STP 599-1976 (Soil Specimen Preparations Laboratory) PDF

SOIL SPECIM EN
PREPARATION FOR
LABORATORY TESTING
A symposium
presented at the
Seventy-eighth Annual Meeting
AMERICAN SOCIETY FOR
TESTING AND MATERIALS
Montreal, Canada, 22-27 June 1975
ASTM SPECIAL TECHNICAL PUBLICATION 599

D. A. Sangrey, symposium co-chairman
R. J. Mitchell, symposium co-chairman
List Price $35.00

04-599000-38
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~L~/~AMER~CAN SOCIETY FOR TESTING AND MATERIALS
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(~) BY AMERICAN SOCIETY FOR TESTING AND MATERIALS 1976
Library o f Congress Catalog Card Number; 76-704
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The society is not responsible, as a body,
for the statements and opinions
advanced in this publication.
Printed in Bahimore, Md.

June 1976
Foreword
The symposium on Soil Specimen Preparation for Laboratory Testing
was presented at the Seventy-eighth Annual Meeting of the American
Society for Testing and Materials held in Montreal, Canada, 22-27 June
1975. Committee D-18 on Soil and Rock for Engineering Purposes spon-
sored the symposium. D. A. Sangrey, Cornell University, and R. J.
Mitchell, Queen's University of Kingston, presided as symposium co-
chairmen.
Related
ASTM Publications
Performance Monitoring for Geotechnical Construction, STP 584 (1975),
$14.00, 04-584000-38
Field Testing and Instrumentation of Rock, STP 554 (1974), $18.75,

04-554000-38
Analytical Methods Developed for Application to Lunar Sample Analysis,

STP 539 (1973), $15.00, 04-539000-38
A Note of Appreciation
to Reviewers
This publication is made possible by the authors and, also, the un-
heralded efforts of the reviewers. This body of technical experts whose
dedication, sacrifice of time and effort, and collective wisdom in review-
ing the papers must be acknowledged. The quality level of ASTM publica-
tions is a direct function of their respected opinions. On behalf of ASTM
we acknowledge with appreciation their contribution.
A S T M Committee on Publications
University of British Columbia Library pursuant to License Agreement. No further reproductions aut
Editorial Staff
Jane B. Wheeler, Managing Editor
Helen M. Hoersch, Associate Editor
Charlotte E. DeFranco, Senior Assistant Editor
Ellen J. McGlinchey, Assistant Editor
Contents
Introduction
Effect of Water Saturation History on the Strength of

Low-Porosity Rocks--G. BALLIW, B. LADANYI,AND
D. E. GILL 4
Testing Equipment 5
Rock Types 7
Specimen Preparation 8
Testing Procedures 11
Experimental Results 12
Conclusions 19
Four Factors Influencing Observed Rock Properties--

P. G. CHAMBERLAIN,E. M. VAN EECKHOUT,AND
E. R. PODNIEKS 21
Discussion of Critical Factors 22
Summary 34
Trimming Device for Obtaining Direct Shear Specimens from

Samples of Stiff Fissured Clay Shale--G. N. DURHAM 37
Residual Shear Test Procedures 38
Waterways Experiment Station Residual Shear Testing 38
WES Direct Shear Trimming Device 39
Discussion 42
Effects of Specimen Type on the Residual Strength of Clays and

Clay Shales--F. C. TOWNSENDAND P. A. GILBERT 43
Previous Investigations 44
Materials and Equipment 45
Test Results and Analyses 49
Conclusions 63
Effects of Storage and Extrusion on Sample Properties--

ARA ARMANAND S. L. MCMANIS 66
Literature Survey 67
Sampling and Field Testing 68
Laboratory Tests and Results 69
Selection of Representative Specimens 80
General Conclusions 85
Transportation, Preparation, and Storage of Frozen Soil Samples
for Laboratory Testing--T. H. W. BAKER 88
Factors Affecting Laboratory Tests on Frozen Soils 89
Frozen Soil Samples 89
Machining and Preparation of Specimens for Testing 97
Rough Cutting Methods 98
Finishing Methods 98
Storage and Protection During Laboratory Testing 104
Conclusions 111
Temperature-Controlled Humid Storage Room--

MICItAEL BOZOZUK 113
Design 115
Closed Flow Conditioning System 119
Handling and Preparation of Samples for Storage 122
Effect of Storage Time on Test Results 122
Summary 125
Effect of Storage and Reconsolidation on the Properties of

Champlain Clays--P. LA ROCHELLE, J. SARRAILH,AND
F. A. TAVENAS 126
Characteristics of the Cemented Clays 128
Water Migration Following Sampling 130
Influence of Reconsolidation 137
Influence of Storage Time 140
Conclusion 144
Pore Water Extraction and the Effect of Sample Storage on the

Pore Water Chemistry of Leda Ciay--J. K. TORRANCE 147
Soil Material 149
Storage Procedures 149
Pore Water Extraction 150
Results and Discussions 151
Conclusions and Recommendations 155
Variation in Atterberg Limits of Soils Due to Hydration

History and Specimen PreparationmD. A. SANGREY,D. K.
NOONAN, AND G. S. WEBB 158
Test Program 160
Conclusions 167
Effect of Specimen Preparation Method on Grain Arrangement

and Compressibility in SandmARsHUD MAHMOOD,J. K.
MITCHELL, AND ULF LINDBLOM 169
Soil Fabric 170
One-Dimensional Compressibility 171
Experimental Investigation 171
Fabric Results 178
Compression Test Results 180
Conclusions 190
A Technique for the Preparation of Specimens of Loose

Layered Silts--V. A. NACCIAND R. A. D'ANDR~A 193
Soil Description 195
Typical Testing Procedure and Result 198
Conclusions 200
Shrinkage of Soil Specimens During Preparation for

Porosimetry Tests--T. F. ZIMMIEAND L. J. ALMALEH 202
Equipment 204
Experimental Work 211
Conclusions 214
Compaction and Preparation of Soil Specimens for

Oedometer Testing--A. R. BOOTH 216
Choice of Compaction Method 217
Construction of Mold 218
Method of Compaction 219
Adjustment of the Degree of Saturation 221
Comparison of Specimens 223
Effect on Results 224
Conclusions 225
Laboratory Preparation of Specimens for Simulating Field

Moisture Conditions of Partially Saturated Soils--T. Y.
CHH AND S. N. CHEN 229
Review of Current Methods for Pretesting Treatment 230
Development of Equipment and Procedures for Pretesting
Treatment 232
Test Results and Discussion 236
General Conclusion 243
Scalping and Replacement Effects on the Compaction

Characteristics of Earth-Rock MixturesmR. T. DONAGHE
AND F. C. TOWNSEND 248
Procedure 249
Test Results and Discussion 257
Conclusions 274
Study of Irregular Compaction Curves--P. Y. LEE 278

Laboratory Investigation 281
Discussion of Test Results 282
Conclusions 287
Importance of Specimen Preparation in Microscopy--

J. E. GILLOTT 289
Microscopic Methods 291
Specimen Preparation for Fabric Analysis 293
Specimen Preparation for Analysis of Particle Size
and Shape 299
Ion Bombardment 300
Replication, Shadowing, and Coating 302
Discussion 304
Conclusions 305
Use of Ultrasonic Energy for Disaggregation of Soil

SamplesmA. I. JOHNSONAND R. P. MOSTON 308
Ultrasonic Equipment 308
Testing Methods 311
Summary 312
Soil Drying by Microwave Oven--P. V. LADEAND

H. NEJADI-BABADAI 320
Heating with Microwaves 321
Effects of Heating Clay Mineral Systems 322
Preliminary Investigations 323
Determination of Water Content 324
Effects of Microwave Heating on Soil Characteristics 330
Summary and Conclusions 333
Discussion 335
S T P 5 9 9 - E B/J u n. 1976
Introduction
A laboratory test run on an inappropriate specimen is often worse

than no test at all. Certainly there are tests for which the preparation
does not significantly change the measured soil property; but the far
more common situation is to have a real or potential variation in the
measured soil property as a result of alternative specimen preparation
techniques. The objective of this symposium was to collect and exchange
information on this problem. Hopefully this will lead to improvements
in our specimen preparation methods or at least a better understanding
of the influence of our preparation methods on final test results.
The entire question of adverse effects on test results through specimen
preparation needs to be examined in the context of the use being made
of the test results. In some cases, accepted practice or a certain design
method are based on a test result involving a particular specimen
preparation technique. If newer, and clearly better, specimen prepara-
tion methods are proposed for this test, there will often be reluctance
on the part of users to change, simply because they are accustomed to
the older methods and have a strong empirical experience to account
for the poorer specimen preparation. Another common situation is
that there are some test parameters which can be used in different de-
sign methods. For some of these design methods, the specimen prepara-
tion is very important, while for others it is much less important.
What general principles, if any, can be applied to the preparation of
soil specimens for laboratory testing? In general, laboratory soil testing
should be done on specimens as nearly identical to field deposits as
possible. For natural soils, this means a minimum of disturbance, con-
tamination, and alteration. For artificially prepared, Or reconstructed,
soils, the objective is to duplicate the in situ structure and state of the
soil, at least in those ways that would influence test results. An overall
objective should be to define methods of specimen preparation and
testing which achieve the smallest variability in the end result. Some
methods are inherently less variable than others, and these will produce
more accurate and more predictable end results.
An objective of the ASTM symposium is to provide a forum for the
exchange of information on a topic of interest or concern. The morning
session of this symposium was separated into two major topic areas.
The first group of papers was concerned with rock as an engineering
material, with stress-strain and strength behavior being the main subjects.
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Copyright 1976 byby ASTM International www.astm.org
2 SOIL SPECIMEN PREPARATION FOR LABORATORY TESTING
From the interest shown for this session it is clear that geotechnical
engineers are becoming increasingly sensitive to the problems of rock
engineering and the role of geotechnical engineering methods in solving
rock mechanics problems.
Storage, extrusion, and predrying effects were covered during the
second part of the morning session. The overall conclusion to be drawn
from this group of papers is that there exists a great potential for
change in soil and rock specimens and their measured properties if
samples are handled poorly and stored for long periods of time. Results
from this group of papers have a direct bearing on present ASTM
standard methods and, in some cases, clearly indicate a need for re-
consideration of existing specifications.
Three major topic areas were included in the afternoon session.
Methods for preparing reconstructed loose cohesionless soil specimens
in the laboratory were discussed in the first group of papers. These
specimens were intended for studies of liquefaction potential and similar
large deformation response. This very current subject was of particular
interest to a large part of the symposium audience.
Preparation of compacted soil specimens was a second topic area
dealing with reconstructing soil specimens in the laboratory. Papers in
this part of the symposium were primarily concerned with the problems
of preparing a laboratory specimen which represented the field situation.
As in the case of the second half of the morning session, there were
some direct implications for present ASTM standard methods indicated
in these papers.
The final session of the symposium was appropriately concerned with
recent techniques applied to laboratory preparation of soil specimens.
All of the papers described new equipment or new techniques for
preparing and testing soil specimens. None of the methods described
are presently covered by ASTM standard methods, but it is reasonable
to expect a need for standards in the near future if there is more wide-
spread use of these new techniques.
A number of present ASTM standard methods were included in the
studies reported in this special technical publication. In several cases,
the results of these research studies indicated a need to reconsider the
present specification, or at least some of its details. Whether it is
appropriate to change an existing standard method or add a method is
an important decision which cannot be based on a single research
study; however, users of specifications should be aware of potential
problems even if the specification is not changed. The listing in Table 1
summarizes the papers included in this special technical publication
and the ASTM standard methods to which they apply. Only the major
associations are noted and there are numerous minor specification refer-
ences which have not been included.
INTRODUCTION 3
TABLE 1--ASTM standards and relevant papers.

ASTM Designation RelevantPapers from This Symposium
D 421 Sangrey, Noonan, and Webb
Johnson and Moston
D 422 Johnson and Moston
D 698 Chu and Chen
Donaghe and Townsend
Lee
D 1140 Johnson and Moston
D 1557 Chu and Chen
Donaghe and Townsend
Lee
D 1587 Arman and McManis
Bozozuk
LaRochelle, Sarrailh, Roy, and Tavenas
Torrance
D 2049 Mahmood,Mitchell, and Lindblom
D 2216 Lade and Nejadi-Babadai
Johnson and Moston
D 2664 Ballivy, Ladanyi, and Gill
D 2936 Chamberlain,Van Eeckhout, and
D 2938 Podnieks
D 3080 Durham
Townsend and Gilbert
This ASTM special technical publication contains a group o f sympo-

sium papers addressing a broad range of materials and testing methods.
It is clearly shown that in most cases the methods of specimen prepara-
tion have a pronounced influence on the subsequent test results. In a
few cases, the opposite conclusion is drawn, for example, in the paper
by Townsend and Gilbert, but it is equally important to know about
minor effects as it is major ones. Several o f the papers present results
and conclusions which have a direct bearing on present ASTM standard
methods. Collecting such information is a major reason for having a
symposium and special technical publication supported by ASTM. The
responsibility for critically reviewing these research studies and, where
appropriate, making modifications to existing standards rests with the
A S T M committee structure.
D. A . S a n g r e y
Cornell University, Ithaca, N.Y.;
symposium co-chairman.
R . J. M i t c h e l l
Queen's University at Kingston, Ontario,
Canada; symposium co-chairman.
G. Ballivy, ~ B. Ladanyi, 2 a n d D. E. Gill 2
Effect of Water Saturation History

on the Strength of
Low-Porosity Rocks
REFERENCE: Ballivy, G., Ladanyi, B., and Gill, D. E., "Effect of Water Saturation
History on the Strength of Low-Porosity Rocks," Soil Specimen Preparation for Labora-
tory Testing, ASTM STP 599, American Society for Testing and Materials, 1976, pp.
4--20.
ABSTRACT: The purpose of the tests described in this paper was to investigate how
the mechanical properties of rock observed in the tests are influenced by the whole satura-
tion history of the specimen prior to testing. Three aspects of the saturation history were
studied in this paper: the effect of drying and resaturating the specimen prior to testing,
the effect of resaturation method, and the effect of the chemical nature of the resaturating
fluid. Three rock types were used in the tests: a gneiss, a cemented sandstone, and a fine
grained limestone. All three rocks had apparent porosities below 2 percent.
Results of triaxial and splitting tests are reported in the paper. One series of specimens
was brought from the site in its natural saturated state and tested without drying while
the others were either air or oven dried and then resaturated prior to testing. The resatura-
tion was performed either by immersing the specimen in water under vacuum, or by
injecting the saturation fluid, under pressure, through a thin channel drilled along the
specimen axis. Either distilled or seawater were used as the resaturating fluid.
The results show that the inclusion of a drying and wetting cycle prior to testing has a
clear overconsolidation effect on the rock behavior, that is, it increases its apparent
strength. On the other hand, the channel saturation technique gives a better saturation
of the specimen and results in a strength decrease. Finally, the results show that the chemi-
cal composition of the saturation fluid has also a significant effect on the measured rock
strength.
The practical conclusion to be drawn from this study is that representative rock
samples, taken in connection with a given project, should, from the moment of coring
until they are tested, be held under environmental conditions that are as close as possible
to those which will prevail after the completion of the project. This implies that no drying
and wetting cycles should be included if they are not expected to occur in practice. If this
condition cannot be met, specimens should be saturated using a natural saturation fluid
and using an efficient saturation technique such as the described axial channel satura-
tion method.
KEY WORDS: soils, rock mechanics, rock sampling, splitting tests, triaxial tests, satura-
tion methods, pore pressure
~Geotechnical engineer, Lalonde, Girouard, Letendre and Associates, Montreal, P.Q.,
Canada.
ZProfessor and associate professor, respectively, Department of Mineral Engineering,
Ecol6 Polytechnique, Montreal, P.Q. Canada.
4
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BALLIVY ET AL ON LOW-POROSITY ROCKS 5
It is well known [1-5] 3 that the strength of rock depends, in large

measure, on the degree of saturation of specimens at the monent of
testing. In fact, it has been stated, in ASTM Test for Triaxial Compres-
sive Strength of Undrained Rock Core Specimens Without Pore Pressure
(D 2664-67) "that the field moisture condition of the specimen should
be preserved until time of test . . . or should be tailored to the problem
at hand."
The wetting of specimens prior to testing has a strength reduction
effect which is generally very large for all kinds of rocks. This effect
results essentially from a reduction of the free surface energy of the
material [3]. This phenomenon is well known, but its physical and
thermodynamic aspects have not been completely clarified to date [6].
The intent of the present study is to illustrate more specifically the
effect of water saturation history on the strength of low apparent
porosity rocks. Three types of rocks have been tested, namely, a
cemented cambrian sandstone, a lithographic ordovician limestone, and
a charnokite (archaean granito-gneiss).
As it is not usual to preserve the field moisture conditions of the
specimen until laboratory testing, this paper also examines the effects
of various resaturation processes on rock strength. Study of these
processes included development of new resaturation equipment, special
specimen preparation, and the use of two different pore fluids.
Testing Equipment
The rock cutting was performed with a circular watercooled diamond
saw blade. Whenever required, the ends of the specimens were ground
flat on a lathe. The specimens were weighed on electronic balances,
and calipers were used to measure their final dimensions.
The oven used for drying the specimens was built in such a way that
the air, heated to 40.5~ as it entered the oven, was forced to circulate
throughout it; the total volume of air in the oven was renewed every
minute.
Resaturation by fluid injection was done with the apparatus shown
schematically in Fig. 1. It consists essentially of a pressure vessel (A),
through the cover of which eight specially prepared specimens can be
connected to eight tubes; these tubes are all connected to a second
pressure vessel (B) which acts as a saturation fluid reservoir. A nitrogen
gas bottle (C) pressurizes, through a regulator, the saturation fluid con-
tained in the vessel (B); this pressurized fluid is injected, by means of
the tubes, through a channel drilled along the axis of each of the
specimens. A second nitrogen gas bottle (D) applies a pressure, also
3 The italic numbers in brackets refer to the list o f references appended to this paper.
FIG. l--Apparatus for saturation of rock specimens by radial divergentflow from a central
channel; (a) view of the apparatus; (b) scheme of the saturation system.
through a regulator, on the saturation fluid contained in the vessel (A),

thus providing a constant fluid pressure at the outside surface of the
specimens.
The saturation fluid pressure gradient results from the difference be-
tween the pressures produced by the nitrogen gas bottles C and D. This
gradient produces radial divergent flow within the specimens. The
apparatus was constructed in such a way that all steel surfaces coming
into contact with the saturation fluid were lined with plastic material.
For the tests results reported in this paper, the pressure in C was 300
psi (2.07 MPa), and in D, 50 psi (0.34 MPa). The photograph in Fig. 1
shows the apparatus just described.
Both a standard testing machine and, more often, a programmable
universal testing machine (Tinius Olsen) were used for loading the speci-
mens to failure. Diametral splitting tests were conducted between rigid
plattens. Triaxial tests were performed in a modified Hock cell, in which
the confining pressure was supplied by a pump (Structural Behavior
Engineering Laboratories, Model 100 LP + 100 P). To test the specimens
which had been resatured by fluid injection, the plattens were modified as
shown in Fig. 2b. As far as the pore pressure is concerned, a nitrogen gas
bottle, combined with a pore fluid reservoir, was used whenever the back
pressure to be maintained during testing was less than 500 psi (3.45 MPa);
otherwise, the back pressure was provided by the pump. Figure 2a is a
photograph of the Hoek cell with modified plattens. Specimen deforma-
tions were measured with electromechanical extensometers, in which
sensors were linear potentiometers. The longitudinal deformation of the
triaxially tested specimens was measured outside the cell; the signal output
by the measuring devices was recorded against the load applied by the
testing machine on a standard X - Y recorder. In the case of the splitting
tests, the changes in both the vertical and the horizontal diameter were
measured and recorded, as for the triaxial tests.
Rock Types
The tests were performed on three types of rocks from various locations
in the province of Quebec.
Cambrian Cemented Sandstone (Potsdam Group)

It is predominantly a white to off-white orthoquartzite with dolomitic
cement; the apparent porosity of this bed is less than 2 percent.
Ordovician Sublithographic Limestone (Trenton Group, Tdtreauville

Formation)
It consists of beds of dense bluish-black limestone up to 6 in. in thick-
ness, separated by shale partings; it has a lithographic stone appearance
[7]. The total porosity of this rock is low (1.2 to 1.9 percent) [8], and its
apparent porosity is less than 1 percent.
Charnokite
This is an Archaean granito-gneiss from the Quebec City area.
FIG. 2--Hoek's cell with modified plattens; (a) view of the cell and the plattens; (b) modi-
fied bottom platten.
Specimen Preparation
General
All the specimens were prepared from NX (diameter: 2~ in. or 5.38 cm)
core samples. The present study involved two types of samples which
have been cored below the water table.
Saturated Samples--Samples selected were kept immersed in water at
the drilling site and delivered to the laboratory, where they were submitted
to various procedures, including drying and resaturation.
Air-Dried Samples--In the other cases, the samples selected at the
drilling site were kept under ambient conditions and delivered to the
laboratory where they were submitted to various procedures.
In all cases, the core specimens were cut to the desired lengths a short
time after delivery, and the effect of wetting caused by the cooling water
during the cutting was considered insignificant as far as mechanical pro-
perties are concerned.
The control of specimen saturation was made by a periodical weighing.
Usually, a specimen was considered to have reached a given saturation
degree when periodical weighings showed constant weight for at least
three consecutive days.
Specimens f o r Tensile Splitting (diametral compression) Tests

As a rule, specimen disks submitted to splitting tests were about 90 of
an in. (1.90 cm) thick. The following groups of specimens were prepared
from the two previously described types of samples (see Table 1).
TABLE l--Groups of specimens prepared by different methods

and number of tests in each group.
Triaxial
Group Tension Splitting Tests Compression Tests
Air-Dried Specimens
A 42
AO 9 50
AS 19
AOS 17 97
AOSC 80
AOC 8
Saturated Specimens
S 57
SO 23
SOS 42
From saturated samples (S):

Group S--The specimens of this group, prepared from saturated samples,
were obtained by cutting specimens of core into disks which had been
temporarily removed from their water bath. The specimens were then
measured, weighed, and tested.
Group SO--The specimens of this group were the same as in group S,
except that they were oven dried before testing.
Group SOS--This group is the same as group S, except that the speci-
mens, after being measured, were oven dried and resaturated by immersion
before testing.
From air-dried samples (A):
Group A--The specimens of core, selected from air-dried sample lots,
were cut into disks. The specimens were measured, weighed, and tested.
Group AO--The specimens of this group were prepared as were those
in group A, except that they were oven dried before testing.
Group AS--These specimens were prepared as those in group A, except
that they were resaturated by immersion prior to testing.
Group AOS--The specimens in this group were prepared as were those
of group A, except that they were oven dried and subsequently resaturated
by immersion prior to testing.
Specimensfor Triaxial Compression Tests

Specimens submitted to triaxial compression tests were about 4 88
long (10.80 cm) cylinders. They were all prepared from the samples of
C opyri ght by ASTM Int ' l ( a l l r i g h t s r e s e r v e d ) ; W e d De c 2 2 1 4 : 0 0 : 0 0 E S T 2 0 1 0

D ownloaded/printed by
U ni vers ity of Britis h Co l u m b i a Li b r a r y p u r s u a n t t o Li c e n se A g r eem en t . N o f u r t h er r ep r o d u ct i o n s au
Type A, that is, the air-dried samples, and they fall into one of the
following groups:
Group AO--This group is the same as AO, described for specimens
for tensile splitting.
Group AOS--This group is the same as AOS, described for specimens
for tensile splitting.
Group AOSC--The specimens in this group were prepared as were
those in the splitting tests, except that a 89 hole was drilled along each
of their axes for about 80 percent of their length [11]. No cooling fluid
was used during this operation.
Figure 3 shows a specimen into which a hole has been drilled, as
FIG. 3--Specimens with central channel; (a) radially saturated sandstone specimens with
cut fitting, ready for testing; (b) section of a specimen with complete fitting.
described previously. This figure shows also the brass fitting that was
cemented to the collar of the channel, in order to enable the specimen to
be mounted on the resaturation apparatus described previously. This fitting
covers the hole wall for a length equal to about 30 percent the specimen
length, leaving an unlined cylindrical channel in the central portion of
the specimen; the length of this cavity is then about 60 percent of that of
the rock specimen. Figure 3a is a photograph of such a specimen. Note
that the threaded part of the fitting was cut away before testing.
Group AOC--The specimens in this group were as in group AOSC,

except that they were not submitted to resaturation, although they were
provided with a central channel.
A review o f the groups and the tests made in each group is presented in
Table 1.
Testing Procedures
Splitting Tests
Specimens were mounted on the testing machine in such a way that the
loading could be performed along two diametrically opposite lines on the
lateral surface o f the disks. The electromechanical extensometers were
then mounted and set to zero. The loading proceeded at such a speed
that the minor principal stress increased at a rate o f 100 psi/s. Tensile
strengths were calculated from the usual formula
2P
To - (1)
nDL
where
To = tensile strength,
P = maximum load applied,
D = diameter of the specimen, and
L = thickness o f the specimen.
Only the tests in which failure started at the center o f the cross section
o f the specimen, and in which failure plane coincided with the loaded
diametrical plane, were considered to be valid.
Triaxial Compression Tests

Jacketed specimens were mounted in the triaxial cell with proper spheri-
cally seated plattens. The cell was placed subsequently into the testing
machine, and the extensometer was installed. The loads were applied at
such a speed t h a t the major principal stress within the specimens increased
at a rate of 100 psi/s. Prior to the test, the confining pressure was applied
to the specimen by increasing simultaneously the axial and the cell pressure.
Whenever required, back pressure was raised to the desired level (200 psi
= 1.38 MPa with limestone specimens, 300 psi = 2.07 M P a with charno-
kite specimens, and up to 5000 psi = 34.5 MPa with sandstone specimens).
Pore pressure was applied from the bottom plattens, and the testing was
started only when the same pore pressure could be read at the top plat-
tens. Similar procedures have been reported in the literature already [8].
The extensometer was then set to zero, and the specimens were brought
to failure by increasing the axial stress.
Experimental Results
Check o f Pore Pressure Distribution in Triaxial Specimens

Before starting the study of the effect of specimen preparation history
on its strength, a check of the system of pore pressure application in the
triaxial cell was made by a series of triaxiai tests on cemented Potsdam
sandstone. All the specimens in these tests were of the AOSC group, that
is, they had a central hole and were resaturated by immersion after being
air and oven dried. The triaxial tests were conducted according to the
Heck's procedure [9], but the pore pressure u was kept constant during
the tests.
Such a system, if working well, that is, if resulting in a uniform dis-
tribution of the applied pore pressure (back pressure) throughout the
specimen at failure, should result in essentially drained test conditions.
According to the concept of effective stress, failure strengths of such a
series of tests, plotted against the effective confining pressure, should fall
on a single failure line [10].
Figure 4 shows that, with the usual scatter of results, this assumption
was found to be valid in the tests with the Potsdam sandstone. These
results illustrate that the pore pressure application system used in the tests
was quite effective, even for rocks of such a low porosity.
Effect o f Specimen Preparation History on the Results o f Tension

Splitting Tests
Figures 5 and 6 show the results of a large series of tension splitting
tests carried out on specimens of Trenton limestone, prepared according
to various procedures. The results show clearly that tensile strength is
affected very much by the specimen preparation history. In fact, three
different groups of results can be seen in Figs. 5 and 6. The lowest strengths
were found for specimens saturated without over drying (groups S and
AS), the highest, for those that were air and oven dried (group AO), while
the strengths of those tested air or oven dry (A and SO), as well as those
tested after having been saturated following air or oven drying (AOS and
SOS), were located between the two extremes.
These results lead to the conclusion that an oven drying, or a severe air
drying, produces a clear overconsolidation effect on the strength of rock,
and that the effect is irreversible, that is, it cannot be eliminated by sub-
sequent resaturation of specimens. On the other hand, Fig. 5 shows that
University of British Columbia Library pursuant to License Agreement. No further reproductions authoriz
ksi ' MPo /

~,o
- 4O0
I--
z
w
40. ~35~(
LEGEND:
Test with opplied

e pressure
u= 8 0 0 psi
t,~176 Specimen:Cemented sondstone~

group AOSC
,o] , L,o
20 MPo
3 ksi
EFFECTIVE CONFINING PRESSURE O''5
FIG. 4--Results of triaxial compression tests with Potsdam sandstone.
the overconsolidation effect seems to affect much less the modulus of

elasticity of rock, because the peak strength points, shown in Fig. 5, are
distributed around a mean straight line without any systematic trend.
Effect of Specimen Preparation History on the Results of Triaxial Tests

Figure 7 shows, in terms of principal stresses at failure, a summary of
all triaxial test results obtained with specimens of Trenton limestone and
charnokite prepared by various described methods. In addition, the median
failure line for AOSC specimens of Potsdam sandstone is shown also in
the figure for comparison. The tests with Trenton limestone were made
at different confining pressures varying from 500 to 5000 psi, while those
with charnokite were all at an effective confining pressure of 1000 psi
(6.9 MPa). Some results for the latter are summarized also in Table 2,
together with the corresponding water contents after immersion in the
distilled and the seawater, respectively.
The test results lead to a number of interesting conclusions concerning
psi MPa
1500 /
I0
/
A0
bJ
I-
co
I000,
'AOS,
-6
w
I
-4
500-
/ IM P a [ ~ e d l o n
LEGEND
-2 / vol~e
of To ond F~v
0.5%
/ 19 ~ ' ~ - s t a n d o r d deviotion
/ number of tests
, , II,
0 0'5 Ii0 1',5 210 25 per cent
VERTICAL STRAIN 8v = A.~I
I
FIG. 5--Effect of mode o f saturation on splitting tensile strength and failure strain of
Trenton limestone. For the definition o f symbols, see Table 1.
the effect of preparation history on the failure behavior of rocks under

triaxial test conditions. The results show clearly that:
1. The strength of dry specimens is from 20 to 30 percent higher than
that of comparable specimens when tested saturated, at any confining
pressure.
2. The presence of a central hole in the specimen improves and accelerates
considerably the resaturation of the specimen. This is seen clearly in the
results obtained for the charnokite. This method, however, could not
have been applied to the specimens of Trenton limestone, which had a
tendency to fracture along bedding planes during pressure saturation. The
limestone, therefore, was soaked in water, and a back pressure of 200 psi
was applied through the central channel. This saturation method was
clearly less effective, which explains the much smaller difference between
BALLIVY ET A L O N LOW-POROSITY ROCKS 15
Initml conditions: S or A -~...._....~ A
@l To. (29Opsi)
,,o~s,
S , ~e,ts AS
TO= 740psi / on
@ (160psi)
saturated
/4-- samples ~
~ TO = 780psi
(260psi)
SO AO
~ tests on
TO = 1150psi oven dried ID @ TO= 1290psi
(;500 psi) samples (~90psi)
SOS AOS
4--- tests on
TO= 1090psi resaturated
L (280psi) samples 9 (150psi)
LEGEND= 5~ number of tests (160psi) =standard

deviation
To = median tensile
strength Ips== 6.9 kPo
FIG. 6--Effect of drying and saturation history on tensile splitting strength To of Trenton
limestone. For the definition of symbols, see Table 1.
/, AOSC j POTSDAMSANDSTONE
psi MPa /
- 400
%,o /
9 AOS(sea water)
-~- 50 /
I- -300 ~z 9 A/0SC (sea water) .

. Q.~ (~
=- 3o-L2oo/ I" ~ o _ ~ ~ ~''
t,,-
"EOENO
~oo , - -
J ~T~,~"5 =median effective stresses
ioJ ~. R,H.=relotive humidity
l 5 ~ number of tests
J L/~30(016~1 :median water content=0.30%
~ standard devJation=O.16%
/ ,o ~ - ~ - ,-~-=~
O 2 5 4 5 ksi
EFFECTIVE CONFINING PRESSURE 0"5
FIG. 7--Effect of mode of saturation on triaxial compression strengths of Trenton limestone

and charnokite. For the definition of symbols, see Table 1.
..L
_o
t-
m
TABLE 2--Influence of mode of saturation and composition of pore fluid on the triaxial compression
strength of charnokite.
m
z
Fluid of Saturation "U
1'I
m
Distilled Water Seawater
Mode of Saturation n ol ult psi s 070 W , 070 n Ol ult, psi s ~0 W , 070

-4
AOS 24 43 100 2.9 0.22 24 50 500 3.1 0.28 Z

(7 600) (0.4) (0.9) (7 100) (0.4) (0.11) 11
AOSC 13 35 700 2.7 1.11 14 43 800 2.8 0.97 O
2O
(8 300) (0.5) (0.5) (5 900) (0.3) (0.37)
Oven-dried r-
specimens 16 53 800 3.17
(12 000) (0.6) O
-n
-4
NOTE--n = number o f tests. (7 600 psi) = standard deviation. 1 psi = 6.9 kPa. O
Period of saturation: 8 to 42 days. .<
ol ult = median ultimate axial strength.
o3 = 1 000 psi for all the tests. m
(D
Eult = median peak deformation.
W, % = water content in percent. z
AOS and AOSC lines for Trenton limestone. The difference increases
slightly, however, with increasing confining pressure, which is due probably
to an increase in the degree of saturation because of increasing consolidation
of the rock under confining pressure.
3. For an intermediate saturation in a 75 percent relative humidity
atmosphere [12], the strengths are located, as expected, between those of
dry and completely saturated specimens. However, for the reason outlined
previously, there is a tendency for consolidation under a high confining
pressure to increase the degree of saturation; this leads to an apparent
decrease of strength at higher pressures.
Effect o f Type o f Pore Fluid on the Results o f Triaxial Tests

As shown by Colback and Wiid [2], the type of pore fluid in the rock
may have considerable effect on strength. This phenomenon is thought to
be due to a combination of thermodynamic and mechanical effects. In
fact, Colback and Wiid have shown that the type of fluid has an effect
on the free surface energy in rocks. On the other hand, there is no doubt
that the fluid viscosity plays also an important role in determining the
level of pore pressures at failure, as shown by Brace and Martin [13].
The results of triaxial tests with specimens of charnokite soaked in
distilled and seawater (with 3.4 percent salt content), respectively, are
shown in Fig. 7 and summarized also in Table 2. It is seen clearly that the
seawater has the effect of increasing apparent strength of this rock by
about 20 percent, no matter which method of saturation is used. However,
the saturation by radial flow remains still much more effective than by
simple immersion, leading to about five times higher water contents and
to a corresponding decrease of strength of the order of 20 percent.
Effect o f the Time o f Saturation on the Water Content

Figure 8 shows a plot of water contents achieved after different periods
of continuous saturation of charnokite specimens, using two different
methods.
The results indicate that simple immersion of specimens leads in a
short period to an upper level of saturation, which remains practically
constant with time, even after six weeks of immersion. On the other hand,
saturation by radial flow from a central channel shows a continuous
increase in water content for a long period of time, attaining a maximum
only after about three weeks. Since this maximum water content is about
five times higher than that after simple immersion, these results indicate
clearly the importance of using a proper saturation method if one wants
to obtain a true saturated strength of rock.
--L
Go
oo
0
r
LEGEND : (I)
"o
m
(~ DISTILLEDWATER o_
8 days 21 doys 42doys AOSC ~ SEA WATER m
z
water 1)
:TJ
content
I
t" m
-o
),
2% AOS~ ~ D,ST,LLEDWATE~
>
SEA WATER -t
5
z
( 8 ) : 8 TESTS
"11
02D
'~176 I
j J loo Isl ffJ
0
0 . . . . . . . . . [o.tT(e) - - -
1 0
-n
-<
TIME OF SATURATION m
.-~
FIG. 8--Variation o f water content with time o f saturation in charnokite specimens, using two different saturation techniques: A O S =
air dried, oven dried, resaturated; A O S C = air dried, oven dried, saturated through a central hole. if)
Conclusions
This experimental investigation shows that the specimen preparation
history has a great influence on the strength of ordinary rocks o f low
porosity. Three factors affecting strength have been identified: the oven
drying, the final water content, and the chemical composition of pore
water.
In particular, oven drying leads to an irreversible overconsolidation
effect, which may be due to a modification in the structure of hydrosili-
cates, resulting in petrification o f bonds. On the other hand, an ordinary
air drying at 60 to 70~ and a relative humidity o f less than 45 per-
cent has a much smaller overconsolidation effect, as found in the tension
splitting tests. This means that, for ordinary rock testing purposes, air
drying with subsequent resaturation may be acceptable, but oven drying
should be avoided.
The water content o f rock at failure was found to be an important
factor in determining its strength. Since the water content attained by
radial flow and back pressure through a central channel can be up to five
times higher than that after a simple immersion of the specimen, it is not
sufficient to indicate only that the specimen was saturated during the
test; its water content at failure should also be identified. In general, it is
clear that the results closest to reality will be obtained if the specimens
are tested at their natural, or maximum expected, water content, without
being subjected to drying prior to testing.
Finally, these results show that even small amounts o f chemicals in the
pore water, such as the salts in the seawater, may affect the strength o f
rock considerably. This result indicates that using distilled water for rock
saturation is not always the best method for finding its expected strength.
Acknowledgments
The experimental work described in this paper was carried out at the
Rock Mechanics Laboratory o f Ecole Polytechnique, Montreal, and was
supported by the National Research Council of Canada Grants 1801 and
3412.
References
[1] Robinson, L. H., Quarterly of the Colorado School of Mines, Vol. 54, No. 3, July
1959, pp. 177-200.
[2] Colback, P. S. B. and Wiid, B. L. in Proceedings, Third Canadian Symposium Rock
Mechanics, Toronto, 1965, pp. 65-83.
[3] Wild, B. L., "The Influenceof Moisture upon the Strength Behaviourof Rock," Ph.D.
thesis, Universityof the Witwatersrand, Johannesburg, South Africa, 1967.
[4] Morlier, P., "R61e des Fluides en M~canique des Roches," Proceedings of the 2nd
Congress of the International Societyof Rock Mechanics, Belgrade, 1970.
[5] Mellor, M., "Strength and Deformabifity of Rocks at Low Temperatures," Research
Report 294, U.S. Army Cold Regions Research and Engineering Laboratory, Hanover,
N.H., 1971.
[6] Chenevert, M. E., in Rock Mechanics-Theory and Practice, W. H. Somerton, Ed.,
Society of Mining Engineers of The American Institute of Mining, Metallurgical, and
Petroleum Engineers, New York, 1970, pp. 599-627.
[7] Clark, T. H., "Montreal Area," Geological Report 152, Minist~re des Richesses
Naturelles, Qu6bec, 1972.
[8] Durand, M., "Etude de propri~t~s Physiques et Chimiques de Calcaires de la R6gion de
Montreal," Thb,se M.Sc.A., Ecole Polytechnique de Montr~.al, Montr6al, Qu6bec, 1969.
[9] Heck, W. J. in Basic and Applied Rock Mechanics, K. E. Gray, Ed., Society of Mining
Engineers of The American Institute of Mining, Metallurgical, and Petroleum Engineers,
New York, 1972, pp. 243-266.
[16] Robinson, L. H., on Quarterly of the Colorado School of Mines, Vol. 54, No. 3,
July 1959, pp. 177-200.
[11] Bernaix, J. Etude G~otechnique de la Roche de Malpasset, Dunod, Paris, 1967.
[12] Dunn, J. R. and Hudec, P. P., "The Influence of Clays on Water and Ice in Rock
Pores," Part II, Physical Research Report RR 65-5, Department of Public Works,
State of New York, 1965.
[13] Brace, W. F. and Martin, R. J., III, International Journal of Rock Mechanics and
Mineral Science, Vol. 5, No. 5, Sept. 1968, pp. 415-426.
P. G. Chamberlain, ~ E. M. Van Eeckhout, 2
and E. R. Podnieks'
Four Factors Influencing Observed

Rock Properties
REFERENCE: Chamberlain, P. G., Van Eeckhout, E. M., and Podnieks, E. R., "Four
Factors Influencing Observed Rock Properties," Soil Specimen Preparation for Labora-
tory Testing, ASTM STP 599, American Society for Testing and Materials, 1976, pp.
21-36.
ABSTRACT: This paper presents a review of the effects of four factors in specimen
preparation that influence mechanical property tests--moisture content, orientation
with respect to rock fabric, fractures, and specimen tolerances--and discusses methods
developed during various Bureau of Mines testing programs for controlling these factors.
Bureau and other research is cited to present problems in obtaining suitable property
data arising from these factors and to define solutions to the problems. Rock mechanics
researchers dealing with field sampling and laboratory testing should find the material
helpful in establishing specimen handling and preparation procedures for obtaining
relevant test results.
KEY WORDS: soils, rocks, rock properties, specimen preparation, laboratory tests,
moisture content
The U. S. Bureau o f Mines has measured numerous rock properties for

a variety of field projects over the years. Many factors influencing mechanical
p r o p e r t y testing h a v e been i d e n t i f i e d a n d investigated. This p a p e r discusses
f o u r critical f a c t o r s - - m o i s t u r e c o n t e n t , o r i e n t a t i o n with respect to r o c k
f a b r i c , f r a c t u r e occurrence, a n d s p e c i m e n t o l e r a n c e s - - a n d presents m e t h o d s
for alleviating p r o b l e m s arising f r o m these f a c t o r s .
O b v i o u s l y , these a r e n o t the o n l y critical f a c t o r s influencing r o c k p r o -
perties; t h e r e m a y be several features o f a n y p a r t i c u l a r field site which exert
g r e a t c o n t r o l over the b e h a v i o r o f r o c k at t h e site, yet which c a n n o t be sim-
u l a t e d in a l a b o r a t o r y testing p r o g r a m . T h e f o u r factors p r e s e n t e d are, h o w -
ever, b o t h significant a n d c o m m o n . A l l can be c o n t r o l l e d t h r o u g h p r o p e r
I Geophysicist and supervisory mechanical engineer, respectively, Twin Cities Mining Re-
search Center, Bureau of Mines, U. S. Department of the Interior, Minneapolis, Minn. 55111.
2Research engineer, Mining Research Division, Continental Oil Co., Ponca City, Okla.
(formerly Geophysicist, Twin Cities Mining Research Center, Bureau of Mines, U. S. Depart-
ment of Interior, Minneapolis, Minn. 55111).
21
Downloaded/printed
Copyright9 1976 by by ASTM International www.astm.org
specimen handling procedures. The order of factor presentation does not

imply relative importance since, in different rocks, under given circum-
stances, the ranking of factor importance would change.
Discussion of Critical Factors
M o i s t u r e Con ten t
There is little doubt that moisture content affects the mechanical properties
of various rock types, sedimentary rocks in particular [1-5] .3 This effect is
usually a lowering of strength with increased moisture, as well as an increase
in mechanical compliances in certain rocks. For example, Table 1 shows how
T A B L E 1--Strength and Young "s modulus o f shale as a function o f relative humidity.
Relative
Relative Relative Young's
Source Humidity, ~ Strength a Modulus ~
Beatrice mine 0 1.0 1.0

48 0.52 0.72
100 0.31 0.39
Matthews mine 0 1.0 1.0
48 0.68 0.86
100 0.32 0.41
A R M C O mine 0 1.0 1.0
48 0.83 0.93
100 0.48 0.90
"All specimens compressed paraUd to bedding; values represent average o f two to six tests.
strength and Young's modulus values for coal mine shales varied after stabili-
zation at three humidities [3]. Further examples are shown in Figs. 1,2, and 3.
It follows that, if meaningful data are to be obtained in the laboratory, sam-
ples should not lose or gain water in transit from the field. Care must be taken
also in the laboratory to prevent changes in moisture content during storage
and specimen preparation.
Many methods are available for stabilizing water content in samples trans-
ported from the field to the laboratory. The methods range from waxing the
sample to enclosing it in airtight steel drums [6] or dipping in cellulose ace-
tate butyrite [7]. The Bureau of Mines has encased some large coal samples
in concrete, but the shrinkage characteristics of certain cements make this
potentially harmful for structurally weak specimens. Although plastic
bags are the easiest sealant to use, they are difficult to seal and tend to rip
easily. During a recent coal sampling trip to Illinois, representative samples
3 The italic numbers in brackets refer to the list o f references appended to this paper.
CHAMBERLAIN ET AL ON OBSERVED ROCK PROPERTIES 23
9,000 - - 1 I i I- -
~ Dried
8,000
Sandstone
7,000
9~ 6,000
c~
E
z 5,000
% ~ - ' ~ = ~ ' ~ Submerged

4,000 Sample 1005/31 in woter
w
~E
o 5,000
~ idity
Sample 1 0 0 5 / 7
Submerged
in water
50 pct relative [
2,000 humidity as zero
datum
1,0OO
0 I I I I
-2.0 O 2.0 4.0 6.0 8.0
MOISTURE CONTENT, wf-pct
FIG. l--Effect of moisture content on compressive strength [l ].
of coal wrapped in plastic bags lost 1 percent in weight during three days
transportation to Minnesota. This weight was regained upon placing the
coal in a 100 percent relative humidity chamber. Such weight changes
vary, of course, with initial moisture content and climatic conditions dur-
ing transportation. If convenient, it is best to coat samples with wax or
other vapor sealant.
Once the samples have been transported to the laboratory, the question
of storage until specimen preparation arises. If there is a good vapor sealant
on the samples, there is no problem unless the sealant cracks. Samples without
a proper sealant should be stored at a humidity which maintains the as-col-
lected moisture content in the rock, as evidenced by weight measurements.
The samples can be stored in an enclosure where the air above a saturated
salt solution is stabilized at the desired humidity (see Winston and Bates [8]
for a list of possible chemicals) or in an enclosure containing the proper mix-
ture of wet and dry air [9]. A problem arises if the equilibrium humidity for
maintaining the original moisture content is not known for a given rock.
20,000 I I I I I I I I
+ Illinois No. 6cool (Inland Mine)

0 Illinois No.6 cool (Orient M i n e No. 4)
~. Illinois No, Scool ( S a h a r a M i n e No. 20)
0 Illinois No. 6cool (Old Ben M i n e )
I 5,000
x Illinois No. 6cool (Montery Coal Co.)
"7.
0.
~E
Z
W
CE
I0,000 §
x x
0.
oo 5,000
I I I I I I I I I
0 I0 20 30 40 50 60 70 80 90 I O0
RELATIVE HUMIDITY, pct
FIG. 2--Effect of humidity on compressive strength of coal [4].
LATERAL STRAIN, / = i n / i n
0 5 O0 1,000 1,500 2,000 2,500
5,000 ! I 1 I
Dry Wet Dry Wet

lateral lateral a axial ,J axial ~A
4,000
~" 3,000
2,000
/," S" / ; / ' ..::.-' . / y . ..,s;-'
/,'/s/ - ~anderasa._d,,on.
,/I J ' ..,:.S,-"
I,OCO
~ "S~ I I I
0 1,000 2,000 3,000 4,000 5,000
AXIAL STRAIN, /=in/in
FIG. 3--Effect of moisture content on deformation of sandstone [5].
Equilibrium humidity can be determined by placing samples in a variety of

dessicator-stabilized humidities and monitoring the weight changes. For
example, see Table 2 for the weight changes an Illinois coal gave after one
TABLE 2--Moisture content changes in coal as a

function o f humidity environment.
Relative Humidity, 070 Specimen Weight Loss, ~
100 0.0
78 1.2
48 5.0
12 6.3
0 6.8
month at the indicated humidities. This particular coal needed to be stored

at nearly 100 percent humidity to maintain moisture content stability, and a
plastic enclosure was built subsequently for this purpose. Relative humidities
of less than 100 percent will be required to maintain original moisture con-
tent for some shales and other rocks which can absorb water in higher humid-
ity environments [3, 4].
During specimen preparation in the laboratory, water is used most
often as a coolant and flushing agent for the drilling and cutting opera-
tions. Although contact between rock and water is generally brief, rock
types very sensitive to water should be cut dry or with a substitute liquid.
After preparing specimens from the collected samples and before test-
ing, specimens again need to be stored at equilibrium humidity. Des-
sicators stabilized at the proper humidity as described earlier are ideal for
this purpose. Testing at a room humidity other than the stabilization
humidity will have little or no effect on test results if the test is of short
duration (less than 30 min).
Orientation
Although it has been well established that mechanical properties of
rock vary with specimen orientation [10-12], many engineers still do not
realize the importance of preparing test specimens properly oriented with
respect to geologic structure to obtain valid test results. Rock property
anisotropy was demonstrated in one study [13] which showed that com-
pressive strength of granites varied approximately 20 percent, while
Young's modulus varied up to 100 percent with direction (Fig. 4). An-
other study [3] showed that Young's modulus of coal mine shale was 30
to 80 percent higher whenspecimens were loaded parallel to the bedding
rather than perpendicular to it. Tensile strength results varied several
hundred percent with direction for shales and other layered sedimentary
rocks [14] (Fig. 5). Indirect tensile strength of coal varied threefold with
different orientations in the horizontal plane [15]. Shear strength of a
schistose gneiss, as determined from confining pressure tests (triaxial com-
pression tests), varied significantly as a function of direction [16] (Fig. 6).
800 / I I e i
7oaf J. Hordwoy / / " J. Groin.*'~ .L Rift~.~

~.6OO I'- Stonsteod granite /-/ ~" /// .
/ - - - - / / j~'/ // //
,oo ,// .// _ / ..
~,oo //~ /C-~ -/ ."
I1" ./I"" .-" /'//
~-i.iL-_-4 ..... I I i
O 500 I ,OOO 1,5OO 2,000 2,500
AXIAL STRAIN, Fin/in
F I G . 4--A nisotropic deformationol characteristics of granite [13].
2,000 [ I I I I I I
Idaho
pS p r i n q s
gneiss
r I
Green River
1,500 Pshole (rich)
Green River
shale (leon)
Z
1,000 Sandstone
Z
tAi
p-
500 Blockhowk
.____._x/-'x "X-
i
,.
15
I
30
I
45
I
60 75
I
90
I I
105
I
120
INCLINATION OF LAYERING TO ~3' de?
FIG. 5--Effect o f orientation on tensile strength [14].
o"3
T
15 J f I l J t i i I
-,r
i-
w
i1c
oc
O 30 60 90
/~'-SCHISTOSITY ANGLE, (:leg
FIG. 6--Effect of orientation and confining pressure on shear strength [16].
Consequently, techniques for orienting specimens are very important to

ensure that measured properties are relevant.
Orientation begins at the field site, where samples of rock to be sent to
the laboratory are marked with a cardinal compass and vertical directions
before being removed from their in situ positions for shipment [17]. Cores
being drilled in the field can be oriented by drilling with special core
barrels which cut a pattern of grooves along the length of the core. The
field orientation must be, of course, maintained throughout the specimen
preparation process to be meaningful.
How does one determine the direction in which specimens should be
cored for laboratory tests from the samples collected in the field? Gen-
erally, the directions of interest are the principal mechanical property axes
which coincide usually with axes of petrofabric symmetry [13,18]. Some-

times visual examination of rock samples lets the investigator establish the
axes; frequently, however, this is impossible. For these rocks, acoustic
wave velocity measurements are made on an oriented sphere cut from the
rock sample [19], with the resultant velocities plotted on a stereonet or an
equal area net [20]. The principal velocity directions determined from the
nets coincide with preferred orientation of rock fabric [20], which, in
turn, correlates with principal mechanical properties. For example, the
stereonets in Fig. 7 show a direct comparison between principal velocity
H=Hlgh value axis

M=Medium value axis
L=Low value axis
H=4.75 km/sec H=59.0 GN/m2 H=20.4 GN/m2

M=4.45 km/sec M=52.9 GN/m 2 M= 17.4 GN/m2
L=5.44km/sec L=20.1 GN/m2 L=16.4 GN/m2
Pulse velocity Young's modulus, Young's modulus,

compression tension
FIG. 7--Stereonet plots of principal velocity and mechanicalproperty directionsfor shale [3].
directions and principal moduli of elasticity poles in a roof shale from

Consolidation Coal Company's Matthews mine, Middlesboro, Kentucky
[3]. Since the sphere is oriented with respect to the rock sample from
which it was cut, specimens can be prepared from the rock sample with
their axes of symmetry oriented according to the directions determined
from the acoustic measurements on the sphere. Tests on these properly
oriented specimens will provide the principal mechanical properties from
which properties in any other direction can be transformed mathematically.
Although preparing and testing a sphere may seem unnecessarily com-
plicated, the entire process is quite routine and inexpensive. It is the best
method of assuring properly oriented specimens for any mechanical
property testing program. With the increasing use of anisotropic rock
properties in analyzing rock mechanics problems, significant time and
cost savings can result from using the techniques described.
Fractures
The fact that rock is cracked or fractured has long caused consternation
to people attempting to characterize a rock mass using laboratory property
tests. Fractures or joints can provide a domineering influence on rock
properties; the effects of fracture systems are similar to those of bedding

planes or other planar features but are frequently of significantly higher
magnitude [21,22].
Characterizing rock from a particular site requires a distribution of frac-
tures in the specimen that represents the distribution of fractures at the
field site. Obtaining representative rock blocks from a test site in frac-
tured rock is, however, no easy matter, since the fractures tend to sepa-
rate easily. Large fracture spacing may preclude obtaining representa-
tive samples that can be handled readily. Preparing specimens from frac-
tured samples borders on the impossible frequently. For most researchers,
the usual procedure is to gather intact portions of rock from a site and to
characterize the site based on the intact rock properties. While such
characterizations are valid for certain applications, they do not reflect
accurately the strength or deformability of the entire rock formation. The
difficulties in collecting samples and testing representative fractured rock
specimens sometimes lead to research on blocks of artificial material con-
taining joints [23-25]. This does not, however, solve the problem faced by
the design engineer--characterizing a specific field site. Collecting rock
blocks in the field for characterizing a site should be preceded by geologic
reconnaissance to determine the fracture distribution at the site [It)]. Fol-
lowing this, rock blocks containing as representative a fracture system as
possible are selected for the laboratory testing program.
Transporting samples must be done carefully to minimize alterations in
the fracture system. For example, a recent shipment of cores from a field
site in Arizona, packed in the usual core boxes, suffered significant changes
in the size distribution of intact pieces, which indicated introduction of new
,51
fractures during transit (Fig. 8). Where it is of interest to preserve the
w
E
20
II Before shipment
Eg After shipment
~ 5
2
I
to to
4
4
to
5
5
to
6
6
to
7
?
to
8
8
to
9
to
I0
l
I0
to
Id
ll ll n
II 12 13 14 15 16
to to to to to to
12 13 I~ 15 16 17
CORE PIECE LENGTH, in
,
17 18 19 20
to to to to
18 19 2 0 21
FIG. 8--Core piece size distribution before and after transportation.
original fracture pattern, the cores should be packed in foam rubber or

newspaper inside wooden core boxes. Large blocks should be strapped to
University of British Columbia Library pursuant to License Agreement. No further reproductions authorized
pallets placed on old tires or other shock absorbent materials in the truck
bed.
Specimens prepared from the collected samples should be large enough
to include a unit cell or one repetition of the fracture pattern as measured
during the geologic reconnaissance. If this would produce a specimen too
large for available testing systems, specimens must be cut as large as feasi-
ble from selected locations in the sample that will provide realistic charac-
terization of the site.
If a desirable specimen size cannot be determined by examining frac-
tures, preliminary tests can be run on various size specimens. Strength and
moduli decrease generally with increased specimen size up to a size con-
taining a representative fracture system [26-28]. The size above which the
properties measured in the preliminary tests do not change, if the size
range includes that specimen containing a representative fracture distribution,
would then be the desired specimen size for the testing program.
Fracture separation is frequently a problem during specimen preparation.
Generally, larger specimens are less prone to separation along fracture
planes than are small specimens. Careful attention must be given to specimen
preparation details such as drilling or cutting speed, torque, flushing fluid
flow etc. to minimize vibrations and reduce stresses induced in specimens
during the preparation process. Structural integrity of specimens with a
tendency to separate can be maintained sometimes with a thin " b e a d " of
cement along one side. Although tension tests cannot be run on such speci-
mens, triaxial or uniaxial compression test results are not affected signifi-
cantly by the cement.
Material that is very friable--coal for example--can sometimes be cut
from original samples with a bandsaw, thus minimizing separation of pre-
existing fractures by eliminating the torques associated with coting. Sawing
specimens with an appropriate bandsaw blade can be done without water
coolant, thereby preventing undue damage to cracks filled with water solu-
ble minerals or clays. Casting rough blocks of coal in concrete or hydro-
stone before sawing helps prevent damage during cutting also.
Where a testing program is being conducted for theoretical studies of
rock behavior, precautions must be taken to ensure that all specimens are
similar. This uniformity can be accomplished by testing specimens with:
(1) no flaws; (2) similar natural fracture distributions; or (3) uniform in-
duced fracture systems. Flawless specimens are obtained by drilling slender
cores and discarding those segments containing fractures. Commercially
available dye-penetrant flaw detecting techniques can be used to find de-
fects not otherwise visible [9]. Obtaining specimens that all contain similar
natural fracture distributions is difficult, especially since no acceptable
method exists for judging their similarity. Generally, a rock sample con-
taining a uniform fracture system throughout is selected; identically oriented
specimens are then prepared from this sample. Care must be taken while
preparing these specimens to prevent alterations in the fracture system.

Specimens with a uniform distribution of induced fractures can be prepared
by line-loading a rock block at intervals corresponding to the desired frac-
ture spacing. The pieces of the rock block are then cemented back together
for additional preparation such as coring, sawing, or grinding. The cement
is then dissolved with an appropriate solvent which does not affect the rock
[29] (Fig. 9). With servo-controlled testing machines, it is possible to load
Load o pplicotion
~Frocture
FIG. 9--Preparingspecimenscontainingfractures.
intact specimens beyond the peak load, inducing a fracture regime in the
specimen, then to remove the load before complete loss of cohesion. Subse-
quent testing can then be performed on the fractured specimen.
Specimen Tolerances
Failure to adhere to prescribed specimen tolerances during specimen
preparation can yield misleading test results. Excessive side roughness, end
roughness, end parallelism, and end perpendicularity to the core axis (or
sides if prismatic specimens are used) can all cause problems (Fig. 10).
End roughness greater than 0.001 in. can create nonuniform stresses near
the ends and decrease the apparent strength of the specimen [30] (Fig. 11).
Ends which are not parallel to each other or perpendicular to the core axis
within 0.25 deg can also alter the apparent strength and deformation
moduli [9,30]. Figure 12, for example, shows affects of excessive end inclina-
tion on typical load-deformation curves. Side roughness becomes important
I1 II
End porollelism End inclination
l
End roughness Side roughness
FIG. lO~Critical specimen tolerances.
because stress concentrations may develop along rough sides and because
it creates difficulties in preparing the ends parallel and perpendicular to
the axis. ASTM Test for Unconfined Compressive Strength of Rock Core
Specimens (D 2938-71), Test for Direct Tensile Strength of Rock Core
Specimens (D 2936-71), Test for Triaxial Compressive Strength of Undrained
Rock Core Specimens Without Pore Pressure Measurement (D 2664-67),
Test for Flexural Strength of Concrete (Using Single Beam With Third-
Point Loading) (C 78-67), and the Bureau guidelines [31] spell out accept-
able specimen tolerances.
Adherance to nominal dimensions is generally not critical. Gross changes
in length-to-diameter ratios (L/D) can, however, make significant differences
in property test results due to end constraint [26] (Fig. 13). Hawkes and
MeUor [32], after surveying a variety of studies on length-to-diameter ratio
effects, have recommended a L / D of 2.5.
For competent rock types, it is fairly easy to circumvent problems of
poor specimens. If cylindrical specimens are desired, cores can be ground
on their cylindrical surface to remove side roughness. It is then simple to
clamp the cores in a V-block to surface grind the rough-sawn ends parallel
to each other and perpendicular to the core axis. Lapping techniques are
not acceptable, due to the complete lack of control on end parallelism and
perpendicularity to the core axis. Prismatic specimens can be machined
48 I 0 i I I
8o
o 0 0
o
0
0
Granite
4O
0 0
0
,,
Q.
32
I..- 0
z
~ 24 ic~
Q
000
0 0
p- I ~ So ndsto~ne
0
00
w 0
Marble A
0 A
(..)
8
0 ~:~Limestone O0 0
T y p i c a l end s u r f a c e
texture variation
measurement
Sm t _ Medium ..L Rough
r 7-
i I
I I I
o 1,000 2,000 3,000 4,000 5,000
W, END SURFACE TEXTURE VARIATION, /=in
F I G . 1 1 - - E f f e c t of specimen end surface texture variation on compressive strength [30].
accurately by damping the rough-sawn specimens in a f'~ture that will hold

a surface perpendicular to a vertical reference plane of the surface grinder.
Accurate specimens of friable rocks are harder to prepare. Clamping
must be done delicately, if at all. Extremely incompetent rocks must be
tested in the rough-sawn condition. Such materials usually have such variable
properties that the effects of poor tolerances are overshadowed. These
weaker materials exhibit also greater ability to adjust internally to ir-
regularities in the surface, thus minimizing stress concentration around
such irregularities. Gypsum compound caps may be cast on the end of
poor specimens of weak rock to create acceptable end conditions.
ST CLOUO GRAY GRANODIORITE DEVILIS HILL DACITE

55, 7, i i 1
-,~G_
6l , 0(. = . 0 8 ~
_
d
o<25 5
~ 2o 4
0(-2= .35' 3
~ ~o 2 (Z = 53 ~
g
~ 5 I
x
< 0 5.0 I0.0 15.0 O 5.0 IO.O 150
AXIAL DEFORMATION. IO-3 m
FIG. 12--Effect of end inclination on the load~deformation behavior of rock [9].
~ 1.6 I I | I I I I I
b
-.r
I-
o'CN = c o m p r e s s i v e strencjth normalize?
~ 1.4
I-
~ 1.2
~ 1.0
O
r
N .8
..J
I I I I I I I I I
0 0.2 0.4 0.6 0.8 I .0 1.2 1.4 1,6 1.8 2.0
L/D, lencjth-to-diam ratio
FIG. t3--Effect of length-to-diameter ratio on compressive strength [26].
Summary
The increased use of computer modeling in the design of openings in
rock and foundations on rock has made it more and more important to
know relevent and accurate rock properties. From the time of sampling a
field site to the completion of property tests on the rock in the laboratory,
many factors in specimen handling may alter their apparent properties.
Moisture content, orientation, crack or fracture occurrence, and specimen
tolerances are four factors that need to be considered in any laboratory
testing program. The negative influences of these factors can be minimized,
however, by giving careful attention to sampling, transporting, storing, and
preparing specimens.
References
[1] Colback, P. S. B. and Wild, B. L. in Proceedings, 3rd Canadian Symposium on Rock
Mechanics, 1965, pp. 65-83.
[2] Parker, J., Transactions, Society of Mining Engineers, American Institute of Mining,
Metallurgical, and Petroleum Engineers, Vol. 247, June 1970, pp. 142-144.
[3] Van Eeckhout, E. M., "The Effect of Moisture on the Mechanical Properties of Coal
Mine Shales," P h . D . thesis, University of Minnesota, Minneapolis, Minn., Dec. 1974.
[4] Aughenbaugh, N. B. and Bruzewski, R. F., "Investigation of the Failure of Roofs in
Coal Mines," Final Report on Bureau of Mines Contract HOI 11462, Oct. 1973.
[5] Mann, R. L. and Fatt, I., Geophysics, Vol. 25, No. 2, April 1960, pp. 433-444.
[6] "Recommended Practice for Core-Analysis Procedure," API RC 40, American Pe-
troleum Institute, 1960.
[7] Oitto, R., Zona, A., and Stears, J., Coal Mining and Processing, Vol. 7, No. 12, Dec.
1970.
[8] Winston, P. W. and Bates, D. H., Ecology, Vol. 41, No. 1, 1960, pp. 232-237.
[9] Podnieks, E. R., Chamberlain, P. G., and Thill, R. E. in Proceedings, 10th Symposium
on Rock Mechanics, Austin, Tex., 20-22 May 1968, American Institute of Mining,
Metallurgical, and Petroleum Engineers, pp. 215-241.
[10] McGill, E. and Raney, J. A., Geological Society o f America Bulletin, Vol. 81, Oct.
1970, pp. 2949-2958.
[ll] Hock, E., South African Institute Mining and Metallurgy Journal, Vol. 64, No. 10, 1964,
pp. 510-518.
[12] Jaeger, J. C., GeologicalMagazine, Vol. 97, 1960, pp. 65-72.
[13] Douglass, P. M. and Voight, B., Geotechnique, Vol. 9, No. 3, 1968, pp. 376-398.
[14] Youash, Y., Geological Society of America Bulletin, Vol. 80, Feb. 1969, pp. 303-306.
[15] Komar, C. A., Overbey, W. K., Jr., and Pasini, J., III, "Directional Properties of Coal
and Their Utilization in Underground Gasification Experiments," Technical Progress
Report 73, Bureau of Mines, Nov. 1973.
[16] Deklotz, E. J. and Brown, J. W., "Tests for Strength Characteristics of a Schistose
Gneiss, Mechanical Anisotropy," Technical Report 1-67, Department of Army, Missouri
River Division, Corps of Engineers, Omaha, Neb., May 1967.
[17] Steckley, R. C., Podnieks, E. R., Chamberlain, P. G., and Pugliese, J. M. in Field
Testing and Instrumentation of Rock, ASTM STP 554, American Society for Testing
and Materials, 1974, pp. 100-115.
[18] McWilliams, J. R. in Testing Techniques for Rock Mechanics, ASTM STP 402, Ameri-
can Society for Testing and Materials, 1966, pp. 175-189.
[19] Vickers, B. L. and Thill, R. E., Journal of Science Instruments, Series 2, Vol. 2 Oct.
1969, pp. 901-902.
[20] Thill, R. E., Willard, R. J., and Bur, T. R., Journal o f Geophysical Research, Vol.
74, No. 20, Sept. 1969, pp. 4897-4909.
[21] Mogilevskanza, S. E. M. in Proceedings, 2nd Congress of the International Society for
Rock Mechanics, Vol. 1, Privredni pregled, Belgrade, Yugoslavia, 1970, pp. 333-339.
[22] Lane, K. S. and Heck, W. J. in Proceedings, 6th Symposium on Rock Mechanics,
University of Missouri-Rolla, 1964, pp. 98-108.
[23] ErgQn, I. in Proceedings, 2nd Congress of International Society for Rock Mechanics,
Vol. 1, Privredni preglad, Belgrade, Yugoslavia, 1970, pp. 497-507.
[24] Brown, E. T., Journal ofSoilMechanics, Vol. 96, No. SM6, Dec. 1970, pp. 1935-1949.
[25] Einstein, H. H., Nelson, R. A., Bruhn, R. W., and Hirshfeld, R. C. in Rock Mechanics
Theory and Practice, Proceedings, l l t h Symposium on Rock Mechanics, New York,
American Institute of Mining, Metallurgical, and Petroleum Engineers, 1970, pp. 83-103.
[26] Obert, L., Windes, S. L., and Duvall, W. I., "Standardized Tests for Determining the
Physical Properties of Mine Rock," Report of Investigations 3891, Bureau of Mines,
1946.
[27] Bieniawski, Z. T. in Proceedings, 10th Symposium on Rock Mechanics, American
Institute of Mining, Metallurgical, and Petroleum Engineers, 1972, pp. 409-427.
[28] Dhir, R. K. and Sangha, C. M., Colliery Guardian, VoL 220, No. 1, Jan. 1972, pp.
75-78.
[29] Wawersik, W. R. and Brown, W. S., "Creep Fracture of Rock," University of Utah
Report, UTC-ME 73-197, Final Report on Bureau of Mines Contract HO220007, July
1973.
[30] Hoskins, J. R. and Horino, F. G., "Effect of End Conditions on Determining Com-
pressive Strength of Rock Samples," Report of Investigations 7171, Bureau of Mines,
1968.
[31] "Bureau of Mines Test Procedures for Rocks," Information Circular 8628, U.S. Bureau
of Mines, 1974, pp. 120-126.
[32] Hawkes, I. and MeUor M., Engineering Geology, Vol. 4, No. 3, July 1970, pp. 177-285.
G. N . D u r h a m I
Trimming Device for Obtaining

Direct Shear Specimens from
Samples of Stiff Fissured Clay Shale
REFERENCE: Durham, G. N., "Trimming Device for Obtaining Direct Shear Spec-
imens from Samples of Stiff Fissured Clay Shale," Soil Specimen Preparation for Labo-
ratory Testing, ASTM STP 599, American Society for Testing and Materials, 1976,
pp. 37-42.
ABSTRACT: A device has been developed at the U. S. Army Engineer Waterways Exper-
iment Station for obtaining direct shear specimens of hard, brittle soils, the use of which
has resulted in a reduction in man-hours for specimen preparation from 3 or 4 h to 50 or
60 min per specimen. This device, which has proved to be superior to any previous ap-
paratus used for obtaining direct shear specimens of such soils, is fitted to the base of a
commercially available unconfined compression apparatus of the hand-operated type.
Samples found untrimmable heretofore can now be tested, because a sample is held
rigidly during trimrning operations, and the time of exposure to air drying (and sub-
sequent deterioration) has been reduced substantially.
KEY WORDS: soils, soil tests, shear properties, clays, shales, residual stress
The concept of residual strength suggested by Skempton 2 has contributed

greatly toward a better understanding of the magnitude and mechanism of
shearing resistance of highly overconsolidated clays and clay shales. Typi-
cally, clay shale materials exhibit significant differences in the effective shear
strength parameters, c and +, corresponding to peak strength and residual
strength. The shearing resistance of a clay shale undergoing displacement will
decrease substantially after failure and ultimately stabilize at a constant
residual shear strength.
The laboratory determination of the residual strength requires unconven-
tional apparatus and techniques for producing a large displacement. Two
methods are most prevalent for measuring residual shear strength--annular
torsion tests and repeated direct shear tests. Townsend and Gilbert 3 reported
t Research civil engineer, Mobility and Environmental Systems Laboratory, U. S. Army
Engineer Waterways Experiment Station, Vicksburg, Miss. 39180.
2Skempton, A. W., Geotechnique, Vol. 14, No. 2, June 1964, pp. 77-101.
3Townsend, F. C. and Gilbert, P. A., "Engineering Properties of Clay Shales; Residual
Shear Strength and Classification Indexes of Clay Shales," Technical Report S-716, Report 2,
U. S. Army Engineer Waterways Experiment Station, Corps of Engineers, Vicksburg, Miss.,
Aug. 1974.
37
Downloaded/printed
the results of residual shear strength tests performed on samples of highly

overconsolidated clay shales from numerous geological deposits. With regard
to this discussion, two of their more significant findings were:
1. The variation of residual friction angles measured by repeated direct
shear tests, annular shear tests, or rotational shear tests were very small and
well within the range of experimental error.
2. Residual shear strengths were found to be independent of specimen
preparation procedures with comparable values being obtained from intact,
precut, and remolded specimens of a clay shale sample.
Residual Shear Test Procedures

Annular shear apparatus tend to be expensive and require elaborate pro-
cedures and a trimming device for intact specimen preparation. Hence, an-
nular shear devices are usually found only in research-oriented or advanced
soil testing facilities. However, most facilities for testing physical properties
of soil are equipped with direct shear testing equipment that may be adapted
to residual direct shear testing with perhaps only minor modifications. A
controlled strain device, in which the direction of shear can be reversed,
should be used to apply the horizontal shear force to the specimens.
The shear surface or zone can be formed by (a) shearing an intact spec-
imen, (b) cutting a plane surface through an intact specimen or (c) shearing
a completely remolded specimen. Practical laboratory considerations favor
the use of a precut shear plane, since producing a plane surface by shearing an
intact stiff-to-hard specimen may be difficult. Any irregularities of the shear
surface would introduce an added resistance that would not be a measure
of the shear strength of the material.
More often than not, stiff and hard clays and clay shales are jointed or
fissured or both. In addition, shales and clay shales often contain faults and
shear zones. These formations usually contain partings of soil, silt, sand-
stone, or siltstone, and, occasionally, partings or layers of bentonite. These
characteristics of clay shale formations tend to complicate the trimming of
intact direct shear specimens, resulting in a time-consuming, tedious task.
Waterway Experiment Station Residual Shear Testing

Since 1968, the U. S. Army Engineer Waterways Experiment Station
(WES) has become extensively engaged in residual shear testing of clay shale.
The only previous method, of many tried at WES, that produced satisfactory
3 by 3-in. (76 by 76-mm) square direct shear specimens of hard soils consisted
of the following steps: with a bandsaw, a horizontal slice ~ in. (3.2 mm)
thicker than desired was c u t from a 5-in. (127-mm)-diameter undisturbed
sample; the horizontal surfaces were made parallel and brought to the desired
DURHAM ON SHEAR SPECIMENS OF STIFF FISSURED CLAY SHALE 39
thickness by fitting the slice in a 6-in. (152.4-mm)-diameter ring and planing

the surfaces with the knife edge of a hardened steel straightedge. A square
approximately 388 in. (77.8 mm) on the side was cut with the handsaw, and
the sides were trimmed with the steel straightedge and stationary cutting
guides to form an exact 3 by 3-in. (76 by 76-mm) specimen. This process took
approximately 3 to 4 h, with a high rate of specimen breakage, especially
in final stages of preparation. These lost specimens were probably due to the
large amount of handling and the deterioration of the soil during the 4 h of
air drying (even though trimming was done in a room with controlled tem-
perature and humidity).
Earlier attempts to prepare direct shear specimens consisted of forcing a
standard direct shear specimen cutter into an approximate 3 by 3-in. (76 by
76-mm) horizontal slice with the aid of an unconfined compression testing
frame. However, the ~-in. (3.2-mm)-thick walls of the cutter deformed out-
wardly during these operations, resulting in a specimen of irregular shape.
Furthermore, because of the stresses imposed by the walls of the cutter, the
specimen tended to break when extruded from the cutter into the shear box.
The foregoing problems and experiences resulted in the development of a
trimming device that has thus far proved to be far superior to any of the pre-
vious apparatus used at WES for obtaining direct shear specimens of hard,
brittle soils.
WES Direct Shear Trimming Device

A direct shear trimming device was designed and fabricated at WES in
1971. The trimming device (Fig. 1) is fitted to the base of a commercially
available unconfined compression apparatus (Soiltest Model U-160; a hand-
operated device). The loading frame of this apparatus was removed, with
the gearing arrangement located in the inclosed base used to push the spec-
imen through the specimen cutter blade and into the specimen holder.
The trimming device consists of two principal components, the specimen
holder and the specimen cutter blade. The two parts are detachable for trim-
ming procedures (reasons discussed later) and for convenient sharpening
or replacing of a worn cutter blade. The specimen holder consists of four
sides fastened with machine bolts; this not only facilitates fabrication but
also allows the prepared specimen to be extracted without extrusion from
the specimen holder. Two specimen holders were fabricated for an 0.25
(6.4-mm) or an 0.50-in. (12.8-mm)-thick specimen. Normally, two 0.25-in.
(6.4-mm) specimens are trimmed from a single sample to form the upper
and lower halves of a direct shear specimen with a precut shear plane.
U. S. Army Engineer Manual EM-1110-2-19064 suggests that a direct shear
4"Engineeringand Design:LaboratorySoilsTesting,"EngineeringManualEM 1110-2-1906,
Appendix IX(A), Officeof the Chiefof Engineers, Headquarters, Departmentof the Army,
Washington,D. C., 30 Nov. 1970.
FIG. 1-- WES direct shear trimming device.
specimen should be 3 by 3 in. (76 by 76 mm) square, trimmed from a 5-in.

(127-mm)-diameter undisturbed sample. For direct shear devices equipped to
test smaller circular specimens, a device similar to that in Fig. 1 could be con-
structed, probably with a less complicated design and more efficient and less
expensive fabrication procedures.
A horizontal slice of soil, approximately ~ in. (3.2 mm) thicker than the
desired final height and approximately 388 by 388 in. (77.8 by 77.8 mm)
DURHAM ON SHEAR SPECIMENS OF STIFF FISSURED CLAY SHALE 41
square, is placed on a soft wood block about 4 by 4 by 88in. (102 by 102 by

6.4 mm), which rests on a piston (Fig. 2a). By means of a hand crank, the
piston pushes the soil vertically upward through the cutter blade until the
blade comes into contact with the wood block. The wood block is used to
prevent corners of the specimen's bottom surface from shearing away under
the force of the cutting action. The piston is then lowered slightly and the
FIG.2-- Typicalprocedurefor trimming directshearspecimenfrom clay-shalesample.
block removed; wall friction prevents the specimen from moving. The piston
is then brought into contact with the specimen and moved upward until the
upper surface of the soil extends slightly above the specimen holder. The
excess soil above the specimen holder is removed with a hardened steel straight-
edge (Fig. 2b). The cutter blade is disconnected from the specimen holder,
which, in turn, is removed from the stanchions and fastened inverted to a
89 (12.7-mm)-thick machined steel plate. The excess material from the
bottom surface is then removed (Figs. 2c and d), the sides of the specimen
holder are disconnected, and the specimen is placed in the shear box for test-
ing.
Discussion
Use of the WES direct shear trimming device has resulted in a reduction in
man-hours for preparation from 3 to 4 h to 50 to 60 min per specimen. Sam-
ples heretofore found untrimmable can now be tested for residual strength
parameters because the sample is held rigidly during trimming operations and
the time of exposure to air drying (and subsequent deterioration) has been
reduced substantially.
Acknowledgment
Acknowledgment is made to W. J. Hughes, civil engineer technician, and
J. P. Wislocki, mechanical engineer, both of the WES, for their significant
contributions in the development and design of the WES direct shear trim-
ming device. The author wishes to thank M. L. Doiron for her editorial review
of this paper and K. M. Jennings, who typed and assembled the paper.
F. C. Townsend' and P. A. Gilbert'
Effects of Specimen Type on the

Residual Strength of Clays and
Clay Shales
REFERENCE: Townsend, F. C. and Gilbert, P. A., "Effects of Specimen Type on

the Residual Strength of Clays and Clay Shales," Soil Specimen Preparation for
Laboratory Testing, ASTM STP 599, American Society for Testing and Materials,
1976, pp. 43-65.
ABSTRACT: This investigation was an examination of the effects of testing apparatus,

specimen type and density, normal stress, and sequence of loading on the residual
strength of various clays and clay shales. Annular shear and repeated direct shear
tests were conducted on intact shale specimens with precut failure planes, while com-
parison rotational shear tests were conducted on the same shale material subjected to
various degrees of remolding. Test results indicate that comparable residual strengths
can be obtained, regardless of equipment type and procedure or degree of remolding.
Supplemental annular shear tests on residual clay and silty sand show that precutting
of the failure plane or the specimen density has no effect on the ~/value. The residual
friction angle is independent of stress history and normal load [when greater than
2 kg/cm 2 (1.96 X 105 Pa)].
KEY WORDS: clays, shales, residual shear stress, direct shear tests, annular shear
tests, soils
The concept o f residual strength has contributed greatly towards a better

u n d e r s t a n d i n g o f t h e m a g n i t u d e o f shearing resistance t h a t is o p e r a t i v e in
o v e r c o n s o l i d a t e d clays a n d c l a y shales a f t e r large d i s p l a c e m e n t s h a v e
o c c u r r e d . This residual s h e a r i n g resistance is quite low in c o m p a r i s o n to
p e a k strengths determined b y conventional l a b o r a t o r y procedures a n d equip-
m e n t , a n d special a p p a r a t u s a n d t e c h n i q u e s c a p a b l e o f p r o d u c i n g large
displacements are required for the accurate l a b o r a t o r y determination o f the
r e s i d u a l s h e a r strength. T y p i c a l l y , a n n u l a r s h e a r o r r e p e a t e d direct s h e a r
tests using intact specimens with o r w i t h o u t p r e c u t failure p l a n e s o r speci-
m e n s o f r e m o l d e d m a t e r i a l a r e u s e d to e v a l u a t e the r e s i d u a l strength o f a
m a t e r i a l . T h e tests a r e o f t e n c o n d u c t e d in m u l t i s t a g e f a s h i o n ; t h a t is, a
Research civil engineers, Soil Mechanics Division, U.S. Army Engineer Waterways Experi-
ment Station, Vicksburg, Miss. 39180.
43
Downloaded/printed
single specimen is tested under various normal stresses in order to define

the residual envelope. Currently, only a few investigators [1-3] 5 have ex-
amined various facets o f equipment and procedural effects in residual
strength.
The objective o f this investigation was to examine the effects o f equip-
ment type and associated procedure, specimen type, normal stress, and
loading sequence on the residual strength of various clay shales and clays.
These effects were evaluated by conducting annular shear and repeated
direct shear tests on shale specimens with precut failure planes. Comparison
rotational shear tests were conducted on remolded specimens subjected to
different processing procedures. Additional annular shear tests on a clay
and micaceous silty sand were used to evaluate the effects of precutting
and initial specimen density.
Previous Investigations
Equipment
The repeated direct shear method using conventional apparatus was de-
veloped by Skempton [4] and has been adapted as a uniform procedure by
the Corps of Engineers. This method involves shearing the specimen a
limited distance in one direction and then either reversing the direction o f
shear or relieving the normal load and pushing the movable half o f the
shear box back to its initial position before shearing again. These opera-
tions are repeated until sufficient displacements are accumulated to reach
a residual condition. A characteristic stepped displacement-shear stress
curve is produced in which the succeeding peaks are due to particle reorienta-
tion or to the formation of new slip planes with each cycle. 3 The less com-
mon ring torsion method was used first in the 1930's by early investigators
[5,6]. The method provides continuous displacements in one direction of
an annular specimen; this feature is desirable in research evaluation of
residual strength [3,4, 7].
Specimen Type
A general agreement exists in the literature [3,8] that residual shear
strength is independent of stress history and that the alignment o f clay
particles in a failure zone o f remolded material controls the value o f +r '
Consequently, three basic specimen types, (a) intact, (b) precut, and (c) re-
sedimented or remolded-reconsolidated, are being tested by various labora-
tories. Testing on intact specimens o f clay shale poses several problems,
2The italic numbers in brackets refer to the list of referencesappended to this paper.
3Skempton himself recognizedthat the method was imperfect and suggested that ideally
the displacement should be continuouslyin one direction, as occurs in field situations.
TOWNSEND AND GILBERT ON CLAYS AND CLAY SHALES 45
namely, (a) preventing slippage between the specimen and torque plate
and (b) having equipment capable of applying high shearing stresses to
initially shear the material and yet sensitive enough to measure low residual
strengths. As a result of these difficulties and Skempton's [9] observation
that precutting ensures the lowest shearing resistance and most conserva-
tive result, the present trend in testing clay shales is to use precut specimens.
Alternatively, since any effects of stress history of the sample on +r ' are
obliterated by the remolding action occurring in and along the failure zone,
the use of remolded samples offers another method for specimen prepara-
tion in residual strength testing. Tiedermann [5], Skempton [4], and Petley
[7] demonstrated that the residual strength of clays normally consolidated
from a slurry was equivalent to that of undisturbed overconsolidated clay.
Effects of Loading Sequence

Based upon the assumption that ~br' is independent of stress history
(previous loading and unloading), a laboratory practice of using multistage
loading tests has developed, that is, a single specimen is tested under various
normal stresses in order to define the residual strength envelope. Kenney
[10] presents results of tests under o, ' from 0.8 to 8.0 and 0.6 to 6.0 kg/cm ~
(0.78 x 105 to 7.8 x 105 and 0.58 x 105 to 5.8 x 105Pa)thatshowed
that ~r' values were essentially the same for a given o~' value, regardless of
loading sequence. Bishop et al [3] likewise stated that, based on ring shear
tests on Weald and brown London clay, ~r ' is independent of stress history.
Materials and Equipment
Materials
Various clay shales from foundations at Corps of Engineers' projects
were tested using repeated direct shear, annular shear, and rotational shear
equipment and techniques. These were:
(a) Dawson shale, Chatfield Dam, South Platte River, Colorado,
(b) Taylor I shale, Laneport Dam, San Gabriel River, Texas,
(c) Strawn shale, Proctor Dam, Leon River, Texas,
(d) Kincaid shale, Cooper Dam, Sulphur River, Texas,
(e) Bearpaw shale, Fort Peck Dam, Missouri River, Montana, and
(1") Pierre shale, Oahe Dam, Missouri River, South Dakota.
Since shearing an intact specimen of clay shale by annular shear equip-
ment is virtually impossible, the effects of precutting and compacted density
were evaluated on softer materials. These were:
(a) Residual clay, Volta Grande, Brazil,
(b) Micaceous silty sand, Rio Paraibuna, Brazil, and
(c) Micaceous silty sand, Rio Paraitinga, Brazil.
Table 1 presents the classification indexes of the materials tested. The

classification indexes of clay shales are greatly influenced by test procedures
[11], so all specimens reported in Table 1 were subjected to the three Corps
of Engineers processing procedures for clay shales, namely, (a) undried,
(b) air dried, and (c) blenderized. Complete descriptions of these procedures
are published elsewhere [11-13].
TABLE 1--Classification indexes of clay shales and clays tested for this study.
Activity
Plasticity
Processing Liquid Plastic Plasticity <2/am, Index
Material Method" Limit Limit Index % <2/am, ~
Dawson shale undried 61 20 41 35 1.17

Chatfield Dam air dried 65 23 42 50 0.84
blenderized 84 25 59 56 1.05
Taylor I shale undried 65 22 43 47 0.91
Laneport Dam air dried 65 21 44 50 0.88
blenderized 79 21 58 57 1.02
Strawn shale undried 51 23 28 47 0.59
Proctor Dam mr dried 52 21 31 48 0.64
blenderized 62 24 38 64 0.59
Kincaid shale undried 88 22 66 35 1.88
Cooper Dam mr dried 78 23 55 46 1.17
blenderized 113 22 91 52 1.75
Bearpaw shale undried 95 29 66
Ft. Peck Dam air dried 128 31 97 61' 1.59
blenderized 161 29 132 64 2.06
Pierre shale undried 83 41 42 34 1.23
Oahe Dam air dried 91 40 51 47 1.08
specimen U-22 blenderized 140 38 112 56 2.00
Pierre shale undried 178 34 144 75 1.92
Oahe Dam air dried 297 34 263 80 3.28
specimen U-28 blenderized 351 31 320 85 3.76
Micaceous silty sand 39 28 11 12 0.92
Rio Paraitinga
Micaceous silty sand ..." 33 27 6 5 1.20
Rio Paraibuna
Residual clay ...~ 96 38 58 40 1.45
Volta Grande
* In accordance with procedures in EM 1110-2-1906 [13].
Equipment
The apparatus used for determining the residual shear strength of the
shales consisted of an annular shear device, a repeated direct shear
machine, and a rotational shear machine. Brief descriptions of the equip-
ment follow.
Waterways Experiment Station Low-Capacity Annular Shear Apparatus--

The annular shear apparatus used in these tests is based on previous
designs by Hvorslev. 4 The annular specimen is 4.00 in. (10.16 cm) outside
diameter, 2.03 in. (5.16 cm) inside diameter, and 0.75 in. (1.91 cm) thick.
The normal stress is applied by a pneumatic stress cell which pulis on a
cable bearing against the loading platen on top of the specimen. A maxi-
mum normal stress of 15 kg/cm ~ (14.7 • 105 Pa) can be applied. The
shear stress (maximum 2.5 kg/cm ~ (2.45 • 105 Pa)) is measured by a
torque plate through torque arms mounted on the top loading platen. An
electrical motor and gear box rotate the lower half of the specimen. The
specimen is confined between upper and lower confining rings, and the
gap can be adjusted by differential screws as the specimen consolidates
during shear.
Geonor Direct Simple Shear Machine--The reversal direct shear tests
were conducted in a Geonor, direct-simple shear apparatus which was
modified to accept a 2.78-in. (7.06 cm)-square direct shear, 0.59-in. (1.50
cm)-thick specimen. The lower half of the shear box is fixed, and the top
half can be displaced 0.3 in. (0.76 cm) to either side of center. The upper
half of the shear box has knife edges; the lower half is Teflon coated to
minimize any metal-to-metal friction should the gap close. The gap is
adjusted manually by inserting a feeler gage. To minimize geometric effects
and area corrections, only those shear stresses measured when the box is
centered are used in plotting residual strength against deformation curves.
Harvard Rotational Shear Apparatus--The rotational shear apparatus
was developed at Harvard University by La Gatta [8]. The apparatus
tests annular specimens (2.8 in. (7.11 cm) outside diameter, 2.0 in. (5.08
cm) inside diameter, and 0.14 in. (0.36 cm) high) of remolded material
prepared from the trimming scraps of the annular shear specimens and
processed by the Corps of Engineers [13] undried, air dried, or blenderized
procedures. Shear stresses are generated by rotating a porous disk at the
bottom of the specimen and using two electrical force transducers to
measure the couple required to keep the top half of the specimen stationary.
Testing of clay shale materials was conducted either on specimens of
intact material with precut failure planes or on specimens composed of
remolded material. Specimens with precut failure planes were prepared by
separately trimming the top and bottom specimen halves from the shale
cores and placing them in confining rings or shear boxes. These specimen
halves were then placed in their respective shearing devices (annular shear
4Construction or modificationwas accomplished at the WaterwaysExperiment Station
under the generalsupervisionof B. N. Maclver.
or direct shear) and allowed to consolidate under the applied normal

stress. This method of preparation facilitates reproducible results and
ensures the lowest possible shear resistance that can be mobilized by the
shale [9].
Annular shear specimens of Volta Grande clay for investigating the
effects of precut failure planes were prepared by either trimming intact
specimens from a block sample or separately trimming the top and bottom
specimen halves in the procedure used for shale specimens.
Annular shear specimens of micaceous silty sand for investigating the
effects of density were prepared by trimming intact specimens from an
undisturbed block sample or by compacting specimens, prepared from
trimming scraps of the intact specimens, in the confining rings to the
selected density and water content. Compaction was accomplished using
a hand-held pneumatic tamping miniature compactor (similar to the
spring-loaded Harvard miniature compactor) with a Teflon section-shaped
foot. Loosely or densely compacted specimens were prepared at 90 or
100 percent, respectively, of maximum standard density.
Annular Torsion Tests Conducted in Waterways Experiment Station

Low-Capacity Annular Shear Apparatus
Annular shear specimens were allowed to consolidate or swell under
selected normal stresses until equilibrium was achieved (usually two to
three days). Shear was then initiated at a slow rate of displacement5 (1.75
cm/day) until the peak strength had been achieved (usually when only
several millimetres of displacement had occurred). The rate of displace-
ment was then increased to 14.0 cm/day until an apparent ~r' condition
was reached. Then the rate of displacement was reduced to its original
value. It was anticipated that using a rapid rate of displacement to pro-
duce large displacements, followed by a reduced rate of displacement for
the final evaluation of d~r', would prove to be a satisfactory and less
time-consuming method of determining ~r' than the use Of a constant low
rate of displacement method [14]. After 4,' had been determined under a
specific normal stress, shear was terminated. The specimen was then
either consolidated or allowed to rebound under a new normal stress.
After equilibrium had been reestablished, shear was reinitiated at a rate of
displacement consistent with that used under the initial normal stress.
Repeated Direct Shear Tests Conducted in Modified Geonor Direct

Simple Shear Apparatus
Repeated direct shear tests are the most common method presently
used for measuring ~ ' . However, the validity and effects of repetitive
5Displacement is measured along the circumferencecalculated from the mean specimen
radius.
back-and-forth movement as opposed to continuous one-directional shear

have not been fully investigated. Accordingly, this series of tests was
made for comparison of d~,' values measured by annular tests. The speci-
mens were precut, consolidated to equilibrium under various normal
stresses corresponding to those used in the annular tests, and generally
sheared at a slow rate of displacement (1.16 cm/day). After ~ / h a d been
clearly defined, as shown by a ~ / versus logarithm displacement graph,
the specimen was returned to its center position, a new normal stress was
applied, and shearing was reinitiated after consolidation equilibrium had
been achieved.
Rotational Shear Tests Conducted in Harvard Apparatus

This series of tests evaluated the effects of material processing on ~r'
values of remolded specimens prepared through use of the three proce-
dures: undried, air dried, and blenderized. The remolded specimens at
water contents above the liquid limit were consolidated under a normal
stress of 6 kg/cm 2 (5.88 x 105 Pa) until observation of vertical displace-
ments indicated that equilibrium had been reached. To prevent excessive
extrusion during consolidation, loads were applied incrementally until a
normal stress of 6 kg/cm 2 (5.88 x l0 s Pa) was reached. A pilot test series
was conducted to determine the effects, if any, of displacement rate d on
d?r'. Based upon these pilot tests, the rate of displacement used for the
tests discussed herein was 69.1 cm/day. Each specimen was displaced an
additional several centimetres after de/ had been reached, as determined
by a dCr' versus log displacement plot [6, 8].
Test Results and Analyses

Tables 2 and 3 summarize the annular shear, repeated direct shear, and
rotational shear test results. The order of normal stress listing refers to
the sequence in which the normal stresses were applied during multistage
tests.
Effect of Equipment Type

Figure 1 presents the residual strength envelopes of companion an-
nular shear, repeated direct shear, and rotational shear tests. Since the
residual shear stress is quite small, tile vertical scales of the graphs have
been exaggerated to provide better comparison between types of tests.
From these results, it is evident that very little difference exists between
the residual shear strength values of clay shale specimens with precut
failure planes, whether measured by annular shear or repeated direct
shear tests (compare circles and triangles). Herrmann and Wolfskill [1]
T A B L E 2--Summary o f residual shear strength tests on clay shales, tl~
0
Residual Displacement per
r
Normal Rate of Shear Stage Required to o
Stress, Displacement, Strength, Achieve ~r ', cmb r"
Shale/Test Test Type~ kg/cm 2 cm/day ~r ', deg (not cumulative) Comments r
-o
m
Dawson
ASI3 AS 6.1 1.75 5.7 cyclic annular shear tests;
m
sample sheared for 1.75 cm in z
one direction; normal load -u
removed and sample manu-
ally returned to initial starting m
-u
point
6.1 1.75 4.9 38.4 continuous annular shear, one
direction --4
5
DS-16 RDS 6.0 1.163 4.9 8.5 Z
6.0 0.593 4.6 4.8 "11
0
RS
H A 316 undried 6.0 69 7.3 73.1
W
H A 310 air dried 6.0 ~ 7.0 31.9 0..n
H A 288 blenderized 6.0 ~ 6.8 19.5 -t
0
Taylor I .<
AS-20 AS 6.1 1.75 12.8 13.0 residual was not yet achieved -t
6.1 14.03 10.6 61.0 residual was not yet achieved m
12.1 1.75 10.6 0.5 .-t
12.1 14.03 11.7 13.0
0
3.1 1.75 10.3 11.3
3.1 14.03 8.8 68.3
1.6 1.75 8.6 0.2 residual was not yet achieved
1.6 14.03 8.2 35.4
1.6 1.75 8.3 3.3
DS-17 RDS 6.0 1.16 9.6 33.0
12.0 1.16 10.3 10,0
H A 285 RS, blenderized 6.0 69 9.8 20.9 tests on material prepared by
undried and air-dried proce-
dures could not be conduc-
ted as peak strengths over- -4
loaded force transducers O
Strawn Z
AS-23 AS 6.1 1.75 8.2 1.7 residual not achieved prior to m
6.1 14.03 8.5 17.1 increase in rate of displace- z
o
6.1 1.75 8.7 1.5 ment
12.1 1.75 1.7 peak not achieved prior to in- z
12.1 14.03 9.5 18.5 crease in displacement rate o
12.1 1.75 9.5 1.7
3.1 1.75 10.0 3.9 residual not achieved prior to F
3.1 14.03 9.3 37.7 increase in rate of displace- ~0
m
3,1 1,75 9.3 3.3 ment 30
-4
1,6 1.75 9.3 5.3
1.6 14.03 9.2 28.0 o
Z
1.6 1.75 9.4 5.0
0r'-
DS-5 RDS 6.0 0.59 9.2 3.0
12.0 0.59 9.8 0.35
RS
H A 323 undried 6.0 69 9.6 91,2 z
H A 321 air dried 6.0 69 9.1 6.0

H A 292 blenderized 6.0 69 7.2 1.4
.<
Kincald -r
AS-25 AS 1.6 1.75 14.6 2.0 residual not developed prior to f-
1.6 14.03 5.7 58.4 increase in rate of displace- m
co
1.6 1.75 5.5 3.4 ment
3.1 1.75 5.3 12.6
Grl
3.1 14.03 5.0 28.0 =,.k
T A B L E 2--Summary o f residual shear strength tests on clay shales--Continued, t.~
Residual Displacement per fD

Normal Rate of Shear Stage Required to _o
Stress, Displacement, Strength, Achieve ~r ', cm b r"
Shale/Test Test Type" kg/cm 2 cm/day ~, ', deg (not cumulative) Comments f/J
"u
I"11
3.1 1.75 4.7 3.8 o_
6.1 1.75 4.8 14.2
m
6.1 14.03 4.9 13.2 Z
12.1 1.75 5.2 2.3 "o
12.1 14.03 5.8 25.9 :D
m
12.1 1.75 5.5 6.4 "13
3.1 1.75 5.7 8.8 :23
3.1 14.03 5.7 28.1
-4
1.6 1.75 5.9 6.0
1.6 14.03 5.9 55.9 z
1.6 1.75 5.6 ll.O "rl
DS- 15 RDS 6.0 0.59 5.5 25.3 o
:23
12.0 0.59 5.3 28.5
r"
RS, blenderized rotational shear tests could not
be successfully completed due 03
o
to "grittiness" of material
Bearpaw -4
6.1 1.75 7.4 2.4 0.75 N solution of Na2SO4 used o
AS-26 AS ,-n
.,<
6.1 14.03 6.5 55.7 as saturating fluid
6.1 1.75 6.9 6.8 -4
l'rl
12.1 1.75 6.6 3.5
12.1 14.03 6.8 J4.0
12.1 1.75 6,6 7.0
3.1 1.75 7.4 7.6
3.1 14.03 7.1 75.0
1.6 1.75 8.2 5.2
1.6 14.03 8.0 14.0
1.6 1.75 8.0 3.5
CopyrightbyASTMInt'l(allrightsreserved);WedDec2214:00:00EST2010
Downloaded/printedby
UniversityofBritishColumbiaLibrarypursuanttoLicenseAgreement.Nofurtherreproductionsauthorized.
DS-10 RDS 6.0 0.59 6.3 15.7 0.75 N solution of NazSO4 used
12,0 0.59 6.2 3.6 as saturating fluid
H A 197 RS, air dried 6.0 69.0 5.0 8.6
RS, blenderized
with distilled
water 6.0 69.0 4.7 15.0
H A 222 RS, blenderized
in 0.75 N Z
Na2SO4 6.0 69.0 6.4 8.9
m
Z
Pierre shale
low plasticity
AS-28 AS 6.1 1.75 7.0 21.0 Z
6.1 14.03 7.1 43.0
6.1 1.75 6.9 1.2
12.1 1.75 8.8 peak not achieved prior to in- 0o
12.1 14.03 10,4 62.8 crease in displacement rate m
~D
12.1 1.75 10.2 4.1 .-I
6.1 1.75 7.7 5.3
0
6.1 14.03 8.3 68.5 Z
6.1 1.75 7.8 4.2 0
3.1 1.75 8.1 33.3
3.1 14.03 8.6 5.0
3.1 1.75 7.5 1.7
DS-12 RDS 6.0 0.59 7.1 25.7 Z
12.0 0.59 7,1 2.4
0
high plasticity
AS-29 AS 6.1 1.75 3.0 12.2
12.1 1.75 3.6 2.3
12.1 14.03 3.8 41.7 I
12.1 1.75 4.0 1.2 f-
6.1 1.75 3.7 1.7 ro
6.1 14.03 3.5 30.2
6.1 1.75 3.5 6.1
O1
3.1 1.75 3.7 3.5
01
0~
O
I"
fD
T A B L E 2--Summary o f residual shear strength tests on clay shales--Continued. "U
Residual Displacement per

ITI
Normal Rate of Shear Stage Required to Z
Stress, Displacement, Strength, Achieve ~r ', cm ~
Shale/Test Test Type" kg/cm 2 cm/day ~r ', deg (not cumulative) Comments -m
i"1'1
"U
3.1 14.03 3.6 57.6 ),
:]0
3.1 1.75 3.1 3.5 3>
--I
1.6 1.75 3.7 35.1
1.6 14.03 3.8 5.1 O
Z
1.6 1.75 3.7 1.7
-11
DS-!3 RDS 6.0 0.59 3.1 15.0 O
:D
12.0 0.59 3.6 6.0
t-
H A Ii5 RS, undried 6.0 69 2.0 191.2
O
H A 122 RS, air dried 6.0 69 3.3 480.4 ~D
H A 119 RS, blenderized 6.0 69 3.2 5.3

0
NOTE--All specimens except those tested in the rotational shear apparatus were intact except that the failure surface was precut prior -<
to testing. --4
~ AS = annular shear; RDS = repeated direct shear; RS = rotational shear. m
b If residual not achieved for stage, displacement shown is total displacement for stage at specified displacement rate.
Z
fi3
TABLE 3--Summary o f results o f annular shear tests.
Residual Displacement
Normal Rate of Shear per Stage
Stress, Displacement, Strength, Required to
Specimen Description kg/cm 2 cm/day d~r', deg Achieve ~r ', cmb
Paraitinga, undisturbed 3.1 1.75 31.3 8.7

block, 94.7 lb/ft 3 3.1 7.02 31.2 49.8
3.1 1.75 31.1" 11.7
1.1 1.75 33.6 9.6
1.1 7.02 33.1 29.4
1.1 1.75 32.9" 10.4
Paraibuna, undisturbed 3.1 1.75 29.5 9.8
block, 100.9 lb/ft 3 3.1 7.02 28.7 48.7
3.1 1.75 28.5" 8.5
1.1 1.75 27.4 9.6
1.1 7.02 27.8 29.4
1.1 1.75 27.4" 10.9
9.1 1.75 28.4 16.1
9.1 1.02 27.4 51.5
9.1 1.75 26.7" 16.1
Paraitinga, bag 1.1 1.75 34.5 25.3
specimen, loosely 1.1 7.02 33.5 28.1
compacted, 95.5 lb/ft~ 1.1 1.75 32.7" 12.3
3.1 1.75 29.4 19.0
3.1 7.02 27.8 47.1
3.1 1.75 27.7~ 15.4
Paraitinga, block 1.1 1.75 32.0 17.7
compacted, 96.1 lb/ft3 1.1 1.75 31.2" 5.9
3.1 1.75 30.5 3.8
3.1 7.02 29.6 48.7
3.1 1.75 30.0" 2.8
5.1 1.75 29.5 13.8
5.1 7.02 28.6 79.9
5.1 1.75 28.2" 6.4
Paraibuna, block 1.1 1.75 30.1 28.0
compacted, 98.0 lb/ft3 1.1 1.75 29.3 a 2.7
3.1 1.75 28.5 13.8
3.1 7.02 28.0 79.9
3.1 1.75 26.9 a 6.4
Paraitinga, block 1.1 1.75 33.8 15.6
specimen, densely 1.1 7.02 32.3 35.8
compacted, 106.8 1.1 1.75 32.4 ~ 2.7
lb/ft 3 3.1 1.75 30.8 13.7
3.1 7.02 29.8 79.9
3.1 1.75 29.6 a 6.4
9.1 1.75 28.1 23.7
9.1 7.02 28.1 21.2
9.1 1.75 27.7" 28.5
Paraibuna, block 1.1 1.75 28.3 38.2
specimen, densely 1.1 7.02 28.1 14.0
compacted, 108.9 1.1 1.75 28.5* 1.7
lb/ft 3 3.1 1.75 29.6 15.5
T A B L E 3--Summary of results of annular shear tests--Continued.
Residual Displacement
Normal Rate of Shear per Stage
Stress, Displacement, Strength, Required to
Specimen Description kg/cm 2 cm/day ~, ', deg Achieve ~r ', cmb
3.1 7.02 28.6 52.7

3.1 1.75 28.4* 8.4
9.1 1.75 27.9 15.1
9.1 7.02 27.4 44.3
9.1 1.75 27.1 a 2.3
Volta Grande precut 3.1 1.75 8.9 29.6
failure plane 3.1 14.05 9.5 72.9
3.1 1.75 8.6 80.9
1.6 1.75 9.3 10.5
1.6 14.05 10.0 70.8
1.6 1.75 9.1 83.1
6.1 1.75 8.3 12.1
6.1 14.05 9.2 49.3
6.1 1.75 8.6 73.0
12.1 1.75 8.6 8.7
12.1 14.05 ... 8.7
12.1 1.75 10.7 c 94.5
Volta Grande intact 3.1 1.75 8.8 24.4
specimen 3.1 14.05 8.8 72.9
3.1 1.75 8.5 80.9
6.1 1.75 7.9 10.5
6.1 14.05 9.3 70.8
6.1 1.75 8.0 83.1
12.1 1.75 8.1 11.0
12.1 14.05 10.6 50.6
12.1 1.75 9.5 c 69.4
6.1 1.75 9.0 7.4
6.1 14.05 ~10 88.9
6.1 1.75 9.7 94.5
3.1 1.75 9.7 19.3
* Residual strength for a given normal load, taken at slowest displacement rate at greatest
cumulative a m o u n t of displacement.
b Not cumulative.
c Considered incorrect.
likewise demonstrated that residual shear strength values for repeated

direct shear and annular shear tests on resedimented Cucaracha shale were
similar. On the other hand, in a series of companion repeated direct
shear and annular shear tests on five different over-consolidated fine-
grained soils, Bishop et al [3] observed that only in the case of remolded
Cucaracha shale were residual shear strength values approximately the
same. They reported that residual shear strengths of stiff clays determined
by repeated direct shear tests were 13 to 58 percent higher than values
measured by annular shear tests.
In addition to the fundamental difference between the two tests relative
I , ~|
jb~#:7o* As|
o I~-'~'~ I I I I I
o 2..5 s.o 7.s ~o.o ~z.s 0 2..5 .5.0 7.5 IC*.D 12.5 Z
a. DAWSON S H A L E , CHATF'IELD DAM d. KINCAID S H A L E j C O O P E R DAM 9" PIERRE S H A L E (HIGH P L A S T I C I T Y ' ) m
OAHE DAM Z
0
2 A~ 2 NOTE: TESTS CONDUCTED IN O,75N NclzSO 4 .
Z
1:7
LEGEND
, REPEATED DIRECT SHEAR "~ PRECUT r-

O ANNULAR SHEAR ~ SPECIMENS
| m
9 ROTATIONAL SHEAR (UNDRIED}
9 ROTATIONAL SHEAR (AIR-DRIED)
o I I I I I o .~!" I I I I I 9 ROTATIONAL SHEAR (BLENDERIZE0)
2,5 s.o 7.5 ~o,o Jz.5 2S s.o 7.5 ~0.O Iz.s o
Z
Q: b. TAYLOR I S H A L E , L A N E P O R T DAM e. BEARPAW S H A L E , FT. PECK DAM NOTE N U M B E R S IN S Y M B O L S INDICATE
S E Q U E N C E OF L O A D I N G FOR 0
M U L T I S T A G E LOADING TESTS.
SYMBOLS CORRESPOND WITH .<
T E S T TYPE.
I~ V A L U E S GIVEN A R E VALID W H E N
P L O T T E D TO E Q U A L SCALES,
1 , . a Z
0
r"
0 ~ I
0 2.5 .5.0 7.5 IO.O 12.5 0 2.5 5 0 7.5 IO,O 12.5
EFFECTIVE NORMAL STRESS ~ r KG/CMZ
c. STRAWN S H A L E , PROCTOR DAM f . PIERRE S H A L E (LOW P L A S T I C I T Y ) "1"
O A H E DAM r-
FIG. 1--Residual strength envelopes o f various clay shale specimens with precut failure
planes.
OI
"M
5{} SOIL SPECIMEN PREPARATION FOR LABORATORY TESTING
to direction of displacement along the failure plane, repeated direct shear

tests on soft materials may be impeded by testing difficulties, for example,
excessive extrusion, box tilt, and failure to control the gap between the
top and bottom halves of the shear box, which might lead to a premature
termination of the test. However, these problems do not manifest them-
selves to such a degree in tests of stiff clay shales for specimens with
precut failure planes. These results (summarized in Fig. 2) show that
repeated direct shear test results fall within or near the range of { / v a l u e s
measured by annular shear tests.
MATERIAL RANGE OF r VALUES FOR VARfOUS TEST TYPES AND TECHNIQUES 1

TESTED O 2 4 6 8 IO 12
DAWSON SHALE
TAYLOR I SHALE
STRAWN SHALE
K INCAID SHALE
SEA RPAW SHALE
PIERRE SHALE
(LOW PLASTICITY)
PIERRE SHALE
(HIGH PLASTiCITy) RA•""'NGE
OF VALUES FOR
ANNULAR SHEAR TESTS
i
LE, ,END
O A N N U L A R SHEAR I. EFFECTS OF O'n IGNORED, s CM/DAY
{3 REPEATED DIRECT SHEAR 2. REPEATED A N N U L A R TEST - N O T
A ROTATIONAL SHEAR ONE- DIRECTIONAL SHEARING
FIG. 2--Range in ~r' values measuredby various test techniques and methods.
Effect o f Remolding
Figure 1 indicates that comparable residual shear strengths are mea-
sured by annular shear or repeated direct shear tests on intact specimens
with precut failure planes and by rotational shear tests on specimens
of remolded material. Although remolded material was not tested in
annular shear or repeated direct shear in this study, Bishop et al [3] and
LaGatta [8] demonstrated that nearly identical residual shear strength
values were measured on remolded and intact specimens. These results
suggest that the use of remolded material offers an alternative method of
specimen preparation for determining ~r' values. However, the problems
associated with soft materials tested in repeated direct shear tests men-
tioned in the preceding paragraph may seriously restrict this procedure
unless the overestimation of ~,' by repeated direct shear tests is acceptable.
The results listed in Tables 1 and 2 and presented in Fig. 1 demonstrate
that, although the classification indexes vary dramatically with processing
procedure, the method of processing has little effect on measured
residual shear strengths. Generally, blenderization produces somewhat

lower residual strength values than those measured for undried or air-dried
material. Apparently, blenderization causes a greater disaggregation of
the soil particles than is achieved during shear strains. It may be observed
that greater displacements are required to achieve the residual condition
in tests using less disaggregated (undried and air-dried) materials than in
tests using well-disaggregated (blenderized) materials. It appears, there-
fore, that while the processing method has little effect on measured +r'
values, greater disaggregation reduces the test duration. LaGatta [8]
observed similar results on crushed versus uncrushed Cucaracha shale;
tenfold displacements were required for the uncrushed material to reach
the same ddr' as that obtained for the crushed material.
Although determination of residual strength by testing remolded speci-
mens using the Harvard rotational shear apparatus is attractive, due to
the ease of specimen preparation and short time required for testing, that
is, three to four days versus the three to four weeks required for annular
shear or repeated direct shear, the apparatus has one basic limitation, in
that materials with fine sand or coarse silt sizes cannot be tested. For
example, the Kincaid shale contained approximately 45 percent mont-
morillonite, which normally would facilitate rotational shear testing.
However, hydrometer analyses revealed that the blenderized material
contained only 52 percent minus 2/am size particles, and reliable results
of rotational shear tests were unobtainable due to the grittiness of the
material. The effects of coarse particles are quite evident because very
thin specimens (0.2 cm thick) are tested in the Harvard rotational shear
apparatus. Waterways Experiment Station experience indicates that results
of tests on blenderized material containing less than 55 to 60 percent
minus 2/am sizes may be questionable.
Effect of Precut Failure Plane

The results of annular shear tests on both precut and intact specimens
of a soft, Volta Grande Brazilian clay that could be sheared intact in the
annular shear apparatus are listed in Table 3 and presented in Fig. 3. The
excellent agreement of the results for the intact and precut specimens
indicates that precutting has little effect on residual strength and at least
ensures determination of the lowest possible residual value.
Effect of Density
The annular shear test results for dense and loosely compacted intact
specimens of micaceous silty sand are listed in Table 3 and presented in
Figs. 4 and 5. These results show that ddr' is independent of initial specimen
density. Obviously, the large deformations required to achieve a residual
3.0
LEGEND
SPECIMEN NOTE: NUMBERS BESIDE DATA POINTS
TYPE REFER TO SEQUENCE OF LOADING.
I 0 ~NTACT ~ = 8.7 ~ WHEN PLOTTED
PRECUT TO EQUAL SCALES.
0
z 2.0
m ~
+;
g
zj~ 8,s ~
o I I Z I I
a.s 5.o 7.5 ~o.o ~z.5
NORMAL STRESS ~ 9 KG/CM 2
FIG. 3--Residual strength for annular shear tests on precut and intact specimens of soft,
Volta Grande Brazilian clay.
condition alter any structure imposed by compaction, and the final void
ratio in the failure zone is dependent only upon the effective normal
stress, that is, the critical void ratio.
E f f e c t o f N o r m a l Stress
The residual strength envelopes presented in Figs. 1 and 3 are satis-

factorily represented by straight lines through the origin. Thus, for these
materials, with the testing conditions and range of normal stresses in-
volved, ~r' is independent of normal stress. However, the micaceous silty
sand residual envelopes shown in Figs. 4 and 5 exhibit a slight curvature
at lower normal stresses. This slight curvature at lower normal stresses is
in agreement with the literature [3,8,15]: that up to a stress level of about
2 kg/cm 2 (1.96 • 105 Pa), ~r' decreases as the normal stress increases
(that is, the failure envelope is curved at lower stresses and ~?r' is dependent
upon the normal stress). This decrease in 4 / w i t h increasing normal stress
is possibly due to the higher normal stresses forcing the clay platelets
into a more oriented structure. Under lower normal stresses, a more
random orientation exists.
The degree of dependence of d~r' on normal stress appears to vary with
material; for example, annular shear tests indicate that, for all practical
purposes, blue London clay and Studenterlunden clay exhibit an inde-
pendence of ~ ' with respect to normal stress, whereas brown London
clay and Weald clay exhibit markedly curved residual strength envelopes
[3]. Repeated direct shear test results at the Norwegian Geotechnical
- LEGEND
9 LOOSELY COMPACTED: FROM BAG S A M P L E

-t
9 LOOSELY COMPACTED: FP,OM BLOCK SAMPLE
_ 9 DENSELY COMPACTED: FROM BLOCK SAMPLE
9 UNDISTURBED SAMPLE z
o m
Z
0
i o
to Z
to 0
M
O3 r-
m
tO
I
to 0
.J
D 0
o
(,q
&J
rr
Z
0
o I
o [ 2 3 4 5 6 7 8 9 IO
i
NORMAL STRESS O-'n} KG/CM 2 -r
I-
F I G . 4 - - R e s i d u a l shear strength e n v e l o p e f o r Paraitinga material.
O3
-- O
It
',,(
r
W 6J
J d t~
D_ 0_
UU
O0
d J z
mnn
~"~I O 0
zE~ ~3
"9 W w~ \
uo~: \
O~Z \
I I I I I O
O
Institute [10] also indicated that d?~' for Bearpaw shale varies only slightly
with normal stress, while similar tests on Pepper shale show a marked
dependence of ~ ' on o, '. Kenney [16] suggested that this dependence of
~r' upon the normal stress would be greater for highly montmorillonitic
clays than for soils composed of massive minerals.
Effect of Loading Sequence

The residual shear strength envelopes presented in Figs. 1, 3, 4, and 5
for annular shear tests indicate that sequence of shearing under various
normal stresses has little or no effect and thus that ~r' is independent of
stress history. Although it might appear that ~r' values determined by
subsequent rebounding under lower normal stresses would be prejudiced
by the residual structure preimposed under the higher normal stresses, this
apparently is not the case. Evidently the large displacements required to
achieve a residual state under each normal stress completely destroy any
structure preimposed at a higher normal stress, and the practice of multi-
stage testing is feasible. It was observed in these tests and those by Bishop
et al [3] that, although a residual condition had been achieved for a
particular normal stress, a further displacement of several centimetres was
required to reestablish the residual condition under a subsequent lesser
normal stress. Hence, it is imperative in multistage tests that sufficient
displacements be achieved to reestablish a residual condition, particularly
for rebound conditions.
Conclusions
Within the bounds of this investigation (the testing methods employed
and the procedures and equipment used) and from published information
of similar studies, the following conclusions are drawn.
(a) The difference in residual friction angles, ~r ', measured by re-
peated direct shear tests, annular shear tests, or rotational shear tests
for different hard clay shales, varied from a minimum of 1.0 to a maximum
of 3.3 deg and averaged 2.4 deg for the various materials tested. These
variations include effects of different testing procedures and types of
tests and are considered to be small. However, other investigators have
indicated greater differences between results of repeated direct shear tests
and annular shear tests on soft clays.
(b) The residual friction angle is, for practical purposes, independent
of specimen preparation procedure and density, and comparable residual
shear strengths were obtained on intact, precut, and remolded specimens.
The residual friction angle is also independent of ~nor~al stress; the
residual strength envelope is accurately described by a straight line through
the origin. However, some investigators have indicated that, for normal
stresses less than 2.0 kg/cm 2 (1.96 x l0 s Pa), the residual envelope is
curved; that is, the residual friction angle is dependent upon normal stress.
(c) The sequence of application of normal stresses in a given test has
no significant effect on the residual strength envelope. However, several
centimetres of additional displacement may be required to establish
residual conditions under reduced stresses.
(d) The Harvard rotational shear device offers a rapid, satisfactory,
and low-cost means for determining ~r' for many, but not all, clay shales.
Tests in which the Harvard rotational shear apparatus is used should be
restricted to shales with a minus 2/am content (blenderized) greater than
55 to 60 percent because of the adverse effects of the coarser particles.
A cknowledgments
The tests described and the resulting data presented herein, unless other-
wise noted, were obtained from research conducted under the Civil Works
Investigation Program of the U. S. Army Corps of Engineers by the
Waterways Experiment Station. Permission was granted by the Chief of
Engineers to publish this information.
References
[1] Herrmann, H. G. and Wolfskill, L. A., "Engineering Properties of Nuclear Craters;
Residual Shear Strength of Weak Shales," Technical Report 3-699, Report 5, U. S.
Army Engineer Waterways Experiment Station, Corps of Engineers, Vicksburg, Miss.,
Dee. 1966.
[2] De Beer, E. in Proceedings, Geotechnical Conference, Vol. 1, Oslo, Norway, 1967,
pp. 83-88.
[3] Bishop, A. W. et al, Geotechnique, Vol. 21, No. 4, Dec. 1971, pp. 273-328.
[4] Skempton, A. W., Geotechnique, Vol. 14, No. 2, June 1964, pp. 77-101.
[5] Tiedemann, B., Bautechnik, Vol. 15, Nos. 30 and 33, 1937, pp. 400-403 and 433-435.
[6] Hvorslev, M. J., "Uber die Festigkeitseigenschaften Gestorter Bindiger Boden," In-
geniorvidenskabelige Skrifter A-Nr. 45, Danmarks Naturvidenskabelige Samfund,
Copenhagen, Denmark, 1937 ("Physical Properties of Remolded Cohesive Soils,"
Translation No. 69-5, June 1969, U. S. Army Engineer Waterways Experiment Station,
Corps of Engineers, Vicksburg, Miss.).
[7] Petley, D. J., "The Shear Strength of Soils at Large Strains," Ph.D. dissertation,
University of London, London, England, 1966.
[8] LaGatta, D. P., "Residual Strength of Clays and Clay-Shales by Rotation Shear Tests,"
Contract Report S-70-5, U. S. Army Engineer Waterways Experiment Station, Corps of
Engineers, Vicksburg, Miss., June 1970; prepared by Harvard University under Contract
Nos. DACW39-67-C-0024 and DACW39-69-C-0028 (Harvard Soil Mechanics Series
No. 86, July 1970).
[9] Skempton, A. W. in Proceedings, Sixth International Conference on Soil Mechanics
and Foundation Engineering, Vol. III, Discussion, Session 8, Montreal, 1965, pp.
551-552.
[10] Kenney, T. C., "Direct-Shear Tests on Samples of Pepper and Bearpaw Shales,"
Internal Report F.24-13.01, Norwegian Geotechnical Institute, Oslo, Norway, May 1965.
[11] Townsend, F. C. and Banks, D. C., "Preparation Effects on Clay Shale Classification
Indexes," Preprint 2140, American Society of Civil Engineers National Meeting on

Water Resources Engineering, Los Angeles, Calif., Jan. 1974.
[12] Hdey, W. and MacIver, B. N., "Engineering Properties of Clay Shales; Development
of Classification Indexes for Clay Shales," Technical Report S-71-6, Report 1, U. S.
Army Engineer Waterways Experiment Station, Corps of Engineers, Vicksburg, Miss.,
June 1971.
[13] "Engineering and Design, Laboratory Soils Testing," Engineer Manual EM 1110-2-1906,
Headquarters of the Department of the Army, Corps of Engineers, Washington,
D. C., Nov. 1970.
[14] LaGatta, D. P., "The Effect of Rate of Displacement on Measuring the Residual
Strength of Clays," Contract Report S-71-5, U. S. Army Engineer Waterways Experi-
ment Station, Corps of Engineers, Vicksburg, Miss.; prepared by Harvard University
under Contract No. DACW39-69-C-0028,Aug. 1971.
[15] Chattopadhyay, P. K., "Residual Shear Strength of Some Pure Clay Minerals," Ph.D.
dissertation, 1972, University of Alberta, Edmonton, Canada.
[16] Kenney, T. C. in Proceedings, Geotechnical Conference, Vol. 1, Oslo, Norway, 1967,
pp. 123-129.
A r a A r m a n 1 a n d K . L. M c M a n i s ~
Effects of Storage and Extrusion on

Sample Properties
REFERENCE: Arman, Ara and McManis, K. L., "Effects of Storage and Extrusion
on Sample Properties," Soil Specimen Preparation for Laboratory Testing, ASTM
STP 599, American Society for Testing and Materials, 1976, pp. 66-87.
ABSTRACT: The shear strength of specimens obtained with thin-walled tubes de-
creased as a result of long-term storage. The preconsolidation pressure of stored
tube samples also followed a similar trend. Specimens obtained from hand-cut blocks
did not show a decrease in strength or preconsolidation pressure with time. Samples
stored by wrapping in plastic film and aluminum foil were found to be preserved
as well as those stored after coating with paraffin. Stresses applied to samples for
extruding from thin-wailed tubes were found to be in excess of the shear strength of
the soils. X-ray radiographs of specimens obtained with thin-walled tubes showed
excessive disturbances caused by sampling and extrusion.
KEY WORDS: soils, storage, tubes, shear strength, radiography, penetrometers

(radiation)
I n g e o t e c h n i c a l engineering, the decision m a k i n g a n d design is o f t e n

d e p e n d e n t o n the p r o p e r t i e s o f the f o u n d a t i o n m a t e r i a l available. I n these
cases, it is o f u t m o s t i m p o r t a n c e t h a t the p h y s i c a l p r o p e r t i e s o f t h e soil
m a t e r i a l s be a c c u r a t e l y d e t e r m i n e d regardless o f the s o p h i s t i c a t i o n a n d
accuracy of the analytical methods. The structural integrity and economy
o f t h e final s t r u c t u r e will d e p e n d largely o n the j u d i c i a l choice o f repre-
sentative s a m p l e s a n d specimens a n d o n t h e m e t h o d s o f testing.
S a m p l e d i s t u r b a n c e occurs g e n e r a l l y d u r i n g t w o essential stages o f the
s a m p l i n g o p e r a t i o n : p o s s i b l e m a j o r d i s t u r b a n c e s w h e n t h e s a m p l e s are
r e m o v e d f r o m their p a r e n t d e p o s i t s (not discussed in this p a p e r ) ; a n d
d i s t u r b a n c e due t o e x t r u s i o n , p r o t e c t i o n , storage, t r a n s p o r t a t i o n , a n d
s p e c i m e n p r e p a r a t i o n . This p a p e r p r e s e n t s s o m e t y p i c a l results f r o m a
c o m p r e h e n s i v e s t u d y c o n c e r n i n g the effects o n test specimens due to
s t o r a g e , e x t r u s i o n , m e t h o d s o f selecting r e p r e s e n t a t i v e specimens, a n d
t Professor, Department of Civil Engineering, Louisiana State University, Baton Rouge,
La. 70803, and Dean of Engineering, Delgado College, New Orleans, La. 70119, respectively.
66
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ARMAN AND McMANIS ON STORAGE AND EXTRUSION 67
inherent variations within samples. Six sample sites, representing several

typical geologic formations in Louisiana, provided about 1800 samples
for more than 6500 laboratory and 1700 field tests of stiff pleistocene
clays, soft silty marine clays, and highly organic silts and clays.
Literature Survey
Hvorslev [1],2 in his classical work on subsurface exploration, listed the
requirements for a suitable, undisturbed laboratory specimen: no distur-
bance of the soil structure, no change in water content or void ratio, and
no alteration in constituents or chemical composition. At the same time,
he acknowledged the fact that such criteria are impossible to meet. Most
geotechnical engineers, realizing the limitations of sampling, use test data
with caution. Often, however, uncertainties arising from sample distur-
bance become glossed over by sophistications involving the analysis and
design of foundations.
Various methods and tools for borehole sampling have evolved, and
cores obtained with thin-walled tubes have been accepted universally. In
spite of warnings, such as one by Terzaghi and Peck [2], that, " I f tube
samples have been taken . . . . it is always desirable to investigate the
extent to which the consistency of the clay has been affected . . . . " little
attention is paid to the extent of disturbance in most daily work.
Bozozuk [3] showed that the long-term storage of marine clays reduced
the measured preconsolidation pressure by 4.8 percent. Thus, consolida-
tion tests should be conducted as soon as possible after sampling. Kall-
stenius [4] found a general lowering of the strength of samples with
storage time.
Many investigators have found that tube sampling causes disturbance,
resulting from excessive friction along the wall of the tube. It is logical
to expect, therefore, that similar disturbances also occur during the extru-
sion of samples. Lang [5] measured the forces acting on a stiff clay in an
open-drive, thin-walled tube sampler and, by two different methods,
determined the ratio of peak forces (inside force/outside force) to be
0.48 and 0.28, respectively. The average friction along the tube wall was
64 percent of the shear strength of the soil. The peak axial stress in the
core had a mean value of 13.4 times its uniaxial shear strength. Sone [6]
found the pressure required for extrusion of an alluvial clayey silt to be
several times larger than its unconfined compressive strength, and the
compression during extrusion was almost equivalent to the failure axial
strain measured in the unconfined compression test. Nuclear techniques
to determine changes in the bulk density of soil samples resulting from
sampling and extrusion showed only minor changes resulting from extru-
sion [7].
2The italic numbersin brackets refer to the list of referencesappendedto this paper.
Various techniques have been used to determine visually the extent of

structural disturbances. Terzaghi, Hvorslev, and others sliced and slow-
dried their specimens to enhance the structural features. Even though this
technique is very effective, it not only destroys the sample, but also af-
fords visual examination of only one plane. Radiography has been used
successfully for geotechnical investigations [8] and for studying varved
clays [9].
The selection of typical specimens, as well as specimen size, is still
largely left to personal preference and convenience. Past work indicates
that small specimens trimmed from large samples provide better test
results. One recommendation is that the trimmed surfaces should be as
small as possible in relation to the original size of the specimen [5].
To avoid disturbance caused by remolding of the outer surfaces, large
samples should be obtained and trimmed so that any remolded material
will be removed [10]. The shear strength of Leda clay was shown also to
be affected by the sample diameter [11]. It was shown that sample size
is the most important factor influencing the shear behavior of specimens
[121.
Several investigators have shown that hand-cut (bench-cut) block
samples are less disturbed structurally at almost all stages of the sampling
operation. Block samples are often uneconomical or cannot be physically
obtained to the required depths.
Sampling and Field Testing
Penetration Tests
The ASTM Penetration Test and Split-Barrel Sampling of Soils (ASTM
D 1586-67) were made for visual classification and determination of nat-
ural moisture content to assure that all later tests would be performed
in the same soil deposit.
The ASTM Thin-Walled Tube Sampling of Soils (D 1587-67) was made
with 2.8-in. tubes to obtain cores for several experiments. Except for
certain samples to be used for extrusion tests in the laboratory, the cores
were extruded in the field with a hydraulic ram, classified visually, cut
into 10 in. lengths, and then wrapped or coated. The samples for extru-
sion testing were sent to the laboratory in sealed tubes.
Sample Protection
Because two methods of sealing the extruded cores were to be com-
pared, identical samples were eitheff immersed completely in melted
paraffin or wrapped first in household polyethylene film and aluminum
foil and then sealed in household polyethylene bags. All samples were
transported in specially molded styrofoam boxes (Fig. 1).
FIG. 1--Tubesamples and special container.
B l o c k Samples
Hand-cut block samples (1 ft cubes) were obtained from only two of
the sites because of the difficulty of obtaining such samples from deep
layers. One set of these was obtained from a deposit of stiff pleistocene
clay in southeast Louisiana at depths of 15 to 35 ft. A second set was
obtained from a soft highly-dessicated fat clay (recent Mississippi River
alluvial deposit) at depths of 5 to 15 ft. Standard penetration tests and
tube sampling were performed at the natural ground surface within a
radius of 15 ft of the block sampling sites.
The samples were cut by chain saw and hand tools from active borrow
pits which were excavated immediatley preceding the tube sampling. They
were covered with several layers of aluminum foil and paraffin and placed
in specially fabricated boxes with 1 in. of sawdust insulation all around.
Laboratory Tests and Results

For all the soil tests except radiography and photoelastic analysis, the
following standard procedures were used: ASTM Laboratory Determina-
tion of Moisture Content of Soil (D 2216-66); ASTM Particle-Size Analy-
sis of Soils (D 422-63); ASTM Test for Liquid Limit of Soils (D 423-66);
and ASTM Test for Plastic Limit and Plasticity Index of Soils (D 424-59).
Long-term storage effects required, in addition: ASTM Tests for Uncon-
fined Compressive Strength of Cohesive Soils (D 2166-66); ASTM Test
for Unconsolidated, Undrained Strength of Cohesive Soils in Triaxial
Compression (D 2850-70); and ASTM Test for One-Dimensional Con-
solidation Properties of Soils (D 2435-70). The effects of core extrusion
from thin-walled tubes were studied from the unconfined compressive
strengths, consolidation, and radiographs.
Sample Protection
The coating of undisturbed samples with paraffin has been accepted
universally as one method of preserving sample integrity. However, earlier
laboratory observations indicated that even experienced and careful tech-
nicians had difficulties in removing the hardened paraffin without damage
to the samples, Sweating under the paraffin was noted also. A sample
from a depth of 40 ft has a temperature of about 65~ (18~ When
it is wrapped in foil and dipped in hot paraffin 120~ (49~ consider-
able sweating results, with an increase of moisture content in a zone
adjacent to the outer surface of the sample. The potential sudden effects
of water migration on the pore pressure and moisture distribution, as well
as the homogeneity of the soil, would be highly undesirable. The use of
aluminum foil and plastic film as an alternative protective coating was
studied.
Approximately 100 tube samples (about 18 in. long) of three types of
soil were split immediately after sampling to make three specimens. One
of these, to be used for determining the natural moisture content, was
wrapped in a plastic bag. The others were used to determine the effective-
ness of alternative protective coatings. One slice, after being wrapped in
foil, was placed in a 6-in. round ice cream carton which, in turn, was
filled with melted paraffin (the usual field procedure). The other specimen
was wrapped in aluminum foil and sealed with household plastic film.
The three specimens from one sample were then placed in a clear plastic
bag that was sealed partially with a twist wire tie and sent immediately
to the laboratory in a styrofoam container.
The natural moisture contents were determined immediately upon arrival
at the laboratory. Both the paraffin-coated and the foil/plastic-wrapped
specimens were stored at 100 percent relative humidity and 72~ (22~
After random storage periods of 14 to 33 days, the two specimens of a
set were tested for moisture content.
The results indicated that the foil/plastic wrapping maintained the
moisture content of a specimen just as well as the paraffin coating (Table
1). After these tests, the Louisiana Department of Highways adopted
University of British Columbia Library pursuant to License Agreement. No further reproductions authorize
TABLE 1--Test o f sample protection methods (typical soft and

stiff heavy clays)--14 to 31 days at 72~ and lOOpercent humidity.
Average Moisture Content, ~

Natural Paraffin Coated Foil Plastic Wrapped
29 26 27
27 29 30
39 37 38
35 35 31
39 38 40
51 48 53
53 54 53
57 53 55
22 21 21
22 24 22
24 19 24
64 64 64
67 65 67
19 16 17
21 21 20
17 18 19
20 20 20
13 13 11
12 12 12
the use o f foil/plastic protection instead o f paraffin. Samples are stored

and transported in a specially designed insulated styrofoam container
(Fig. 1).
S i m u l a t e d F i e l d Storage
Earlier observations had shown that sampling crews remain in the field
usually about five days before bringing samples to the laboratory. These
samples are generally extruded in the field, wrapped, placed in the special
s t y r o f o a m boxes (Fig. 1), and stored in covered trucks. The temperature
in the storage part o f these trucks often rose to and remained at I I 0 ~
(43 ~ for about 10 h each day.
To study the effect o f such storage on moisture content, 10-in.-long
samples (2.8 in. diameter) were brought in plastic bags to the laboratory
immediately after extrusion. A Y2-in.-thick specimen was cut f r o m the
middle to determine the natural moisture content. The remaining two end
sections (about 4.5 in. long) were then rewrapped and placed in the styro-
f o a m containers. One set of containers was kept in a forced-draft oven
at l l 0 ~ (43~ the other set at 72~ (22~ and 100 percent relative
humidity. After five days, the specimens were removed and the moisture
contents determined f r o m the entire 4.5 in. length.
Because no appreciable difference in moisture content was found
University of British Columbia Library pursuant to License Agreement. No further reproductions autho
among the three sets, it is evident that the storage methods and the two
protective coatings caused no changes in the moisture content (Table 2).
Thus, any observed differences in the moisture content of samples are
inherent--probably due to silt and calcareous intrusions, etc.
TABLE 2--Simulated field storage o f extruded cores.
Moisture Content, %
5 Days at 72 ~ and
Soil Type Natural 5 Days at 100~ 100 Percent Humidity
Heavy clay 56.0 63 62

Heavy clay 69,0 63 71
Silty clay 19.3 19 14
Light silty clay 29.0 29 3O
Clay 23.0 23
Clay 56.0 63
Clay 69.0 70
Clay 66.0 69
Clay 67.0 72
Clay 64.0 64
Long- Term Storage

The effects of long storage times on the shear strength and consolida-
tion characteristics were determined from three types of samples: 12-in.
hand-cut cubes, 5-in. cores, and 2.8-in. cores. All samples were sent to the
laboratory immediately after protective coatings had been applied. Initial
testing was performed on 2.5-in.-diameter cylindrical specimens trimmed
from identical companion samples to determine the moisture content,
unconfined compressive strength, undrained triaxial shear strength, and
consolidation characteristics without long-term storage effects. The re-
maining samples were stored for different times at 72~ (22~ and 100
percent relative humidity in the field-applied wrappings.
In the case of the unstored samples, the initial (four to seven day) un-
drained triaxiai shear strengths of specimens from the 5-in. cores were
slightly lower than those from the large hand-cut blocks. Specimens from
2.8-in. cores had much lower strengths (Fig. 2). Such effects must be
attributed to disturbances of the outer zones during tube driving and
core extrusion.
At the end of randomly chosen periods, the stored samples were re-
moved from their containers, trimmed to cylindrical specimens (2.5 in.
30
&
Block-trimmed to 2 . 5 m. r & & &

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I i i I | I t i I t I , I , I , tl I I I I
5 I0 50 I00 500 o
LOG TIME (DAYS) Z
FIG. 2--Storage time versus strength. ".,I
diameter), and tested for unconfined compressive strengths, undrained

triaxial shear strength, and consolidation characteristics. Only samples
with similar moisture contents, densities, and classifications were used.
Up through the first ten days of storage, the decrease in shear strengths
for specimens from the three sizes of samples was small--practically
indiscernable. However, the specimen strength of both the 2.8 and 5-in.
cores deteriorated at an increasing rate after the first ten days (Fig. 2).
Any attempt to analyze this strength deterioration versus time numeri-
cally would be of no value and might be misleading, because each type of
soil reacts differently to storage time, as well as other disturbances. How-
ever, it is of the utmost importance to know that extended storage af-
fects the strength and that it should be avoided. The derivation of a uni-
versai correction factor or formula does not appear feasible due to all
the variables involved.
The relaxation of overburden stresses, changes in pore pressure, and
unavoidable migration of water within the sample, as some of the reasons
for changes in the measured soil characteristics, are supported by the
lack of strength reduction in specimens from the block samples (Fig. 2).
The results agree with those of Kallstenius [5].
Extended storage times also bring about a reduction of the preconsoli-
dation pressure by as much as 30 percent (Fig. 3) for specimens from the
tube cores. By contrast, no change occurred in the block samples, except
for some scatter after 100 days. Bozozuk [3] found much less reduction
(only 4.8 percent).
Evidence of disturbance in 2.8-in. cores is shown in Fig. 4. The void
ratio/log pressure curves approach those obtained for the same soils after
they had been remolded and compacted under static loads that approxi-
mated the original overburden pressures.
The average moisture contents during extended storage remained un-
changed. Conceivably, some change in moisture content or dry density
should occur also. However, all determinations of these properties showed
only small variations, due to natural inherent scatter.
Extrusion Effects
Several methods are used to extrude soil cores from sampling tubes.
Pressurized water, as well as hydraulic rams, are used in the field or lab-
oratory. Each method affects the soil properties, depending on the soil
type, its condition, and the type of sampling tube, etc.
Several replicate samples were obtained with a 2.8-in. thin-walled tube
from each type of soil deposit. Some cores were extruded hydraulically
in the field and placed in a protective coating. Others were sealed in the
tubes. All samples were transported without delay to the laboratory.
University of British Columbia Library pursuant to License Agreement. No further reproductions authori
Biock - trimmed to 2.5 in. r

s A
2.5 in. # sample trimmed from 2.81n.

~4
o
v
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LOG TIME (DAYS)
FIG. 3--Storage time versus preconsolidation pressure.
The field-extruded samples were tested for unconfined compressive

strength after being radiographed.
The sealed samples were used to determine the extrusion pressure and
the resulting strains. At first, strain cells attached to the piston of the
hydraulic ram were used to determine the extrusion forces. More con-
sistent results were obtained later with a calibrated pressure gage attached
to the oil cylinder. The displacements at the ends of the cores were
measured with two extensiometers.
After a core had been extruded, a portion of it was trimmed and tested
for unconfined compressive strength. Another section was sliced for
X-ray radiography. Some test specimens were radiographed also before
the unconfined compression test.
1.2
I.I
'.o F
0.9
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g~ Remolded
0.5
0.41 I I I I ~r
I 2 4 8 16 32
LOG PRESSURE (tons/ft 2)
F I G . 4--Storage effect on e versus log p plots.
During core extrusion, the end of the sample in contact with the piston
began to show measurable displacements before the opposite end. Thus,
internal displacements were occurring within the tube. The maximum
strain (the strain at the piston end before steady movement at the opposite
end) varied from 0.001 to 0.005. The average strain was 0.003 (Table 3).
In all cases, the applied stress exceeded the unconfined compressive
strength of the soil to a maximum of 900 percent. This is somewhat less
than the 1340 percent measured by Sone [5].
TABLE 3--Typical extrusion stresses and unconfined compressive strengths

(heavy stiff clay at 35 f t depth).
Max Unconfined Unconfiried

Sample Extrusion Max Composition Composition
Length, Stress, Extrusion Strength," Strength,b
in. psi Strain psi psi
22 69 0.005 17
33 150 0.004 12 "14"'
32 137 0.004 20 18
33 94 0.003 20 19
33 129 0.003 14 ...
33 159 0.003 20 o H
25 78 0.001 6 9
33 198 0.003 28 ...
=Laboratory extruded.
bField extruded.
Radiography
Radiographs showed two distinct distorting effects caused by sampling

and extrusion processes. The first type of distortion, observed in all cores,
was a gradual bending of the soil layers, with a m a x i m u m at the tube
surface and decreasing toward the center. The bending was a symmetrical
dome-like effect around the longitudinal axis. This effect was more pro-
nounced in the soft marine deposits (Fig. 5) tested than it was in the stiff
pleistocene clays (Fig. 6).
A comparison o f the layers in the hand-cut samples (Fig. 7) and the
tube samples (Figs. 5 and 6) demonstrates the effects of tube driving and
extrusion. Note that reference grids were superimposed photographically
on the X-ray films to aid in visual analysis.
A second, more serious type of disturbance shown by the radiographs
was a definite failure plane pattern in some of the untested stiff clays
(Fig. 8). These failure planes, either at a 50 deg angle or with a classical
cone shape, occurred at intervals along the longitudinal axis of some
specimens.
To determine if the failure planes had occurred during either sampling
or extrusion, radiographs o f specimens in tubes were made also. H o w -
ever, because o f parallax effects caused by the roundness o f the sample
and shadowing of the high-intensity X-rays necessary to penetrate the
steel tubes, the tests were inconclusive. Thus, it could not be determined
clearly when these failures occurred. However, edge turning could be
observed in the radiographs of unextruded c o r e s - - a n indication that at
least some o f the edge distortion took place during tube driving. H o w -
ever, it is more likely that most of the failure planes appeared during
extrusion because the sample was in compression.
FIG. 5--Edge turning in marine clays.
ARMAN AND MCMANIS ON STORAGE AND EXTRUSION 79
FIG. 6--Edge turning in stiff clays.
Photoelastic Analysis
To obtain a qualitative analysis of the stress patterns developed during
sampling, a photoelastic analysis was performed with a thin-walled tube
that had two opposite 90 deg arcs of the wall removed.
A gelatin/water mixture was poured into a 4 by 5-ft by 3-in. glass-
walled tank with cross polorizing filters on the walls. After the gelatin
had set, the tube sampler was driven in slowly by hand. The developed
stress patterns (resulting from bi-refringence of gelation) were recorded
on color movie film and color still photographs (Fig. 9). These patterns,
FIG. 7--Lack of distortion in block speciman (stiff clay).
covering the full volume of the driven tube, were very similar to the bent
layers in soft soils that had been observed in the radiographs (Fig. 6).
However, no failure planes developed.
Although this experiment showed that distortion occurs during sampler
driving, it did not disprove the earlier stated contention; friction, due to
adhesion of the soil to the tube wall, increases the distortion during extru-
sion.
Selection of Representative Specimens
Importance f o r Design
The selection of a specimen to represent a specific soil deposit is critical
to soil data acquisition. Once the choice has been made, the designer
FIG. 8--Failure plane in 5-in.-diameter specimen.
receives only the data obtained from that particular point in the ground,
or for the whole deposit, from a few selected samples. In special cases,
when all the samples are used for testing, any errors that may result from
specimen choice can be eliminated.
In order to observe and analyze the specimen selection process, the
authors made long-term observations in several soil laboratories, as well
as testing samples obtained from various sources. A review of the soil
profiles at several agencies indicated that the soil characteristics were
plotted as neatly divided 3-ft layers. If one considers that thin-walled tube
samples are 3 ft long, such plots indicate arbitrary specimen selection in
the laboratory. However, soils do not always become deposited as homo-
geneous 3-ft layers. Without the benefit of the observations of a well-
qualified soil exploration technician or engineer, a high risk factor may
be introduced into geotechnical engineering.
FIG. 9--Photoelastic simulation of tube sampling.
Variations in 36-In.-Long Cores

Figure 10 shows the erratic physical variations along a typical 36-in.-
long tube sample obtained from a soil that is considered locally to be
uniform. (It should be noted that the core was classified as a silty clay
for its full length.) All the specimens showed similar variations in the
Atterberg limits. With the unconfined compressive strength varying from
1100 to 2700 psi, the arbitrary selection of a representative single speci-
men from this sample could result in either underdesign or overdesign.
It should be emphasized that some of these variations are probably
due to sampling and extrusion disturbance. However, slickensides not
visible to the naked eye, very thin sand and silt layers, calcareous nodules,
and marine shells were observed in radiographs of parts of these speci-
mens (Fig. 11).
P o c k e t Penetrometers
The use of pocket penetrometers to assist the laboratory technicians
Top of somple
0 rm l i | i i
9
k-
Z
~m
~ 24
3O
36
I I I I I I I
50 I00 150 30 40 50 0 I000 2000 3000 4000
DRY U N I T W E I G H T MOISTURE CONTENT UNCONFINED STRENGTH

( I b / f t 3) (%) ( I b l f t 2)
FIG. lO--Variations in sample properties,
or engineer in specimen selection has been studied also. (This instrument

is presently in use by some agencies for this purpose.)
One hundred and fifty strength tests, obtained from one site by uncon-
fined compression, undrained triaxial compression, and pocket penetro-
meter tests (Fig. 12), show wide scatter, with the plots distributed un-
equally above a 45 deg line (representing one-to-one agreement).
Because of inherent scatter in both the triaxial and unconfined com-
pressive strengths of soils, all the scatter in Fig. 12 should not be attri-
buted to the pocket penetrometer.
Statistical analysis shows the error distribution of pocket penetrometer
readings to be a band, in which they were at least one half the laboratory
strengths 97 percent of the time and not more than one and one-fourth
the laboratory strengths 94 percent of the time (Fig. 13). On the average,
the errors vary from 90 to 120 percent. Based on this evaluation, the
pocket penetrometer has been considered satisfactory for selection, but
not for testing. It may reduce the probability of gross errors, but it will
not solve completely the problem of selecting typical specimens.
Field N o t e s
Many errors in the selection of a representative specimen can be elim-

inated by a thorough study of the field notes taken by a well-qualified,
observant exploration engineer or technician. The penetration test record,
comments on the terrain, as well as careful notes (for example, of sample
separation after extrusion because of slickensides or very thin silt or sand
FIG. 11--Embedded shells and silt planes in 2,8-in. tube sample.
FIG. 12--Pocket penetrometer versus laboratory strength.
lenses, or obnoxious odors) serve as a warning to the laboratory tech-

nicians and the engineer who makes the final selection of the most repre-
sentative specimens.
General Conclusions
Undisturbed tube samples do not have to be coated with paraffin for
protection. A wrapping of household polyethelyene film covered by
aluminum foil, followed by sealing in common household polyethelyene
FIG. 13--Error distribution in strength.
bags, is satisfactory protection, provided that they are stored also in

containers insulating them against impact and direct exposure to the
elements.
Long-term storage of soil cores results in serious deterioration of the
shear strength and lowering of the measured preconsolidation pressure.
Tube samples should be tested within 15 days after sampling to prevent
erroneous results, due to the deteriorating effects of long-term storage.
The extrusion of soil cores from thin-walled tubes required friction
stresses and axial compression greatly in excess of the unconfined shear
strength. Soil reorientation, as well as internal failures, may occur during
tube driving and core extrusion. Immediate attention should be given to
the development of a thin, low-friction lining for sampling tubes.
Radiography is useful for determining the extent of the disturbances,
as well as the presence of anomalies, in soil cores. It should be made
part of the soil testing program in critical foundation projects.
The pocket penetrometer is a useful, inexpensive, and a simple tool for
identifying and selecting representative soil specimens.
Soils should be tested within two weeks after sampling to prevent test
errors due to the deteriorating effects of long-term storage. If practical,
large (at least 5-in.) diameter tube samples should be obtained. They
could then be trimmed to small specimens, in which the trimmed-down

distorted outer portions have been eliminated. However, for critical
designs involving soft soils, in situ tests must be made in addition to
laboratory tests and should be given prominence when the acquisition of
large tube or block samples is impractical or uneconomical.
Acknowledgment
This study was conducted as part of a research project financed by
the Louisiana Department of Highways and the U.S. Department of
Transportation, Federal Highway Administration.
The authors express their gratitude to the Louisiana Department of
Highways for the personnel and equipment they provided. Thanks are
due to Charles Hill, engineering editor, and Norma Duffy, draftswoman,
for their invaluable assistance. The dedicated work of many student work-
ers who spent their time collecting data is gratefully acknowledged.
References
[1] Hvorslev, M. J., Subsurface Exploration and Sampling of Soils for Civil Engineering
Purposes, reprint, Engineering Foundation, 1965.
[2] Terzaghi, K. and Peck, R. B., Soil Mechanics in Engineering Practice, 2nd Edition,
Wiley, New York, 1968.
[3] Bozozuk, M. in Samplings of Soil and Rock, ASTM STP 483, American Society for
Testing and Materials, 1970, pp. 121-131.
[4] Kallstenius, T. in Proceedings, Specialty Session on Quality in Soil Sampling, Fourth
Asian Conference, International Society for Soil Mechanics and Foundation Engineer-
ing, Bangkok, July 1971.
[5] Lang, J. G. in Proceedings, Fourth Asian Conference, International Society for Soil
Mechanics and Foundation Engineering, Bangkok, July 1971.
[6] Sone, S. in Proceedings, Fourth Asian Conference, International Society for Soil
[7] Shackel, B. in Proceedings, Fourth Asian Conference, International Society for Soil
[8] Krinitzsky, E. L., Radiography in the Earth Sciences and Soil Mechanics, Plenum
Press, New York-London, 1970.
[9] Kenny, T. C. and Chan, H. T., Canadian Geotechnical Journal, Vol. 9, 1972, p. 195.
[10] Holtz, W. G. in Laboratory Shear Testing of Soils, ASTM STP 361, American Society
for Testing and Materials, 1963, p. 417.
[11] Coats, D. F. and McRostie, G. C. in Laboratory Shear Testing of Soils, ASTM STP
361, American Society for Testing and Materials, 1963, p. 459.
[12] Lo, K. Y., Seychuk, J. L., and Adams, J. I. in Sampling of Soil and Rock, ASTM
STP 483, American Society for Testing and Materials, June 1970, pp. 60-71.
T. H. IV. Baker'
Transportation, Preparation,
and Storage of Frozen Soil Samples
for Laboratory Testing
REFERENCE: Baker, T. H. W., "Transportation, Preparation, and Storage

of Frozen Soil Samples for Laboratory Testing," Soil Specimen Preparation
for Laboratory Testing, ASTM STP 599, American Society for Testing and Materials,
1976, pp. 88-112.
ABSTRACT: Increased construction activities in cold regions require a better

understanding of the behavior of frozen soil. Although in situ testing pro-
cedures are being improved or developed, the highly variable and complicated
conditions usually encountered in the field make it difficult to formulate inter-
pretations that are useful in practice. Controlled laboratory tests on frozen
soils are helpful, therefore, in determining behavior indicative of diverse field
conditions and will assist in establishing design information. This paper is a
review of the procedures used and the difficulties encountered in the transporta-
tion, preparation, and storage of naturally and artificially frozen soil samples
required for testing in the laboratory. The effective control of sample dis-
turbance by temperature variation and sublimation and the need for further in-
vestigation as to their effect on the mechanical properties of frozen soil are discussed.
KEY WORDS: soils, frozen soils, transportation, preparation, preserving, sub-

limation, thermal degradation, mechanical properties, laboratory tests
Procedures for transporting, preparing, and storing the naturally

and artificially frozen soil samples that are required for laboratory
testing are still in the formative stages. This paper reviews the cur-
rent practices used for naturally frozen field samples from the time
of sampling, and for artificially prepared laboratory samples from
the start of the molding operation. A review of the literature is
included, as well as the experiences of industry, university groups,
and government departments and agencies.
'Research officer, Division of Building Research, National Research Council of

Canada, Ottawa, Ont., Canada.
88
Downloaded/printed9 by
Copyright 1976byASTMInternational www.astm.org
BAKER ON FROZEN SOIL SAMPLES 89
Factors Affecting Laboratory Tests on Frozen Soils

Laboratory tests are performed on naturally and artificially pre-
pared frozen soil samples to investigate (a) strength and creep de-
formation behavior and (b) volume change.
Tests conducted under (a) include: stress and strain controlled un-
confined compression tests, stress and strain controlled triaxial shear
tests, ring shear tests, Brazilian tests, tension tests, load-controlled
indentation tests, flexural strength tests, dynamic loading tests, and
torsion tests.
Tests conducted under (b) include: uniaxial consolidation upon
thawing under constant stress, triaxial consolidation upon thawing
under constant stress, and uniaxial heave during freezing.
The strength and deformation properties of frozen soil samples
are known to be affected by sublimation, evaporation, and thermal
disturbance. Their effect is in the redistribution and ultimate loss of
moisture from the specimen as the result of a temperature gradient or
low humidity environment or both. Loss of moisture reduces the
cohesion between soil particles and may reduce the strength (which
is dependent on temperature). The effects of moisture redistribution
in frozen soil are not known, but are thought to change the strength
and creep behavior.
Thermal disturbance of a frozen sample refers not only to thawing,
but also to temperature fluctuations. Soil structure may be changed
completely if the sample is thawed and then refrozen. Temperature
fluctuations can set up thermal gradients, causing moisture redis-
tribution and possible change in the unfrozen moisture content. Care
must be taken, therefore, to ensure that frozen soil specimens remain
in their natural or prepared states and that they are protected
against the detrimental effects of sublimation and thermal disturbance
until testing is completed. The type of laboratory test to be con-
ducted will determine the degree of care required in providing this
protection.
Frozen Soil Samples
Naturally Frozen
Undisturbed block and core samples of frozen soil must be pro-
tected from thawing and loss of moisture, from the time they are
taken from the ground, throughout the period of transportation,
storage, machining, and testing. In most cases, the sample must be
maintained under the same thermal and moisture conditions existing
at the time of sampling. The implications and practicality of this
will be discussed later.
Methods of handling frozen soil samples in the field have not changed
greatly in recent years. When the samples have been examined visually
and logged at the field site, most investigators wrap the frozen samples in
cellophane and place them in polyethylene bags (6 mil) (Fig. 1). All air
FIG. 1--Large block sample of frozen soil delivered from the fieM in a polyethylene bag
(scale in tenths of afoot).
must be evacuated from the bag, and it must be sealed to prevent sub-
limation. This is accomplished best by using a vacuum pump, but can be
done by forcing most of the air out by hand before sealing. Humidity can
be maintained by placing some snow or crushed ice in the bag. Heat
sealing the plastic bag after de-airing gives the most permanent seal, but a
locking nylon tie (of the type used for bundling electric cables) is adequate
if it is fastened properly. The seal should be checked regularly; any air
that has entered the bag should be removed, and the bag should be re-
sealed. This packaging procedure keeps moisture loss from the sample
within acceptable limits and has been used successfully by the author to
store frozen samples for periods of eight months or more. To minimize

still further the moisture loss due to transfer of vapor through the plastic,
Roggensack [1] 2 suggested that the wrapped samples should be packed in
snow or ice chips. This will reduce vapor pressure gradients. Even with
these precautions, some water loss occurs as vapor leaves the sample and
crystallizes on the inside of the plastic wrapper. This will be discussed in
the section on sublimation.
After the sample has been packaged to keep sublimation to a minimum,
some facility is required at the site to prevent thermal disturbance. For
example, if unfrozen samples have been obtained for frost heaving experi-
ments, they must not be allowed to freeze so that they can be tested in
truly undisturbed conditions. If ambient temperatures are below 0~
these samples should be placed in well-insulated boxes and kept in heated
tents or some other warm enclosure until they are shipped. On the other
hand, when frozen soil samples are obtained for thaw consolidation,
strength, and creep tests, the in situ temperature must be maintained. As
ground temperatures vary with depth during the year, the temperature
should be determined at the time of sampling. In addition, depending on
the tests to be conducted, it may be necessary to determine the annual
amplitude of the temperature fluctuations at the sample depth.
Maintaining the in situ temperature of the frozen samples has been
attempted, using several methods. Portable refrigerators powered by
110-V generators have been used successfully at field sites to store frozen
soil samples. These can control adequately the thermal environment and
can be set to maintain the temperature measured at the field site when
the sample was obtained. Insulated boxes packed with ice, dry ice, or
freezer "jelly" packs have been used also to prevent thawing of frozen
samples in the field. This is considerably less expensive than the use of
portable refrigerators, but, of course, temperature cannot be controlled
accurately. A typical insulated box used for field storage and shipping
by the University of Alberta [1] is shown in Fig. 2. When using solid
slabs of dry ice, thin sheets (25 mm) of insulation must be placed between
the dry ice and the soil samples to minimize "burning" effects caused by
contact with carbon dioxide. The dry ice is placed between the insulation
and the top, bottom, and sides of the box. If freezer packs are used, they
can be arranged in the same manner. A double-walled insulated box has
been used, where dry ice is placed in the space between the two walls. The
temperatures of samples, packed in this manner, are not constant; they
will undergo a fairly rapid drop in temperature, the rate depending on
how well protected they are by insulation. The dry ice evaporates slowly,
and the temperature of the box (and consequently of the samples) will
~The italic numbers in brackets refer to the list of references appended to this
paper.
STRONG LATCH SASH CHAIN TO

WITH PROVISION ~ PREVENT LID PROM
LOCKING ~'~ ~ FALLING BACK
FOR ~ , 1 1 ' ~ , [ i i ~ MINIMUM OF
THREE HINGES
[ ALONG BACK
3" (760ram) HIGH-
OENSITY URETHANE
RTV CAULKING i i i q iNSULATION INSIDE
IN INBULATIO N ~" (12ram) GOOD
JOINTS QUALITY PLYWOOD
LARGE D-HANDLES
BOLTED TO BOX
i:
METAL BANDING
FOR REINFORCEMENT
2"x4" (S0mm BY 100ram)

BOLTED TO BOX BOTTOM
SO IT CAN BE
AS A PALLET (ALSO
KEEPS BOX BOTTOM
AWAY FROM MOISTURE)
FIG. 2--Typical insulated box used for field storage and shipping.
increase. When ice or freezer packs are used, there is no drastic cooling
of the samples, but, in time, the temperature of the insulated box and
samples will increase unless the ice is rel~laced periodically.
If the boxes are to be stored for any length of time (for example, a few
weeks), it is advisable to pack snow or crushed ice around the sample
bags to prevent sublimation and to fill any air spaces with crushed news-
paper to provide added insulation and reduce movement of air in the box.
The cover of the box should be fastened securely and made airtight by
applying a thin bead of room temperature vulcanizing silicone rubber
(RTV) caulking compound around the edge of the lid before the box is
closed.
Although not entirely satisfactory, tempory measures to protect
samples in the field can be used in some instances. During the winter,
frozen soil samples, packaged in polyethylene bags, can be buried in snow
drifts, or, if the ambient air temperature is below 0~ they can be left in
the open air but must be protected (shaded) from the sunlight. During the
summer, frozen samples have been stored successfully for up to three
days in shallow pits dug in the frozen ground or put into plastic sleeves
and stored in the boreholes from which they were taken. The pit should
be lined and covered with some insulating material. Moss serves quite
well for this purpose. The top of boreholes, used to store samples, should
be covered or plugged with insulation to prevent thawing and closing of
the hole.
If adequate storage facilities are not available at the field site and the
samples are to remain frozen, they must be transported immediately to a
temperature- and humidity-controlled storage area. The frozen soil sam-

pies must be shipped in refrigerated containers or insulated boxes. Power
requirements for shipping a typical refrigerated unit by aircraft are out-
lined in Fig. 3 [2]. A competent person should accompany frozen samples
FIELD SITE
GAS DRIVEN GENERATOR I

IlOV l SINGLE PHASE
PORTABLE REFRIGERATED UNIT I
O.3m3 (10 fl 3)
10V l SINGLE PHASE
AIRCRAFT
DYNAMOTOR I
28V l DC
I RECTIFIER I
I0V l 3 PHASE
l AIRCRAFT POWER I
FIG. 3 --Power for refrigerated units.
transported by commercial airlines from the field to the laboratory.

(Refrigerated units not attended could be left unplugged on the parking
apron or in a storage area, and thawing or undesirable temperature changes
of the samples might occur.) Arrangements can be made to have the
insulated boxes placed in airport freezers between flights. Cold storage
areas are not always available, but restaurants and cafeterias at airports
are usually most helpful in allowing their facilities to be used for this
purpose if the containers are not too large or too many; arrangements
for storage en route should be made prior to shipment. The author has
found that insulated boxes packed properly can be left without auxiliary
freezing up to 8 or 9 h without apparent deterioration of the samples. The
samples can be left in the insulated containers and placed in cold storage
upon arrival at the laboratory until required for testing.
Preparing and transporting naturally frozen undisturbed soil samples
for laboratory testing is a very difficult and costly operation. In most
cases, and for most purposes, insulated boxes have been used successfully
to transport frozen samples to the laboratory, provided care has been
taken in packaging, storing, and handling the containers.
Artificially Frozen
The physical properties that affect the mechanical behavior of soil, for
example, homogeneity, grain size, moisture content, compaction, and, to
some extent, ice lens structure, should be closely controlled. This can be
achieved in the laboratory by using special molds and controlled methods
of freezing.
The steps followed in the preparation of laboratory frozen soil speci-
mens are:
1. Assembly of the mold.
2. Compaction of the soil sample.
3. Saturation of the sample.
4. Freezing.
5. Disassembly of the mold and removal of the sample.
The geometry of the mold is determined by the desired shape of the
test specimen. Rectangular, cylindrical, and dumbbell specimen shapes
commonly are used, depending on the test to be performed. As unidirec-
tional freezing of the sample is usually desirable, the mold is fabricated
from or covered with materials having good insulating properties. Use of
split molds with all joints ,fastened by easily removed connectors greatly
facilitates specimen removal after freezing. All interfacing surfaces of the
mold and all threads on metal connectors should be coated with a lubri-
cant to ensure a tight fit for evacuating the air from the samples and to
aid in extracting the sample from the mold in the cold room. Care must
be taken to prevent the lubricant (especially the silicone types) from
coming in contact with the sample.
Air-dried soil usually is placed into a mold in 30-mm-thick layers and
compacted by a drop hammer or vibration action, following standard soil
mechanics procedures (for example, Modified Proctor, American Association
of State Highway Officials' Standard). Each layer should be scarified to a
depth of approximately 5 mm before the next layer is placed. If the soil
has a wide range of grain sizes, vibration may cause the particles to separate
into layers of uniform size. For sands, the vibratory technique is the
better compaction method.
The following method of evacuation and saturation has been found by
Haynes [3] to give a fully saturated compact sample.
After the sample has been compacted, caps can be placed on each end
of the mold. Both end caps should be fitted with hose connections, which
include porous stones, to prevent the loss of soil during the air evacuation
and water saturation phase. Plastic tubes are connected to both of the end
caps. The tube from the top cap is connected to a vacuum pump; the tube
from the bottom cap leads to an o n / o f f valve and then to a reservoir of
distilled water. A vacuum pump is also connected to the water reservoir.
The on/off valve allows for separate deaeration of the mold and the
reservoir. A photograph of the apparatus is shown in Fig. 4.
A vacuum is applied to the top of the mold with the o n / o f f valve
closed. At the same time the distilled water reservoir is placed under a
FIG. 4--Apparatus for molding and saturating artifical samples.
vacuum to remove as much air as possible. After about 2 h, the vacuum

pressure in the reservoir is decreased, and the valve is opened. A differen-
tia/ pressure between the mold vacuum and the water tank vacuum is
maintained so that the water travels up through the sample and saturates
it at a slow steady rate. Fast saturation must be avoided to prevent: (a)
piping o f water through channels along the outside o f the sample; (b) a
" q u i c k " condition disturbing the dense packing obtained in compaction;
or (c) incomplete evacuation of air. When the samples appear to be sat-
urated (that is, water can be seen in the top tube), the vacuum pumps are
turned off, and the sample is allowed to saturate under a 0.5-m head of
water for about 1 h.
Goughnour and Andersland [4] and H o o k e et al [5] prepared sand-ice
specimens by mixing natural snow uniformly with a selected proportion o f
precooled sand. This mixture was compacted in the mold, and water, pre-
cooled to 1 ~ was admitted under pressure. Little snow melted during
this process, and the sand particles remained dispersed during freezing.
Using this procedure, frozen sand specimens were obtained with large ice
contents.
Vyalov [6] reported that frozen soil without ice segregation can be ob-
tained by freezing samples rapidly at temperature below - 3 0 ~ To obtain
specimens having a layered or reticulate structure (that is, horizontal or

randomly oriented in layers, respectively), the soil samples should be fro-
zen at temperatures of about - 6 ~ or above. A layered, ice-lensed struc-
ture is obtained by cooling one end of the sample and providing free
access to a constant supply of water at the other end.
Tsytovich and Sumgin [7] investigated the influence of the freezing
method on the unconfined compressive strength. The results indicated
that a freezing temperature between - 1 2 and - 1 7 ~ gave a relatively
lower strength if the freezing time was less than three days for sand and
four days for clay. They also found that the strength properties were not
affected significantly if the freezing occurred from all sides or only from
the top down.
To achieve a uniform moisture content throughout a sample of Fair-
banks silt, Haynes [3] froze specimens unidirectionally in a cold chamber
at a temperature of - 37 ~ The bottom mold connection was attached to
a water supply; the top of the mold was exposed to freezing temperatures.
Loose insulation (granulated cork) was placed under and around the mold
to reduce radial heat loss and to allow the sample to freeze from the top
down. Vermiculite can be used for this purpose instead of granulated cork
(Fig. 5). A constant supply of water was maintained at the bottom of the
mold to replenish the water that migrated upward from the unfrozen zone
FIG. 5--Vermiculite placed around the mold to allow the sample to freeze unidirectionally.
to the freezing front. Thermistors, placed at locations along the center

line of the specimen, recorded the freezing rate.
Cold rooms, refrigerated cabinets, and constant temperature baths have
been used by many investigators to control the freezing rate of remolded
soils. Many cooling systems have slow response times, so that rapid ad-
justment of the rate of heat extraction from the sample is usually very
difficult.
More accurate control of the freezing process can be obtained, using a
thermoelectric cooling plate which operates on the Peltier effect [8]. The
design of a cooling plate (Peltier module) is described in detail elsewhere
[9,10]. The temperature of the plate can be maintained with an accuracy
of at least _+0.02~ As heat removal from the sample is uniaxial, this
method is well suited for unidirectional freezing of a soil specimen. Sam-
pies of various sizes, with variations in moisture content of + 1.5 percent
by dry weight, have benn frozen succesfully under many different test
conditions, using a thermoelectric plate at the Division of Building Re-
search (DBR), National Research Council of Canada (NRC) [9].
Rapid sample freezing minimizes redistribution of soil moisture. Freez-
ing too rapidly, however, can cause entrapment of air bubbles in the
specimen and tensile failures due to thermal shock. Typical freezing rates
used by Sayles and Haines [11,12] on small specimens (69 mm diameter
by 140 mm high) were:
Ottawa sand (20 to 30
mesh) 38 mm/day
Manchester fine sand 40 mm/day
Hanover silt 80 mm/day
Suffield clay 170 mm/day
Methods of freezing large remolded soil specimens have been reported by
Warder and Andersland [13] (125 mm diameter by 300 mm high) and
Laba [14] (100 mm diameter by 241 mm high), but no reference was made
to their homogeneity. It is not known whether it is possible to produce
large uniform samples using existing freezing techniques. Samples frozen
in the laboratory are molded normally in the test apparatus and frozen
just prior to testing, thus eliminating the difficulties associated with the
storage of frozen specimens.
Machining and Preparation of Specimens for Testing

The machining and preparation procedures used for frozen soils depend
upon the size and shape of the specimen required, the type of soil, and
the particular test being performed. Similar procedures are followed for
cutting and machining both naturally frozen and artificially frozen sam-
ples.
Frozen soil samples should be handled with gloves and all tools and
equipment kept in the cold room to avoid sample damage by localized
thawing. A temperature of - 5 _+1 ~ is the most suitable ambient tem-
perature for machining with respect to material workability and personal
comfort. At warmer temperatures, surface thawing is a problem, and
cutting tools must be cleaned frequently, for they become coated and
clogged with frozen soil, reducing their cutting efficiency. Working at
colder temperatures is uncomfortable and slow. The soil is also difficult
to work with because of increased hardness; cracks can be formed easily
in it, due to increased brittleness.
Any cracking induced in the specimen during preparation will reduce
the load-carrying capability and influence the test results. Thermal dis-
turbance, due to frictional melting by a cutting tool, may be insignificant
when preparing specimens for thaw consolidation tests, but it may be very
significant for strength tests. Extreme care must be taken when machining
frozen soil samples for testing to keep disturbance to an absolute mini-
mum.
Various cutting and grinding techniques have been used to machine
specimens to the shape required for the test to be performed.
Rough Cutting Methods

A number of methods for cutting frozen soil, including using a hand,
band, or chain saw, forcing a cutting edge into the frozen soil, and using
a hot wire have been investigated at NRC. Others have found rotary dia-
mond saws satisfactory. The advantages and disadvantages of these meth-
ods are summarized in Table 1.
Finishing Methods
After being cut roughly to the required dimension, rectangular speci-
mens are finished usually by one, or a combination, of the following
methods, listed in increasing order of precision:
1. Hand shaving with a sharp, straight cutting edge (for example, a
draw knife).
2. A coarse wood rasp or file.
3. Grinding with several grades of emery paper or grinding stone.
4. Milling machine equipped with heavy-duty cutters.
5. Drill press (heavy-duty) equipped with an end milling tool.
These methods have been used on a wide range of frozen soils, and the
particular application of each is dependent upon the required specimen
tolerances. The allowable specimen tolerance is dependent on the type of
test to be preformed and is discussed next.
Cylindrical specimens are machined either on a metal working lathe or

cut carefully with a coring tube in the laboratory.
A lathe is being used extensively at the Division of Building Research to
obtain well finished cylindrical specimens of most types of frozen soils up
to 150 mm in diameter. Soils containing pebbles are extremely difficult to
machine on a lathe. If pebbles are not plucked out by the lathe, the speci-
men becomes jammed on the cutting tool and breaks between the tool
post and the chuck. The various steps in the preparation of specimens on
a lathe are outlined pictorially in Figs. 8-10.
Samples are cut initially to eight-sided cylinders on the bandsaw. A
V-block is used to hold the specimen so that the ends can be squared on
the handsaw. The dimensions of the eight-sided cylinder are chosen so
that the specimen can be turned to a right cylinder with both ends faced.
A finished specimen 75 mm in diameter by 150 mm long is turned from
an eight-sided cylinder 85 mm across the end and 200 mm long.
The eight-sided cylinder is placed on the lathe, with one end supported
in a four-jaw chuck and the other end supported by the tallstock. The
tailstock is separated from the specimen by the round wooden block which
has sandpaper glued to one side and a cone seat (for the tailstock) on the
other. Pressure applied to the specimen by the tailstock is distributed
evenly over the face of the specimen by the wooden block.
Best results are obtained when the frozen soil specimen is turned at 690
rpm and the carriage feed set at 30 mm/36 revolutions. The maximum
depth of cut should be limited to 0.38 mm. A tungsten carbide cutting
tool, with a minimunrback clearance of 45 deg, gives the best results. For
clean cuts, the tool has to be sharpened often, as the abrasive action of
the soil dulls the edge quickly.
A tool post grinder can be used for dressing coarse-grained soils.
Grinding efficiency for fine-gra/ned soils is reduced by buildup of material
on the grindstone. A special holder that screws onto the spindle of the
lathe and allows the ends of the specimen to be squared and faced with
the cutting tool is shown in Fig. 10.
Cylindrical samples can be cored from block samples in the laboratory,
using a diamond set core barrel and a large industrial drill press. The
block is held to the drill press flame by clamps. This procedure has been
used in Alaska to produce sand and gravel specimens with less than 0.5
percent variation in diameter and for silt and clay samples with less than
0.4 percent variation [15]. The drill press was fitted with a gas swivel
through which pressurized liquid nitrogen vapor was passed to blow the
cuttings away. The configuration of the diamond matrix and vents on the
core bit was varied in order to core each type of soil most effectively. To
obtain specimens of consistent diameter, the internal diameter of the core
bit must be checked often and the diamond matrix replaced if the allow-
able tolerances are exceeded.
TABLE 1--Rough cutting methods. Q
Method Advantages Disadvantages

_o
Sharp edge poor, as the ice in front of the cutting 1.-
Axe (for example) edge chipped, leaving voids in the O)
sample "0
m
o_
Hot wire (piano) wire passed quickly through 10-cm speci- a cheese cutter frame was rigged with a
23 kg weights men of frozen clay hot wire, but not enough pressure could m
2to4V be applied by hand to obtain efficient z
cutting; it is suggested that this method ~D
not be used to cut laboratory specimens m
of frozen soil due to its thawing action "0
~D
Hand saws a swede saw was used for rough cutting inadequate due to slow progress and poor -4
Miter saw large blocks of frozen clay (Fig. 6); use geometric control; for effective cutting
Hack saw of a miter box improves geometric the blade had to be continually cleaned Z
Swede saw control to remove partially thawed clay and to "TI
prevent binding 0
Chain s a w excellent for rough cutting large blocks of ineffective in cutting frozen clay with the
Electric powered 254 frozen peat and silt which have high teeth and chain becoming clogged with 0
"11
mm arm ice contents clay and the blade binding in the cut
---I
Gas powered 381 mm 0
arm
Band saw very satisfactory for cutting fine-grain largest sample that could be cut was 159 .--t
m
1/2 hp, 1725 rpm specimens; quite adequate for coarse mm thick, but with height attachment --4
sands (Fig. 7) up to 311 mm
5 mm blade, 2 teeth/cm fast cut blade wanders when cutting specimens 60 if)
to 200 mm thick
10 mm blade, 1 tooth/cm straight cut cuts slowly and dulls very quickly due to
the abrasive action of the frozen soil;
tooth life very short with no significant
difference between ferrous, non-ferrous
and wood cutting blades
Diamond saw in conjunction with table and guide, it is depth of cut restricted by the radius of
the most desirable method for cutting the blade; clayey soils greatly reduce
frozen soils; very clean straight cut cutting efficiency of the saw blade as
even in coarse-grain pebbly soils the blade must be cleaned regularly
7~
Ill
2O
O
Z
"r
-n
O
N
m
z
o')
0
"o
I-"
m
FIG. 6--Use o f a swede saw f o r rough cutting large block samples.
At the University of Alberta, a core barrel attached to a milling ma-

chine was used to core cylindrical specimens from block samples [1]. An
80 mm length of steel tubing (67 mm inside diameter) was fabricated with
a cutting edge on one end. The cutting edge was formed by rolling the lip
of the tube inward and sharpening it to an inside diameter of 64 mm. The
core barrel, clamped in the drive chuck of a milling machine, was rotated
at 300 rpm. Only short specimens were prepared for testing. Long speci-
mens break during coring, particularly if the frozen soil has a high ice
content.
Dumbbell-shaped specimens for tensile testing are prepared in molds or
by machining samples on the lathe, using these procedures.
Greater care is necessary in machining naturally frozen samples, as they
FIG. 7--Use o f band saw to cut smaller samples.
may contain large ice inclusions (lenses, etc.) that are very fragile and
easily chipped. Unexpected occurrences of pebbles can ruin many hours
of machining if care is not taken when they are detected. Many samples,
obtained at high cost in the field, have not been tested because they were
too difficult to machine.
These combined cutting and coring processes are used to prepare frozen
soil specimens for all forms of load testing. Dimensional tolerances for
uniaxial thaw-consolidation test specimens are particularly critical, as the
sample must fit tightly into the consolidometer ring. The nature of the
other tests is such that the dimensions of specimens are less critical.
It is important that the ends of the specimens are parallel and plane, so
that intimate contact occurs with the loading platens. Seating errors have
been observed on many loading curves [4]. Eccentric loading can give
lower strength values [3], but these are often ignored.
Although the effects of thermal disturbance induced by machining pro-
cedures have not been investigated, every effort should be made to elimi-
nate or reduce them, especially on clay samples. Surface thawing has been
noticed on several occasions when machining specimens of frozen day.
FIG. 8--Eight-sided cylinder cut on band saw.
Storage and Protection During Laboratory Testing

Careful control of temperature and humidity in storage areas is necessary
to protect the frozen sample from sublimation and thermal disturbance,
from the time it has been molded or machined or both until testing has
been completed. Protection methods are similar to those used when trans-
porting frozen samples from the field. Samples should be wrapped in an
impermeable material and stored in a refrigerated room or freezer.
Khomichevskaya, one of the earlier Russian investigators, wrapped naturally
frozen samples in insulation and stored them in underground rooms for
up to seven days with good results [16].
Sublimation of samples can be minimized by controlling the humidity
and reducing air flow around the specimen. Most small capacity freezers
do not have air circulation fans in the freezing compartments, and air
FIG. 9--Specimen turned on lathe to required diameter.
flow is limited to that caused by convection currents. Large walk-in freezers

rely on fans to circulate the air and control the temperature effectively
throughout the storage chamber. Frozen samples can be protected from
these air currents by wrapping them in cellophane and placing them in
plastic bags. Snow or ice shavings can be placed in the bags to raise the
humidity around the sample. The bags should then be evacuated to re-
move as much air as possible and heat sealed. These procedures are
shown in Figs. 11 and 12.
In studies of ways to store and preserve frozen samples, Livingston [17]
found that samples lost considerable weight, due to surface evaporation,
when the storage temperature ranged from 0 to - 6 ~ To study the effect
of the storage temperature on surface evaporation and sublimation, small
specimens of frozen Keweenaw silt (approximately 25 mm cubes with
polished surfaces) were prepared and stored at various temperatures. The
results indicated that storage at temperatures between - 8 and - 12~ re-
duced the rate of surface evaporation to an acceptable value. Various
methods were investigated to reduce sublimation further, as failure to
control this moisture loss affects test results. Synthetic resins, silicone oil,
varnishes, natural oils, and other commercially available products were
sprayed or painted on the surface of the specimens. Vegetable and min-
FIG. lO--Facing specimen ends on the lathe using special holder.
eral waxes could not be used as they must be heated. Although many of
the surface coatings reduced the rate o f surface evaporation, none o f the
materials investigated provided satisfactory protection for more than one
week.
Frozen soil specimens at the University of Alberta have been coated
with a thin layer of ice by applying a fine spray of supercooled distilled
water [I]. This film o f ice prevents sublimation of the sample and is re-
moved easily prior to testing.
Yershov et al [18] published information on the sublimation o f frozen
soils. As shown in Fig. 13, different soil types have different sublimation
rates. Finer grained clay soils have a higher evaporation rate than do
coarser sands. The rate o f sublimation is affected greatly by the ambient
temperature (Fig. 14). The parameters studied were temperature, relative
humidity, and air velocity, but no details were given on how the experi-
ments were undertaken nor on the apparatus used.
A similar study was undertaken by the author to determine the rate of
sublimation on three soil types: Ottawa sand (20 to 30 mesh), Niagara silt,
and Leda clay. Four specimens of each soil type were prepared by adding
50 g o f water to equal volumes o f each soil and placing the mixture in
FIG. 11--Evacuatingplastic bag to prevent sublimation.
plastic boxes 1.9 • 10-2 m deep, having a surface area o f 3.31 • 10-3 m 2.
Two samples of each soil type had their surfaces covered with cellophane;
the others were left uncovered. All the samples were weighed and placed
in the cold room to freeze at a temperature o f - 4 . 4 ~ and a relative hu-
midity of 37 percent. The specimens were weighed after 8 h and then once
a day for 23 days. Results are presented in Fig. 15.
The sublimation rates of the frozen soils investigated by the author are
within the same range as those reported by Yershov et al [18]. Similarly, it
was found that the finer clay soils have higher sublimation rates than the
coarser sands. This is because the larger particle surface area in fine-grained
soils allows for film flow, which brings the water to the surface o f the
sample. Samples that were covered with cellophane had significantly
lower sublimation rates than those that were left uncovered.
Many investigators [5,7,17,19-21] have found that the compressive
strength of frozen soil is greatly dependent on its overall moisture con-
tent. Compressive strength increased with increasing moisture content. It
FIG. 12--Heat sealing the plastic bag.
reached a maximum when the soil was saturated completely and then de-
creased to the strength of ice. Any loss of moisture from a specimen,
therefore, will cause a change in its compressive strength.
The compressive behavior of frozen soil is also affected greatly by tem-
perature and by temperature fluctuations. It is imperative, therefore, that
specimens be stored and tested in a freezing chamber that has only a small
temperature fluctuation to minimize thermal disturbance. The effect of
fluctuations in temperature can be reduced by enclosing the specimen in
an insulating jacket during storage and testing. Vyalov [6] suggested the
following permissible temperature variations when storing and testing
frozen soils within different ranges:
Temperature, ~ up t o - 2 -2to -5 -5to-10 below-10
Permissible devia- _+0.1 _+0.2 __.0.5 ___1.0
tion
Guarded hot plate experiments carried out by Hoekstra [22] using Fair-
banks silt (see Fig. 16) show that any thermal gradient in the sample, even
at temperatures below freezing, will cause moisture redistribution in fro-
I I I I I J
TEMP.: -1.6deg C
REL. HUM,: 65% I I I I I
A I R V E L . : 4 . 2 m/sec
O MOSCOW LOAM
9 KIEV CLAY
9 MOSCOW SANDY LOAM

?
o o
HUM.: 60%
x 30 VEL.: 4 . 5 m/see
2
s
~E
GLUKHOV KAOLIN
I
20
< go
>
z z
0 2(1 o m
..n
BENTONITE
O O
z
D
"11
10 __ ~o
O
M ~ v N
10 m
ISANDY LOAM \ Z
q')
0
9...... TIME = 600h I--
0 I >
0 -2 -4 -6 -8 -10 -12 -14
0 L I I I I I I TEMPERATURE, deg C -o
t-
0 100 200 300 400 500 600 700 in
TIME, h
if)
FIG. 14--Sublimation and temperature ( Yershov et al [18])
FIG. 13--Sublimation rates o f frozen soils ( Yershov et al [18])
O
(.O
4o t I I I I I I
TEMP.: -4.4 de9 C

REL. HUM.: 37%
ONE SIDE EXPOSED
3O
2O
z
o
CELLOPHANE COVERED(ALL THREESOILS)
I00
.[ _ I
200 300 400
TIME, h
I I
500 600
t 700
FIG. 15--Sublimation in N R C / D B R cold room.
0.35 I I I I I I I [ I I I
I
k .ICE LAYER
0 30 I~'x
E ~''"/,'~',k INITIAL WATER CONTENT
~-"
Z ~ ~ S = 0.73 r t40 MIN
TIME = R _-,
Z 0.25 1 6 0 _ - - -B'" - --'
< 0.20 /\~X//~NNOTE: ARROWS POINT-_

~ \I\/A. t TO BOUNDARY
~/~bX-' BENT~ R ~ E NFRsO~,ELN A N g -
I 2 3 4 5
DISTANCE FROM COLD PLATE, inches
FIG. 16--Effect o f temperature gradient on moisture redistribution in frozen Fairbanks

silt ( Hoekstra [22]).
zen soil. This moisture movement will increase the sublimation/evapora-

tion rate, as well as change the fabric of the specimen.
Many investigators [19,23] have found that the unfrozen moisture con-
tent will influence greatly the compressive strength of frozen soils. Wil-
liams [24], using calorimetric methods, found that there was a hysteresis
effect in the temperature dependence of the unfrozen water content. The
unfrozen water content of a frozen soil, at a given temperature, is depend-
ent on whether the temperature is reached by cooling or warming. If
temperature fluctuations occur, even though the specimen remains below
0 ~ the unfrozen moisture content will change. This is of great concern
when testing frozen soils at temperatures above - 5 ~
The cold rooms at DBR/NRC provide good examples of well controlled
environments. The temperature of the cold rooms can be controlled
accurately by a reheat system to within ___0.1~ at any location in the
room. Each refrigeration unit is operated by a two-stage compressor with
a capacity of 3.5 tons of refrigeration circulating Freon 22. The cooling
capacity is adjusted automatically to be in excess of that required, and the
temperature is controlled by electric reheating. The reheat unit has a
capacity of 12 kW and is operated by a solid state controller. Two evap-
oration units are located in each of the cold rooms so that one unit can be
defrosted without shutting the cold rooms down. A separate auxiliary
compressor and control system is available in case one of the main sys-
tems becomes inoperative. In addition, a freezer of 1 m 3 capacity is avail-
able also in the laboratory as a backup system. Samples can be transferred
to the freezer in case of emergency shutdown. The need for an alarm sys-
tem to provide warning of equipment failure and for several backup sys-
tems is appreciated only after samples are lost due to thawing because of
unexpected equipment breakdowns.
Conclusions
The important factors to be considered in transporting, preparing, and
storing frozen soils for laboratory testing are the control of the effects of
sublimation/evaporation and minimization of thermal disturbance. Their
effect on the ice content, fabric, and unfrozen moisture content of the
specimen, and, therefore, on the strength and deformation behavior of
the material, is of great significance. Further evaluation of existing proce-
dures and development of new or improved techniques are required be-
fore standard methods can be proposed for the laboratory testing of fro-
zen soils.
Acknowledgments
The author wishes to acknowledge the assistance of W. D. Roggensack,
University of Alberta, M. S. King, University of Saskatchewan, and W.
A. Slusarchuk, Northern Engineering Services Ltd. (formerly of the Divi-

sion of Building Research) in the development of this reveiw paper.
References
[ll goggensack, W. D., University of Alberta, personal communication, 1974.
[2] Slusarchuk, W. A., Northern Engineering Services Ltd., Calgary, Alta., personal com-
munication, 1974.
[3] Haynes, F. D., U.S. Army Cold Regions Research and Engineering Laboratory, personal
communication, 1974.
[4] Goughnour, R. and Andersland, O. B., Journal of the Soil Mechanics and Foundation
Division, American Society of Civil Engineers, Vol. 94, No. SMI, 1968, pp. 923-950.
[5] Hooke, R. L., Dahlin, B. B., and Kauper, M. T., Journal of Glaciology, Vol. 11, 1972,
pp. 327-336.
[6] Vyalov, S. S., "Methods of Determining Creep, Long-Term Strength, and Compres-
sibility Characteristics of Frozen Soils," National Research Council Technical Transla-
tion, T'r-1364, Ottawa, 1969.
[7] Tsytovich, N. A. and Sumgin, M. I. "Principles of Mechanics of Frozen Ground,"
U.S. Army, Snow, Ice, Permafrost Research Establishment, Translation No. 19, 1959.
[8] Lechner, W., "Peltier Cooling," Philips Technical Review, No. 27, 1966, pp. 113-130.
[9] Williams, P. J., Canadian Geotechnical Journal, Vol. 5, No. 4, 1968, pp. 264-266.
[10] Webb, E. L. R., "Equivalent Circuit Model for Thermoelectric Temperature Con-
trollers," Bulletin No. 18, Radio and Electrical Engineering Division, National Research
Council of Canada, Ottawa, 1968.
[11] Sayles, F. H., "Creep of Frozen Sands," U.S. Army, Cold Regions Research and
Engineering Laboratory, Technical Report No. 190, 1968.
[12] Sayles, F. H. and Haines, D., "Creep of Frozen Silt and Clay," U.S. Army, Cold Re-
gions Research and Engineering Laboratory, Technical Report No. 252, 1974.
[13] Warder, D. L, and Andersland, O. B., Canadian Geotechnical Journal, Vol. 8, No. 1,
1971, pp. 46-68.
[14] Laba, J. T., Highway Research Record, No. 360, 1971, pp. 26-36.
[15] Shuster, J. A. in Proceedings o f the Symposium on Cold Regions Engineering, Ameri-
can Society of Civil Engineering, University of Alaska, Vol. 1, 1971, pp. 73-117.
[16"1 Khomichevskaya, L. S., "Compressive Strength of Permafrost and Ice in Their Natural
States," U.S. Army, Arctic Construction and Frost Effects Laboratory, Translation
No. 20, 1951.
[17] Livingston, C. W., "Explosion Tests in Keweenaw Silt," U.S. Army, Snow, Ice,
Permafrost Research Establishment, Report No. 30, 1956, pp. 25-40.
[18] Yershov, E. D., Gurov, V. V., and Dostovalov, B. N., "Ice Sublimation in Fine-Grained
Soil of Various Cryogenic Structure During its Interaction with an Air-Current," U.S.
Army, Cold Regions Research and Engineering Laboratory, Translation No. 439, 1973,
pp. 2477_251.
llgl Yong, R. N. in Proceedings of the Permafrost International Conference, National
Academy of Sciences-National Research Council, 1963, pp. 315-319.
[20] Kaplar, C. W., "Some Strength Properties of Frozen Soil and Effect of Loading Rate,"
U.S. Army, Cold Regions Research and Engineering Laboratory, Special Report No.
159, 1971.
[21] Andersland, O. B., The Northern Engineer, Vol. 3, No. 3, 1971, pp. 4-6.
[22] Hoekstra, P., Water Resources Research, Vol. 2, No. 2, 1966, pp. 241-250.
[23] Sanger, F. J., "Foundations of Structures in Cold Regions," U.S. Army, Cold Regions
Research and Engineering Laboratory, Monograph No. III-CA, 1969.
[24] Williams, P. J. in Proceedings of the Permafrost International Conference, National
Academy of Sciences-National Research Council, 1963, pp. 225-229.
Michael Bozozuk'
Temperature-Controlled Humid
Storage Room
REFERENCE: Bozozuk, Michael, "Temperature-ControlledHumid Storage Room,"

Soil Specimen Preparation for Laboratory Testing, ASTM STP 599, American So-
ciety for Testing and Materials, 1976, pp. 113-125.
ABSTRACT: The design of a soil sample storage room that has been in operation
since 1954 is described. The room provides a storage environment with a constant
temperature of 55 ~ and relative humidities of 90 to 97 percent. It is of wood frame
construction, lined with copper sheeting, forming a watertight interior. The desired
temperature and humidities are obtained by running water down the walls of the
room and circulating it through a heat exchanger. The preparation of samples for
storage and the effect of storage times on softs are discussed.
KEY WORDS: soils, design, storage room, constant temperature, humidity, samples,
storage time
The purpose of a storage room for soils is to retain soil specimens in

their original condition at time of sampling until testing can be under-
taken. The functional requirements for such facilities will depend upon
the nature and quality of the samples to be stored, as well as the use to
be made of them. Granular soils obtained for grain size or compaction
tests can be kept in ordinary burlap sacks and stored almost any place for
years, even in an unheated shack. On the other hand, high quality undis-
turbed samples of sensitive marine clays, obtained for consolidation,
undrained triaxial strength, or other special engineering tests, require
careful handling and ideal storage conditions. These samples should be
wrapped, waxed, labelled, and stored properly, free of shocks or vibra-
tions, in a humid environment at a constant temperature near that which
prevailed in the ground at the time of sampling.
Unless these storage requirements are met, high quality undisturbed
soils will deteriorate, and the results of the special engineering tests would
be questionable. The storing of soils in a warm, humid environment is
conducive to high rates of oxidation causing chemical changes in the soil,
1Research officer, Geotechnical Section, Division of Building Research, National Re-
search Council of Canada, Ottawa, Ont., Canada.
113
Downloaded/printed
Copyright 9 1976 byby ASTM International www.astm.org
deterioration of the sealing wax, and formation of water blisters (Fig. 1),
and sometimes breeds bacteria that feed upon the soils or the wax. High
temperatures permit dissolved gases in saturated clays to come out of
solution, causing expansion and deterioration of the soil skeleton. If
stored in a dry and warm environment, soil moisture may escape, causing
FIG. 1--Poorly stored samples.
the soils to shrink; on the other hand, samples stored submerged in

water containers may absorb water and swell. Consequently, the clays
could change both physically and chemically so that they would no longer
exhibit the engineering properties of the in situ soil they are supposed to
represent.
In 1954, the Division of Building Research, National Research Council
of Canada, designed and constructed a temperature-controlled humid
storage room (Fig. 2), to reduce or minimize the effects of improper
storage; it has operated continuously since then. The room is approxi-
mately 13 ft long, 6 89ft wide, and 9 ft high. A removable wooden floor
provides a relatively dry walking area and supports the storage shelves
and working table. This paper discusses the design of the room, the han-
dling and preparation of samples for storage, and the effect that long stor-
age times can have on engineering properties.
BOZOZUK ON TEMPERATURE CONTROLLED HUMID STORAGE ROOM 115
FIG. 2a--Constant temperature humid storage room.
Design
The storage room was designed as a necessary accessory to laboratory
soil testing facilities. Its purpose is to keep the soil samples in the best
possible condition, that is, to bridge the period from the time they are
obtained in the field until they are tested and to provide a conditioned
environment for performing certain special engineering tests, when re-
quired.
The principle of operation is as follows. Water is directed to flow down
the inside walls of the room to the floor, where it is ponded. Natural
evaporation from the wetted walls and the reservoir that covers the
entire floor area provides relative humidities from 90 to 97 percent. The
temperature control is obtained by circulating the ponded water through a
heat exchanger located outside the room. After it is cooled, it is pumped
back to the top of the room, where it is directed against the walls through
nozzles to complete the flow cycle. Any heat gain through the walls is
picked up by the flowing water and dispelled through the heat exchanger.
The storage room is essentially a copper tank enclosed in an insulated
wood frame. A plan view (Fig. 3) shows the layout of the sample racks
and worktable, relative to the door and window. It was constructed on 2
by 2-in. wood sleepers laid on the concrete floor of the laboratory. Set at
12 in. centers and running parallel to the length of the room, they were
covered with 88 plywood and nailed together (Fig. 4). The
FIG. 2b--Mechancal plant: (a) chilled liquid and (b) heat exchanger.
purpose of the sleepers was to provide an air space and ventilation for the
floor and adequate support for the superstructure, in case it had to be
moved. The plywood was then covered with a vapor barrier that projected
about 2 in. beyond the perimeter.
To facilitate circulation of the ponded water, the floor was sloped 1 in.
to the drain located at the back o f the room by tapering the 2 by 6-in.
floor joists. They were placed across the sleepers to form the floor of the
room. The wall frames, made o f 2 by 3-in. studs, were erected on the
joists, which, in turn, supported the frame roof made up of 2 by 4-in.
joists. All joists and studs were placed at 16 in. centers whenever possible.
The spaces between the studs and joists in the floor and ceiling were
insulated with 2-in.-thick mineral wool insulation. The exterior of the
room was first sheathed with a layer o f 5/16-in. plywood, then covered
completely with a vapor barrier that overlapped at the ends and corners.
It was, in turn, protected with a second layer of 5/16-in. plywood.
The walls, floor, and ceiling inside the room were covered with Y2-in.-
thick fir plywood. Finally, it was covered completely with 20-gage copper
sheeting to form a watertight interior.
FIG. 2c--Interior of humid storage room.
L. 12'- I0'~ _1
PUMP a MOTOR
CHILLED
HEAT EXCHANGER l --WATER
SUPPLY
t~"FLOOR DRAIN
? j 3 ' x 4'
~ /SAMRLE
r
I
/
RACKS
WORK
TABLE
THERMOPANE
W~NOOW
6L( I
I ~_~---REMOVABLE FLOOR-..~
e-~-r~-(///i SECTIONS ~%"2" OIA. ACCESS
HOLE
I
t~NSITE BAFFLE
INTERIOR SHEET " / SEAL'~WOOD FRAME WALL

COPPER W{TH 2"x 3" STUDS ~ 16"C.C.
SPRAY NOZZLES 3'x7' REFRIGERATOR
DOOR
FIG. 3--Floor plan o f storage room.
Two thermopane windows were provided for lighting. A 3 by 4-ft

window installed at one end of the room allowed ordinary light from
the laboratory to illuminate the worktable (Fig. 3). A second 2 by 4-ft
window was installed in the ceiling to permit artificial lighting of the
room, using a fluorescent ceiling lamp suspended above it (Figure 4). For
.•(fEXJSTING CEILING IN LABORATORY
; LU~RES~ENTT -J" THERMOPANE

2"x4"@ 16" C.C.-~ /COPPER~, LIGHTsO C) 0 / WINDOW
WATER
= INLET
T'I"
i,l.._~_
CL A M p
c 2" INSULATION
r-
I/4" TRANSITE 6' - I0 5/B"

BAFFLE
/I/2" FIR PLYWOOD

8'- I/4"
~ 2 " x 3" STUDS
@ =6 " Cl C. 20 GAUGE COPPER
TO FORM WATERPROOF
INTERIOR.~
~TWO LAYERS 5/16" PLYWOOD
WITH VAPOUR BARRIER
IN BETWEEN.
~2 1/2"
_ 5~L_ 4'- 11Y4"
;I 5 / 8 II X I 5/8"
~ 12' C.C. 3/4" SYLVAPLY PLYWO
~/ Fo,~
LEVELLING JO,ST ~' / 2 "
JL,~ , ~ ~ ------CEOA,, , "r
2" DIA.
S/B"nnnn/J TAPEREB JO,ST ""-,/2" FIR PLYWOOD ~,,/'~/'~'.-I-':: ~"OUTLET
pq I~ E,~ II. [X] D..r-Ji
#
EXISTING FLOOR IN LABORATORYj LSLEEPERS X~l/4" PLYWOOD
FIG. 4--Design section o f storage room.
safety reasons, no electric outlets or fixtures were permitted inside the

room. If power is required, it is brought in through the 2-in. diameter
access or service hole through the wall, 5 in. from the ceiling above
the window (Fig. 3). The hole is left open to dissipate the air cushion
effect every time the door was opened or closed.
A 3 by 7-ft refrigerator door with a two-way latch, insulated and
covered with sheet copper, was installed on the outside to close against a
rubber seal placed around the doorway.
Three removable floor sections were constructed to provide the walking
area and support for the racks and table above the reservoir (Fig. 3).
These consisted of 90 sylvaply plywood sections nailed to 2 by 2-in.
cedar sleepers, which, in turn, were nailed to 2-in.-thick tapered cedar
levelling joists (Fig. 4). The removable floor facilitates maintenance

when required. A 5 in. clearance was provided, adjacent to the sprayed
walls (Figs. 3,4), to ensure an adequate circulation of air under the floor.
Closed Flow Conditioning System

The desired storage temperature and relative humidity are obtained by
continuously circulating the ponded water from the reservoir through a
heat exchanger and back into the top of the room, where it is directed to
flow down the walls. This is achieved by pumping the preconditioned
water into a copper tube header, fastened to the ceiling about 89 in. away
from the walls, and covering most of the room perimeter (Fig. 3).
Originally, the header was fitted with eleven flat atomizer jets spaced
relatively uniformly, but this mixed the air and water to such an extent
that it created fog. Any objects placed in the room collected water im-
mediately. Even beakers filled up within a short time. Such an environ-
ment was satisfactory for storing and curing concrete specimens but was
not considered satisfactory for soil samples. Consequently, the atomizer
jets were replaced with 10 in. lengths of 88 copper tubing. It
was possible, by bending the tubing to direct the flow along the walls, to
create the flow pattern illustrated in Fig. 5, and to wet the walls below
24"C C.
PER TUBE NOZZLE,lO"

LO?0 GBE ,IZ0 0,REGT LOW
l // /
the header completely. A 88

RUNNING DOWN WALLS
PONDED WATER
S, TTooLgVEL
9 FLOOR OF RESERVOIR
,/
FIG. 5 Flow pattern o f water along walls o f storage room.
transite (asbestos) baffle, installed in

4-ft-wide sections and set 2 89 in. away from the walls, prevented splash-
ing of the interior (Fig. 4). It also increased the wetted surface area from
which water evaporated into the room. The bottom of the baffle was
kept about 2 in. above the surface of the ponded water to ensure proper
circulation of air.
The storage room requires about 75 Imperial gallons of water to create
a pond 1 89 in. deep at the shallow end. Slimacide V-10, with a pine root
oil base, is added to the circulating water to prevent bacterial growth.
The water is pumped from the reservoir, through a strainer, to the heat
exchanger, as shown in Fig. 6, where it is cooled, then back to the room
E__-~ ..... ~_--_~_--_~

~NOZZLES
TEMPERATURE CONDITIONED WATER
CONTROL TO HUMID ROOM
t [ ~ i HERMOMETER
SERVO TEMPERATURE
ENSOR
MOTOR THERMOMETER
CHILLED ~
VALVF,I
E Jil I
WATER IL " ~ I ~ HEATEXCHANGER
SUPPLY ~ ~ -~ .j I ;
VALVE ALVE THERMOMETER TEMPERATURE SENSOR
PRESSURE GAUGE
BYPASSVALVE/ / ~'I
WATERFROMROOM
TEMPERATURE / CENTRIFUGAL
SENSOR / PUMP
THERMOMETER ~ !
\STR%ER
DRAIN
FIG. 6--Conditioning equipment and controls.
at a rate of 15 Imperial gal/min, under a pressure of 16 psi. A single

phase l l0-V 60-cycle 3450-rpm V2-hp motor powers the centrifugal
pump. The temperature of the chilled water supply feeding the heat ex-
changer is about 41 ~ it is exhausted at about47 ~
The temperature o f the storage room is regulated by the control panel
and three temperature sensors installed at the locations shown. The panel
operates the servo motor driving the by pass valve mounted on the
chilled water supply line, thus controlling the amount of cooling required
to maintain a room temperature of 55 ~ which is about the mean annual
ground temperature in the Ottawa region. Four thermometers, located
as shown, provide an easy check on the operation of the system. In
assembling the plumbing system, air bleed valves were provided at all
high points and drains at all low points. To facilitate maintenance and
flushing of the room, it is connected permanently to a floor drain in the
laboratory.
The storage room is furnished with four sample racks and a worktable
laid out as shown on Fig. 3. The support frames are made of aluminum
angles and the shelves of asbestos sheeting. The design details are given
on Figs. 7 and 8.
ALUMINUM FRAMING
~ IlL'ix I I,/21'X3/f6" THK.
~21 821
ASBESTOS BOARD SHELF

/47 5/8" , 12"X I14'l THK,
,//
===:
~ALUMINUM BASE PLATES ~

UNDER EACH UNIT
48" t25/8"x II~'x 3/16" THK, 12"
FIG. 7--Storage room racks.
SECURE SYLVAPLY TO FRAME USING

N-I/4'L20 BRASS BOLTS ~ NUTS 8r
SCREW I/2" ASBESTOS SHEETING
WrTH VB" F/HD BRASS SCREWS.~
SYLVAPLY
G6" | 26"
I
/ J
~3" -- 112" ASBESTOS SHEETING BOLTED 15, --i 112"
TO SHELF FRAME WtTH 4-I~L20
BOLTS B NUTS',,
35'
14'
_ r ,4 )"
ALUMINUM FRAMING LUMINUM BASE PLAT[ ~
[12" x ~ ~/2" X ~ / 4 II THK. 25"x 3 " x 3/16" THK.
FIG. 8--Worktable.
Handling and Preparation of Samples for Storage

Careful handling and protection of high-quality undisturbed samples
start in the field. As soon as the sample tubes are removed from the bore-
hole, they are numbered, sealed and capped, and placed in special carry-
ing cases lined with styrofoam and foam rubber. Consequently, the
samples are protected from extreme temperature changes, shocks, and
vibrations until they reach the laboratory.
At the laboratory, they are recorded immediately and placed in the
storage room. If the sample tubes are made of stainless steel, the soil
cores can be left in them until needed. If rusting or corrosion is a pos-
sibility, or if the tubes are needed for continuing the sampling program,
the soils should be extruded and waxed for storage.
The cores are extruded vertically, using a hydraulic extruder. They are
extruded in lengths of 4 or 8 in. at a time, cut o f f with a wire saw,
covered with thin plastic film and coated by dipping them carefully
several times into melted wax. For very weak or soft soils, the cores are
wrapped with cheesecloth to provide lateral support as they are extruded,
then cut off, wrapped in plastic film, and waxed. The wax used in the
laboratory is a Grade 175 microwax (Imperial Oil Co.), that has a
congealing temperature of 78 ~ Labels are applied and coated with wax
before the samples are placed on the storage racks. Block samples are
prepared for storage in a similar way, except that the wax is applied by
brush.
Effect of Storage Time on Test Results

Grain size analysis and Atterberg limits of sensitive marine clays do not
appear to be affected significantly by long periods of storage, even
though the samples change color frequently, indicating that some
chemical changes have occurred. La Rochelle et al, 2 on the other hand,
found that the shear strength of some Champlain clays was reduced after
long periods of storage. Similar results were obtained from strength tests
performed on marine clays f r o m Canadian Forces Station (CFS) Glou-
cester, which had been stored for seven years. The results, summarized in
Table 1, show that generally the degree of saturation and wet density
decreased, and the water content increased somewhat by extending the
storage time f r o m one to seven years. There was also a reduction in
shear strength, averaging 11.2 percent and a small decrease in strain at
failure.
Some investigators ~'4 have found that long storage times reduce the
2La Rochelle, P., Sarrailh, J., Roy, M., and Tavenas, F. A., this publication, pp. 126-146.
3Leonards, G. A. and Altschaeffl, A. G., Journal o f Soil Mechanics and Foundations
Division, Vol. 5, Sept. 1964, pp. 133-155.
4Bozozuk, Michael in Sampling o f Soil and Rock, A S T M STP 483, American Society
for Testing and Materials, 1971, pp. 121-131.
O
TABLE 1--Effect o f storage on triaxial consolidated anisotropically undrained strengths, measured on undisturbed N
tube samples o f marine clay, obtained from CFS Gloucester, Dec. 196Z c
O
Consolidation Z
Stress, k g / c m ~ Tested, Nov. 1968 Tested, Dec. 1974 -I
Depth, m
+ 0 . 3 ft Oo' o', S, 070 w, 070 y, 6Q, ~s, 07o S, 070 w, ~ r. 6Q, Es, 07o "u
lb/fP kg/cm 2 lb/ft a kg/cmz rn
nn
7.2 0.38 0.24 99.3 80.7 96.4 0.348 0.93 97.8 77.9 96.3 0.300 0.91 c
16.2 0.50 0.31 99.8 52.1 107.6 0.546 1.03 100.3 76.7 96.4 0.273 0.69
m
25.5 0.62 0.39 99.8 85.3 95.4 0.493 0.68 96.5 95.8 90.5 0.460 0.66
36.9 0.76 0.47 99.8 88.7 94.5 0.706 0.56 99.8 84.5 95.6 0.621 0.38 0
0
43.0 0.74 0.51 100.0 79.1 97.3 0.716 1.03 97.1 77.2 96.0 0.812 1.07 z-H
48.8 0.95 0.58 98.9 50.0 108.5 0.818 0.84 96.7 49.8 107.2 0.772 1.23
57.0 1.31 0.75 99.2 70.5 99.7 0.774 0.86 98.9 61.7 102.8 0.650 0.93 0
i-
63.0 1.39 0.86 99.3 35.6 117.8 0.734 0.67 96.8 36.5 115.6 0.672 0.58 r-
m
O
Average
"1"
99.5 67.7 102.1 0.642 0.83 98.0 70.0 100.1 0.570 0.81 C
Change, ~
. . . . . . . . . . . . . . . -1.5 +3.4 -2.1 -11.2 -2.3 O

22
NOTES---O 'o = in situ vertical effective stress. fi)
Ill
o'c = effective confining pressure.
S = degree of saturation at start of test. :Ij
0
w = water content at start of test. 0
y= wet density at start of test.
/IQ = maximum deviator stress at failure, A(m - o~)y.
~, = axial strain at failure (rate of strain 2070/h.
r
124 SOIL SPECIMEN PREPARATION FOR L A B O R A T O R Y TESTING
measured preconsolidation pressure, whereas others a found no effect. To

investigate this point further, additional consolidation tests were
performed on undisturbed samples of clay from CFS Gloucester that
had been stored in the temperature-controlled humid storage room from
five to seven years. In Fig. 9, the results are compared with the original
tests reported by Bozozuk and Leonards. ~ The measured preconsolidation
VERTICAL EFFECTIVE STRESS

TONSIFT2, kglcm 2
SOIL PROFILE O 0.5 1.0 1.5 2.0 2.5 3.0 3.5
0 ~ ...... IN I I I I I 1 O
BLACK ORGANIC TOPSOIL I~
5
TAN COLOURED \
FINE SAND AND SILT
DESICCATED GREY-BROWN
I0 SILTY CLAY
SOFT GREY-BROWN SILTY CLAY
WITH OCCASIONAL DECAYEDROOTS,
15 ROOTHOLES, AND SOME SMALL
FLAT STONES
PRECONSOLIDATION PRESSURE
20 SOFT GREYSILTY CLAY WITH MEASURED I TO 4 MONTHS
SOMECLAM SHELLS AFTER SAMPLING
(BOZOZUK AND LEONARDS, 19/21
25 GREY SILTY CLAY WITH
PRECONSOLIDATION PRESSURE, E
SOME SHELLS
MEASURED 5 TO I YEARS
30 AFTER SAMPLING
GREY CLAY WITH BLACK
MOTTLING, AND OCCASIONAL l0 w
% 351 SMALL FLAT STONES CONSOLIDATION TESTS
MEASURED 5 TO 7 YEARS
AFTER SAMPLING
40
45 IN SITU VERTICAL
EFFECTIVE STRESS
[5
50
GREY SILTY CLAY WITH BLACK

55 MOTTLING, OCCASIONAL SHELLS
AND SMALL STONES
60 I I I \ I I I I
F I G . 9--Effect of storage time on preconsolidation pressure measured on undisturbed

samples obtained from CFS Gloucester.
pressure was reduced only slightly in the lightly overconsolidated clay

formation from 6 to 18 ft (1.8 to 5.5 m). Below this depth, the measured
overconsolidation pressure of 0.25 kg/cm 2 was 40 percent lower than the
originally measured value of 0.42 kg/cm ~. Below the 50 ft (15.2 m) depth,
the reduction was about 35 percent. As the loading schedules in both
~Bozozuk, Michael and Leonards, G. A . in Proceedings, Specialty Conference on
Performance of Earth and Earth-Supported Structures, American Society of Civil Engineers,
Purdue University, West Lafayette, I n d . , Vol. 1, P a r t 1, 11-14 J u n e 1972, pp. 229-317.
testing programs were identical and the test specimens were the same size,
the observed reduction in preconsolidation pressure must be attributed to
storage time.
The evidence concerning the detrimental effects of storage time on the
engineering properties of soils is accumulating but is still not entirely
conclusive. Detrimental effects, as noted previously, have been observed
under the best storage conditions, and it is known that a relaxation of
stresses with time may cause changes in soil structure. In planning a soil
testing program, therefore, consolidation, undrained triaxial strength, and
other special engineering tests should be performed as soon as possible
after the samples are obtained. Atterberg limits, grain size analysis, and
other classification or index tests may be performed after long periods of
storage without affecting the results seriously.
Summary
In 1954, a controlled-temperature humid storage room was designed
and constructed in the Geotechnical Laboratory of the Division of Build-
ing Research, National Research Council of Canada. The room is a wood
frame construction, lined completely with sheet copper on the inside. The
desired temperature and humidity are achieved by running water down the
walls to the floor, where it is ponded below a removable floor. Heat gain
into the room is removed by pumping the water through a heat exchanger
fed by chilled water. The paper discusses the design, the preparation of
samples for storage, and the effects that long storage times may have on
test results.
A ckno wledgmen ts
Thanks are due to K. R. Solvason, Research Officer, Building Services
Section, who designed the mechanical plant for the storage room.
This paper is a contribution from the Division of Building Research,
National Research Council of Canada and is published with the approval
of the Director of the Division.
P. L a Rochelle, ~ J. Sarrailh, ~ M. R o y , 1 a n d F. A . Tavenas ~
Effect of Storage and

Reconsolidation on the Properties
of Champlain Clays
REFERENCE: La Rochelle, P., Sarrailh, J., Roy, M., and Tavenas, F. A., "Effect
of Storage and Reconsolidation on the Properties of Champlain Clays," Soil
Specimen Preparation for Laboratory Testing, ASTM STP 599, American Society
for Testing and Materials, 1976, pp. 126-146.
ABSTRACT: A testing program has been made on samples of sensitive cemented

clays at different times after sampling. When comparing results of unconfined
compression tests performed on the field immediately after sampling or in the
laboratory the following week, it is observed that there is a decrease in the measured
strength which may be attributed to water migration; however, this effect was
minimized or eliminated completely by keeping the samples in the tubes or by
trimming the samples immediately after sampling. The reconsolidation of the samples
to the in situ stresses restored an appreciable part of the strength lost by sampling
disturbance; this effect is negligible in the case of good quality samples. Tests
made on block samples which had been stored for many years in a humid room
have shown a decrease in the shearing of the clay, but the preconsolidation pressure
has not been affected.
KEY WORDS: soils, cohesive soils, tests, samples, preservation, storage
T h e h i s t o r y o f a c l a y s a m p l e p r i o r t o testing m a y have a n a p p r e c i a b l e
effect o n the p r o p e r t i e s o f t h e c l a y m e a s u r e d in the l a b o r a t o r y . I n t h e case
o f the soft sensitive clays, o b s e r v a t i o n s b y d i f f e r e n t a u t h o r s h a v e s h o w n
t h a t t h e s a m p l e s s h o u l d be m a n i p u l a t e d with great c a r e d u r i n g t r a n s p o r -
t a t i o n , p r e p a r a t i o n , a n d t r i m m i n g so as to a v o i d a n y shocks, v i b r a t i o n s ,
o r stress c o n c e n t r a t i o n s , w h i c h a r e b o u n d to d i s t u r b the clay s t r u c t u r e a n d
affect the measured properties.
In spite o f all due p r e c a u t i o n s with regard to m a n i p u l a t i o n , the p r o p -
erties o f the clay s a m p l e s m a y b e altered b y o t h e r p h e n o m e n a , s u c h as
the w a t e r m i g r a t i o n within the s a m p l e . T h a t p r o b l e m was r e c o g n i z e d b y
H v o r s l e v [1]z w h o suggested t h a t " s e r i o u s l y d i s t u r b e d parts o f t h e s a m p l e
Professor, graduate student, and associate professors, respectively, Department of Civil
Engineering, Universit6 Laval, Quebec, Canada.
2The italic numbers in brackets refer to the list of references appended to this paper.
126
Copyright 1976byASTMInternational www.astm.org
LA ROCHELLE ET AL ON STORAGE AND RECONSOLIDATION 127
should, as far as possible, be separated from the undisturbed parts in

order to avoid migration of pore water from the disturbed to the un-
disturbed parts." More recently, Bjerrum [2] has reported on some
observations made at Norwegian Geotechnical Institute (NGI) on Norwegian
clays. Clay samples were tested immediately after sampling and after a
storage time of three days; during this relatively short storage time, water
migration resulted in water contents which were 3 to 4 percent higher
in the core than in the outer zone of the samples; moreover, a reduction
of 15 percent of the undrained shear strength was observed even if the
samples had been reconsolidated to the field stresses. The reduction was
attributed to the internal swelling which had occurred within the sampling
tube during that fairly short period of time.
Following such observations, many questions arise concerning the
behavior of the sensitive clays of eastern Canada. These clays are known
to have a strongly bonded structure [3-7], which is a major difference
when compared to the Scandinavian clays. Is it then possible that the
cementation bonds have the ability to preserve the properties of the clay
during a change in stresses, thus preventing the clay from swelling as
suggested by Bjerrum [2]? Is it of essential importance that the samples
be reconsolidated to the same pressure they carried in the field in order
to yield representative test results? And finally, what is the influence of
the storage time on the cementation bonds, and how does it affect the
test results?
This paper presents the results of a testing program which was carried
out with the purpose of providing answers to these questions. Samples
of the cemented Champlain clays were used to study the occurrence of
the water migration and its influence on the undrained shear strength, the
importance of the reconsolidation to the in situ stresses, and the effect
of prolonged storage time on the characteristics of the bonds.
The present study is then aiming at determining differences in soil
properties resulting from some variations in sample treatment. It must be
realized that, in the case of natural soil deposits, such differences may
be fairly small when compared to the natural scatter of the soil properties,
further amplified by the variability of the sample quality. Hence, a very
large number of tests would have to be performed in order to arrive at
definite conclusions based on sound statistical analysis; this point has
not always been fully realized by previous authors involved in similar
testing programs. In the present study, if the large number of tests
required to reach definite conclusions had been performed, the publication
of the results would have been delayed considerably; however, the authors
believe that the available results show strong tendencies which are of some
importance to the engineering profession and should be known at this
time, pending confirmation by further studies.
Characteristics of the Cemented Clays

The geology and the general physical and mechnical properties of the
Champlain clay deposits have been discussed by many authors [3-71. The
deposits which are found in the Saint-Laurent, Ottawa, and Saguenay
river valleys have been known, for many decades, to be composed mainly
o f an extremely sensitive clay, but it is only recently that the presence
and significance o f the cementation bonds in the clay structure was fully
appreciated. Although their exact nature is not completely understood,
the cementation bonds are known to be the main cause for the relatively
high rigidity and strength of that clay; similarly, the fact that the pre-
consolidation pressures pc measured on the clay samples are appreciably
higher than the maximum loads which the deposit has ever carried in
nature has also been explained by the presence o f the cementation bonds.
The intensity o f cementation bonding in the clay may vary considerably
from one area to the other; for the purpose o f the present study, three
sites were chosen.
Saint-Aiban
The site o f Saint-Alban is located 80 km from Quebec City at the
northern fringe o f the Champlain clay deposits in that area. The clay
found on that site, which has been described previously in the literature
[8,9], is very soft and sensitive below a desiccated crust 2 m thick; the
strength, measured by means o f a Nilcon vane apparatus, increases from
10 kPa (210 lb/ft 2) below the crust at 2 m depth to 21 kPa (440 lb/ft 2) at
7.5 m depth. As seen f r o m Table 1, the water contents, the limits, the
indices, and the clay contents decrease with depth. In terms of the pre-
vious loads carried by the deposit, the clay is nearly normally consolidated;
TABLE 1--Typical properties of the clays studied.
Saint-Alban
Saint-Jean-
Soil Properties 2 m depth 7.5 m depth Saint-Louis Vianney
Water content, % 95.0 50 69.0 42.0
Plastic limit, ~ 27.0 20 27.0 18.0
Liquid limit, % 55.0 35 50.0 29.0
Plasticity index, % 28.0 15 23.0 11.0
Liquidity index 2.4 2 1.8 2.2
Clay content, % 80.0 35 80.0 60.0
Sensitivity(by lab. vane) 14.0 22 50.0 >500.0
Field vane strength, kPa 10.0 21 43.0 240.0
pc - po, kPa 18.0 45 102.0 640.0
however, the difference (Pc - Po) between the preconsolidation pressure

Pc and the effective overburden pressure Po, as given in Table 1, indicates
that the clay has gained a pseudo-preconsolidation which may be attributed
to a delayed consolidation during the aging of the deposit [10] and which
is locked into the clay structure by the cementation bonds.
Saint-Louis
The properties of the d a y at Saint-Louis, Yamaska, which is located
160 km southwest of Quebec City, have also been discussed in detail in
previous papers [6,11]. The typical values given in Table 1 correspond to
the elevation at which block samples were cut out from a trench dug in
a landslide crater. The clay plasticity on that site is more uniform with
depth than in Saint-Alban, and the vane strength at block level is 43 kPa
(900 lb/ftz). The clay is slightly overconsolidated by previous loads, but
the major part of (pc - po) is estimated to be due to delayed consolidation
and bonding. In terms of undrained strength and bonding, this clay may
be considered representative of the average clay encountered in the Saint-
Laurent lowlands.
Saint-Jean. Vianney
The village of Saint-Jean-Vianney, which was located approximately
200 km north of Quebec City on the northern side of the Saguenay
river valley, was the site of a disastrous landslide in 1971, which was
reported in the literature [12]. In many regards, the clay on that site
is similar to the Toulnustouc clay reported on by Conlon [4]. The typical
properties listed in Table 1 correspond to the elevation of block samples
cut out from a trench dug in the crater of the landslide. The clay is very
stiff, the vane strength being 240 kPa (5000 lb/ft2); it has a low plasticity
and is extremely sensitive. When compared to the average Champlain
clay deposits, the clay at Saint-Jean-Vianney is highly overconsolidated;
the measured preconsolidation pressure at the level of the block samples
is 900 kPa (8.4 T/ft 2) and it is estimated that half the value of (Pc - Po)
given in Table 1 is due to delayed consolidation and bonding.
When comparing the properties measured on the three sites, it becomes
obvious that the clay of Saint-Alban is the least cemented; as a matter of
fact, of all the Champlain clay deposits studied, that clay probably lies
close to the lower end of the scale in terms of intensity of cementation.
As the cementation bonds are believed to prevent swelling following a
stress release, the clay from Saint-Alban was chosen for the study since
it was considered to be the most susceptible to water migration within the
clay samples after sampling. On the other hand, the effect of storage time
on the bonds was evaluated on block samples from the two other sites
where the cementation is more important.
Water Migration Following Sampling

In order to find out whether any water migration takes place within
the samples o f cemented clays following sampling, two types of checks
were made: the first one consisted o f a direct comparison of the results
of unconfined compression tests made at different times after sampling,
and the second check consisted o f measuring the water contents across
the clay samples a few days after sampling.
The samples were taken at the site o f Saint-Alban by means o f a NGI
thin-wall stationary piston sampler; the stainless steel tubes used had a
diameter of 73 mm, a length of 1 m, an area ratio o f 9 percent, and an
internal clearance of 0.25 percent. Tube samples were taken in adjacent
boreholes over an area of 4 by 4 m at two different elevations (Fig. 1);
Cu-kPo
0 I0 20 30 40 50
o T
S T-AL BAN
I
~ 1~o
2
I tube somples
(upper level)
3
4
E
6
~~c I tube somples
1 (lower level )
7
o vane I
9 - o vane 2
e,--e average
,o I i
FIG. l--Undrained strength profile at Saint-Alban.
the useable length o f sample was on the order of 80 cm per tube. Five
tubes were taken at depths between 2.1 and 3.0 m, and nine tubes were
between 6.1 and 7.0 m.
Unconfined Compression Tests

The undrained strength at different times after sampling was measured
by unconfined compression tests made on specimens trimmed to a di-
LA ROCHELLE El" AL ON STORAGE AND RECONSOLIDATION 131
ameter of 3.8 cm and a height of 7.6 cm. A press, a triaxial cell, and the
necessary equipment for extruding and trimming the samples were
installed in a shanty on the site, so as to make compression tests im-
mediately after sampling.
In order to study the effect of short storage time on the undrained
strength, four series of tests were made on the samples taken at the two
different levels:
Series A--The samples were extruded, trimmed, and tested immediately

after sampling on the field.
Series B--The samples were extruded, trimmed, and paraffined on the
field and tested in the laboratory about one week later.
Series C--The samples were extruded and paraffined on the field, and
they were trimmed and tested in the laboratory about one week later.
Series /)---The tube samples were transported to the laboratory and
stored in the humid room; the samples were extruded, trimmed, and
tested the following week.
All compression tests in the field and in the laboratory were made by
the same operator, using the same apparatus. It may be worthwhile to
mention that the so-called paraffined samples were, in fact, wrapped
in plastic films which were sandwiched between layers of a mixture of
paraffin and vaseline; this technique was found to be very efficient in
preventing any measurable loss or gain of moisture during storage periods
of more than three years in a humid room.
Comparison o f the Results--When comparing the results in such a
study, problems arise due to the variation of strength of the specimens,
even when tested under exactly the same conditions. In the present case,
two types of variations are encountered: the first one is the natural
variation of the undrained strength profile along the length of the tubes,
and the second is the variability in the quality of the tube samples and
also of the specimens within one tube, resulting from the disturbance due
to the sampling operation.
Strength Profile--From previous studies in Saint-Alban, the strength pro-
files are known to be fairly uniform throughout the site; nevertheless,
two vane profiles were determined 2 m apart in the central part of the
sampling area, and the results are given in Fig. 1. It is seen that both
profiles coincide fairly well. On the same figure, the positions of the tube
samples have been drawn for the two levels studied; it may be observed
that the vane strength varies by an appreciable amount in the depth in-
crease, corresponding to the length of the tubes. At the upper level, the
vane strength is 10 kPa (210 lb/ft 2) at the elevation of the top of the tube
and 12.5 kPa (260 lb/ft 2) at the elevation of the bottom, thus increasing
by 25 percent. At the lower level, there is an increase in strength of about
15 percent from the top to the middle of the tube sample and then a
slight decrease in the bottom half.
In order to make the strength results of the compression tests com-
parable, they were all referred to the vane strength measured at the
elevation of the specimens within the tube and were expressed by the
ratio C~
c~, = c . ~ / c . (l)
where C~r is the undrained shear strength given by the unconfined com-
pression test at failure, and C,v is the vane strength measured at the same
elevation.
The vane strength was taken as a reference because it indicated, in a
very consistent manner, the variation of undrained strength along the
profile. Any elaborate discussion on the significance and value of the
vane strength is beyond the scope of the present paper.
Variability o f the Quality o f Samples--In spite of all the care taken
during the sampling operations in the field, there is an appreciable
variation in the quality of the samples obtained in such deposits of soft
sensitive clays. Figure 2 gives the results of unconfined compression tests
strength ratio, Cfv
top 0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1,8
, !
2 f
~ tube I
}- 4 I I / '
f
i
/
-- [
bo~'m
FIG. 2--Variability of the quality of tube samples.
made on specimens trimmed from two tubes taken in two adjacent holes
at the lower depth (Fig 1). It may be seen that the results from Tube I
are much higher than those from Tube H, although the field technique,
the sampling apparatus, the operators, and the testing method were the
same for both tubes. Moreover, the strength of the specimens within the
same tube sample varies appreciably, depending on the position of the
specimens in the tube; this variability may be attributed to sampling

disturbance [13]. Of the eight 10-cm-long specimens, which can be cut
from each tube, Specimen I, located at the top, was systematically elim-
inated as being disturbed; compression tests on Specimen 1 would give
only 20 to 30 percent of the vane strength at that elevation. Even Speci-
mens 2 and 3 (Table 2) give results which are questionable. Hence, the
variability of the quality of the tube samples and of the specimens
within each tube requires that the results be analysed carefully.
Analysis of the Results--The results of the comparative study of the
four test series are given in Table 2. Three different approaches were
used to analyse the results.
In a first approach, all tests were included to compute the average CM
thus, the corresponding values of N given in Table 2 represent the total
number of tests made for each series in this program. As some tests were
giving exceptionally low values of C~, and others, exceptionally high
values, the second approach, called the statistical approach in Table 2,
consisted in eliminating the results lying outside _+1 standard deviation
from the average, and a new average value was recalculated with the
results that were not rejected; their number and the corresponding average
C~ are given in Table 2, for each case. The third approach was based
on an arbitrary rule whereby only the best results were used, up to a
number equal to half the total number of tests available in each case.
When comparing the results of the three different approaches given
in Table 2, it is seen that, as expected, the first two approaches yield
average values of C~ which are nearly identical; as for the third approach,
it is quite normal that the average values of C~ be appreciably higher.
However, for the purpose of the present study, it is not so much the
absolute magnitude of Civ which is of interest, but rather its variation
from one series to the other. In this respect, it is interesting to note that
the three approaches used to analyze the results give essentially the same
tendency. As the number of tests at either of the sampling levels is rather
small in some of the series, and as the ratio C~ takes into account the
variation of strength with depth, it is believed that the averages computed
for both levels combined are more representative and should be used for
the comparison of the different series. Moreover, as the three approaches
are equally justifiable and show essentially the same tendency, the overall
averages of the values of the three different approaches may be used for
the sake of simplicity in the discussion; these averages are given at the
bottom of Table 2.
Discussion--It is seen that the same strength values are obtained from
the unconfined compression tests in both Series A and B; in both cases,
the samples were trimmed on the site, immediately after sampling, thus
preventing water migration from the disturbed zone to the undisturbed
core of the sample. As the compression tests were made on the field for
O
w
r-
T A B L E 2--Comparison of unconfined compression tests. m

tD
Series m
"u
A B C D
Sampling m
-u
Choice of Tests Level Na C/~ avg N C~ avg N C/v avg N C/~ avg
All tests upper 9 0.85 8 0.92 5 0.73 7 0.81 -t

lower 28 0.87 6 0.87 6 0.81 20 0.84 5
both 37 0.87 14 0.90 11 0.78 27 0.83 z
-i"1
Statistical upper 8 0.78 5 0.88 3 , 0.73 4 0.81 O
lower 15 0.95 4 0.83 3 0.82 14 0.84
both 23 0.89 10 0.85 6 0.77 19 0.85
Best tests upper 4 1.14 4 1.17 3 0.85 4 1.01 O
lower 14 1.12 3 1.14 3 0.86 10 1.06
both 18 1.12 7 1.16 6 0.85 14 1.05
O
Overall average both 0.96 0.97 0.80 0.91
-<
aN is the number of test results used to c o m p u t e the corresponding average value of Cir. --I
m
-I
Series A and in the laboratory for Series B, the identical results confirm
that the testing conditions were comparable. The strength values obtained
in Series C are appreciably lower, by about 17 percent, than in Series A
and B; in this case, the samples were extruded and paraffined on the field,
and they were trimmed only one week later, just before being tested in
the laboratory. Thus it would seem that under the conditions of complete
stress release, and given sufficient time, the undrained strength may be
affected by water migration within the sample. However, if the con-
fining stresses are not released completely, the effect on the strength does
not seem to be as important. This is illustrated by the fact that the
strength measured in Series D is only about 5 percent lower than in Series
A and B and about 12 percent higher than in Series C; in Series D, the
samples were left in the stainless steel tubes and stored in the humid room
for two weeks or more before being tested. It should be noted that the
internal clearance ratio of the tubes is very small, on the order of 0.25
percent, and could then efficiently confine the samples.
These data show a strong indication that the strength of a clay sample
decreases appreciably in a short time after sampling, when stored under
conditions of complete stress release; following the observations made by
other authors [1,2], it is reasoned that water migration within the sample
might be responsible for that decrease.
Water Content Measurements

It may be possible to check whether water migrates within a soil sample
by measuring the water content in a cross section of the cylindrical
sample. This was attempted by cutting 2 cm-thick discs from samples
and taking the water contents on the outer 1-cm ring (Wo), on the central
3-cm-diameter core (we) and on the intermediate ring (wi). These measure-
ments were made on samples which had just been extruded from their
tubes and on samples which had been stored for a certain time after
extrusion. The water content measurements are given in Table 3, together
with the history of the samples. When comparing the water contents
of the core and of the outer ring, A(wc - Wo), it can be seen that there
is no consistent tendency for the core to have a higher water content.
However, it is interesting to note that, in the case of the samples which
have been stored for two to three years after being extruded from their
tubes, the water contents of the intermediate rings are all higher than in
the outer rings and, except for one case, also higher than in the central
core.
It would then seem that, under conditions of complete stress release,
a measurable migration of water from the outer more disturbed zone
towards the center o f the sample takes place, but that it does not affect
the core as much as the intermediate zone. If this is confirmed by further
CO
6o
0
t--
co
TABLE 3--Water content measurements across samples (from Saint-AIban).
nl
Dates o f Water
rrl
Tube No. Depth, m Sampling Extrusion Content Wo~ a(w~ - Wo) wi a A(w, - w~) w~a A(wc - wo) z
..~
N' 6.1 21/0 6/ 74 24/06/74 24/06/74 69.2 -1.5 67.7 -0.6 67.1 -2.1
m
67.7 -0.6 67.1 +0.7 68.8 + 1.1
M 2.1 21/06/74 24/06/74 24/06/74 66.8 -0.8 66.0 +0.9 66.9 +0.1
62.5 +0.4 62.9 -0.6 62.3 -0.2 -t
M' 6.1 21/06/74 13/07/74 13/07/74 70.2 0.0 70.2 -0.3 69.9 -0.3 z
69.3 +0.5 69.8 + 0.3 70.1 + 0.2
C-4-6 4.0 20/1 0/ 72 29/ 01 /73 07/ 01/ 75 73.3 + 0.3 73.6 +0.6 74.2 +0.9
. . . . . . 70.3 -0.6 69.7 . ..
C-26-5 5.6 12/09/72 18/10/72 07/01/75 65.0 + 2.2 67.7 - 1.3 66.4 + 1.4
51.1 + 0.3 51.4 - 1.9 49.5 - 1.6
B-12-G 4.3 05/06/73 12/06/73 07/ 01/ 75 51.2 +0.9 52.1 -0.1 52.0 +0.8
-.I
51.5 +0.4 51.9 - 1.8 50.1 - 1.4 0
-<
awo = water content o f the outer 5-mm ring, we = water content o f the 3-cm-diameter central core, and ..q
wl = water content o f the intermediate ring. t'rl
6o
---I
studies, it would constitute an additional argument in favor of the use of

larger diameter tube samplers.
Influence of Reconsolidation
It is generally agreed that the detrimental effect of water migration and
of some limited sampling disturbance may be remedied partly by recon-
solidating the samples to the in situ stresses [2]. The beneficial effect
of reconsolidation is twofold: first, it squeezes out the excess water
resulting from swelling, and second, it restores the effective stresses
which were acting in the soil element in nature.
The main difficulty of such a procedure lies in the choice of the correct
stress values corresponding to the field stresses. In order to do so, the
value of the coefficient of earth pressure at rest, Ko, should be known;
however, that coefficient remains one of the most elusive parameters of
clay deposits. Many methods have been suggested for the determination
of the Ko values; a recent study [14], comparing different methods of
Ko measurements made on the clay deposits of Salnt-Alban, has shown
that the Ko value may be taken anywhere between 0.4 and 1.2, a probable
lower limit being 0.56.
For the purpose of studying the influence of reconsolidation on the clay
of Saint-Alban, three types of tests were made:
1. Unconsolidated undrained (UU) tests under confinement pressures
equal to half the total vertical overburden pressure.
2. Isotropically consolidated undrained (CIU) tests, with isotropical
consolidation pressures equal to 0.8 times the vertical effective overburden
pressure.
3. Anisotropically consolidated undrained (CAU) tests, with vertical
and horizontal consolidation pressures equal to 1.0 and 0.56 times the
vertical effective overburden pressure, respectively.
In the CIU tests, the consolidation pressures were kept below the
vertical effective overburden pressure to prevent any overstressing of the
clay structure [15] which could affect greatly the strength parameters.
For the CAU tests, a K value of 0.56 was arbitrarily adopted, as this
value corresponds to the modified [16] Jaky's expression (0.95 - sin
d~r'), where ~,' is the friction angle measured on remolded clay. All
tests were made at the same controlled strain rate of 0.3 mm/min.
From the results given in Table 4, the following observations may be
made:
1. The UU tests give strength values (C~, Table 4) which are generally
higher than those obtained by unconfined compression tests (C~, Table
2).
TABLE 4---Influence o f reconsolidation.
Type of Test Sampling Level No. of tests AVJV, % et, % Cs~

UU upper 3 ... 3.10 1.19
lower 4 ... 0.92 1.46
CIU upper 4 4.1 1.60 1.89
lower 4 1.2 1.00 1.99
CAU from 2.3 m
(K = 0.56) to 6.4 m 4 2.2 0.87 1.45
2. The anisotropic consolidation under K = 0.56 does not seem to

improve appreciably the measured strength; this may possibly indicate
that the actual value of/to is higher than 0.56.
3. The CIU tests give strength values which are considerably higher
than the values obtained by UU tests and are nearly twice the vane
strength. The stress-strain curves for UU and CIU tests are compared
in Fig. 3; it can be seen that both the peak strength and the rigidity are
improved.
II
~o
8
_o
x
o 7
13_
~6
b
J
b-~
o
o 2 4 6 8 I0 12
E,deforrnation,%
FIG. 3--Comparison o f UU and C I U tests.
Discussion--From these results, it is evident that a reconsolidation in

the isotropical conditions restores the strength to an appreciable degree.
Questions may be raised as to the significance of the fairly large change
of volume (AVJV) encountered during consolidation (Table 4) when
compared to the small amount of water migration observed. However,
the increase of strength, which may seem quite important, is not outside
the order of magnitude of the undrained strength, which is expected
on these soils, when compared to the vane strength. Previous studies [6],
have shown that the undrained strength obtained by compression tests,
U or UU tests, on good quality samples amounts to 1.5 times the value of
the vane strength measured at the elevation of the samples, or more.
Hence, it should be realized that these observed differences between UU,
CAU, and CIU results for cemented clays are due to the fact that the
clay structure has suffered from the sampling operation. For good
quality samples, such differences may not be so evident; this is illustrated
by the results of UU and CAU tests (Fig. 4) made on samples which
T
_0
x
0 2 4 6 8 I0 12
~, d6formation, %
FIG. 4--Comparison o f UU and CA U tests on good quality samples.
have been taken by means of a new tube sampler developed at Laval

University. It is seen that the stress-strain curves are comparable, and
the undrained strengths measured for the CAU and UU tests are
1.80 and 1.85 times the vane strength, respectively. Although all these
results emphasize the importance of good sampling techniques, they also
show that it is possible, after sampling, to restore part of the characteristic

of brittleness in the sensitive cemented clays, provided that the clay
structure has not been affected too much.
It should be emphasized that this testing program has been performed
on the clay of Saint-Alban, which is among the least cemented clays
encountered in the Saint-Laurent lowlands, as may be appreciated from
the values given in Table 1. The detrimental effect of water migration
and stress release should normally be less pronounced in more intensely
cemented clays; however, no data are available to confirm that assertion.
Influence of Storage Time

The influence of storage time on the characteristics of undisturbed soil
samples is of some importance for research or even commercial labora-
tories which get involved in long-term testing programs. Unfortunately,
very little is known of that influence on the sensitive cemented clays.
Bozozuk [17] has reported a reduction of 4.8 percent of the precon-
solidation pressure in samples of the sensitive clay from the Ottawa
Sewer Plant, after 17 months of storage; no data are available on the
variation of the strength with storage time.
In the present testing program, compression and consolidation tests
were made on block samples taken from two sites and stored for long
periods of time. Block samples were preferred to tube samples for such
a study because the tests are reproducible with very small dispersion,
and, if the blocks are properly wrapped and stored in a humid room, no
water migration should take place and affect the test results appreciably.
For such samples, it was thought that any change in the strength of con-
solidation characteristics would result in a chemical change, which would
mainly affect the cementation bonds.
The typical properties for the clay of these two sites, Saint-Louis
and Saint-Jean-Vianney, are given in Table 1. In both cases, the block
samples were cut from a trench dug in the craters of landslides; they were
wrapped in plastic sheets, sandwiched between layers of a mixture
of paraffin and vaseline, and were transported on a foam mattress to
the laboratory, where they were kept in a humid room at a temperature
of 70~ and a relative humidity of 95 percent. There were occasional
failures of the climatizing apparatus of the humid room, which resulted
in spells of three to five days with a temperature of 75 ~ and relative
humidity of 60 percent. The sample from Saint-Louis has been stored
for more than six years and that from Saint-Jean-Vianney for more than
three years. The first test on the Saint-Louis blocks were made five
months after sampling, and on Saint-Jean-Vianney blocks, within six
weeks after sampling.
From the data available from adjacent blocks taken at the same time,
no noticeable change in the water content could be detected after these

long periods of storage. It was observed that a green moss had formed
on the face of the blocks under the paraffin; consequently, a 2.5-cm-thick
layer of soil was removed from the faces of the blocks before cutting the
test specimens. All cutting and trimming operations were made by a thin
wire saw.
Undrained Strength
In order to examine whether the undrained strength has been affected
by the long period of storage time, CIU tests were performed under
exactly the same testing conditions as similar tests which were made on
adjacent blocks, within a few weeks after sampling. The CIU tests were
chosen, as they are considered to be an efficient means of evaluating the
intensity of bonding in cemented clays [4,6,18]. From the comparative
results given in Table 5, the following observations may be made:
1. The change of volume during consolidation has increased con-
siderably and has more than doubled in some cases; this may be indicative
of a certain weakening of the clay structure.
2. The deviator stress at failure (ol - o3)t has decreased by 10 to 15
percent for Saint-Louis clay and by 14 to 21 percent for Saint-Jean-
Vianney.
3. The strain at failure ~r has increased appreciably in the case of Saint-
Louis but not in the case of Saint-Jean-Vianney.
4. The pore pressure generated by shear deformation has a tendency
to be lower at failure for the Saint-Louis clays.
Figure 5 gives the stress-strain and pore pressure curves obtained from
CIU tests performed on block and tube samples after five months of
storage by Lefebvre [19] and on block samples after six years of storage;
this comparison indicates that the effect of storage is somewhat similar
to the disturbance resulting from tube sampling but not as severe.
Consolidation Characteristics
The consolidation characteristics, and especially the preconsolidation
pressure pc, may be considered as an indication of the presence of cemen-
tation bonds in the sensitive clays, where the magnitude of pc is appreciably
larger than the maximum load which has ever been carried by the soil
element. The consolidation curves of cemented clays are characterized
by a well-defined knee at pressures corresponding to Pc; the better the
sample quality, the more pronounced the knee. Hence, any appreciable
change in the shape of the consolidation curve and in the value of Pc
would be an indication of alteration or disturbance of the soil sample.
...g
4~
PO
Oo
o
r'-
Go
-o
m
o_
TABLE 5--1nfluence o f storage on CIU tests. m
z
Date of Date of (ol - oa)j, "10
20
Site Sampling Test oo ', kPa AVJV, % kPa eI, ~ u/, kPa m
"1o
1969 69 0.3 132 0.9 48 2o
1974 69 0.7 112 1.5 35 --I
Saint-Louis summer 1969 83 -- 131 1.1 56 6
1968 1974 83 2.3 112 1.3 32 z
1969 103 1.7 129 1.0 60
1974 103 2.6 116 1.2 56 8-n
1971 103 1.1 703 0.7 101
1974 103 1.3 554 0.8 85
Saint-Jean-Vianney summer 1971 345 1.1 831 1.0 258 O
1971 1974 345 2.6 712 0.8 255
1971 483 1.4 931 0.6 310 --4
O
1974 483 3.4 777 0.7 331
-<
"-4
t'tl
0~
--4
T~
fi)
LA ROCHELLE ET AL ON STORAGE A N D RECONSOLIDATION 143
200
I
ST-LOUIS
180
I
160
140
n~ 12o
-~ moo
g
_L ;I =L~..~ . . . . .
',F I _..-
b-
60
4t'
IJ--; h / ~ -
40
20
g ,
lq~,c~ClU (block)
' v-'~CIU(tube)
(C~_O-3)Au
o
o
9
9
1974 CIU(block) = ,L
0 I I
0 I 2 3 4 5 6
e, deformotlon,%
FIG. 5--Comparison between CIU tests on block sample after storage with C I U tests
on block and tube samples made after sampling by Lefebvre [19].
Consolidation tests were made on the block samples of Saint-Louis

and of Saint-Jean-Vianney after prolonged periods of storage, and the
results were compared with those obtained from initial tests made within
a few weeks or months after sampling. As illustrated by the data given
in Table 6, the values of pc have not changed during storage on either
site. The consolidation curves remain essentially of the same shape as may
be observed from the comparison of curves given in Fig. 6 for Saint-Jean-
Vianney.
Discussion--It thus seems that storage affects the strength character-
istics of the cemented clays but has no influence on the consolidation
characteristics. This paradoxical behavior may be explained by an adequate
clay structure model and is not inconsistent with previous observations
[6], in that limited sampling disturbance of cemented clays decreases the
strength of the samples but has no influence on the value of pc. The
observation that Pc is not affected by storage is contrary to previous
findings by Bozozuk [17], who has found a decrease of 4.8 percent on
samples which have been stored for 17 months; it should be noted,
however, that tube samples were used by Bozozuk, and, again, this may
show the importance of obtaining good quality samples for long periods
of testing. Obviously, these results imply that the samples should be
tested as soon after sampling as possible, especially if shear strength
parameters are to be determined.
TABLE 6--Influence of storage on the preconsolidation pressure.
Preconsolidation
Date of Pressure-pc,
Site Sampling Date of Test No. of Tests kPa
Saint-Louis 1969 1969 3 164

1969 1974 2 164
Saint-Jean-Vianney 1971 1971 6 900
1971 1974 2 900
1.4
1.5
1.2
I.I
o
>o
I0
09
0.8
0'75 6 789 2 3 4 5 6 789 2 3 4 5 6 789 2 3

I0 I00 I000
pressure, kPo
FIG. 6----Comparison of consolidation curves from block samples before and after storage
period.
Conclusion
The present paper is a report on a study o f the influence o f recon-
solidation and storage time on the strength and consolidation character-
istics o f sensitive cemented clays from eastern Canada. From the data
presented, the following tentative conclusions are suggested.
1. In the case of tube samples of soft and weakly cemented clays, a

decrease of undrained strength on the order of 15 percent takes place
during the first "few days after sampling, under conditions of complete
stress release.
2. The decrease of strength may possibly be attributed to water migration
from the disturbed outer zone of the sample towards the central part.
From the water content measurements across samples, it is reasoned that
larger diameter samplers would attenuate this detrimental effect. It is also
suggested, pending further studies, that, in more strongly cemented clays,
the effect of water migration might not be as pronounced.
3. The reconsolidation of samples under the field stresses does restore
at least part of the lost strength and rigidity. However, it is also shown
that, on good quality samples, the effect of reconsolidation is negligible.
4. During long periods of storage in humid rooms, block samples of
medium and strongly-cemented clays have suffered a reduction of undrained
shear strength on the order of 10 to 20 percent. However, the preconsoli-
dation pressure and the general shape of the consolidation curve have not
been affected by storage.
Many of the observations presented in this paper stress the detrimental
effect of sampling disturbance and the importance of obtaining good
quality samples for elaborate programs of testing.
Acknowledgments
The field and laboratory work reported in this paper were carried out
by J. Sarrailh, graduate student. The help of J. P. Dussault, J. Y. Julien,
S. Par6, and M. Pouliot, technicians, is appreciated greatly. This investi-
gation was carried out with the financial support of the Ministry of Edu-
cation of the Province of Quebec and the National Research Council of
Canada.
References
[1] Hvorslev, J., "Subsurface Exploration and Sampling of Soils for Civil Engineering
Purposes," Waterways Experiment Station, Vicksburg, Miss., 1949, pp. 163-164.
[2] Bjerrum, L. "Problems of Soil Mechanics and Construction on Soft Clays," State-
of-the-Art Report to Session IV, 8th International Conference on Soil Mech~ics and
Foundation Engineering, Moscow, Vol. 3, 1973, pp. 1l 1-159.
[3] Crawford, C. B., Geotechnique, Vol. 13, No. 2, 1963, pp. 132-146.
[4] Conlon, R. J., Canadian Geotechnical Journal, Vol. 3, No. 3, 1966, pp. 113-144.
[5] Mitchell, R. J., Canadian Geotechnical Journal, Vol. 7, No. 3, 1970, pp. 297-312.
[6] La Rochelle, P. and Lefebvre, G. in Sampling of Soil and Rock, ASTM STP 483,
American Society for Testing and Materials, 1971, pp. 143-163.
[7] Sangrey, D. A., Geotechnique, Vol. 22, No. 1, pp. 139-152.
[8] Tavenas, F. A., Chapeau, C., La Rochelle, P., and Roy, M., Canadian Geo-
technical Journal, Vol. 11, No. 1, 1974, pp. 109-141.
[9] La Rochelle, P., Trak, B., Travenas, F. A., and Roy, M., Canadian Geotechnical
Journal, Vol. 11, No. 1, 1974, pp. 142-164.
[10] Bjerrum, L., Geotechnique, Vol. 17, No. 2, 1967, pp. 83-119.
[11] Lefebvre, G. and La Rochelle, P., Canadian Geotechnical Journal, Vol. 11, No. 1,
1974, pp. 89-108.
[12] Tavenas, F. A., Chagnon, J. Y., and La Rochelle, P., Canadian Geotechnical
Journal, Vol. 8, No. 3, 1971, pp. 463-478.
[13] La Rochelle, P., discussion on the State-of-the-Art Report to Session IV, 8th Inter-
national Conference on Soil Mechanics and Foundation Engineering, Vol. 4.2, Moscow,
1973, pp. 102-108.
[14] Tavenas, F. A., Blanchette, G., Leroueil, S., Roy, M., and La Rochefie P., "Dif-
ficulties in the In Situ Determination of Ko in Soft Sensitive Clays," Specialty Con-
ference on In Situ Measurement of Soil Properties, American Society of Civil Engineers,
Raleigh, N.C., June 1975, Vol. 1, pp. 450--476.
[15] Raymond, G. P., Townsend, D. L., and Lojkasek, M. J., Canadian Geotechnical
Journal, Vol. 8, No. 4, 1971, pp. 546-557.
[16] Brooker, E. W. and Ireland, H. O., Canadian Geotechnical Journal, Vol. 2, No. 1,
1965, pp. 1-15.
[17] Bozozuk, M. in Sampling of Soil and Rock, A S T M STP 483, American Society for
[18] Lo, K. Y. and Morin, J. P., Canadian Geotechnical Journal, Vol. 9, No. 3, 1972,
pp. 261-277.
[19] Lefebvre, G., "Contribution h l'~tude de la stabilit6 des pentes dans les argiles
ciment6es," Ph.D. thesis, Universitd Laval, Qu6bec, Canada, 1970.
J. K. Torrance'
Pore Water Extraction and the Effect

of Sample Storage on the Pore Water
Chemistry of Leda Clay
REFERENCE: Torrance, J. K., "Pore Water Extraction and the Effect of Sample
Storage on the Pore Water Chemistry of Leda Clay," Soil Specimen Preparation for
Laboratory Testing, ASTM STP 599, American Society for Testing and Materials,
1976, pp. 147-157.
ABSTRACT: In recent years, the potential significance of chemical and mineralogical

influences on the behavior of the post-glacial marine clays has been increasingly
recognized by the soils engineering community. The precise relationships are not
known, but it seems probable that, in some cases, small differences in chemical
factors may explain the differences in behavior between otherwise similar samples. In
connection with an investigation of these relationships, the experiments reported in
this paper were undertaken to examine the magnitude of chemical change which may
occur in low-salinity Leda clay during periods o f storage. Pore water extraction de-
vices are described, and the effects on the pore water chemistry of three months
storage, under a variety of standard and modified storage procedures, are reported.
It is concluded that none of the storage procedures tested is entirely satisfactory, in
that potentially significant changes in the pore water chemistry occurred. Finally, it is
recommended that pore water chemistry be assessed more often than is the present
practice when soils engineering tests are performed on Leda clay and that this be done
as soon as possible after the sample is obtained from the field.
KEY WORDS: soils, tests, clays, water chemistry, moisture content, storage pro-
cedures
In most soils engineering studies, it is considered sufficient, in addition

to the standard engineering measurements, to describe the geological origin
of the material, certain physical properties such as texture and density,
and the dominant minerals present. Rarely is any description of the
chemical state of the soil system included. This is acceptable for many soil
materials, but there are instances where the lack of chemical information
may lead to incomplete understanding of results or to misinterpretation.
An example of the latter possibility occurs when one is working with the
'Associate professor, Department of Geography, Carleton University, Ottawa, Ont.
Canada.
147
Downloaded/printed by ASTM International www.astm.org
Copyright 9 1976by
post-glacial marine clays. The influence of chemical factors on marine

clay behavior has been examined in Norway by various investigators work-
ing at the Norwegian Geotechnical Institute [1-3]. 2 In Canada, the main
work to date has been published by Penner [4], Sangrey and Paul [5], and
Torrance [6].
Bjerrum [1] found that, for the Norwegian marine clays, a relationship
exists between the sensitivity and the salinity; namely, the sensitivity in-
creases as the salinity decreases. In these materials, it also has been
found [2,3] that relatively small differences in the concentrations of certain
ions, at low but essentially constant pore water salinity, can explain dif-
ferences in behavior between otherwise similar soils. The investigation of
the role of chemical factors in the Canadian Leda clay has been less exten-
sive. Penner [4] observed a relationship between electrokinetic potential
and sensitivity for the Leda clays and noted that certain chemicals added
to the soil affected its behavior. Sangrey and Paul [5] investigated the in situ
pore water chemistry at sites in the Ottawa area and suggested that the
sodium/calcium ratio in the pore water was an index of the depositional
origin of the material and its susceptibility to a certain type of landslide.
Further work at the Geotechnical Science Laboratories at Carleton Univer-
sity in Ottawa has extended these investigations and has shown, for individ-
ual samples of Leda clay, that a salinity-sensitivity relationship exists,
similar to that observed in Norway [6]. The relationship, however, may
vary greatly from one sample to another. These differences are thought to
be related to other differences, that is, physical, mineralogical, and chem-
ical, between samples. It was noted that, as in Norway, the various cations
have different effectiveness in altering the soil behavior. It also has been
found that the soduim/calcium ratio is inadequate as an index of origin
since it depends on both the depositional origin and the degree of leaching
and weathering of the Leda clay [7].
The problem of determining the importance of chemical factors in Leda
clay is Complicated by the extreme variability of other factors known to
influence its behavior. Experiments to date indicate that the relationships
to be expected, at least for certain variants of Leda clay, will follow a
pattern similar to that observed in Scandinavia. Among the most interesting
of the Norwegian findings is the effect of low concentrations of various
ions on the soil behavior [2,3,8]. If similar effects are important in Canada,
then, in view of the nonuniformity of Leda clay, care must be taken to
obtain the most reliable chemical information possible. In many engineering
investigations there is a period of storage, usually under controlled condi-
tions, before the laboratory investigation is undertaken or before all tests
are completed. This storage period represents a time during which chemical
changes may occur within the sample. The present investigation was under-
2Theitalic numbers in brackets refer to the list of referencesappended to this paper.
TORRANCE ON PORE WATER CHEMISTRY OF LEDA CLAY 149
taken to determine the possible magnitude of changes in the pore water

chemistry of a low-salinity Leda clay during storage under a variety of
conditions.
Soil Material
The soil material used in this investigation was taken in September 1974
from the site of the landslide of May 1973, north of Chelsea, Quebec. The
Shelby tube samples were taken by hand from the base of the scarp at the
side of the landslide scar. All samples were obtained from 10 to 12 ft below
the surface and from an area measuring approximately 1 by 3 ft. The
natural water content of the soil was normally between 55 and 65 percent
(although higher and lower values were observed), the liquid limit ranged
from 37 to 41 percent, and the plastic limit from 21 to 25 percent. Sensi-
tivity, determined by the fall cone method, was between 10 and 20. This
low value for the sensitivity was the result of the soil material coming from
a near-surface location, in which it had been mildly affected by weathering.
This weathering has caused an increase in the remolded shear strength.
Storage Procedures
Standard storage techniques and some modifications of standard methods
were tested to assess the amount of change which occurred in the pore
water chemistry. The following storage procedures were used:
1. Left in the original Shelby tube.
2. Aluminum foil wrapped and waxed.
3. Plastic film wrapped and waxed.
4. Waxed only.
5. Extruded and placed in sealed plastic container with a nitrogen
atmosphere.
6. Extruded, wrapped in plastic film, and placed in a sealed plastic
container with a nitrogen atmosphere.
7. Extruded, and placed in a sealed plastic container with an air
atmosphere.
For all treatments except Treatment 1, the soil was extruded from the
sample tube Within four days of sampling.
Four inch samples of soil were used in each test. Before being prepared
for storage, a slice of soil was taken along the full length of each segment.
The surface of this slice, which had been in contact with the tube, was
removed by scraping, and the remainder was subdivided lengthwise to allow
water content determination on one portion and pore water extraction
from the other. This procedure allowed the initial water content and pore
water chemistry of the sample to be determined for comparison with the results
obtained after storage.
Samples prepared in the manner described were stored under conditions
o f room temperature (20~ and under conditions of high humidity at a

temperature approximating the mean annual temperature of the sampling
site (7 ~ Treatment 1 was carried out only under the latter conditions.
The storage period reported in this paper was three months. While longer
duration storage periods are being studied, three months is considered
applicable to most commercial situations and is, therefore, of practical
interest.
Pore Water Extraction

The quality o f a pore water sample depends on the method by which it
is obtained. Pore water extraction apparatus should meet certain basic
requirements as to the amount of pressure that can be applied, and, at the
same time, evaporation of water from the soil during extraction and from
the extract while it is being collected should be minimal. Two different
devices which are used in our laboratories to extract pore water from Leda
clay will be described. The choice o f device depends mainly on the remolded
shear strength of the soil.
When samples with a remolded shear strength below approximately
0.5 t o n / m ~ are encountered, an air-activated pore water press has proven
satisfactory (Fig. 1). This device consists o f a plastic sample chamber into
which a disturbed sample of the soil is placed. At one end, there is a 1 mm
pressure applied f r o m air c y l i n d e r
tcm
I I
/ I/
-metal top plate
-rubber gasket
- dental dam
- s a m p l e chamber
-connecting bolt
-protective filter paper
-fine-pored filter paper
. . . . . . . . . . . . . . . . plastic outflow tube
T
to test tube
FIG. l--Air-activated pore water press (schematic).
diameter opening which, during operation, is covered by a fine-pored filter

paper. This, in turn, is protected physically by one or more standard filter
papers. A fine plastic tube (as used with atomic absorption photometers)
is connected to the opening and leads to the collecting test tube. The other
end of the chamber is covered by a thin rubber membrane (dental dam)
and a rigid top plate (which is fitted with connections to allow application
of air pressure). A rubber gasket between the dental dam and the top plate
has been found to lengthen the membrane life. The apparatus is assembled
and pressure applied (slowly at first to prevent puncture of the filter paper)
from a cylinder of compressed air. The thin rubber membrane applies
pressure to the sample, while preventing the air from passing through the
sample and evaporating an unknown quantity of pore water. The present
apparatus resists air leakage for pressures up to 6 to 7 atm. If the sample
chamber which measures 1 in. depp by 2 in. diameter is half full or more,
1 to 5 ml of pore water can be usually obtained in less than 1 h. This
apparatus in inexpensive and fast, and it is possible to use the same air
cylinder to apply pressure to a number of sample chambers simultaneously.
When pore water is required from stiffer samples, a mechanical pore
water press is used (Fig. 2). The design is a minor modification of a pore
water press that the author first saw in operation at the Norwegian Geo-
technical Institute. The soil chamber is constructed of steel, the 1-mm-
diameter exit is protected by layers of filter paper, and pressure is applied
to the disturbed soil sample through a steel piston. This device is slow to
operate but is necessary with stiff samples and in cases when only a small
amount of soil is available.
The concentrations of sodium, calcium, magnesium, and potassium in
the extracted pore water were determined using a Jarrell-Ash atomic ab-
sorption spectrophotometer.
Results and Discussions

The concentrations of sodium, calcium, magnesium, and potassium found
in the pore water and the water contents at the start of the experiments
and those found after three months storage for each treatment are presented
in Table 1. The results show that considerable change in the pore water
chemistry can occur over this time period. The differences in water con-
tents before and after storage create a problem in making comparisons with
the aluminum foil wrapped and waxed samples at 7 ~ and with the waxed
only samples at both temperatures. In these cases, the data suggest that
significant water loss occurred during storage. The samples, however,
showed no visual evidence of major water loss, and it seems probable that
the differing water contents before and after storage represent, in large
measure, natural water content variations. The substantial increase in
water content for one of the plastic wrapped and waxed samples and the
i 1 cm I
~. . . . . . . . . . . . . plunger
[ ~'~::'J" . . . . O-rings
......... sample chamber
.......... protective filter paper

~ ~----i~------fone'iP;~ ed f'lter paper
............... plastic outflow tube
FIG. 2--Mechanical pore water press--all materials are steel unless otherwise indicated.
TABLE l--Chemical analysis of pore waterfor Leda clay samples from Chelsea, Quebec at beginning of experiments and after three months storage.
Water Content, o7o Na Ca Mg K :~

"In
2:
Storage 3 3 3 3 O
Tempera- 3 Initial, Months, Change, Initial, Months, Change, Initial, Months, Change, Initial, Months, Change, ITI
Treatment ture Initial Months ppm ppm ~ ppm ppm 07o ppm ppm ~ ppm ppm ~ 0
z
Shelby tube, ends waxed (4 49.6 18.8 48 26 40
"o
samples from tube) 48.7 19.5 57 31 33 0
7 70.5 16 to 34 22.5 14 to 25 55 7 to 12 27 17 to 22 31 ~o
64.2 16.5 36 15 24 m
Aluminum foil, waxed (dupli- 7 57.5 48.4 24 20 -17 23 28 22 9.7 13 34 19 20 5

cate samples) 20 57.1 45.0 16 49 200 21 72 240 10 41 310 17 33 95
53.0 51.3 23 35 52 18 25 39 8.2 12 45 19 17 - lO m
58.4 61.4 16 56 250 14 21 50 7.9 13 65 17 18 6
0
Plastic wrapwaxed(duplicate 7 55.5 50.3 24 45 88 18 30 67 7.2 12 67 20 32 60 I
samples) 20 55.1 50.9 29 21 - 27 18 26 44 7.8 13 40 Ig 24 33 m
59.3 56.0 34 29 - 15 20 26 30 8.1 13 38 20 22 lO
Waxed 7 50.7 44.0 28 39 40 18 31 72 7.4 16.5 110 20 24 20

20 58.5 50.4 30 20 - 33 20 31 55 8.2 16 95 22 29 32 .<
Container N~ 7 58.0 58.7 18 27 50 23 129 460 11.5 93 7(30 20 49 145 0
64.2 65.5 20 34 70 17 107 530 8.2 67 720 19 48 150 "11
20
r-
Container, plastic wrap I',I2 7 58.7 57.1 22 20 -9 25 77 210 11 43 290 26 34 30 m
20 56.4 53.5 26 30 15 19 77 300 8.2 45 450 20 36 80 o
Container, air 7 51.9 49.4 34 32 -6 18 65 260 7.9 40 400 21 42 100 0

2O 55.8 49.9 24 61 150 22 107 390 11.5 68 490 21 42 100 r-
..k
ol
initial water content differences between samples support this interpretation.

In any case, the water content differences are insufficient to explain the
magnitude of the variations in pore water chemistry.
The chemical changes which occurred are not encouraging with regard
to the possibility of storing samples for anything but short periods without
the danger of unknown changes in total concentration and the concentration
of various elements. In most cases, the concentrations of all elements in
the pore water increased, and it should be noted that the percentage increase
was different for each element. It would appear that reactions occur
which attack the soil minerals to varying degrees. Any cation released from
the structure of the minerals would engage in cation exchange such that
the relative strengths of adsorption of these ions and those satisfying
exchange sites also influence the pore water concentrations that result. It
is the author's opinion that in no instances are the measured changes small
enough to ignore. Furthermore, the duplicates for the aluminum foil wrapped
samples and for storage in the Shelby tube indicate that the degree of
change is not necessarily consistent for identical or similar storage proce-
dures. With the paucity of information relating to the effect of chemical
factors on Leda clay behavior, it is not possible to state what degree of
change during storage should be considered an acceptable maximum.
The two most common methods of storing samples are (1) in the original
sample tube and (2) wrapped in aluminum foil and waxed. In Table l, the
pore water chemistry at four positions in the Shelby tube after storage for
three months are compared with the lower and upper limits of concentra-
tion found initially in all other samples. With the exception of sodium, all
concentrations observed after storage in the tube were considerably higher
than the maximum observed in any sample at the beginning of the experi-
ment. With the second common storage method, the samples wrapped in
aluminum foil, evidence of reaction (probably biologically aided) between
the foil and the soil sample was present in all samples, as was indicated by
discoloration of the foil. Additionally, in those aluminum foil wrapped
samples stored at 20~ there was a buildup of gas pressure within the
sample and a smell of hydrogen sulfide when the samples were opened. In
this case, the magnitude of the pore water chemistry changes varied con-
siderably for the duplicate samples at 7~ but the changes, with the
exception of sodium, were relatively small and consistent at 20~ Redox
potential measurements on the 20~ samples indicated that extreme reduc-
ing conditions had developed. Presumably, the reducing conditions enhanced
the stability of the minerals, thus decreasing the magnitude of change.
Despite the small chemical changes observed, it does not seem reasonable
to recommend a storage procedure during which the redox potential under-
goes major change.
It was hoped that the use of plastic wrap in place of aluminum foil
would eliminate these chemical reactions and decrease the magnitude of
University of British Columbia Library pursuant to License Agreement. No further reproductions auth
chemical change during storage. The improvement was marginal, but the
degree of change appears to be somewhat more consistent. Likewise, the
samples which were only waxed exhibited considerable change, some of
which may be attributable to water loss.
The other storage procedures tested all involved storage of the samples
in air-tight plastic containers. This types of storage might be used with
sample trimmings or with material after other tests have been performed.
In all cases, evaporation-condensation processes resulted in loss of water
from the soil (as evidenced by free water in the container), even though
water was not lost from the container. The wrapping of the sample in
plastic to inhibit water transfer and the presence of the nitrogen atmosphere
to inhibit oxidation reactions gave no improvement over storage with air.
With all the samples stored in the containers there was a dramatic increase
in the amount of calcium and magnesium in the pore water. The change
cannot be explained by the water transfer within the container and is prob-
ably related to attack on the carbonates which are present in the soil. Long
term storage in plastic containers cannot be recommended. It is not known
whether storage in sealed glass jars would be superior.
Conclusions and Recommendations

The conclusion drawn from these experiments is that, regardless of the
method of storage, chemical changes which will increase the concentrations
of most cations in the pore water can be expected to occur during storage.
The results of pore water analysis carried out after extended periods of
storage should not be expected to accurately represent the in situ chemistry
of that material. The best storage procedures, as indicated by least overall
change, are to extrude the sample and to wrap and wax it. The type of
wrap, aluminum, or plastic made little difference. Likewise, the tempera-
ture of storage was not particularly important, although it does not seem
reasonable to recommend any procedure where there is clear evidence of
biological activity. This last consideration means that aluminum-wrapped
samples should preferably be refrigerated. A temperature of 7 ~ which
represents the mean annual ground temperature at Ottawa, is not necessarily
the optimum storage temperature for inhibiting chemical change. Presumably,
lower temperatures would be better.
It has been found that the stability of sodium-montmorillonite increases
as the salinity of the surrounding water increases [9]. If this observation
can be applied to the marine clays, then it would be expected that the lower
the electrolyte concentration of the pore water, the greater would be the
degree of chemical change during storage. Thus, pore water chemistry
changes in high-salinity Leda clay during storage may be small, but the
dilemma exists that the low-salinity clays, which are the most susceptible
to change in behavior when the pore water chemistry changes, are the ones
that are most susceptible to chemical alteration during storage. Since the
precise relationship between s0il behavior and pore water chemistry for the
Leda clays has not been established, it must be assumed that these changes
in pore water chemistry during storage may be of importance.
Knowledge as to the role of chemical factors in Leda clay behavior is
limited. The relationships and interactions that occur between the various
chemical elements and the soil are complicated. Preliminary laboratory
investigations with chemical additions to Leda clay and investigations of the
in situ chemistry of Leda clay give promise of leading to a more complete
understanding of the behavior of this soil [6, 7]. Much more work is needed
on the relationships between chemical and physical factors and the soil
behavior as observed in the field and laboratory. In this regard, the author
recommends that more investigators assess the chemical, mineralogical,
and physical nature of the specimens that are tested. Pore water chemistry
investigations should take place as soon as possible after the sample is
obtained if in situ chemical information is desired. If research is being
performed, knowledge of the chemical state of the soil should be obtained.
The chemical investigations should be carried out at the beginning of the
experiment on a sample of soil immediately adjacent to the specimen tested
(to obtain initial chemical data), and on the specimen itself after the test
is completed (to determine if changes have occurred during testing).
The results presented in this paper suggest that pore water chemistry
should be assessed as soon as possible after the sample is obtained from
the field and that, if storage is necessary, the sample should be wrapped
with aluminum foil or plastic wrap and sealed with wax. It is preferable that
the sample be stored under refrigerated conditions. Evaporation of pore
water during and after extraction should be kept to a minimum. The
unpredictable and nonreproduceable nature of the chemical change during
storage must be emphasized.
Preliminary experiments with certain Leda clays and the experience from
Norway indicate that relatively small differences in pore water chemistry
can lead to differences in the remolded behavior of this type of soil. Only
with good chemical and engineering data on a large number of samples
can the actual relationships be determined.
A ckn o wledgm en ts
The author wishes to acknowledge the support of the National Research
Council of Canada and the assistance of L. Cowe in the laboratory portion
of this investigation.
References
[1] Bjerrum, L., Geotechnique, Vol. 4, 1954, pp. 49-69.
[2] Mourn, J., L6ken, T., and Torrance, J. K., Geotechnique, VoL 21, 1971, pp. 329-340.
[3] Moum, J, L6ken, T., and Torrance, J. K., Geotechnique, Vol. 22, 1972, pp. 675-676.
[4] Penner, E., Canadian Journal of Earth Science, Vol. 2, 1965, pp. 425-441.
[5] Sangrey, D. A. and Paul, M. J., Canadian Geotechnical Journal, Vol. 8, 1971, pp.
315-335.
[6] Torrance, J. K., Canadian Geotechnical Journal, Vol. 12, 1975, pp. 326-335.
[7] Torrance, J. K., "Leaching, Weathering, and Origin of Leda Clay in the Ottawa Area,"
Guelph Symposium on Geomorpholoty, in press.
[8] Torrance, J. K., Geotechnique, Vol. 24, 1974, pp. 155-173.
[9] Shainberg, I., Proceedings, Soil Science Society of America, Vol. 38, 1973, pp. 689-694.
D. A . Sangrey, ~ D. K. N o o n a n , 2 and G. S. W e b b 2
Variation in Atterberg Limits of

Soils Due to Hydration History
and Specimen Preparation
REFERENCE: Sangrey, D. A., Noonan, D. K., and Webb, G. S., "Variation in

Atterberg Limits of Soils Due to Hydration History and Specimen Preparation,"
ABSTRACT: Drying and rewetting of soils, as presently required in preparing ma-

terial for Atterberg limit tests, causes significant variation in the liquid limit. Once
dried, the rehydration of fine grained soils is time-dependent, requiring typically
several weeks rather than the one day period often used. More important are the
irreversible effects of drying many soils. Because so many applications of the Atter-
berg limit values are related to engineering problems of naturally moist soil, the limits
determined for nondried soil are more appropriate. It is argued that ASTM standards
should reflect this and recognize the ~vere changes brought about by drying. An
alternative method allowing testing of nondried soils should be added to the present
standards.
KEY WORDS: soils, tests, Atterberg limits, liquid limit, soil hydration, swelling, clay
minerals
"The liquid limit of a soil is the water content expressed as a percentage

of the weight of oven-dried soil, at the boundary between the liquid and
plastic states" (ASTM Test for Liquid Limit of Soils (D 423-66)). ASTM
specifications require that the soil to be used in determining the liquid limit
be a prepared dry sample (ASTM Dry Preparation of Soil Samples for
Particle-Size Analysis and Determination of Soil Constants (D 421-58
(1965)), although no specific time for rehydration of the air-dried soil is
defined except for check or referee tests. In these, 24 h of "seasoning" is
JAssociate professor, School of Civil and Environmental Engineering, Cornell University,

Ithaca, N.Y. 14853.
2Engineers, H. Q. Golder and Associates, Mississauga, Ont., Canada.
158
Copyright 1976byASTMIntemational www.astm.org
SANGREY ET AL ON SPECIMEN PREPARATION 159
specified, but no consideration is given allowing for variation in the liquid

limit due to differing times for rehydration.3
In contrast to this standard, there is ample evidence, [1-5] 4 both theo-
retical and observational, that soil consistency, particularly the Atterberg
limits, is significantly influenced by the degree of hydration of clay min-
erals. When air dried, these clay minerals will dehydrate to some degree,
and, when more water becomes available upon rewetting, the clays rehy-
drate. The dehydration-rehydration sequence is time dependent, and
achieving an asymptote to complete hydration may require more than one
month [4] for some clay minerals.
Other effects of the standardization procedure, such as chemical altera-
tion of the soil constituents and irreversible cementing by precipitates, can
also be noted [6-8]. This problem is particularly acute in tropical soils
containing compounds of iron, aluminum, and other metals which form
natural cements. The same factors influencing the formation and stability
of laterite will affect the preparation of these soils for classification tests.
It is reasonable to expect, and it has been demonstrated in a limited amount
of testing [6, 7], 5 that soil plasticity will be irrevisibly changed if the amount
or characteristics of cementing change. This factor may be as significant
in magnitude as dehydration but, in contrast, is a permanent effect. The
specific mechanism of plasticity change due to cementing is unknown. It
is probably due to the aggregation of small particles which act as larger
particles and the water holding capacity of cemented micro peds.
Methods of wet preparation of soil samples have been specified by
ASTM Wet Preparation of Soil Samples for Grain-Size Analysis and
Determination of Soil Constants (D 2217-66), although this specification
is not referenced in other ASTM classification test procedures. Two alterna-
tive methods of wet preparation are described, one from air-dried soil, the
second from naturally moist soil. Oven drying procedures are also used in
some soil preparation. However, these are not part of ASTM procedures
for specimen preparation.
Changes in soil properties might be acceptable if a standard for identifica-
tion were the only objective. For soil, however, the plasticity characteristics
3The association of water to a clay soil is very complicated. Some water is quite free and
mobile while other water is attracted, in varying degrees, to the clay particle. Still other
water is strongly a part of the clay crystal structure. As the water content of a soil changes,
especially as it is dried, all of the modes of associated water are affected, each to differing
degrees, depending on the conditions of temperature, water content, time, etc. Obviously the
detailed explanation of the results of this test program would involve this complicated
problem. However, the main point of this work is to describe the effects of drying. Empha-
sis on explanations for these effects, especially hypotheses about the reasons, is unnecessary.
For this reason, in the paper, the terms dehydration and rehydration will be used to cover
the entire spectrum of water content changes.
*The italic numbers in brackets refer to the list of references appended to this paper.
Communication of test results by S. G. Samuels, Building Research Station, England and
J. Pruntel, Cornell University, Ithaca, N.Y.
are recognized as not only a means of soil classification, but also a rela-
tively inexpensive method for estimating engineering characteristics of
strength and compressibility [9]. Since the engineering application usually
involves a naturally moist soil, it is reasonable to determine the liquid
limit working from natural water content rather than from air-dried soil,
as specified by ASTM. Certainly many engineering organizations and
laboratories are currently testing from the natural water content in spite
of the standard. It is also noteworthy that the British Standards Institu-
tion modified its original specification for liquid limit testing, which had
been similar to ASTM's, to one permitting either naturally moist or rehy-
drated soils [10].
Two separate questions are at issue here, each with its own implications
in terms of the present standards. The first is how long it takes for an air-
dried soil to rehydrate to some reasonably constant condition as far as the
liquid limit test is concerned. I f dehydration-rehydration is simply a re-
versible, but time dependent, phenomenon, and if it is desirable to test a
soil when more or less at equilibrium within this process, then it is suffi-
cient to specify a rehydration time long enough to reach this condition.
Such a rational is implicit in arguments like those of Winslow and Gates
[2] and the current check test procedure of ASTM Method D 423-66
where a specific 24-h rehydration time is specified.
A second question of perhaps even more significance is: to what degree
will soils respond irreversibly to dehydration; in which case, any length of
time for rehydration would not reproduce the natural soil behavior.
Test Program
In an attempt to answer these questions, series of tests were run in
which several different soils were subjected to drying and rewetting. The
liquid limits were measured over a period of up to two months time for
rehydration.
A summary of the characteristics of these soils is presented in Table 1.
Specimens 1 and 3 occurred naturally in deposits of marine or estuarine
silty clay in the Ottawa and St. Lawrence River systems of Eastern Canada,
respectively. They are representatives of the sensitive, naturally cemented,
Leda-type clays. Specimens 2 and 5 were from deposits of normally con-
solidated, post-glacial, varved fresh water lake clays; both were taken in
Eastern Ontario near to Kingston and New Liskeard, respectively. Specimen
4 was a lightly overconsolidated material from the Great Lakes basin near
Lake St. Clair, while the final specimen was of Cretaceous age Bearpaw
shale from Saskatchewan. The liquid and plastic limits listed in Table 1
were obtained by testing soils that had not been air dried but were wetted
directly from the natural water content.
Results of mineral analysis using X-ray diffraction are listed in Table 2.
{D
TABLE 1--Identification characteristics of soils tested.
Z
New Louis - Red Bearpaw m

..<
Parkway Liskeard ville Clay Kingston Shale
Specimen No. I 2 3 4 5 6
Liquid limit, ~ 69.5 34.2 74.0 24.5 42.4 95.0 r"

Plastic limit, 07o 30.3 18.8 27.5 16.9 22.3 27.6
0
Natural water content, 070 70.5 44.4 82.4 22.4 43.5 22.0 Z
Clay (< 2 gin), 07o 72 55 80 27 55 40
Silt (2/~m to 0.06 mm), 070 21 43 12 63 39 46 "13
m
070> 0.06 mm 7 2 8 10 6 14 _o
Activity 0.54 0.28 0.59 0.27 0.37 1.68
m
z
zlJ
m
"10
TABLE 2--Mineralogy of soils tested.
Specimen Abundant Clay Minerals MinorClay Minerals Other Minerals

1 mica group, vermiculite montmorillonite quartz, feldspar, amphi-
bole hornblende, cris-
tobalite
2 mica group vermiculite, chlorite same as 1
3 mica group, chlorite vermiculite same as 1
4 mica group, chlorite quartz
5 mica group chlorite, vermiculite same as 1
6 montmoriUonite,mica
group chlorite quartz
The soils were subjected to the same testing procedure. A portion of

each was air dried in a laboratory at average relative humidity of 55 percent
and temperature o f 22~ for a period o f seven days. Similar portions of
each were oven dried for a period of 20 h at 108~ The specimens were
then mixed throughly with enough water to bring them to approximately
the liquid limit determined from the original tests and listed in Table 1.
At time intervals beginning at 15 min after mixing and continuing at
roughly doubling increments thereafter, the liquid limits were determined
for each soil. The equipment and method o f testing used conformed to
the standards o f ASTM Method D 423-66 except for the method o f speci-
men preparation and the use of the Casagrande-type grooving tool. Between
test periods, the specimens were stored in a cabinet at a relative humidity
of >95 percent and a temperature of approximately 22~ The results of
these tests are presented in Figs. 1-6. The liquid and plastic limits, defined
by testing o f nondried specimens, are indicated on the left margin. Subse-
quent liquid limits for air and oven dried soils rehydrated for various
periods of time are also shown.
These results clearly indicate that the effects of rehydration time and
irreversibility were significant for the soils tested. Previous work on the
Atterberg limits, particularly that of Winslow and Gates, has concluded
that most rehydrating soils reach a practical assymptote after 24 h, but that
more active clay minerals, such as montmorillonite, may require several
days. The results of this study demonstrate that, even for very inactive soils,
24 h is insufficient and that liquid limit changes due to rehydration may
be significant for at least several weeks. It does appear that the time
required increases with activity, or at least that the changes are more
significant with the more active soils (for example, Bearpaw shale--No. 6.).
A second significant observation is that the drying of soils, either in
air or oven, does not necessarily lower the liquid limit, as is usually as-
sumed [1] and frequently referenced in textbooks. This test program showed
that, for three out of six air-dried and one of six oven-dried ones, the
initial liquid limit was higher than that determined from the nondried speci-
SANGREY ET A L ON SPECIMEN PREPARATION 163
70
wL
PARKWAY (LEDA CLAY)-AIR 9
60 PARKWAY (LEDA CLAY)-OVEN +--
z I & 9 9
LU 50 -
F- I I| "1" ? §
Z
0 I
o
r~ 40 -
hi
I--
<
30 =Wp
20-
t5 L I I
I I0 I00 I000
REHYDRATION TIME-HOURS
FIG. 1--Liquid limits measured for rehydrating Specimen 1, Parkway soil (note changes
with additional cycle o f drying of the oven dried soil after 60 h).
70
NEW LISKEARD CLAY-AIR 9
60 NEW LISKEARD CLAY-OVEN +
I
I.- 50
z
hi
I'--
Z
0 40
0
(Z:
ILl
NL ,, .I,.
I--
'< 30 4- 4, Ilk '1" '@ i 6 9 4. ;_
4- v
20
9Wp
15 I I I
I I0 I00 I000
FIG. 2--Liquid limits measured for rehydrating Specimen 2, New Liskeard clay.
80
LOUISEVILLE (LEDA CLAY)- AIR 9
-w L
70 LOUISEVILLE (LEDA CLAY)-OVEN +-
60
I-
Z
MJ 50
I.-
z
0
tt,- 4-0
I.LI
I,-
,<
30
wp
20
15
I I I 1
I IO I00 I000
FIG. 3--Liquid fimits measured for Specimen 3, Louiseville soil.
80
RED CLAY- AIR 9

70 RED CLAY-OVEN +
I 60
I,-
Z
WJ
l--
50
Z
0
0
Iv
40
I,LI
I.--
30
: +" 9 : $ $ ; : .
wL
20 m
--Wp
15 1 I I
I IO IOO I000
FIG. 4---Liquid limits measuredfor Specimen 4, red clay.
80
KINGSTON CLAY - AIR 9
70 KINGSTON CLAY -OVEN §
60
I
t-
z
LLJ 50
D--
Z
0
0
WL w ,~ 9 9 -
-
r~ 40
§ + + 4- I I I + +
p-
,<
30
Wp
20
15 I I J I
I I0 I00 I000
FIG. 5--Liquid limits measured for Specimen 5, Kingston clay.
150
130
I10
r
z
IJJ wL
I,- 90
Z
0
0
70
bJ
t.-
<
50
BEARPAW SHALE-AIR e"
BEARPAW SHALE-OVEN +
30
wp
I0 - - I I I I
I I0 I00 I000
FIG. 6--Liquid limits measured for Specimen 6, Bearpaw shale.
men. A similar observation was noted by Torrance [1] for a Norwegian

clay soil.
The question of irreversibility is the most significant one with respect to
drying of specimens for plasticity tests. If the effects of drying are not
reversible, then the soil has certainly experienced major structural change
and may be very different from the original material. The results of this
testing program clearly show that irreversibility is very common, perhaps
more common than not. Explanations for this probably involve several
phenomena.
The single effect most likely in the tests reported herein is irreversible
precipitation of natural cements from the soil or soil water [2]. Because
four of the six soils in this test program (No. 1, 2, 3, and 5) were of this
type, the results may not be representative of the percentages of all soils
which behave in this way. However, naturally cemented soils are extremely
common in some parts of the world, and organic material in almost any
soil could produce the same effect [3].
Low permeability is a second reason for irreversibility, or apparent ir-
reversibility, as demonstrated by the montmorillonitic Bearpaw shale (No.
6). This soil had a natural water content (22 percent) below its plastic limit
and was extremely overconsolidated. The liquid limit determined by
wetting of this soil directly from the natural water content was 95 per-
cent; however, with time, even this value changed, assuming an asymptote
to 109 percent only after several weeks of soaking and apparent rehydra-
tion, as shown in Table 3. That a soil can be dehydrated by large consoli-
TABLE 3--Changes in liquid limit for Bearpaw Shale, Specimen 6,

when hydrated from natural water content of 22 percent.
HydrationTime Liquid Limit, %

24 h 95.0
2 days 100.2
3 days 107.5
5 days 107.9
8 days 111.6
21 days 109.0
34 days 108.6
dation stresses even though remaining saturated seems obvious from these
data, and a rehydration time is necessary in order to ensure that some
consistent measurement of the liquid limit is possible. Because of the low
permeability of the Bearpaw shale, the time effects, whether rehydrating
air-dried, oven-dried, or nondried specimens, are so long that asymptotes

may well be impractical to define. As Fig. 6 shows, even after 55 days,
the liquid limit was still varying significantly for the Bearpaw shale.
Conclusions
There are important implications for the present standard of ASTM
Test for Liquid Limit of Soils (D 423-66) in light of the variabilities re-
viewed in this paper. Without question, it is important that a standard
method be as simple as possible and not require excessive time for speci-
men preparation or the test itself. If long time periods were prescribed,
they would, no doubt, be ignored by most testing groups. This would
seem to preclude a change in the present standard to allow for the hydra-
tion times of several weeks that appear to be necessary for most air-dried
soils.
If correlations between engineering behavior of natural soil and the
Atterberg limits are to be meaningful, then the irreversible changes
brought about by drying, as illustrated in most of the specimens tested,
are very significant. As reflected in the British Standards [10], the logical
solution to this problem is to prescribe testing of nondried specimens.
On the other hand, specimen handling and preparation is greatly simpli-
fied if the soil is dry. There may also be instances when it is desirable to
reduce soils to some common state by eliminating extraneous factors in-
herent in the natural material (although the author cannot imagine where
this would really be beneficial). In either case, a method of dry prepara-
tion such as ASTM D 421 is warranted.
In summary, it is necessary that the present standard for ASTM Test
for Liquid Limit of Soils (D 423-66) be changed to provide the option of
testing nondried soil specimens. Such a standard would require a descrip-
tion of the procedure of specimen preparation as part of the reporting of
the liquid limit. A similar change for the plastic limit, ASTM Test for
Plastic Limit and Plasticity Index of Soils, (D 424-59) (1965)) is probably
also justified.
Regardless of the method of test, it is important that engineers recog-
nize the variability of soils as they are dehydrated and rehydrated, es-
pecially with respect to the Atterberg limits. This is particularly important
when irreversible changes result.
Acknowledgments
An ASTM Grant-in-Aid award to the senior author, while on the Staff
of Queen's University at Kingston, supported part of the research re-
ported herein. The assistance of Dr. R. H. M. van de Graaff in soil
mineral analysis and interpretation is gratefully acknowledged.
References
[1] Casagrande, A., Public Roads, Vol. 13, 1932, p. 121.
[2] Winslow, J. D. and Gates, G. R., Materials Research and Standards, Vol. 3, 1963, p.
205.
[3] Muller-Von Moos, M. in Proceedings, International Conference on Soil Mechanics and
Foundation Engineering, Vol. I, 1965, p. 17.
[4] Grim, R. E., Applied Clay Mineralogy, McGraw-Hill, New York, 1962.
[5] van Schuylenborgh, J., Journal of Agricultural Science, Vol. 2, 1954, p. 17.
[6 "Soils of the Humin Tropics," Committee on Tropical Soils, Agricultural Board and
National Research Council, National Academy of Sciences, Washington, D.C., 1972.
[7] Frost, R. K. in Proceedings, First Southeast Asian Conference on Tropical Soils,
Bangkok, 1967, p. 43.
[8] Remillon, A., "Stabilization of Laterite Soils," Bulletin 108, Highway Research Board,
1955, p. 96.
[9] Terzaghi, K. and Peak, R. B., Soil Mechanics in Engineering Practice, Wiley, New
York, 1968.
[lt)] Methods of Test for Soil Classification and Compaction, British Standards Institution,
1968.
[11] Torrance, J. K., discussion in Engineering Geology, Vol. 4, p. 353.
[12] Sangrey, D. A., Geotechnique, Vol. 22, No. l, p. 139.
Arshud Mahmood,' J. K. Mitchell, 2 and Ulf Lh~dblom 3
Effect of Specimen Preparation

Method on Grain Arrangement
and Compressibility in Sand
REFERENCE: Mahmood, Arshud, Mitchell, J. K., and Lindblom, Ulf, "Effect of

Specimen Preparation Method on Grain Arrangement and Compressibility in Sand,"
ABSTRACT: Effects of methods of specimenpreparation on fabric and compressibility

were investigated in a medium grain-sized sand. The effect of vibratory compaction
was compared with the effect of pluviation by characterizing the particle arrangements
and measuring compressibility in a specially fabricated oedometer. The lateral stresses
during compression were also measured.
Specimens densified by vibration in layers had random grain orientation up to 100
percent relative density. When vibration was continued beyond the time interval needed
for achieving 100 percent relative density, the grains acquired a preferred orientation.
Pluviated specimens had randomly oriented grains at both low and high densities.
The loose, pluviated specimens were much more compressible than the dense speci-
mens prepared by the same procedure. The dense specimens when prepared by vibra-
tion were less compressible than the pluviated specimens. The lateral stresses were
higher in the loose pluviated specimens than in the dense pluviated specimens during
loading. On unloading, the same trend was present initially but reversed at lower
axial loads. This trend was also measured in the specimens prepared by vibration.
KEY WORDS: sands, soils, tests, specimen preparation, fabric, compressibility,

vibration, laboratory studies, oedometers
This study was carried o u t to investigate the possible effects o f the

method of specimen preparation o n fabric a n d compressibility in a m e d i u m
grain-sized sand. T h e objective was to d e t e r m i n e whether or n o t such a
m a t e r i a l acquires different fabrics w h e n deposited in different ways; a n d ,
if so, whether different fabrics are associated with different compressibilities.
I n s i m u l a t i n g the b e h a v i o r o f sands i n the l a b o r a t o r y , it has c o m m o n l y
b e e n deemed sufficient to merely r e p r o d u c e the in situ relative density b y
'Project engineer, Woodward-Clyde Consultants, Orange, Calif. 92668.
2Professor of civil engineering, University of California, Berkeley, Calif. 94720.
3Head, Research Department, Hagconsult, Banergaten 37, 115 22 Stockholm, Sweden.
169
Downloaded/printed
Copyright9 1976 byby ASTMInternational www.astm.org
any means whatsoever. Engineered construction is being carried out to in-

creasingly exacting specifications on more and more unsuitable sites, and
it is becoming clear that a pertinent question is: How was this soil depos-
ited? Significant aspects of such a question are: (1) what fabric did the
soil acquire and (2) what is its stress history? In answering this question, it
is possible to determine how to prepare the laboratory specimens to
simulate the field density, the particle arrangement, and the in situ stress.
This study represents a first step in answering these questions and deals
with the effects of the method of specimen preparation and grain arrange-
ment on one-dimensional compressibility.
Scope
As prior tests have already shown that specimen preparation effects are
significant in influencing the fabric and properties of a sand with elongate,
angular particles [1,2], 4 a material that was likely to be far less suscep-
tible to such behavior was used for the present study: Monterey No. 0
sand, a medium beach sand with rounded and only slightly elongate parti-
cles. The effect of vibratory compaction on fabric and properties was com-
pared with the effects of specimen preparation by pluviation by charac-
terizing the particle arrangements and measuring compressibility in a spe-
ciaUy fabricated oedometer. ,The lateral stresses during compression were
also measured.
Soil Fabric
The term fabric describes the basic framework or arrangement of in-
dividual constituents of an assemblage consisting of different components.
A comprehensive description of the fabric of a soil sample [3,4,5] would
involve reconstruction of a complex, three-dimensional spatial arrange-
ment of individual grains, multigrained units, and pores. In biological and
material sciences, the principles of stereology have long been applied in
studying the internal structure of many objects by looking at thin slices or
sections [6, 7]. Thin sections and broken, ground, or polished surfaces can
be studied in several ways, depending upon the type and extent of informa-
tion required and the nature and grain size of material being studied [8].
Observation by means of optical [9] or electron microscopes [10-14] has
been employed. Impregnation with resins has been used for friable or cohe-
sionless soils such as sands [2,15]. Arrangement and planar displacements
can also be measured by X-radiography [16].
If the soil grains have shapes such that their geometrical axes coincide
with the crystal axes, then some property of the mineral crystals can be
used to define the particle arrangement, without having to define the
4The italic numbersin brackets refer to the list of referencesappendedto this paper.
MAHMOOD ET AL ON PREPARATION METHODS FOR SAND 171
geometrical outlines of grains. For platy clay particles, the difference in

refractive indices in the direction of long and short axes has been used in
determining particle orientation [11]. X-ray diffraction has also been used
for characterizing clay mineral particle orientations in soil specimens [17,18].
Other properties that have been used are magnetic anisotropy [19], dielec-
tric anisotropy [20], dielectric dispersion [21,22], sonic and thermal aniso-
tropies [23], permeability [24], and inductive conductivity [25].
One-Dimensional Compressibility
Although compressibility characterized in the field by such means as the
standard penetration test (through relationships with relative density) and
static cone bearing capacity [26] may provide a basis for reasonable settle-
ment predictions in specific cases, oedometer results obtained from labo-
ratory prepared specimens are important in understanding factors con-
trolling the compressibility behavior of sands. Laboratory measurements
of one-dimensional compressibility of sands may also be useful for obtain-
ing settlement estimates of foundations in situations where it can be
assumed that no lateral strain occurs [27], provided correct density and
fabric can be reproduced. Evaluation of relative density is susceptible to
several errors [28], and fabric is even more difficult to evaluate. Measure-
ments of one-dimensional compressibility can be used to characterize non-
linear stress-strain behavior [29,30] and to estimate footing settlements [31].
Measurement
Many of the data on one-dimensional compressibility of sands have
been obtained in conjunction with laboratory studies of at-rest radial earth
pressures. Both types of studies necessitate equipment that permits little
or no lateral deformation of the specimen [32]. Two types of equipment
have generally been used: oedometers and triaxial cells. The oedometers can
either be of a null design [33] or can be allowed to undergo small lateral
deformations [34]. One method of characterizing the effect of lateral
deformation on measured axial strains and radial stresses is by using a
range of oedometer ring thicknesses [35].
The triaxial tests have mostly been an improvement upon and variation
of the procedure suggested by Bishop and Henkel [36]. In some recent
studies, Ko triaxial tests were used to study compressibility [37,38].
Experimental Investigation
Equipment
It was desired to study the compressibility of sands in an apparatus that
would: (a) offer minimum side friction, as large side friction affects meas-
surements of lateral stresses [32]; (b) permit a specimen size tall enough
for mid-height measurements to be free of the end effects that cause errors
in data from short samples [39]; and (c) possess enough lateral rigidity to
permit horizontal stress measurements with very small radial deformations.
An apparatus of the Swedish ring compressionmeter type was fabricated.
These devices are oedometers that are easily compressible in the vertical
direction but possess considerable lateral rigidity. Larger devices, based
on similar principles, have been used in the study of crushed rock [40,41],
and have provided excellent compressibility results. In these earlier investi-
gations, the values of lateral stresses could not be recorded properly due
to low sensitivity of the measurement techniques, and it is believed that an
improvement has been effected in this respect in the present investigation.
The ring device fabricated for the present study was 102 mm inside
diameter and 136 mm high and is shown schematically in Fig. 1. It was
~Neoprene
3m cork
plan
Elevation
FIG. l--Schematic drawing of ring chamber.
made of alternating rings of stainless steel and neoprene impregnated cork,

glued together with an epoxy resin. Several materials were considered
before selecting these two. The stainless steel provided lateral rigidity and
was corrosion resistant. The neoprene rubber-impregnated cork combined
the nearly elastic compression and rebound properties of rubber with the
low Poisson's ratio of cork. The elastic recovery was important during
rebound and for loading-unloading cycles. A low Poisson's ratio (0.21)
ensured that the compressible rings did not disturb the soil specimen by
squeezing inwards into the ring chamber. The high vertical compressibility
and high lateral rigidity were similar in principle to that in devices used
for cubical triaxial tests [42,43].
After connecting the eleven steel rings with ten cork-neoprene rings,
three of the steel rings were made into load cells by mounting strain gages
around their perimeters. The strain gages consisted of 8 mutually perpen-
dicular pairs (16 in all). These were connected together, as shown in Fig. 2,
to compensate for temperature changes. A photograph of the apparatus
is shown in Fig. 3.
Horizontal
Horizontal
(o)
~ Steel ring
Horizontal
(b)
FIG. 2--Arrangement o f strain gages on ring chamber: (a) circuit diagram; (b) location o f
gages.
The chamber was calibrated, using air pressure applied from the inside
through a thin rubber membrane. The changes in the height of specimen
were measured using a linear variable differential transformer (LVDT).
Axial load was measured, using a copper-beryllium load cell that had
been calibrated with dead loads. The loads and height changes were read
out on a digital voltmeter and teleprinter. The setup is shown in Fig. 4.
Test Soil
The soil used in this investigation was a well-sorted beach sand known
as Monterey No. 0 (zero). It is a uniform, medium grain size sand (ds0 =
FIG. 3--Photograph of ring chamber.
0.43 ram; C, = 1.4), composed mostly of quartz and some feldspar. The
grains are rounded and somewhat elongate (mean length/width ratio =
1.39), as shown in Fig. 5. The specific gravity of grains is 2.65, and the
maximum and minimum densities, determined in accordance with ASTM
Test for Relative Density of Cohesionless Soils (D 2049-69), are 1.70 and
1.45 g/cm 3, respectively [44].
Specimens were prepared in the ring chamber either by pluviation (pour-
ing dry) or by vibration. Pouring from zero height was used for obtaining
loose specimens. Dense specimens were produced either by slow pouring
from a height or by vibratory compaction. Vibration was applied on top
of the sand layers by means of a circular plate of the same diameter as the
specimen vibrating vertically (frequency = 30 Hz, amplitude = approxi-
mately 0.5 ram).
FIG. 4--Photograph of experimentalsetup.
As a check on the uniformity of specimens, resin-impregnated tube

specimens were taken, as described in the next section. These cylinders o f
resin-impregnated sand were sawed into V2-in. thick slices. The density o f
these slices was measured by immersion in water, and the density profile
o f specimens was determined. The differences in density of various slices
were less than 1 percent.
FIG. 5--Grain shape distribution of Monterey No. 0 sand based on study of 227particles.
Specimens f o r Fabric Study

Specimens were separately prepared for fabric study in a container
identical to the ring chamber and by the same methods of preparation as
used for making specimens for compressibility and radial stress measure-
ments. A thin-walled acetate tube was pushed slowly into the specimen. In
loose specimen, the tube could easily be pushed nearly to the bottom of
the specimen. In dense specimens, however, tube penetration to a depth
greater than one third of the specimen height caused disturbance. The
fabric of all specimens, therefore, was determined by studying specimens
from the upper third. Epoxy resin was poured into the specimen tube and
permeated the specimen under a head of a few millimetres.The resin was
allowed to harden overnight. The hardened specimens were then sawed to
obtain vertical and horizontal faces, which were ground and finished on a
diamond-cloth grinder. These faces were then photographed and enlarged
by projecting them onto a sheet of paper and tracing the grain boundaries.
Each complete tracing contained the outlines of 400 or more grains.
The best estimates of the apparent long axes of elongated grains were
drawn on the tracings and their orientations determined by assigning them
to one of the eighteen 10-deg intervals between 0 and 180 deg. The num-
ber of particles in each of the 18 intervals was separately totalled and then
computed as percentages of the total number of particles in a tracing.
These percentage values were then plotted on polar coordinate graph paper
as rose diagrams, as shown in Fig. 6. The portion of the diagram from
180 to 360 deg is a duplicate of the portion from zero to 180 deg. If all
particles were randomly oriented, the plot would have been the circle shown
by a broken line.
MAHMOODETALONPREPARATIONMETHODSFORSAND 177
(o)
/
5~176
~ ~ (c)
FIG. 6--Grain orientation diagrams f o r specimens o f Monterey sand: (a) pluviated, density
= 1.58 g / c m 3 Dr = 53 percent; (b)pluviated, density = 1,72 g/cm 3, Dr = 106 percent; (c)
vibrated, density = 1.69 g/crn 3, DR = 97 percent; and (d) vibrated, density = 1.71 g / c m 3,
DR = 104 percent.
Testing Program
Frabric-compressibility relationships in sand were studied by testing

specimens prepared at different densities by either vibration or pluviation.
The as-compacted grain arrangements were determined for both methods
of densification. The vertical compressibility and radial stress were mea-
sured on specimens prepared both ways.
Fabric Results
Particle orientation diagrams, representing the initial or as-compacted
fabrics of four specimens, are presented in Fig. 6. When poured to form
a medium dense specimen, the sand particles acquired a grain orientation
as shown in Fig. 6a. There is no strong preferred orientation of grain axes.
Experiments with materials composed of elongate, angular grains had
shown that pouring resulted in the grains acquiring an arrangement such
that their long axes were preferentially oriented in the horizontal direc-
t i o n - o r normal to the direction of fall [1]. This orientation of grains can
be explained by considering the behavior of flat ellipsoids tumbling in free
fall [45]. On a horizontal surface, more ellipsoids are likely to come to
rest with their long axes normal to the direction of free fall.
In the case of a soil such as the Monterey sand, which is composed of
grains that are only slightly elongate and rounded, no strong orientation
resulted on pouring. Evidently, at the end of fall when the nearly equant,
rounded grains come to rest, they take up random positions. A very slow
rate of pouring was used to obtain dense specimens, and the randomness
of grains was still observed, as shown in Fig. 6b. Densification by vibration
also produced a specimen with reasonably random grains, which can be
seen in Fig. 6c. This grain arrangement resulting from dynamic densification
is similar to that of soils composed of elongate, angular particles [1].
Specimens were prepared by vibrating each layer for a longer period
of time than that required to attain 100 percent relative density, in order
to develop some prestress in the specimen. The grain orientation diagram
for one such overvibrated specimen is shown in Fig. 6d, where it may be
seen that there is a recognizable preferred grain orientation, with the
vector mean oriented at about 40 deg from the horizontal. It appears that,
if the sand is kept in a fluidized state for an extended period by over-
vibration, then the grains get some freedom of mov~nent and gradually
acquire a preferred orientation. That the grain axes become oriented at
40 deg could perhaps be due to the fact that densification to a high
density involves frictional slippage at grain contacts, and the particles
gradually become arranged to resist this change. This happens even
though the vibratory stresses causing densification are cyclic and thus
might not be expected to produce preferred orientation. The sustained
application of vibratory compactive effort results in an incipient frictional
failure. Such a failure in a mass should be evident at two complementary
planes, but two planes might not be seen if the failure is initiated on one
of them first. In Fig. 6d, all the grains are arranged as if in a stack,
an arrangement known to develop when discrete plates are vibrated to a
dense state. Figure 7 suggests how such an arrangement might develop
in a sand with less elongate particles.
In the ASTM Test for Relative Density of Cohesionless Soils, (D 2049-
M A H M O O D ET AL ON PREPARATION METHODS FOR SAND 179
"Stack" Arrangement
FIG. 7--Proposed stack arrangement of particles in an overvibrated specimen of sand.
69) vibratory compaction is specified for determination of maximum den-

sity. It is sometimes stated that any mechanical energy used for obtaining a
densification in excess of the standard maximum density generally results
in grain crushing. Since the vibration applied for preparing the overvibrated
specimens did produce relative densities greater than 100 percent, it was
suspected that grain crushing might have influenced the grain orientation
results. A carefully controlled sieve analysis of a sand specimen before
and after vibratory compaction did not reveal any measurable change in
gradation, as shown in Fig. 8, and it can therefore be inferred that grain
crushing was not significant enough to influence the grain orientation
results obtained.
Sieve Sizes
27O
~ 400 ~ I00 50 302016 8 4
I I
F
I I I I I
O Initiol $ievin 9
8O ~, Sieving after 90 seconds
vibration per layer
g
- 60
g
u
Monterey Sand No. 0
9~ 4C
O
._o
2O
J
AI, = 5 1 1 I I I I I
0.05 0J 0.5 LO 5
Groin Size, mm
FIG. 8--Effect of vibratory compaction on gradation of Monterey No. 0 sand.
The standard maximum density was also exceeded in specimens prepared

by very slow pouring, a procedure in which there is no mechanical energy
applied for compaction, and hence no grain crushing is likely. Other

procedures have also been reported to result in higher densities [46] than
obtained using the ASTM Method D 2049-69.
C o m p r e s s i o n Test Results
Axial deformations and radial stresses measured on sand specimens in
the ring chamber are presented in this section. The effect of relative density
on axial strain is shown in Figs. 9 and 10.
AxioI Stress, ko,/cm z
I I0
Oj ' I I I = , , , ,
I
I Density DI~
ooozi- F~i=~ ~ o ~.4e

9 J la 1.71 104
z_
0.006 - ~ A~....,~
" ~a,l
0 . 0 0 $ --
O.OlC
O.OIZ
Monterey S a n d
I I I L ' I , ,
FIG. 9--Effect of density on axial compression of pluviated specimens.
The effect of specimen density on the lateral stresses is presented in Figs.

11, 12, and 13. The variation of K, the ratio of radial stress to axial stress,
is plotted versus the applied axial stress. This relationship for the loose
and dense pluviated specimens is shown in Fig. 11. The lateral stresses
were slightly higher in the loose specimen upon loading. This would be
expected, as the dense specimen, being more rigid than the loose specimen
resisted the applied vertical stresses better. The loose specimen was less rigid,
and, being softer, it behaved more like fluid, transmitting vertical stress
into the lateral direction.
Axiol Stress,kg~mz
I0
I I I I I I I i
Density DR
g/cm~ %
0.00 P
t~ i.64 80
0002 - %
._
o
. \
0.00,
0.006 MontereySand - ~
0.007 I I I I I i J i
FIG. lO--Effect of relative density on axial compression of specimens densified by vibra-

tion in six layers.
On unloading, the same trend was present initially, but below an axial
stress of about 4 kg/cm 2, the radial stresses in the dense specimen became
higher than in the loose sand, as seen in Fig. 11. The dense specimen was
more rigid than the loose specimen, and hence the static loading resulted
in relatively larger locked-in stresses during loading. During unloading,
these locked-in lateral stresses resulted in higher K values in the dense
specimen. This behavior was observed even when specimens were loaded
only up to 1 kg/cm 2, as shown in Fig. 12. Similar trends showing a reversal
in the comparative magnitudes of radial stresses on unloading were mea-
sured in the specimens prepared by vibration in six layers, as shown in
Fig. 13, but the effect was not as pronounced.
Method of Specimen Preparation

The dense specimens were prepared either by very slow pouring or by
vibratory compaction. The stress-strain plots of dense specimens prepared
by the two methods are compared in Fig. 14. The pluviated specimen was
1.4 I I I I I
Density DR
| Q/cm 5 %
1.2 - t
, PluviotedJ"o 1.46 6
L~ 1.71 104
1.0 -
o
\\
-
, 0 . 8
0.6
_ Loodmg ' ~ ~
~'0.4
0.2 Monterey Sand
0 I I I I i
0 2 4 6 8 iO 12
Axiol Stress, kg/cm 2
FIG. 11--Relationship between axial stress and K in specimens prepared by pluviation;

effect of density.
slightly denser than the specimen vibrated in six layers, yet the pluviated
specimen showed greater deformation under the same load. The greater
compressibility of the pluviated specimen is largely due to the axial de-
formation that occurs at low axial stress (less than 1 kg/cm 2) as may be
seen from Fig. 15, where the data are replotted on a linear scale.
The grain orientation diagrams of the pluviated and vibrated specimens
were shown in Figs. 6b and c, respectively, indicating grain arrangements
that were quite random, yet their axial deformations showed small dif-
ferences. These small differences could have been due to a difference in
the initial state of stress of the poured and the vibrated specimens. If any
such difference existed, it was likely to show up in the initial value of
measured lateral stresses. A plot of K (ratio of radial stress to axial stress)
versus axial stress is shown in Fig. 16 for dense specimens prepared by
pluviation and by vibration. The pluviated specimen had slightly higher
lateral stresses. The vibrated specimen did not show any evidence of high
locked-in stresses.
It is intriguing that the vibrated specimen did not have the high lateral
stresses that might be expected [47], and the behavior could not be explained
on the basis of grain orientations. It may be that the vibrated specimen
was less compressible because the particles had acquired an arrangement
0.9 I I i I I
a ~ Monterey Sond
0.8
\
xA
0.7 \
\
0.6
U')
0.5
K
<z
0 ' u _ ~
=
| 0.4 A
LoodinQ
nO-~ 0.3
Density DR
g/cm3 %
0.2
o ,.46 ~ } P,uviafed
/" 1.71 I
0.1
o I I I I I
O 0.2 0.4 0.6 0.8 I. 0 1.2
Axiol Stress, kQ/cml
F I G . 12--Relationship between axial stress and K in pluviated specimens in the low axial
stress range.
efficient in resisting one type of stress (due to vibratory compaction) that

made it better able to resist a different type of stress also (due to static
load). The pluviated specimen did not achieve its grain arrangement in
order to resist any externally applied stresses and was, therefore, more
compressible even under small axial stresses.
Whatever changes take place in a specimen upon vibration should be
amplified if the vibration is continued for longer periods. An average
vibration time of 30 s per layer produced a specimen of 96 to 100 percent
relative density, and vibration beyond 30 s per layer yielded relatively
small increases in density. The stress-strain plots of three specimens densi-
fied by vibration for 30, 60 and 90 s on each layer are presented in Figs.
17 and 18 (a replot of Fig. 17 on linear axes). All three specimens had an
equal amount of residual strain after complete unloading, as seen in Fig.
18, even though their peak axial strains (at 10 kg/cm 2) were different.
This result points to the uniform efficiency of packing in the three speci-
1.4 I I l I I
Density DR
I,Z 9/~" ~ -
o 1.57 50 /
1.64 80 ~,Vibrated
1.69 97 J
E I.G o -
o
(:16
l,J~loodinQ
0.6
o
^ -"~-~.~-'2~ _
0.4
"~: - ~- --8:-~; --- ~- - - - -o . . . . -o
Loodinq
Monterey Sond
I I I I I
0 Z 4 6 8 I0 12
Axiol S t r e s s , kg/cm 2
FIG. 13--Relationship between axial stress and K in specimens densified by vibration in

six layers.
mens, and shows that the overvibrated grain structure was relatively
more resilient.
The measured lateral stresses during loading of overvibrated specimens,
as shown in Fig. 19, increased with decreasing density, as would be ex-
pected. Evidently, however, density differences were too small to cause a
crossover of the curves on unloading, as was the case in Fig. 12. '
The compression test results shown in Figs. 10, 15, and 18 are replotted
in Fig. 20, expressing compressibility as the ratio of strain to stress
(1/modulus), obtained from the slopes o f stress-strain curves at axial
stress values of 1, 4, and 10 kg/cm'. This figure shows that, at low axial
stresses, the compressiblity is large and gradually decreases at high axial
stresses of 4 and 10 kg/cmL The plots also show that, at each axial stress
value, the compressibility is large at low relative densities, decreases with
increasing relative density to a point, and then increases again. This
optimum value of relative density, at which the lowest compressibility oc-
curs, is about 85 percent for 1 kg/cm 2, 95 percent for 4 kg/cm 2, and
approximately 100 percent for the 10 kg/cm 2 curve.
Long duration of vibration could cause enough particle breakage in
some sands to influence the compression behavior. However, no measura-
ble change in grain size took place here, as already shown in Fig. 8.
Axial Stress, kg/cm 2

IO
I I I I I 1 I I
Densit~E DR
O.OOI g/cm= %
A t.69 97 Vibrated
a 1.71 104 Ruvioted
0.00~
,a o.oo3
s
0.00,
0.005
0.006
Monterey Sond ~o,~
0007 I I I I l i i ,
FIG. 14--Effect of method of specimen preparation on the axial compression of dense sand.
Axial Stress. kg/cm 2

0 2 4 6 8 IO 12
I ! I l I
Monterey Sond
o.o~ 9\ ~ b ~ Vibrated o ~ "9"7

X~ . . Phwioted • I. 71 104
o 0.004
(/1
o
K
-~~ ' ~ , , ~ ~
0.006
0.008 I I I I I
FIG. 15--Effect o f method of specimen preparation on the axial compression of densesand.
1.4 I I I I "1
M o n t e r e y Sand
Oensity D R
~l 4~ 1.69 97 Vibroted
~o o 1.71 104 Pluviofed
1.0
r
~ 0.4
Looding
O.Z
I I I I I
O 2 4 6 El 10 12
AJtiol Stress, k g / c m 2
FIG. 16--Effect o f method o f specimen preparation on the relationship between axial

stress and the ratio o f radial to axial stress.
Observation of long axes of grains showed that the overvibrated grains

had a preferred orientation, as shown in Fig. 6. The vector mean of long
axes of grains was inclined at about 40 deg, which is quite close to the
probable planes of maximum shear under static load. This result points to
the possibility that the larger compressibility of the dense, overvibrated
specimens was related to their grain orientation. The fabric results, how-
ever, do not conclusively explain the changes in compressbility with over-
vibration, and it is believed that a better understanding of grain arrange-
ment is needed, involving perhaps a study of grain contacts and the orienta-
tion of contact planes.
Values o f K
The values of K, the ratio of radial stress to axial stress, are summarized
in Table 1. For comparison, a few measured values of the coefficient of
lateral pressure at rest reported in the literature are also included. The re-
sults from the various laboratory studies seem to be in the same general
range of values. The values measured in the field by D'Appolonia et al
[44] are substantially higher.
MAHMOOD ET A L O N PREPARATION METHODS FOR S A N D 187
Axial Stress. i~/cm 2

01 10
Density D R Vi brotion/Loyelr
g/cm5 % seconds
0.001 o 1.69 95 30
1.70 I01 60
o 17',> 105 90
.~,,,,,,,,~ ~ Loo d i ng
0O02
0.003
0004 ~
0O03
~"-,. ~,, ]
QO06
Monterey Sond
0.007 I I I I I J I I/
FIG. 17--Effect o f overvibration on the axial compression o f dense sand.
Axiol Stress, kg/cm2

O Z 4 6 8 I0 IZ
0 I I ! I I
Density DR Vibrotion//oyer
o/cm3 % seconds
~'~-LoOdin~ 0 ~ ~"
0.00~ ,, ~ ~ 1.70 I01 60
~ 17z io5 ,o
.~ 0.004
o3
o .L UnloOding --''.a . . . . "'~",=..~..~ "~.,,,.~
Monterey Sond
0,008 J I I i t
FIG. 18--Effect o f overvibration on the axial compression o f dense sand, axial stress
plotted to linear scale.
188 SOILSPECIMENPREPARATIONFORLABORATORYTESTING
1.4 I I I I I
Density DR Vibration/Layer
-- I:~ g/01~3 % seconds
I.Z
',I o~- ;; ~ -
~ ~ t704 OI 60
~ o I.Tg 105 90
i i.O
0.8
-,,,,,
O.S
n-
m 0.4
Loadin9
0.2
Monterey Sond
0 I I I I I
0 Z 4 6 8 I0 12
Axiol Stress, kg/cm 2
FIG.
19--Effect o f overvibration on the relationship between axial stress and K in speci-
mens densified by vibration in six layers.
07
i i i I i i
p .o,o k g /
-I~ /
I
,.r
== .ooe Monterey
Vibroted
Sond
Specimens
=- ~, .006
=
.o
o
4 kg/cm;
~ .004
r
I0 k g / c m ~ ~" ~ -
.002 I I I I I I I
30 40 50 60 70 80 90 IO0 I10
Relative Density, D R, %
FIG.20--Relationship between compressibility and relative density.

TABLE l--Comparative summary o f K (ralio o f radial to axial stress) values.
K = Radial Stress/Axial Stress
Unloading "1"
Method of
Initial DR, % ~, deg Loading OCR b = 2 4 8 10 Specimen P r e p a r a t i o n Remarks 0
0
Cl
6 32* 0.46 0.60 0.74 0.85 0.95 pluvialion results f r o m this paper
1.02 1.12 vibration m a x i m u m vertical stress I"11
50 38* 0.42 0.60 0.82 "--I
80 44 ~ 0.39 0.57 0.80 1.02 1.20 vibration o n specimen = 10 k g / c m 2
2~
97 47 ~ 0.35 0.53 0.78 1.02 1.20 vibration r o u n d e d sand grains I-"
104 49 ~ 0.40 0.58 0.85 1.12 1.30 pluviation
O
9 30 0.38 . . . . . . Hendrnn, rounded sands--from Z
... 34 0.33 . . . . . . B r o o k e r a n d Ireland [48] "0
"11
.,. 30 0.50 . . . . . . Hendron, angular sands--from rn
B r o o k e r a n d Ireland [48] "1o
... 36 0.40 . . . . . .
. . . . . . 12.5 kip roller

::0
"-'90 ... 2.7 . . . . . .
27.5 Hz" .-I
D ' A p p o l o n i a et al [47]
. . . . . . 1.5 . . . . . . . . . . . . 6.3 kip roller Z
29.5 Hz" g
Loose ... 0.425 . . . . . . A n d r a w e s a n d EI-Sboby, [46]; Silver

(n = 0.411) sand; r o u n d e d particles I
Dense ... 0.343 . . . . . . 0
(n = 0.352)
0.0 ... 0.37 , .. Obrician [24]coarse to fine sand "11

9 vibration 0
51.6 ... 0.33 0.64 0.90 "n
78.6 ... 0.28 . . . . . . . . . vibration
~ D u r g u n o g l u a n d Mitchell [49], Fig. 5 . 8 b . Z

CI
bOCR = m a x i m u m vertical load/vertical load d u r i n g unloading.
CAfter 40 passes; stresses perpendicular to roller path.
CO
Conclusions
A medium sand, composed of rounded, slightly elongate grains, when
pluviated at both low and high densities, formed specimens with randomly
oriented grains. When specimens were densified by vibration in layers, the
grain orientation was random up to 100 percent relative density. When
vibration was continued beyond the time interval needed for achieving 100
percent relative density, the grains acquired a preferred orientation with a
vector mean at some inclination to the horizontal.
The loose, pluviated specimens were much more compressible than the
dense specimens prepared by the same procedure. On application of verti-
cal load, the particles slide and overturn to reduce the void volume. The
lateral stresses during loading were higher in the loose specimen; being
less rigid, it had a greater tendency for sideward bulge than the dense
specimens. On unloading also, the loose specimen had higher lateral stresses
than the dense specimen, but this trend reversed itself towards the end of
unloading. The same trend was also measured in the specimens prepared
by vibration.
The dense specimens, when prepared by vibration, were less compressi-
ble than the pluviated specimens. This difference in the behavior of speci-
mens prepared by these two methods of preparation cannot be conclusively
explained on the basis of either grain arrangement or locked-in stresses.
The effects of stress history may also contribute to the observed behavior.
The grains are randomly oriented in both pluviated and vibrated speci-
mens, and the measured lateral stresses are slightly higher in the more
compressible, pluviated specimen.
It is believed that this study addressed two important issues bearing on
the specimen preparation of cohesionless materials. First, how meaningful
is a comparison of test results obtained from research efforts in the
absence of fabric studies and, second, how much emphasis should be
placed on fabric when in situ properties of granular materials are estimated
by testing reconstituted specimens in the laboratory. The results of this
study reaffirm that density as well as the method of densification should
be specified in standardized testing procedures. Also, it points to the need
for further research in testing of sands in order to obtain better under-
standing of how the field behavior of sands can be estimated from tests
in the laboratory.
Acknowledgments
The experimental work reported was carried out at the University of
California, Berkeley, and the study was supported by The National
Aeronautics and Space Administration through Grant NGR-05-003-406
and Contract NAS 9-11266. Joyce Blueford and Carl Bellamy helped with
some portions of the fabric study. Addition support from Professional

Development Committee of Woodward-Clyde Consultants is gratefully
acknowledged.
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1629-1953.
[31] D'Appolonia, D. J., D'Appolonia, E., and Brissette, R. F., Proceedings, American
Society of Civil Engineers, Vol. 94, No. SM3, Journal of Soil Mechanics Foundation
Division, May 1968, pp. 735-759.
[32] Schmidt, B. and Steen, O., "Compression of Sands," Bulletin No. 23, The Danish
Geotechnical Institute, 1967.
[33] Hendron, A. J., "The Behavior of Sand in One-dimensional Compression," Ph.D
dissertation, Department of Civil Engineering, University of Illinois, Urbana, 1963.
[34] Obrcian, V., "Determination of Lateral Pressures Associated with Consolidation of
Granular Soils," Highway Research Record 284, Highway Research Board, 1969, pp.
13-24.
[35] Calhoun, D. E. and Triandafilidis, G. E., Proceedings, 7th International Conference on
Soil Mechanics and Foundation Engineering, Mexico City, 1969, Vol. 1, pp. 65-72.
[36] Bishop, A. W. and Henkel, D. J. Measurement of Soil Properties in the Triaxial Test,
Edward Arnold, London, 1962.
[37] Moore, C. A., Proceedings, American Society of Civil Engineers, Vol. 97, No. SM9,
Journal of SoiI Mechanics Foundation Division, Sept. 1971, pp. 1275-1292.
[38] Campanella, R. G. and Vaid, Y. P., Canadian Geotechnical Journal, Vol. 9, Aug. 1972,
pp. 249-260.
[39] Andreasson, L., "Compressibility of Frictional Soils," Ph.D dissertation, Chalmers
University of Technology, Gothenburg, Sweden (in Swedish with English summary).
[40] Fumagalli, E., Proceedings, American Society of Civil Engineers, Vol. 95, No. SM1,
Journal of Soil Mechanics Foundation Division, Jan. 1969, pp. 313-330.
[41] Lindblom, U., "Compression Characteristics of Spread Fills from Blast Rock, with
Special Reference to Settlements of Footings," Ph.D dissertation, Chalmers University
of Technology, 1972, Gothenburg, Sweden (in Swedish with English summary).
[42] Lade, P. V. and Duncan, J. M., Proceedings, American Society of Civil Engineers, Vol.
99, No. SM10, Oct. 1973, pp. 793-812.
[43] Daniel, A. W. T., Harvey, R. C., and Burley, E., Proceedings, American Society of
Civil Engineers, Vol. 101, No. GTS, Journal of Geotechnical Engineering Division,
May 1975, pp. 508-512.
[44] Durgunoglu, H. T., "Static Penetration Resistance of Soils," Ph.D dissertation,
University of California, Berkeley, 1972.
[45] Jizba, Z. V. in Procedures in Sedimentary Petrology, R. E. Carver, Ed., Wiley, New
York, 1971.
[46] Youd, T., Proceedings, American Society of Civil Engineers, Vol. 98, No. SM7, Journal
o f Soil Mechanics Foundation Division, July 1972, pp. 709-726.
[47] D'Appolonia, D., Whitman, R., and D'Appolonia, E., Proceedings, American Society
of Civil Engineers, Vol. 95, No. SM1, Journal of Soil Mechanics Foundation Division,
Jan. 1969, pp. 263-284.
[48] Brooker, E. W. and Ireland, H. O., Canadian Geotechnical Journal, Vol. 2, No. 1,
Feb. 1965, pp. 1-15.
[49] Durgunoglu, H. T. and Mitchell, J. K., "Static Penetration Resistance of Soils,"
Geotechnical Engineering Report by Space Science Laboratory, University of California,
Berkeley, April 1973.
V. A . N a c c i ~ a n d R. A . D ' A n d r e a 2
A Technique for the Preparation of

Specimens of Loose Layered Silts
REFERENCE: Nacci, V. A. and D'Andrea, R. A., "A Technique for the Prepara-
tion of Specimens of Loose Layered Silts," Soil Specimen Preparationfor Laboratory
Testing, ASTM STP 599, American Society for Testing and Materials, 1976, pp.
193-201.
ABSTRACT: A brief review of previously published results of shear strength testing

of silty soils is presented. It is noted that, due to their highly porous structure and the
resultant unfavorable effects derived from sampling, natural silts are among the least
studied deposits in the world. When found in glaciated regions, these deposits are often
laminated, usually contain small amounts of clay, and, when laminated, are invariably
anisotropic.
A typical naturally occurring silt, prevalent in the area of Providence, Rhode
Island, is described in terms of its geologic origin and its in situ index properties.
An experimental procedure which entails laboratory sedimentation, consolidation
under small load increments, and laboratory freezing to obtain a soil specimen which
may be handled without densification, is described. It is shown that these laboratory
produced specimens duplicated the in situ varved structure and index properties of the
natural silt. Although the paper reports in detail on the production of cylindrical triaxial
specimens, the method may be readily adapted to produce specimens of virtually any
size or shape.
In conclusion, it is pointed up that, in utilizing this technique, specimens may be
prepared with virtually any angular relationship between the inclination of the layers
and the directions of the applied principal stresses, facilitating the investigation of
anisotropic strength effects.
KEY WORDS: soils, silts, sedimentation, freezing, anisotropy, shear strength, triaxial
tests
As part of a comprehensive research project dealing with the determina-

tion of the mode of failure and the strength parameters of certain naturally
occurring stratified silty deposits found in Rhode Island, a unique speci-
men preparation technique was devised and is described herein.
Under natural conditions, the liquidity index of these silts is well above
Professor of civil and ocean engineering, University of Rhode Island, Kingston, R.I. 02881.
~Assistant professor of Civil Engineering, Worcester Polytechnic Institute, Worcester,
Mass. 01609.
Copyright 9 1976by ASTM International www.astm.org
1.0, and, in many respects, they behave like loose sands, in that it is not
uncommon for them to lose a high percentage of their undrained strength
when the silt is subjected to limited remolding, which is inevitable in even
the best undisturbed sampling techniques.
A prime prerequisite to the aforementioned study was to obtain samples
which preserved the in situ layering, structure, and porosity variations.
However, conventional sampling techniques, including thin-walled and
block sampling, produced inferior results, since the soil liquefied at the
slightest disturbance. Furthermore, even when good samples were obtained,
some densification took place in transit to the laboratory, and it was
assumed that the resulting laboratory specimen would exhibit a higher
strength than that present in situ, due to its decreased void ratio.
A review of the relevant available literature reveals that the problem of
obtaining adequate samples of silty soils seems almost universal. Some
studies [1,2] 3 have employed remolded triaxial specimens of varying relative
densities, and the large excess pore water pressures developed upon shearing
the loose samples in these studies proved to be a good indicator of the
expected behavior of the silts in question. However, as demonstrated in
strength investigations on layered clays [3,4], it seemed likely that the shear
strength would be dependent upon the shear plane orientation with regard to the
strata, as well as soil structure and void ratio. Furthermore, Bjerrum [5] has
pointed up the importance of anisotropic strength effects and their relevance
to solutions of soil stability problems. Consequently, remolded samples
(which would exhibit no anisotropy) were deemed inappropriate for this
investigation.
Investigations by Fagnoul [6] and Schultze and Odendahl [7] indicate that
undisturbed silt samples were tested, but fail to indicate how these samples
were obtained.
Hirschfeld and Poulos [8] present drained shear test data from samples
extracted from an undisturbed block. Fortunately, their silt was not satu-
rated fully and had a high preconsolidation pressure. Both of these effects
(which are absent in the Rhode Island silts under study) impart some rigidity
to the soil, and thus probably facilitated sampling.
In situ field strength tests, such as the vane shear, provide questionable
results in silt, since drainage conditions are difficult to predict, due to the
silt's relatively high permeability. Tests are likely to be drained partially and
consequently would yield strengths greater than the undrained strength in
the loose silt under consideration. Although Blight [9] presents a technique
for performing drained field vane shear tests, undrained strength para-
meters for the Rhode Island silts were required for certain design purposes.
Thus, field strength testing programs were discarded in favor of laboratory
testing under monitored drainage conditions, and the decision was made
3The italicnumbersin brackets referto the list of referencesappendedto this paper.
NACCI AND D'ANDREA ON LOOSE LAYERED SILTS 195
to attempt to duplicate the sensitivity and layering of the in situ material

with laboratory sedimented specimens.
Soil Description
In many parts of the world which have experienced glaciation, there exist
clay, silt, and sand deposits with a definite banded or varved structure.
The Rhode Island silts are illustrative of such sedimentary glacial lakebed
deposits.
Although the mode of sedimentation and the effects of electrolytes on
deposition may be a matter of dispute, the typical Rhode Island silt is
banded, almost devoid of clay particles, and in a fairly loose condition.
Their characteristic light and dark bands imply an annual deposit, with
the coarser silt and sand sizes having been deposited during periods when
the waters of the parent glacial lake were more turbulent. The silts in the
Providence, Rhode Island area are fairly consistent in lamina thickness,
with natural water contents often well above the liquid limit. It is not un-
common for standard penetration test results to be two blows per foot or
less.
A typical deposit, which was sampled extensively for this investigation,
was discovered at a location 1.5 km south of the Park Avenue overpass
on Interstate Route 95 in Cranston, Rhode Island. The distinguishing
geotechnical features of this deposit may be summarized as follows:
1. The successive layers are on the order of 0.9 cm in thickness and are
composed mainly of a lightly colored coarser portion which grades into a
thick dark band composed of rock flour and clay. No attempt was made
to separate the materials comprising the layers, since the grading was often
almost imperceptible.
2. Natural water contents varied between 30 and 38 percent.
3. The liquid and plastic limits for the material, as a whole, were 28
and 22 percent, respectively.
4. The grain size range and uniformity (again, of the entire mass) are
depicted in Fig. 1.
5. The high natural water contents suggest a metastable soil structure,
and the soil, when sampled, proved highly sensitive to disturbance.
Initially, bulk samples were procured from the site during the con-
struction of Interstate Route 95. The soil was stored in barrels, and, as it
was needed, it was mixed with sufficient distilled water to produce a mass
which could be readily poured through a funnel. The resultant slurry was
stored in sealed glass jars.
Triaxial specimens were prepared by slow sedimentation of this slurry
100.
-.....
a~
Z 40
~o
20 ,,I
.3 .2 .06 .02 .01 .002 .001
SAND I SILT SIZE I CLAY SIZE

J L
DIAMETER ( rnm'~
I
FIG. l--Grain size distribution o f a varved Rhode Island silt.
through a solution of 0.1 normal sodium chloride in 3.48-cm-diameter

solid perspex tubes (see Fig. 2). By varying the size of the tube in which
LOAD
POROUS STONE
VARVED SAMPLE
j BEAKER
PLASTIC TUBE~
....-.----COARSE SAND
FIG. 2--Sedimentation apparatus.
the silt is sedimented, specimens of any size may be obtained. A small

amount of the dilute silt suspension was poured through a funnel into the
tube. The funnel was equipped with an upturned stem so that the soil
would be initially directed upward through the solution inside the tube.
Eventually, the silt began to settle at a rate governed by the prevailing
grain size, thus producing layers graded in a fashion similar to those
found in nature. The quantity of silt poured was determined via trial and
error, until the sedimented varve formed was approximately equal in
thickness and composition to the natural varves. Utilizing a sodium
chloride solution accelerated the settling of the clay sized fraction, and
additional charges could be poured at the rate of one per day until the
cylinder was full.
In order to prepare specimens of varied strata inclinations, Doyle [10]
made modifications to the apparatus shown in Fig. 2 (which produces
specimens with horizontally oriented layers). This apparatus was hinged
at the base so that layers could be deposited at any angle up to 60 deg.
Tilting the tube rack beyond 60 deg, however, caused the soil particles
to fall along the side of the tube, rather than in a vertical direction through
the solution. To obtain specimens whose strata were oriented between
60 and 90 deg with respect to the horizontal, a slotted sediment tube was
used. The silt slurry was poured along the longitudinal axis, rather than
into the end of the tube. Once filled, a plastic insert was pushed across
the tube to act as a seal.
At this point, in order to impart some rigidity to the essentially liquid
sediment, the silt was consolidated under a pressure of slightly less than
89 kg/cm 2. This was accomplished by applying a direct load, as shown in
Fig. 2, for the specimens with strata inclined from 0.0 to 60 deg with
respect to the horizontal. The steeper strata orientations were consolidated,
utilizing a hydraulic ram. In general, consolidation with the major
principal stress perpendicular to the layering would be desired, in order
to assess the effects of rotation of principal stresses on strength. Un-
fortunately, during consolidation for rigidity in either sedimentation
apparatus, the major principal stress is perpendicular to the longitudinal
axis of the tube. However, it was felt that the subsequent freezing of
the specimen, described later in this article, separated the grains, and
ensuing consolidation under the desired stress system could be performed
in the appropriate test apparatus.
After consolidation was completed, the cylinder with sedimented soil
intact could be lifted out of the chamber and extruded into a split mold
for triaxial testing. Unfortunately, the soil densified visibily, even though
vacuum was applied, presumably altering the strength properties. This
development prompted an additional step in specimen preparation
technique, in order that the sample might be set up without undergoing
drastic changes in void ratio.
It was hypothesized that, if the silt exhibited little electrochemical

bonding (that is, its behavior was influenced primarily by gravitational
forces), a freeze-thaw cycle would not alter the particle arrangement
significantly, and densification due to handling could be minimized.
Lambe [11] has shown that differences in axial shrinkage of compacted
samples may be utilized as an indicator of structural differences of samples
of equal dry densities but compacted at different molding water contents.
In order to demonstrate that the silt in question did not display inter-
molecular bonding and the corresponding structural differences at differing
electrolyte concentrations, silt samples were compacted, wet and dry, of
optimum water content, via a kneading type compaction apparatus, and
their axial shrinkage upon drying was measured. Since equal shrinkages
were recorded for equal dry densities, regardless of water content, it was
concluded that the small percentage of clay sizes had little effect, and the
silt's packing arrangement was not influenced by electrochemical effects.
This conclusion led to the following method of placing samples in the
desired shear apparatus without altering their structure.
After the samples were consolidated under the aforementioned sur-
charge loading, the plastic tubes were removed carefully from the sedimen-
tation beaker; excess fluid was drained; and rubber caps were applied
to both ends of the tube. The samples were then placed in a conventional
household freezer, wherein the pore water froze, imparting sufficient
rigidity to the sample to allow handling without densification. Although
the freezing mechanism expanded the silt, it was felt that, upon sub-
sequent thawing, the silt particles would revert to their sedimented con-
figurations. As a further check, X-ray photographs were taken of the
frozen samples. The photos revealed that little ice lensing due to pore
water migration occurred, and that the layering remained intact.
The water content of a frozen sample was in the range of 34 to 35 per-
cent, comparing favorably with the in situ condition.
The freezing procedure would not have been feasible if compaction
results had shown that freezing and thawing would have broken down
intermolecular bonds within the soil. Since there were no such bonds to
begin with, it was assumed that freezing the sample to facilitate installation,
coupled with subsequent thawing before testing, would not change the
structure of the silt significantly. Although many researchers, Fahlquist
[12] included, report field sampling methods which involve freezing the soil
while it is being sampled, to the best of the authors' knowledge, laboratory
freezing as described herein has not been practiced extensively.
Typical Testing Procedure and Result

Triaxial specimens were prepared, as described previously, and trimmed
to proper lengths while still frozen. Experience showed that the samples
NACCI A N D D'ANDREA ON LOOSE LAYERED SILTS 199
should be frozen no more than 24 h to maintain 100 percent saturation,

and that, by setting up the sample in a chilled triaxial chamber, thawing
could be prevented until a small confining pressure could be applied. A
period of 24 h at room temperature was sufficient for complete thawing
and consolidation under the seating consolidation pressure. The confining
pressure required for the test was then applied and volume change versus
time recorded in the normal manner.
As an illustration, the following shear test will be described. The example
specimen had varves perpendicular to its longitudinal axis and was con-
solidated isotropically under a pressure of 1 kg/cm 2 (yielding a post-
consolidation water content of 32.46 percent). After consolidation, the
normal procedure of back pressuring and testing for pore pressure
response [13] was followed. Shearing loads were applied via undrained
triaxial compression, using Geonor equipment [14], at a constant strain
rate of 2.8 percent per hour. This rate was slow enough to ensure that
the pore pressure measured at the specimen base identified an equalized
pore pressure throughout the material.
Figure 3, which is a plot of principal stress difference (o~ - 03) versus
strain, and Fig. 4, depicting principal stress difference versus average
principal effective stress (o~' + 02' + 03 ')/3, portray graphically the
behavior of the example specimen under loading. The behavior is similar
to that observed by Schultze and Odendahl [71, who shear tested a
similar soil.
Again, it must be emphasized that, based on the described research
and 25 years of experience with this material, the authors believe that a
truly undisturbed field sample cannot be obtained and tested successfully.
The silt's behavior under load is essentially that of a slowly draining
80
70 ~,
60 i
z so
~i 4o
0//
3O
10
0 1 2 3 4 5 6
STRaiN C%')
FIG. 3-- Typical stress-strain behavior.
80
/
E
Z
60
/
i 40
20
0
o 2o 4o 6o 80 loo 12o
FIG. 4--Stress t~th for typical test.
granular material: granular, in that the silt's void ratio and stress history
solely govern its strength, and slow draining, in that significant time is
required to dissipate excess pore pressures developed upon application of
shear stresses. Although a complete discussion of application of the
parameters derived from the laboratory sedimented specimens to field
cases is beyond the scope of this paper, use of results from laboratory
specimens whose water contents equaled those of the in situ silt proved to
yield successful solutions (in that no failures were observed) to problems
concerning stability, structural foundations, and slopes of cuts, as well
as reasonable predictions for settlement under preloads.
Conclusions
Due to the highly unstable nature of many sedimentary silt deposits,
even ratively undisturbed samples are difficult to obtain. As a result,
most investigations of such silty sites make use of remolded products or
use natural specimens, on which the effects of sampling and handling
disturbance cannot be quantified.
According to this study, silt samples may be sedimented artificially in
the laboratory and frozen to provide sufficient rigidity to prelude
densification during handling and test setup. The resultant specimens
have the same ~soil solid constituents and similar water content and
layering characteristics as the original in situ deposits.
Acknowledgments
This study forms part of an investigation of the strength characteristics
of saturated varved silts being conducted under the sponsorship of the
Rhode Island Department of Public Works, in cooperation with the U.S.
Department of Transportation Federal Highway Administration, Bureau
of Public Roads. The opinions, findings, and conclusions are those of the
authors and not necessarily those of the Bureau of Public Roads.
References
[1] Penman, A. D. M., Geotechnique, Vol. III, No. 8, Dec. 1953, pp. 312-238.
[2] Schultze, E. and Norn, A. in Proceedings, Sixth International Conference on Soil
Mechanics and Foundation Engineering, Vol. I, Montreal, 1965, pp. 350-353.
[3] Lo, K. Y. and Milligan, V., Journal of the Soil Mechanics and Foundation Division,
American Society of Civil Engineers, Vol. 93, No. SM1, Paper 5056, Jan. 1967,
pp. 1-15.
[4] Milligan, V., Soderman, L. and Rutka, A., Journal of the Soil Mechanics and
Foundation Division, American Society of Civil Engineers, Vol. 88, No. SM4, Paper
3324, Aug. 1962, pp. 31-67.
[5] Bjerrum, L. in Proceedings, Eighth International Conference on Soil Mechanics and
Foundation Engineering, Vol. 3, Moscow, 1973, pp. 111-159.
[6] Fagnoul, A. in Proceedings, Sixth International Conference on Soil Mechanics and
Foundation Engineering, Vol. 1, Montreal, 1965, pp. 213-216.
[7] Schultze, E. and Odendaltl, R. in Proceedings of the Geotechnical Conference, Vol. I,
Oslo, 1967, pp. 239-242.
[8] Hirschfeld, R. C. and Poulos, S. J. in Laboratory Shear Testing of Soils, ASTM STP
351, American Society for Testing and Materials, pp. 329-341.
[9] Blight, G. E., Canadian Geotechnical Journal, Vol. 5, No. 3, Aug. 1968, pp. 142-149.
[10] Doyle, E. H., "Influence of Strata Orientation on the Shear Strength of Varved Silt,"
unpublished M.S. thesis, University of Rhode Island, Kingston, R.I., 1968.
[11] Lambe, T. W., Journal of the Soil Mechanics and Foundation Division, American
Society for Civil Engineers, Vol. 84, No. SM2, Paper 1654, May 1958, pp. 1-34.
[12] Fahlquist, F. E. in SoilMechanics 1941-1953, Boston Society of Civil Engineers, Boston,
1953, pp. 20-44.
[13] Lowe, J., III, and Johnson, T. C. in Proceedings, American Society of Civil Engineers
Research Conference on Shear Strength of Cohesive Soils, Boulder, Color., 1960,
pp. 819-836.
[14] Andersen, A. and Simons, N. in Proceedings, American Society of Civil Engineers
Research Conference on Shear Strength of Cohesive Soils, Boulder, Colo., 1960,
pp. 695-709.
T. F. Z i m m i e ' a n d L. J. A l m a l e h ~
Shrinkage of Soil Specimens During

Preparation for Porosimetry Tests
REFERENCE: Zimmie, T. F. and Almaleh, L. J., "Shrinkage of Soil Specimens

During Preparation for Porosimetry Tests," Soil Specimen Preparation for Laboratory
Testing, ASTM STP 599, American Society for Testing and Materials, 1976, pp.
202-215.
ABSTRACT: Various methods of removing moisture from small soil samples were
investigated. The samples were to be tested by mercury porosimetry, and one
requirement is a constant volume drying process. Air-drying, oven-drying and freeze-
drying procedures were used. Three different clay types were used: kaolinite,
montmorillonite, and an illite. The clays were fully saturated, and compaction was
achieved by using static pressure.
Freeze drying is the best practical method of drying the soil samples, as it produces
the least amount of shrinkage in the soil. In certain instances, air drying and oven
drying may produce satisfactory results. Total drying time for freeze drying can
be accomplished in 5 to 10 h.
A simple laboratory freeze-drying system is described and operating procedures
and principles discussed.
The results are applicable to the preparation of small size soil samples where it is
desired to remove soil moisture and, at the same time, minimize disturbance to the
soil structure.
KEY WORDS: soils, samples, clays, shrinkage, drying, freezing, moisture content,
vacuum, mercury porosimetry, tests
In order to obtain pore size distribution measurements on soil by the

use o f mercury porosimetry, almost all moisture must be removed from
the soil. During the conduct o f a porosimetry test, the soil sample is
subject to a v a c u u m prior to the intrusion of mercury into the soil pores.
At typical natural water content, the vacuum will cause the water to
vaporize, often disintegrating the sample but, in any case, rendering the
pore size measurements useless. At lower water contents, on the order o f
a few percent, the soil moisture can cause errors in the pore size measure-
ments since water is essentially incompressible even at the pressures
utilized for mercury porosimetry. The water content must be reduced to
1Assistant professor and graduate student, respectively, Rensselaer Polytechnic Institute,
Troy, N.Y. 12181.
Copyright9 1976by ASTM International www.astm.org
ZIMMIE AND ALMALEH ON POROSIMETRY TEST SPECIMENS 203
a low value, less than a percent, prior to the performance of a porosimetry

test.
Although this research was conducted for the purpose of determining
the most practical method of sample preparation for mercury porosimetry
tests on clays, the results and methods reported herein would be ap-
plicable to other areas of study where soil moisture must be removed
without disturbing the soil structure and interparticle arrangement, for
example, electron microscopy.
Various methods of soil dehydration are available. Oven drying and
air drying are two of the most common methods, but, in general, they
are not very satisfactory as constant volume dehydration procedures.
Surface tension forces produced by the air-water menisci cause large
amounts of shrinkage, and this structural disturbance effects the pore
size arrangement also.
Critical-region dehydration has been reported to yield successful results
relative to volume change [1-2]. 2 With this method, the soil sample is
subjected to slowly increasing temperature and pressure, regulated to
keep the water in the pores liquid until the critical region is reached. Then
careful regulation of temperature allows vapor transfer to an adjacent
vessel. Since critical conditions occur at about 245 atm and 380 ~ there
is some question about the possibility of modifying the clay minerals.
In most cases, critical-region dehydration is not a practical method of
moisture removal because of the apparatus and procedures required.
Freeze-drying techniques have been used to dehydrate soil samples in
an attempt to obtain a constant volume drying process and retain the
original soil structure [2,3,4]. Vacuum freeze drying consists of rapidly
freezing a specimen and then subjecting it to a vacuum so that the
moisture, in the form of ice, is removed by the process of sublimation.
The triple point of water occurs at a pressure of 4.6 mm Hg and about
0~ Only at the triple point can solid, liquid, and vapor phases exist
simultaneously. At pressures less than 4.6 mm Hg and temperatures below
0~ water can only exist in the solid or vapor form. This sublimation
region is of interest in freeze drying, since water can be directly removed
by changing from the solid state to the vapor phase, that is, sublimation.
Reference can be made to numerous general thermodynamic texts and
chemistry texts for further details on phase diagrams and changes of state.
The success of freeze drying is attributed to the fact that, after freezing,
no shrinkage takes place, at least under ideal conditions, since surface
tension forces caused by the air-water menisci have been eliminated.
As a result of this research, it is concluded that vacuum freeze drying is
the best practical method of dehydrating soil samples in preparation for
mercury porosimetry testing. Therefore, the results and procedures used
2The italic numbers in brackets to refer to the list of references appended to this paper.
will be discussed hereinafter as they apply to the preparation of small size

(volumes of a few cubic centimetres) soil samples. It is beyond the scope
of this paper to cover the subject of freeze drying in detail, and the
reader is referred to other general articles for a more thorough discussion
of freeze-drying techniques [5, 6].
Equipment
General Considerations
The basic elements required for a vacuum freeze-drying system consist
of a specimen container to hold the sample, a condenser or cold trap to
condense the moisture removed from the sample, and a vacuum pump.
A vacuum gage in the system can be considered a convenient addition
in order to monitor the operation. The freeze-drying apparatus used in
this project is shown in Fig. 1, and the basic dements just mentioned
FIG. 1--Freeze-drying apparatus; A--Specimen container, B--Vacuum gage, C--Con-

denser, D m Vacuum pump.
can be identified. This simple and economical laboratory freeze-drying

system is very adequate for small size soil samples.
Commercial freeze-drying units are available, and they will contain the
same basic elements as those just mentioned. In addition, convenience
features may be obtained, such as automation and monitoring devices.
The commercial units are designed normally for handling large volumes
of sample on the order of litres, and, as a result, both initial and operating
costs o f a commercial unit will be higher than the costs for a simple
laboratory system. To the best o f the authors' knowledge, there is no
commercial freeze-drying apparatus available that is specifically tailored
to soils work, and, in most instances, a system similar to the one used
in this project will be satisfactory for freeze drying small volumes o f
soil. Relative to performance, the final freeze-dried product will be
identical whether a commercial unit or apparatus similar to that shown
in Fig. 1 is used, as long as the system characteristics are comparable.
That is, if comparable samples, vacuums, temperatures, refrigerants, and
times are used, the results will be comparable.
Apparatus
The specimen container consisted of a 250-ml glass jar, able to withstand
a vacuum (Fig. 2). In order to minimize handling, the soil samples were
placed on a cage, immersed in liquid nitrogen until frozen, and then
placed in the jar along with the cage. The cage consisted of stainless steel
wire and aluminum screen, since the metals must be resistant to cryo-
genic temperatures. Normally, three soil samples were dried at a time.
However, the volume of the jar and the capacity of the system are
sufficient to produce 10 or 20 samples at a time.
After soil samples are frozen, the freeze-drying process must begin
rapidly so that melting does not occur. The 250-ml jar could be evacuated
in a matter o f seconds, and there was no danger of the samples melting.
A larger volume jar might necessitate a larger vacuum pump or a vacuum
ballast or both in order to produce a vacuum quickly. The system should
be evacuated in about 15 s to be certain that no sample melting occurs.
The vacuum gage utilized was a diaphragm type gage, accurate to about
2 nun Hg. This type o f gage is not precise enough to read the actual
vacuum in the system. Where precise vacuum readings are desired, special
purpose vacuum gages must be used [6]. However, the diaphram gage in
the system can be calibrated against a precision vacuum gage to establish
a zero point, that is, the operating pressure of the system. Then loss o f
vacuum caused by slight leaks or similar problems can be detected easily.
This was the purpose of the gage shown in Fig. 1.
The condenser consisted of a Dewar flask, suitable for cryogenic
liquids, which held the refrigerant, and a commercial vacuum pump
protector. The vacuum pump protector consisted of two compartments,
the first, a condenser compartment which is immersed in the refrigerant
to freeze out the sample moisture, and, the second, a compartment filled
with a chemical dessicating agent to prevent water vapor from entering
the vacuum pump. In order to maintain a proper vacuum, the dessicant
FIG. 2--Specimo7jar for freeze drying.
must be maintained or renewed periodically. Some water vapor will still

pass through to the vacuum pump, and the pump oil must be checked
and changed periodically to remove water from the oil in order to main-
tain the proper vacuum.
The use of different condenser refrigerants will be discussed. However,
if liquefied gases are used as a refrigerant, a Dewar flask, resistant to
cryogenic temperatures, is required to hold the liquid gas. If dry ice and a
solvent such as acetone or alcohol are used as a refrigerant, laboratory
beakers o f the Pyrex type are sufficient. During operation, the condenser
is surrounded with a thick layer o f foam insulation. This minimizes heat
leak and loss of refrigerant.
The vacuum pump was a c o m m o n laboratory Cenco Pressovac 4 pump
available from the Central Scientific Co., Chicago, Illinois. The rated
pumping capacity is 10 litres per minute free air displacement at normal
operating speed, and the nameplate rating states that the pump will
produce a vacuum of 0.015 mm Hg (0.015 torr) or better. In practice,

pumps of this type are capable o f producing much better vacuums, as
low as 0.001 torr in leak-free systems. In an ideal system, water in the
liquid state will not form if the pressure remains below 4.6 mm Hg.
However, above 0~ the ice will turn to vapor, rupturing the sample.
Even at temperatures below 0 ~ the subliming water vapor can become
trapped in pores, causing a local increase in pressure, and the vapor can
condense to the liquid phase. This becomes more probable as the system
pressure approaches 4.6 mm Hg. Therefore, in practice, a vacuum lower
than about 0.015 m m Hg should be maintained. This can be easily
attained with the system and equipment shown in Fig. 1.
The device shown in Fig. 3 was used for volume measurements on the
FIG. 3--Volume measuring device for soil samples.
soil samples. The dial gage can be read to 0.002 ram. The gage force is
only about 50 g, and this force can be reduced by applying a slight
squeezing force to the top extension o f the gage arm as the gage arm is
brought into contact with the sample. As a result, even the softest soil
could be measured without disturbance. The performance o f the volume
measuring device was quite satisfactory, and the measurements were con-
sistently reproducible. George [7], in his shrinkage studies on soil-cement
mixtures, obtained satisfactory results using a dial gage measuring device
similar in concept to the one used for this project. A precision micrometer
accurate to 0.002 m m and a caliper accurate to 0.002 m m were also tried

as volume measuring devices. However, the use o f micrometer devices
were abandoned, as the measurements could not be reproduced very
precisely. A h m e d et al [4] have also reported difficulties in obtaining
volume measurements using micrometers.
Specimens
Most of the tests were performed on two clays, a kaolinite and a sodium
montmorillonite. These clays were selected because they have very differ-
ent properties. In fact, they represent opposite ends of the spectrum
normally encountered. One series of tests were performed using a local
illitic clay o f glacial origin in order to ascertain that results that were
similar to those for the kaolinite and montmorillonite samples could be
obtained. The properties o f the clays are presented in Table 1, and the
hydrometer grain size analysis for the kaolinite is shown in Fig. 4.
TABLE l----Characteristicsof soils used.
Sodium
Property Kaolinite Montmorillonite Illitic Clay
The Georgia Kaolin In situ sample
Co., Dry AmericanColloid eastern New
Supplier Branch, Ga. Co., Chicago, Ill. York State
WL, o70 39 "~500 43
We, % 26 85 29
Specific gravity 2.65 2.70 2.80
Percent finer than #200 sieve 98 95 99.6
Percent finer than 20 t~m 96 90 98
Percent finer than 0.5 lam 67 85 80
The clay samples were remolded with sufficient water to assure com-
plete saturation. The clays were compacted by using a static procedure.
Different pressures were utilized to produce various water contents. The
clays were placed in a standard Proctor mold (volume approximately 1000
cm3), and static pressure was applied by jacking. The compaction was
carried out in stages until the final pressure was reached. The final static
pressure w a s a b o u t 700 k N / m 2 for the highest water contents and about
2800 k N / m 2 for the lowest water contents. Consistent procedures were
used in the mixing and compaction processes, and, for each clay type, the
final water contents and void ratios could be satisfactorily duplicated to
within a few percent. After compaction, the load was removed f r o m the
soil, and the soil was allowed to rebound and come to equilibrium. The
length o f the compaction period ranged f r o m one to three days.
ZIMMIE AND ALMELEH ON POROSIMETRY TEST SPECIMENS 209
I00
~ II I I [ i i]1 [ i E i ~ tl}l
I
i i i i t
90
BO
70
60
I-- 5 O
~40
~ 3o
~ 2O
IAI
z_
u. I 0
13 lill I J I I~ll I i__l llllll ] I I Illll I t III II I I I

.01 .O01 .OOOI .00001 . O00001
DIAMETER (MM)
F I G . 4--Grain size distribution for kaolinite.
Samples for testing were taken from the center of the soil mass, where
they were of uniform water content and void ratio. The outer portions
of the soil mass tended to be more nonuniform than the center. Cube
samples about 7 mm on a side were formed by trimming with a thin wire
cutter.
Procedure
The oven-dried samples were dried at l l0~ and the air-dried samples
at room temperature (20 ~
The samples to be freeze dried were placed on a cage (Fig. 2) and
immersed directly into liquid nitrogen, where they froze in about 5 to 15 s.
It is important that the samples be frozen rapidly and at temperatures
below - 130~ to avoid the formation of ice crystals which can damage
the soil structure [2]. To attain the low temperatures, liquefied gases must
be used, usually liquid nitrogen. When a sample is placed in a liquefied
gas, bubbling occurs from the heat transfer, and the sample becomes
surrounded by a thermally insulating layer of gas which tends to retard
the freezing process. In order to avoid this relative delay in freezing, the
samples can be immersed directly into intermediate cooling liquids, for
example iso-pentane cooled by liquid nitrogen [6]. For the small size
samples used for mercury porosimetry tests, this refinement is not required,
as freezing occurs rapidly. However, if large soil samples are to be frozen
for other applications, the use of intermediate cooling liquids may be
required.
About 30 percent of the samples exhibited large cracks, heaves, and

similar disruptions after freezing in liquid nitrogen (Fig. 5). There did not
appear to be any predictable pattern to the cracking, and it occurred
equally at all water contents and with all the clay types. Accurate volume
FIG. 5--Cracked samples after freezing in liquid nitrogen," 0eft) montmorillonite,

(right) kaolinite; 7-ram cubes.
measurements could not be obtained on cracked samples, and although

porosimetry tests could be run on cracked samples, the results would be
questionable. Therefore, the easiest solution was to allow for a number of
cracked samples and discard them when cracking occurred.
After freezing, the samples were quickly placed in the specimen jar and
the vacuum applied. This transfer operation and the subsequent application
of vacuum must occur rapidly to prevent the sample from melting. As
mentioned in an earlier section, the system could be evacuated in a matter
of seconds, and there was no danger of melting.
The specimen jar remained exposed to room temperature as shown in
Fig. 1. Sublimation is an evaporative process accompanied by cooling, so,
although the specimen container is exposed to room temperature, the
sample temperature will remain well below freezing. The soil samples were
placed on the cage inside the specimen jar, never in direct contact with
the glass. Samples should not make contact with the glass if the specimen
container is exposed to temperatures above freezing, as heat conducted
through the glass could cause sample melting. These observations were
confirmed by using copper-constantan thermocouples inserted into a
number of soil cubes.
The refrigerant used in the condenser was a mixture of acetone and
dry ice ( - 79 ~
After the freeze-drying operation was completed, volume measurements
were made and the samples were oven dried to determine the amount of
moisture remaining after freeze-drying. The above procedure was followed

after drying because this study was conducted to investigate sample
preparation techniques. However, samples to be used for porosimetry
tests are transferred to a glass vacuum dessicator where they can be stored
for lengthly periods. Freeze-dried samples should be exposed to ambient
room conditions for minimal times, since the soil will absorb moisture
rapidly. Montmorillonite can absorb large amounts of moisture, negating
the freeze-drying operation. Kaolinite will absorb much less moisture, and
this can be removed by conventional oven drying without any further
volume change. Nevertheless, as a general rule, freeze-dried samples should
be stored in a moisture-free environment.
Experimental W o r k
R a t e o f Freeze Drying
Freeze-drying times of 5 to 6 h were required for the kaolinite clay, and

9 to 10 h for the montmorillonite. Typical results showing the rate of
moisture removal from kaolinite are presented in Fig. 6. The shape of the
curve is characteristic of the freeze-drying process [8], and, for the
kaolinite, an initial constant-drying rate occured for about the first 3 h,
followed by a falling-rate period from 3 to 6 h.
o 50 i KAOLINITE
t-
g_
~ 2o
~ ,o
0 [ I I I L ~ I
0 I 2 5 4 5 6 7
FREEZE DRYING TIME I HRS.)
FIG. 6---Typicalrate of freeze-drying curve showing soil water content versus time.
Kearsey et al [9] have developed an equation for predicting the rate

of ~ublimation of a slab of ice contained in such a manner that evaporation
can occur from one face only. The rate of sublimation is given by
G = 3600yV(M/2nRT)P (1)
where
G = rate of evaporation in grams per square cm of surface per hour,
y = evaporation coefficient,
M = molecular weight,
R -- gas constant in dyne cm per mole per ~
P = vapor pressure of pure ice at the temperature of evaporation, and
T = temperature in K.
Assuming y to be unity and expressing P in mm of mercury Eq 1 reduces
to
G = 544(PA/--T) (2)
Under ideal conditions, the maximum rate of sublimation will occur at

0~ and a vapor pressure of 4.6 mm Hg (4.6"t:orr). From Eq 2 this rate
is found to be about 150 g/cm2/h. Assuming a sample temperature of
- 3 0 ~ with the corresponding vapor pressure of 0.29 torr, the rate of
evaporation is found to be about 10 g/cm2/h. If one assumes that evapor-
ation occurred on all faces of the 7-mm cube sample of Fig. 6, the rate
of moisture removal was approximately 0.01 g/cm2/h, several orders of
magnitude less than the ideal. Strictly speaking, the above equations are
not applicable to porous media; however, they do show that the rate of
evaporation is dependent on the vapor pressure and temperature of the
sample. In practice, operating temperatures and pressures will be well
below 0~ and 4.6 torr. Operating pressures have been discussed pre-
viously in the apparatus section, and a margin of safety must also be
observed with temperatures to prevent sample melting. However, if the
sample temperature is too low, the rate of sublimation will also be low.
In the freeze-drying experiments of Ahmed et al [4], the specimen con-
tainer was immersed in a refrigerant ( - 4 0 ~ to prevent sample melting,
and liquid nitrogen was used as a condenser refrigerant. Equations 1 and
2 indicate a low rate of evaporation using this method; however, a series
of experiments were performed to determine the amount of sample
shrinkage incurred. The sample jar was placed in an acetone-dry ice bath
(-79~ and the condenser fluid was liquid nitrogen. The procedures
used were the same as outlined by Ahmed et al [4], and total drying times
of about 17 h were required for kaolinite and montmorillonite. Ahmed et
al [4] reported drying times of 12 to 18 h on a Grundite clay.
The shrinkage values obtained were slightly less when the specimen jar
was immersed in a refrigerant; however, no special significance should be
attached to the slight differences in shrinkage values.
There appears to be no advantage to immersing the specimen jar in a
refrigerant. On the other hand, the drying time is extended considerably.
As pointed up previously, there is little danger of small soil samples melt-
ing if the specimen container is exposed to room temperature.
Results
The results of drying tests on approximately 100 soil samples (cubes
7 mm on a side) are presented in Fig. 7. Each data point represents the
AIR DRIED 9
OVEN DRIED 9
FREEZE DRIED 9
30 KAOLINITE MONTMORILL ONTE
T
2s
I
~ 2o NOTE * AIR DRIED I OVEN DRIED
z 15
.I-
u
f SAMPLES DISINTEGRATED.
IO
o 5 11/ ~yl 9 &
0
I1~'
I
IO
I
20 30
I
9
40
I
9
I
50
I
60
I
I00
I
9
150
I I I
200
I
250
I I I
300
WATER CONTENT: % DRY WEIGHT OF SOIL
FIG. 7--Volume change versus water content f o r various drying methods.
mean of a test series. In addition, 15 to 20 pilot tests were performed

to develop techniques, establish drying rates, and check procedures.
Freeze drying produced the best results, that is, the least amount of
shrinkage at all water contents. However, results comparable to freeze
drying could be obtained by oven drying and air drying kaolinite samples
with very low water contents. Montmorillonite samples must be freeze
dried. Virtually all air-dried and oven-dried samples of montmorillonite
disintegrated upon drying due to the large amount of shrinkage that
occurred (Fig. 8).
FIG. 8--Typical montmorillonite samples after drying (left)freeze dried, 7 mm cube;

(center) air dried; (right)oven dried.
A series of the illitic clay samples were freeze dried for comparative
purposes. The water contents were 38 percent, and the mean final shrinkage
value was about 5 percent, a value similar to that obtained for kaolinite.
The shrinkage values for the clays can be considered to represent the
absolute volume change due to drying procedures. Volume measurements
were made on a number of samples after freezing in liquid nitrogen, and
the amount of expansion measured was negligible. Rosenqvist [3] has
reported a value as high as 3 percent expansion when an undisturbed soft
Norwegian marine clay was frozen, and this is probably the highest value
that Would be normally encountered.
For freeze-dried samples, a final water content of 0.5 percent or less
was considered a dry sample. Freeze-dried samples absorb moisture
rapidly; rates of 2 percent water content per minute have been reported [6].
Thus, the sample absorbs moisture even during the weighing process.
Practically speaking, there is no necessity for removing the last 0.5 percent
moisture, since the sample will be exposed to the atmosphere while being
transferred to the mercury porosimeter chamber.
Conclusions
Vacuum freeze drying is the best practical method of preparation of soil
samples for mercury porosimetry tests. Adequate drying can be accom-
plished in 5 to 10 h.
In certain instances, air drying and oven drying may produce satisfactory
samples for use in mercury porosimeter tests.
This research was primarily intended to study soil sample drying
methods for porosimetry testing. However, the results and methods are
applicable to other areas where it is necessary to produce dry soil samples
with minimal structural disturbance.
Acknowledgments
The authors wish to thank T. C. Engel and D. E. Moellman, graduate
ZIMMIE AND ALMALEH ON POROSlMETRY TEST SPECIMENS 215
students at Rensselaer Polytechnic Institute, for their valuable assistance

during this project.
References
[1] Sridharan, Asuri, Altschaeffl, A. G., and Diamond, Sidney, Journal of the Soil
Mechanics and Foundations Division, American Society of Civil Engineers, Vol. 97,
No. SM5, May 1971, pp. 771-787.
[2] Gillott, J. E., Journal of Sedimentary Petrology, Vol. 39, 1969, pp. 90-105.
[3] Rosenqvist, I. T., Journal of the Soil Mechanics and Foundations Division, American
Society of Civil Engineers, Vol. 85, No. SM2, April 1959, pp. 31-53.
[4] Ahmed, Syed, Lovell, C. W. Jr., and Diamond, Sidney, Journal of the Geotechnical
Engineering Division, American Society of Civil Engineers, Vol. 100, No. GT4, April
1974, pp. 407-425.
[5] Meryman, H. T., New York Academy of Science Annals, Vol. 85, March-May 1960,
pp. 630-640.
[6] Rowe, T. W. G., New York Academy o f Science Annals, Vol. 85, March-May, 1960,
pp. 641-679.
[7] George, K. P., Highway Research Record, No. 255, 1968, pp. 42-58.
[8] Broughton, Geoffrey in Technique of Organic Chemistry, Vol. III, 2nd Ed., Arnold
Weissberger, Ed., Interscience Publishers, New York, 1956, Chapter VI, pp. 787-839.
[9] Kearsey, H. S., Strickland-Constable, R. F., and Bruce, E. W. in The Institute of
Refrigeration, Imperial College of Science and Technology, Session 1953-1954,
pp. 5-15.
A. R. Booth'
Compaction and Preparation of Soil

Specimens for Oedometer Testing
REFERENCES: Booth, A. R., "Compaction and Preparation of Soil Specimens for

Oedometer Testing," Soil Specimen Preparation for Laboratory Testing, ASTM STP
599, American Society for Testing and Materials, 1976, pp. 216-228.
ABSTRACT: The paper describes the development of a method for the compaction of
groups of identical pedometer specimens. Groups were compacted from several soils at
various densities and moisture contents. The specimens in each group were tested later
in the pedometer over the complete range of initial saturations, and it was important
that they should be as near as possible to identical after compaction.
The paper considers, by means of a literature review, the various methods of compaction
available. The conclusion reached is that the static method is most suitable for compaction
of relatively thin specimens. Soil was compacted directly into the pedometer rings under
static loading. The advantages and disadvantages of this approach are discussed.
A special mold developed for this purpose is described in detail. This enabled a
known mass of soil to be compacted into a 76.2 by 19.05-mm-thick specimen. The
procedure used in the laboratory is outlined.
It was necessary to allow most specimens to either increase or decrease in moisture
content after compaction so that pedometer tests could be carried out over the complete
range of saturation. The procedures followed are described, and it is stressed that these
model as closely as possible what would happen in a road embankment.
Finally, the paper considers the dry densities of groups of specimens immediately
prior to being placed in the pedometer. It is shown that variations within each group
are lower than those found in undisturbed samples, and it is concluded that the
standardized method produced groups of specimens which were closer to identical than
would have been obtained by other methods. This, in turn, enabled the influence of
other variables, principally the compaction moisture content and initial dry density, to
be studied with more confidence.
KEY WORDS: soils, compaction, embankments, collapse settlement, consolidation,

pedometers, density, partial saturation, roads
T h e r e h a v e b e e n several failures o f r o a d e m b a n k m e n t s in s o u t h e r n A f r i c a
in r e c e n t y e a r s w h i c h c a n b e a t t r i b u t e d t o c o l l a p s e s e t t l e m e n t w i t h i n t h e c o m -
p a c t e d f i l l i n g , f o l l o w i n g w e t t i n g [1]. 2A r e s e a r c h p r o j e c t w a s i n i t i a t e d t o d e t e r -
mFormerly, chief research officer, National Institute for Road Research, Pretoria, South
Africa; presently, senior engineer, Duff and Geddes, Edinburgh, Scotland.
The italic numbers in brackets refer to the list of referencesappended to this paper.
216
Downloaded/printed by ASTM International www.astm.org
Copyright + 1976by
BOOTH ON SOIL SPECIMENS FOR OEDOMETER TESTING 217
mine how variations in the conditions imposed during construction affect the
subsequent settlement of the filling, particularly following wetting. The results
of this investigation are being reported elsewhere [1,2].
The experimental work was carried out in the laboratory, using standard
76.2 by 19.05-mm oedometer specimens. These were loaded, partly saturated,
and soaked, at a particular pressure, in the same way as the partly saturated
half of the double oedometer test [3,4]. Several soils were tested, and variations
were made in the initial dry density, the compaction moisture content, and the
maximum applied pressure. For each combination of imposed conditions, a
group (usually between 6 and 24 in number) of specimens was tested over the
full range of saturation, including one or two under water to represent full
saturation.
Since this work related to road embankments, the oedometer tests were carried
out on compacted soils. In order to make valid comparisons between the results,
it was essential to devise a method of preparation that produced a group of
specimens that were as close to identical as possible after compaction. Most
specimens were loaded at a moisture content other than that used for compac-
tion, and a conditioning procedure was necessary to allow increases or reduc-
tions in moisture content in a way that modelled, as closely as possible, such
changes in the field.
This paper describes the methods that were adopted for the compaction and
conditioning of the oedometer specimens. It also considers the uniformity of
specimens and groups of specimens in the light of the results obtained.
Choice of Compaction Method

Several investigations into the merits of different compaction methods
have been reported. Leonards [5], quoting Mayo [7], used only static compac-
tion to prepare his specimens. A Proctor penetration needle was used to detect
variations in unit weight in a 2.5-in. (63.5-mm) high specimen, compacted
statically. It was found that a diameter of 10 in. (254 mm) was necessary in
order to reduce side friction to the point where the variation in unit weight
within a specimen was less than 0.5 percent.
Dawson [7] measured variation in density within specimens compacted
in layers by dynamic methods in standard 4 and 6-in. (101.6 and 152.4-mm,
respectively) diameter molds. The average density in the bottom third of
the mold exceeded that in the top third, by over 2 percent in some cases.
Dawson cut his specimens carefully into a number of pieces to measure these
variations.
Whitman et al [8] found that static compaction methods gave substantial
density variations within specimens, with a height to diameter ratio of unity.
When this ratio was reduced to 1"2, the density variations ceased to be signifi-
cant.
Shackel [9] devised a nondestructive method of measuring density, using
gamma rays, and could thus measure densities every 0.4 in. (10.2 mm) along
the axis of 4-in. (101.6-mm) diameter specimens compacted statically. He
found significant variations in the density, which increased considerably
when the height to diameter ratio rose above unity.
Gau and Olson [10] compared dynamic, static, and kneading compaction
by means of a miniature penetrometer and concluded that the static method
gave the most uniform specimens, though kneading may be more representative
of field conditions. They agreed with Leonards [5] that greatest uni-
formity is achieved by static compaction in one thin layer.
The general conclusion reached is that static compaction gives the most
uniform specimens, and it as decided therefore to use this to prepare the
oedometer specimens. It is recognized nevertheless, that there may be differences
in the fabric and engineering properties of specimens compacted by other
methods [11].
Construction of Mold
The soils used for the oedometer tests were essentially sandy with a
relatively small proportion of finer particles (Fig. 1). When cutting oedo-
meter specimens from blocks of these soils, it was found that a good deal
of lack of fit occurred at the edges. It was decided therefore to compact
the soil directly into the oedometer ring and accept any slight variation in
density due to side friction. There is also the risk of built-in stresses within
the soil and, more particularly, between the soil and the ring, but silicone
grease was used in an attempt to reduce these.
The mold used for compaction of the specimens is shown schematically in
Fig. 2. It consists of a cylinder of 76.2 mm internal diameter, into which a
standard oedometer ring fits so that the inside faces are flush. Pistons can be
inserted at each end of the mold and are provided with flanges to prevent
them entering the oedometer ring. The mold splits on both vertical and hor-
izontal planes to facilitate the removal of the ring. The vertical joint is neces-
sary because otherwise even slight distortion of the ring during compaction
could lock it in the mold. The horizontal joint is arranged so that the ring is
still supported when the top half of the mold is removed, thus preventing
the ring sliding off the specimen. Figure 3 shows the mold with one side re-
moved to demonstrate the position of the ring.
No drains were provided in this mold since all specimens were compacted
well below the saturation moisture content. Air escapes between the piston
and the mold, provided the former is not inserted too rapidly.
Both the mold and the pistons were made of brass, chosen because of its
low cost and ease of machining during the development period. A large num-
ber of identical oedometer rings were also made from brass. The brass has
not been marked badly by the soil during compaction, but a harder surface
would be advisable if high densities were being used.
SIEVE NUMBERS 200 I00 60 40 2O IO

I00 I I I I
90
8O I SOIL Z - - ~
//
.of
x
7o
60 I /
//
z
u_
50
I j,1
/
/ /
~S'OIL Y
i!
I~ 1/ 7 6
z 30
zo
0-002 0-006 0"02 0-06 0-2 0"6 2

PARTICLE SIZE mm (log scole)
SOIL X DECOMPOSED GRANITE FROM NORTH-EASTERN TRANSVAAL

SOIL Y DECOMPOSED SANDSTONE FROM DURBAN
SOIL Z DECOMPOSED QUARTZITE MELSETTER, RHODESIA
FIG. l--Particle size distribution o f soils tested in the oedometer.
Method of Compaction
The mold was simple to use, and a group o f six specimens took about
2 h to make. The same sequence was used throughout.
The soil was stored dry, having first been wet sieved through a 2 mm
screen. Rather more dry soil than was actually necessary for the number o f
specimens being made was weighed in a bowl o f known weight to an accu-
racy of 0.1 g. Water was added to give the required moisture content and
worked in by hand until the operator was satisfied that it was distributed
evenly. This was not difficult with the types of soil being used. The wet soil
was reweighed to determine the exact moisture content and stored in an
air-tight bag while the amount required for each specimen was calculated.
The assembled mold was placed on the bench with the oedometer ring and
bottom piston in place, the inside faces having been greased sparingly. The
necessary amount o f soil, weighed to an accuracy of 0.01 g, was put into the
mold as shown in Fig. 4. This was probably the step at which the greatest lack
of uniformity occurred, and considerable care was essential to ensure an even
1--,o..o.o-1
2 - ~ i i ' MOLD
'~L~. -tl ",, ~ ~ MOLD SPL,'rs
_L~ \OEOOMETER
IN PLACE
R,NG
i .~,..~../BOTTOM PtSTON
I I
CROSS SECTION THROUGH MOLD AND PISTONS
MOLD SPLITS
ON THIS LINE
PLAN ON MOLD
All dimensions in mm
FIG. 2--Arrangement of mold for compaction of 76.2-ram-diameter by 19.05-ram-thick

oedometer specimens.
distribution of soil. The top piston was inserted and pressed home to compact
the soil into the ring, as in Fig. 5. At higher densities, it was helpful to maintain
the compacting pressure for some time to reduce rebound, and probably
this would be essential if less permeable clayey soils were being compacted.
Removal of the ring and specimen from the mold was relatively easy. The
top piston and top part of the mold were removed (as shown in Fig. 6) and a
porous disk placed over the end of the ring. The whole assembly was inverted,
so that the disk supported both the ring and specimen. The other piston and
the rest of the mold were removed, leaving the specimen in its ring standing on
the porous disk. (Each piston was given a slight twist before being pulled away
from the soil to release fine particles adhering to the face.)
FIG. 3--Mold partly assembled, showing position of ring.
Adjustment of the Degree of Saturation

The testing program required that a group of specimens, identical im-
mediately after compaction, should be tested in the oedometers over the range
of saturations. (It was found to be more convenient to work in terms of the
initial degree of saturation, rather than in terms of moisture contents.) Speci-
mens to be tested at 100 percent saturation were soaked throughout the test
as in the standard consolidation test. All other specimens were loaded, partly
saturated, at constant moisture content, as usual for the partly saturated half
o f the double oedometer test [4,12]. Loads were applied at intervals in log-
arithmic steps up to the chosen maximum, 440 k N / m 2, for most groups of
specimens. At the end of compression under this load, the oedometers were
flooded and the collapse settlement measured.
For those specimens where the selected degree of saturation was higher than
at compaction, it was necessary to introduce additional moisture into the soil.
Specimens were allowed to stand in a humidity room until they had a moisture
content slightly above that required, and, with a little experience, it was possi-
ble to judge the length o f time needed to achieve this. The specimen was then
transferred to a dry porous disk and treated in exactly the same way as those to
to be dried immediately after compaction.
FIG.4--Mold assembled and containing loose soil readyfor compaction.
The behavior of the specimens in the humidity room differed from soil to
soil. In some soils, there was a slow increase in moisture content, suggesting
that it was rising simply by condensation on the exposed surface. Other soils
gained moisture rapidly and, if left in the humidity room, swelled quite con-
siderably within 89 h. The top surface always took a domed shape, presuma-
bly because swelling radially was giving rise to frictional stresses between the
soil and the ring. Specimens which swelled in this way were rejected without
being tested.
The drying part of the process took place in the air-conditioned laboratory.
The specimen, on a porous disk, was allowed to stand in the open and dry
slowly. The process was easy to control by weighing the specimen, including
ring and porous disk, until the mass fell to that required. Possible shrinkage
during drying was checked in many cases by measuring the thickness before
and after the drying stage, but differences were never found in excess of
0.5 percent and were usually much less.
When the required saturation had been reached, the specimen, still on its
disk, was placed in a double polythene bag and stored in the humidity room.
Where possible, this storage extended for at least four days to allow time for
the moisture to distribute more equally within the specimen.
Adjusting the moisture content means following different stress paths,
which may affect the test results to some extent [13]. There is, however, no
other way of bringing the specimens to different initial conditions, and the
methods do, in fact, model changes of moisture content in the field. These are
likely to occur most readily shortly after compaction, before the addition of
more filling.
FIG. 5 - - Top piston being inserted into mold to compact soil.
Comparison of Specimens
The success of the method of compaction and conditioning can be con-
sidered in terms of the dry densities of groups of specimens, The actual dry
density of each specimen immediately prior to testing was calculated, based
on the thickness measured at the time and the mass of the dry soil at the end of
the test. The mean dry density of each group was then determined, though this
differed from that intended by up to 3 percent in extreme cases. As a general-
ization, the mean dry density achieved exceeded that intended when this was
relatively low but, at higher densities, the reverse applied. Increases in the
compaction moisture content gave only marginally higher dry densities.
Specimens were assumed to be sufficiently close to identical if the dry den-
sity was within 1 percent of the mean for that group. A total of 506 specimens
were made and conditioned, as described in this paper (a number of others
were subjected to a cyclic conditioning procedure [1]). These were divided
into 37 groups of between 5 and 72 specimens, though only 6 groups had more
FIG. 6--Mold partly dismantled showing soil compacted into oedometer ring.
than 12. Of these specimens, only 39 fell outside the 1 percent limits. Only 5
groups had more than 15 percent unsatisfactory specimens, and more than
half the groups had none at all [1].
Specimens were also prepared from undisturbed samples taken in the field,
both of natural residual soils and of embankment filling. Sixty-six specimens
were cut from two natural soils and three embankment fills, of which 37 fell
outside the I percent limits. The uniformity within individual specimens can-
not be quantified, but, in purely subjective terms, the laboratory compacted
specimens appeared to be much more homogeneous than those obtained
from the field.
Effect on Results
The test results are not discussed in any detail here, as this has been done
elsewhere [1,2]. Sufficient data will, however, be presented to demonstrate
that the results obtained were adequate for the study being carried out.
The basic analysis was considered in terms of the collapse occurring on
wetting as a function of the moisture content during loading, and it was found
that curves could be plotted. Figure 7 shows such a plot for specimens cut
from a naturally occurring collapsing sand from Durban. The scatter of
points is considerable, though not such as to make the drawing of a curve
impossible. Figures 8 and 9 are typical examples of the plots for groups of speci-
mens compacted in the mold. Figure 8 shows a case where the scatter of points
is at its worst, whereas Fig. 9 is one of the better plots obtained. In neither case
does the scatter of results cause any problems in interpretation.
It might be thought that the scatter of results in Fig. 8 was due to variations
0"14 --
% •
0"12 --
Z COLLAPSING SAND FROM DURBAN

0 MEAN DRY DENSITY 1611kg/m 3
~< 0'~0- -
13-
==
~ •
~J 0 ' 0 8 - X
c~
~0
0"06-
"04-
X
~KK
_Z X•
~ 0"02 --
~ •
I I x-x~-x-x-• I • I x-x-x-I
5 10 15 20 25 30
MOISTURE CONTENT DURING LOADING (%)
FIG. 7-- Typical results obtained from specimens cutfrom undisturbed sample of residual soil.
in density. In fact, none of the 24 specimens in this group fell outside the 1 per-
cent limits. In Fig. 10, the initial dry density has been plotted against moisture
content, with the collapse marked against each point. There is no pattern to
relate particularly the variations in collapse to those in dry density.
It was, nevertheless, found [1,2] that the initial dry density was a major
factor in determining the amount of collapse on wetting. The range of dry
densities existing in any group of specimens, however, does seem to have been
small enough to have prevented excessive variations in the test results.
Such variations as did occur can be probably ascribed to local fluctuations
in density or particle size within the specimen. These fluctuations would have
been caused during the filling of the mold, immediately prior to compaction.
It is doubtful whether any method of compaction can avoid this, since all
require some kind of mold to be filled. Variations in moisture content within
the specimen may have also contributed.
Conclusions
The paper has described a method for compacting and conditioning speci-
mens prior to testing, partly saturated, in the oedometer. The static method of
O-16 - -
0.14 x
•x
X ~
RECOMPACTED DECOMPOSED GRANITE FILLING
FROM NORTH-EASTERN TRANSVAAL
X ~ MEAN DRY DENSITY 1575 kg/m 3
u~
0- 0-I0 _ x ,XXxx
0.08
D
0
I--
0.06 - - X
z ~o4
~ 0"02
Ilg
1 1 ~--x-x-xl ~ I ~ l
5 10 15 20 25 30
MOISTURE CONTENT DURING LOADING (%)
FIG. 8--Relatively poor results obtainedfrom specimens made in the mold.
compaction has been shown, in the past, to give the most uniform specimens.
The conditioning procedure for adjusting the moisture content models, as
closely as practicable, the changes occurring in compacted earthworks.
Measurements of the dry density of the individual specimens immediately
prior to testing have been used to consider the uniformity of each group of
specimens. The variations within a group of laboratory compacted specimens
is considerably less than in those cut from natural or compacted soils in the
field. The homogeneity of individual specimens is also, by visual observation,
markedly better than in the in situ soils.
The results obtained from testing these specimens are adequate to enable con-
clusions to be drawn. Such variations as there were in the collapse settlements
measured cannot be related to the initial dry densities of the specimens. They
are probably caused by unavoidable local variation in dry density or particle
0'14
RECOMPACTEO DECOMPOSED QUARTZITE FROM 1600 - -

COLLAPSE SHOWN AS REDUCTION IN VOIDS RATIO
z MELSETTER, RHODESIA
-,~ O.12 - -
0,r
,r I % ABOVE MEAN
~ % MEAN DRY DENSITY ,520 kg/m 3 O~
~890 . . . . . ~0 0
0
~
m 0.10 - ~ "1-
x0.055 x0
x0 0
3 x0
J _ ~o.io2 ~o.o67 Z
a 1880
xO.I21 xO'100
g ~8
~
Z 0.08 x0.12.80ill x0"095 MEAN
--x' "-~xO.O85 9 xO.046- r-
xO
I- co
"1o
1570 - - xO'O62 m
o ).141 o_
~ O.OB ~O'OB2 x0
xO'050 m
0.080 z
x0"097 l % BELOW MEAN Go
1560
z 0-04 o=
g 0
o ~ 5 5 0 i_
m
I-
8
0,02
m
-,L
m
154C I I I I I I
0 5 I0 15 20 25 50
I I .x- I ,~ I ~_~ MOISTURE CONTENT DURING LOADING (%} m

5 I0 15 20 25 50
MOISTURE C O N T E N T DURING LOADING (%) FIG. 10---Poor resultsreplotted in terms of the dry density of individual
specimens.
FIG. 9--Consistent resultsobtainedfrom specimens compacted in the mold.
bO
",4
size occurring during compaction. It is doubtful if any other method can

eliminate this problem.
Acknowledgments
The work described in this paper was carried out at the National Institute
for Road Research in Pretoria, South Africa and is published by permission
of the director. The author would also like to thank Professor K. Knight of the
University of Natal in Durban, South Africa, for his interest throughout this
work.
References
[1] Booth, A. R., "Collapse Settlement in Compacted Soils," Council for Scientific and Indus-
trial Research, Research Report 324, National Institute for Road Research, Bulletin 13,
Pretoria, South Africa, to be published 1976.
[2] Booth, A. R. in Proceedings, 6th Regional Conference for Africa on Soil Mechanics and
Foundation Engineering, Durban, 1975, Vol. I, pp. 57-63.
[3] Jennings, J. E. B. and Knight, K. in Proceedings, 4th International Conference on Soil
Mechanics and Foundation Engineering, London, 1957, Vol. I, pp. 316-319.
[4] Knight, K., "The Collapse of Structure of Sandy Subsoils on Wetting," Ph.D. thesis,
University of the Witwatersrand, Johannesburg, South Africa, 1961.
[5] Leonards, G. A. "Strength Characteristics of Compacted Clays," Proceedings, American
Society of Civil Engineers, Vol. 79, Paper 360, 1953.
[6] Mayo, R. I. "Compression Tests on Stabilized Soil Mixtures," M.Sc. thesis, Purdue
University, Lafayette, Ind., 1939.
[7] Dawson, R. F. in Papers on 1959 Meetings Soils, ASTM STP 254, American Society for
[8] Whitman, R. V., Roberts, J. E. and Man, S., "One Dimensional Compression and Wave
Velocity Tests, and Responses of Soil to Dynamic Loads," Report 4, Publ. 106, Soil Engi-
neering Division, Department of Civil and Sanitary Engineering, Massachusetts Institute of
of Technology, Cambridge, Mass., 1960.
[9] Shackel, B., Australian Road Research, Vol. 4, No. 5, 1970, pp. 12-31.
[10] Gau, F. L. and Olson, R. E., Journal of Materials, Vol. 6, 1971, pp. 874--888.
[11] Kirkpatrick, W. M. and Rennie, I. A. in Proceedings, International Symposium on Soil
Structure, Gothenburg, 1973, pp. 103-111.
[12] Jennings, J. E. B. and Knight, K., Transactions, South African Institute of Civil
Engineers, Vol. 6, 1956, pp. 255-256.
[13] Barden, L., Madedor, A. O. and Sides, G. R., Journal of Soil Mechanics and Founda-
tions Division, American Society of Civil Engineers, Vol. 95, 1969, pp. 33-51.
T. Y. Chu' and S. N. Chen 2
Laboratory Preparation of
Specimens for Simulating Field
Moisture Conditions of Partially
Saturated Soils
REFERENCE: Chu, T. Y. and Chen, S. N., "Laboratory Preparation of Specimens

for Simulating Field Moisture Conditions of Partially Saturated Soils," Soil Specimen
Preparation for Laboratory Testing, ASTM STP 599, American Society for Testing
ABSTRACT: Due to the significant effect of soil moisture on the behavior character-
istics of a soil, one of the primary requirements in the preparation of specimens of
a partially saturated soil is to simulate the suction in the soil under prevalent field
conditons. This objective may be achieved by the conditioning or pretesting treatment
of a soil specimen, so that a desired suction in the specimen is attained prior to
testing. Relatively simple equipment such as that described in this paper, is suitable
for the required treatment of specimens representing partially saturated soils. This
paper presents results of undrained triaxial tests and repeated loading tests on soil
specimens treated by using the equipment mentioned previously. Test data from
specimens without any suction treatment are presented for comparison purposes.
Information obtained from these experiments indicates that the simulation of the
field moisture condition of a soil cannot be achieved simply by reproducing the
field moisture content of the soil. The conditioning or pretesting treatment of soil
specimens by using apparatus such as that presented in this paper is believed to be
a preferable method for the purpose of simulating field moisture conditions.
KEY WORDS: soils, subgrades, unsaturation, specimens, treatment, soil, water,

suction, triaxial tests
In consideration of the significant effect of soil moisture on the behavioral

characteristics o f a soil, it is evident that a primary requirement in the
preparation o f specimens representing the soil mass at a particular site
is to simulate the field moisture conditions of the soil. The term moisture
condition, as used in this paper, refers to all factors related to the water
in a soil mass, such as the positive or negative pore water pressure, the
] Professor of engineering, University of South Carolina, Columbia, S.C. 29208.

2 Soil engineer, Tippetts-Abbett-McCarthy-Stratton Engineers and Architects, New York,
N.Y. 10022.
229
Downloaded/printed9
Copyright 1976 by by ASTM International www.astm.org
water content, and the degree of saturation. In the case of saturated soils,
the objective of simulating field moisture conditions is often achieved by
saturating specimens of desired density and soil structure with water, as
well as by the application of a back pressure to the soil water, if necessary.
On the other hand, laboratory preparations of specimens for simulating
the field moisture conditions of unsaturated or partially saturated soils
are sometimes rather complicated, due to the need for elaborate equipment
and time-consuming procedures.
This paper presents a relatively simple apparatus which has been
developed primarily for the aforementioned objective in the case of
partially saturated soils. The procedures involved are also comparatively
simple. While the test results presented in this paper are based on the
use of remolded specimens only, the developed equipment and procedures
may be applied equally well in the preparation of undisturbed soil
specimens prior to laboratory testing.
The developed equipment and procedure for specimen treatment prior
to laboratory testing may be applied for determining the behavior charac-
teristics of partially saturated soils, as required in the design of pavements,
foundations, and different types of retaining and earth structures. For
instance, in the design of pavement structures, it is desirable to determine
the subgrade characteristics at the anticipated field moisture conditions.
This objective may be achieved by using the developed method for
specimen treatment prior to subgrade evaluation tests. At the present
time, the commonly used methods for specimen treatment in connection
with subgrade evaluation tests include the saturation of test specimens by
evacuation or complete immersion in water and the capillary absorption
by the Texas procedure, as discussed elsewhere in this paper. In previous
studies [1--4],3 however, subgrade soils below pavements were seldom found
to be saturated or close to saturation, as represented by specimens treated
by the methods mentioned previously. The findings from these studies
indicate that, in areas of relatively high ground-water table, subgrade
moisture variations may be predicted, according to the equilibrium
suctions of the subgrade soils, provided that frost actions are not expected
to occur in the subgrade. For this reason, the developed method for
specimen treatment presented in this paper appears to be a preferable
procedure in comparison with other methods for treating subgrade
specimens prior to testing.
Review of Current Methods for Pretesting Treatment

In the laboratory testing of remolded or compacted soil specimens,
the molding moisture conditions are usually different from those during
~The italic numbers in brackets refer to the list o f references appended to this paper.
CHU AND CHEN ON PARTIALLY SATURATED SOILS 231
testing. Pretesting treatments of such specimens are, therefore, an essential

step in the preparation of specimens for laboratory testing. The commonly
used methods for pretesting treatment are described hereinafter. Many of
these methods were developed in connection with the evaluation of sub-
grade soils, as required in the design of pavement structures.
Kansas Method
In the Kansas method [5] for laboratory preparation prior to testing,
soil specimens are saturated with water by evacuation. In view of the fact
that subgrade soils below pavements usually are not saturated to the same
extent as that of the laboratory specimens prepared according to the
procedure just mentioned, correction factors, such as those formulated
in the Kansas method for pavement design, are to be used in the application
of test results for pavement design purposes.
California Bearing Ratio Test Method

The California Bearing Ratio (CBR) test described in the ASTM Test
for Bearing Ratio of Laboratory-Compacted Soils (D 1883-67, 1967) is
used by the Corps of Engineers and many state highway departments
for subgrade evaluation in connection with pavement design. In this test
method, remolded soil specimens are soaked in water, under a simulated
surcharge pressure, for four days prior to testing. Due to the application
of a surcharge and the confinement of the soil specimen in the mold
during soaking, the four-day soaking normally does not provide full
saturation of the soil. Nevertheless, the degree of saturation of the
soaked specimen might be substantially higher than that of the subgrade
soil under the proposed pavement.
Texas Method
The basic procedure for pretesting treatment in the Texas method [6] is
to allow water to move upward into a remolded soil specimen by
capillary absorption. The capillary flow of water is accomplished by keep-
ing the soil specimen (resting on a porous stone) at 0.5 in. above the
water level in a pan provided in the treatment assembly. While the Texas
method may be considered as an improvement of the other methods
described previously, insofar as the simulation of field moisture con-
ditions of subgrade soils is concerned, it appears that the particular setup
might be satisfactory in simulating the subgrade moisture conditions at
certain sites and might not be satisfactory for the same purpose at other
locations. In other words, some flexibility in the treatment assembly is
believed to be necessary in order to make it possible to achieve the

objective of close simulation of the field moisture conditions of the soils.
Other Methods
Seed et al [7,8] developed a method for preparing and conditioning
soil specimens to simulate closely the field condition of a soil with respect
to its density, soil structure, and degree of saturation. Using their method,
specimens are prepared either by kneading compaction at a moisture
content "dry of optimum" or by static compaction "wet of optimum."
In either case, the compacted specimens are soaked to the desired degree
of saturation. It was reported that the procedure of using kneading com-
paction dry of optimum and subsequent soaking would require considerable
time and effort in achieving the desired degree of saturation. The soil
water suction of a partially saturated soil specimen is not controlled or
measured in this method for specimen preparation and conditioning.
If it is desirable to control the soil water suction of a partially saturated
soil specimen during pretesting treatment, apparatus such as those
developed by Escario [9] and Alpan [10] for conducting swelling tests of
expansive clays might be suitable, provided that necessary modifications
are made in regard to the equipment and the related procedures. The use
of these elaborate apparatus, however, is expected to require considerable
time and effort in carrying out the desired treatment, prior to testing.
For this reason, one of the considerations in developing the new method
for pretesting treatment, as described herein, is to make the equipment
and procedures relatively simple, so that this method may be applicable
for routine tests in connection with subgrade evaluation or for other pur-
poses.
Development of Equipment and Procedures for Pretesting Treatment

The effect of soil water suction on the behavior characteristics of a
partially saturated soil has been emphasized by many investigators.
Recognizing the importance of this factor in laboratory testing, Burland
[11] and Aitchson [12] suggested that one of the primary requirements
in the preparation of specimens of any partially saturated soil should be
the simulation of the soil water suction under field conditions. This
is also the basic concept in developing the equipment and procedures
described in this paper. It is to be noted that, in order to make the equip-
ment as simple as possible, a suction plate device is included in the treat-
ment assembly. The limitation of this device is the relatively low suction
level (not exceeding a suction of 3.0 pF) that can be applied during treat-
ment. The use of a complex equipment, such as an apparatus incorporating
a pressure membrane device, is necessary for the application of relatively
high suction levels during treatment. As mentioned previously, it is

expected that pretesting treatment using a rather complicated equipment
requires considerable time and effort. The discussions presented herein,
will refer only to the simple equipment and procedures developed from
this study.
A schematic diagram of the developed equipment is presented in Fig. 1.
As shown in this figure, a soil specimen, which is 2 in. in diameter and
4 in. high, is placed between the upper and lower cylinder units (denoted
as No. 7 in the figure). These units are connected to the tubing system
and the graduated glass tube. Figure 2 shows the base chamber, including
a ceramic plate at the top of the chamber. The device for providing a
desired lateral pressure on the soil specimen under treatment is similar to
the axial cell used in a capillary wetting assembly suggested by Hunt [13].
The surcharge load on the specimen is provided by placing proper weights
on the upper cylinder units. This unit is free to move in a vertical direction.
While the lateral pressure and the surcharge on the soil specimen may be
adjusted to provide any desired value, the value of 1.0 psi was used as
both the lateral and the surcharge pressure in treating all soil specimens
prior to the tests reported in this paper.
The desired suction in the soil water for specimen treatment is applied
by adjusting the water level in the graduated glass tube shown at the
lower right corner of Fig. 1. In other words, the depth of the water level
below the center of the specimen is a variable which may be determined
in accordance with the desired suction during the treatment. In this
respect, one will note that other expressions such as tension, capillary
potential, and negative pore water pressure, together with soil water suc-
tion or suction, have been used by various investigators in relating the
stress levels of the water in partially saturated soils. These terms are
sometimes defined in a slightly different manner. Discussions of these
expressions and methods for the conversion from one expression to another
are presented in publications by Croney and others [14,15]. It is not the
intention of this paper to suggest specific definitions of these terms and
to discuss other details. In accordance with the information given in the
references indicated previously, it may be stated that, in the case of non-
plastic soils, the depth of the water level (in the graduated tube) below
the center of the specimen represents the applied tension or suction during
treatment. For plastic soils, Croney's method [14] may be used to compute
the required depth of the water level for a desired suction, if the recom-
mended definitions of the various terms given in the aforementioned
references are to be followed. An alternative [16] for providing the
desired suction is to use mercury instead of water in the plastic tubing and
the glass tube, as mentioned previously. This method for providing the
desired suction would be required if it is substantially higher than 3 ft of
water.
arent
c tubing
~ / - - - Graduated
>~ _ _ ~ g ~ lass tube
Legend:
i. 2-in. dia, 4-in. high soil specimen.
2. Ceramic plates.
3. Filter papers.
4. Rubber membrane.
5. Cylinder for providing lateral
pressure on the soil specimen. p l a s t i c tubing
6. Rubber covers.
7. Chambers filled with de-aired water.
8. Transparent plastic cylinder.
9. Guide to keep the upper unit in
proper position.
i0. Cover to prevent evaporation.
ii. Ring to provide a pool of water
during preparation for specimen treatment.
12. Connection for applying desired lateral
pressure.
FIG. l--Setup for pretesting treatment of a soil specimen to simulate field moisture
conditions.
FIG. 2--Photograph showing the base chamber of the apparatus for treating specimens
of partially saturated soils.
As shown in Fig. 1, the movement of water into or from the soil

specimen is through the ceramic plates and the two pieces of filter paper
in contact with the top and bottom of the specimen. The purpose of
allowing flow to occur through both the top and bottom of the specimen
is to reduce the time required for completing the treatment. The rubber
covers (denoted as No. 6 in the figure) near the top and bottom of the
specimen are provided to minimize the loss of moisture from the specimen
due to evaporation.
The treatment assembly illustrated in Fig. 1. is suitable for either
undisturbed or remolded soil specimens. While remolded soil specimens
may be prepared by any desired method of compaction, all specimens
reported in this paper were compacted by using a drop hammer, except
for a limited number of specimens that were prepared by kneading com-
paction. The procedure for the pretesting treatment of partially saturated
soil specimens by the developed equipment is outlined in the following
paragraphs.
1. Prepare soil specimens at the desired density and moisture content.
After a designated waiting period (24 h used in this study), the specimen
is ready for treatment.
2. Prepare the treatment assembly by saturating the ceramic plates and
filter papers and by filling the upper and lower chambers with deaired
water. The valves, which are marked as V-l, V-2, and V-3 in Fig. 1, are
provided for the purpose just mentioned. In addition, a pool of water
above the lower ceramic plate may be created by pouring water into the
area within the ring (marked as No. 11 in Fig. 1). The purpose of pro-
viding this pool of water is to assure that good contact exists among the
specimen, the filter paper, and the ceramic plate. Any air entrapped in
the contact areas may interfere with the successful completion of the
intended treatment.
3. Place the specimen in the treatment assembly and apply the sur-
charge, as well as the confining pressure (lateral pressure), on the speci-
men. At the same time, apply the desired suction by adjusting the water
level in the graduated glass tube. If mercury is used instead of water, as
mentioned previously, adjust the mercury column to provide the desired
suction.
4. When a moisture equilibrium condition is reached (as indicated by a
nearly constant water level in the graduated glass tube over a period of
time), remove the specimen from the treatment assembly.
The height, diameter, and weight of a specimen are to be determined
before and after the treatment to obtain the necessary data for com-
puting the change in density, moisture content, and the degree of satura-
tion. The treated specimens may be used for any desired laboratory test,
such as the undrained triaxial compression test and the repeated loading
test. Both types of test were performed in this study.
Test Results and Discussion

The physical properties of the soils used in this study are summarized
in Table 1. Due to the fact that this study is related to part of a research
project concerning the investigation of subgrade moisture conditions
below pavements in South Carolina, the sampling locations are identified
according to a numbering system used in that project. General informa-
tion regarding the subgrade moisture investigation project was reported
by Chu et al in a separate paper [3]. The samples from Sites 57 and 58
are micaceous soils obtained from the Piedmont region; the one from
Site 80 is a silty sand obtained from the coastal plain area of South
Carolina.
Table 2 presents all data concerning pretesting treatment, as well as the
dry density, moisture content, and the degree of saturation for both the
as-molded condition and the condition before testing. The 3 and 1 ft suc-
tion levels for specimen treatment, as indicated in this table, were provided
by using the equipment illustrated in Fig. 1. On the other hand, the 2.5 in.
suction level for treatment was attained by using a device somewhat
similar to the assembly for the capillary wetting of the soil specimens,
as employed in the Texas method [6]. In other words, the specimen was
placed on a filter paper above a porous stone, and the water level in a pan
(holding the porous stone) was maintained at 0.5 in. below the bottom of

TABLE 1--Physical properties o f soils. 0
I
Cl
Laboratory Compaction
z
Test a E~
Percent Passing Atterberg
0
Sieve No. Limits AASHTO Max Dry Optimum -1-
Classifica- Specific Density, Moisture 111
z
Site No. 4 10 40 200 LL PL PI tion Gravity lb/ft 3 Content, %
0
Z
57 98 95 75 24 ...... NP A-2-4 2.74 101.2 17.5
"o
58 ... 100 95 63 43 37 10 A-5(6) 2.74 97.7 23.5
80 100 97 58 18 ...... NP A-2-4 2.65 120.5 9.3 -4
NOTES-- LL = liquid limit. I'-
I"
-<
PL = plastic limit.
PI = plasticity index. 60
NP = nonplastic.
I lb/ft 3 = 157 N / m L
m
E~
aASTM Tests for Moisture-Density Relations of Soils, Using 5.5-1b Rammer and 12-in. Drop (D 698-70). o
GO
-,,4
co
oo
T A B L E 2--Summary of data from undrained triaxial tests with 10 psi confining pressure.
co
As-molded Condition Condition before Testing O
Modulus Maximum r'-
Suction Level Dry Moisture Degree o f Dry Moisture Degree o f of Deviator o9
-v
in Pretesting Density, Content, Saturation, Density, Content, Saturation, Elasticity, Stress, m
Specimen No. Treatment lb/ft 3 % 07o lb/ft 3 % 07o psi psi _~
tl1
57-1 no treatment 96.6 17.6 62 96.6 17.6 62 1100 16.5 Z
57-2 3 ft 95.5 17.8 62 91.3 22.8 71 670 15.3 "u
~u
57-3 95.5 17.8 62 91.5 22.7 72 700 13.0 m
57-4 1 ft 95.0 17,8 61 89.2 26.5 80 490 9.5
57-5 95.4 17.8 62 90.8 24.5 76 520 11.2 ~
57-6 2.5 in. 95.0 17.8 61 86.0 31.5 88 310 8.0
58-1 no treatment 94.5 23.6 80 94.5 23.6 80 2490 29.5
58-2 93.6 23.6 79 93.6 23.6 79 2780 28.0 Z
58-3 3 ft 93.2 23.5 77 91.8 26.9 86 1300 15.8 -n
58-4 1 ft 93.3 24.0 78 90.7 28.5 89 830 8.4 O
58-5 2.5 in. 93.2 23.5 78 87.3 31.0 88 670 6.2
I'-
58-6 3 ft 98.0 24.0 89 94.6 27.2 92 1500 24.0 3~
58-7 98.0 24.0 89 94.5 26.8 91 1800 28.2 u0
O
58-8 i ft 98.0 24.0 89 94.0 28.4 95 1100 12.2
58-9 2.5 in. 98.0 24.0 89 93.5 28.5 95 600 10.0
80-1 3 ft 121.0 8.8 65 120.8 9.0 66 2280 22.8 O
80-2 1 ft 121.0 8.8 65 120.5 9.4 67 1600 18.5 -<
80-3 2.5 in. 121.0 8.8 65 120.0 11.2 79 930 11.8 .~
ITI
fD
N O T E S - - T h e specimens are numbered in such a way that the first two n u m b e r s are referring to the site where the soil samples were obtained. .-I
I lb/ft 3 = 157 N / m 3, 1 psi = 6900 N / m 2, l ft = 0.3048 m. 1 in. = 0.0254 m,
Specimens 58-1 through 58-5 have relatively low densities.
Specimens 58-6 through 58-9 have relatively high densities.
the specimen. For specimens 4 in. in height, as used in this study, the
average tension in the specimen is 2.5 in. For the low plasticity or non-
plastic soils used in this study, there is little or no difference between the
tension or the suction of these soils. The time required for completing
the treatment of all specimens employed in this study was less than one
week.
As indicated in Table 2, four groups of specimens having similar
initial dry densities and moisture contents (see the columns under "As-
molded Condition" in this table) were prepared in this series of experi-
ments. According to the density and moisture data in the columns under
"Condition before Testing," substantial swelling of the specimens pre-
pared by using soils from Sites 57 and 58 occurred during the treatment.
The appreciable volume change during treatment is believed to be pri-
marily due to the micaceous composition of the soils. If it is desirable
to minimize the volume change of a specimen during the treatment,
extremely high surcharge and lateral pressures would have to be applied
on the specimen. The use of extremely high pressures, however, will
result in an increase in the time needed to complete the treatment.
Furthermore, the high degree of confinement of a specimen during
treatment is likely to cause a less uniform condition with respect to the
density and moisture content within the specimen (after the treatment)
than that found when a relatively low pressure level is maintained during
the treatment.
The modulus of elasticity and the maximum deviator stress determined
by undrained triaxial tests are also presented in Table 2. As expected, the
test data indicate that, in the case of soil specimens subjected to pre-
testing treatment, an increase in the suction level maintained during
treatment results in a corresponding increase in the modulus of elasticity
and the maximum deviator stress of the specimen. This general trend of
variation is true for all the samples tested. It is to be noted that, for soils
from Sites 57 and 58, the triaxial test data obtained from specimens with-
out treatment are included in Table 2. On the basis of the data in regard
to the degree of saturation of the soil specimens before testing and the
information from supplemental experiments, including tensiometer tests
[17] and pressure plate extractor tests [3], the suction in any of the
specimens without treatment was found to be higher than those in the
treated specimens. For this reason, the modulus of elasticity and the
maximum deviator stress of the specimens tested without treatment were
found to be higher than those of the treated specimens. A comparison of
stress-strain curves of both treated specimens and the one without treat-
ment, prepared by using the soil from Site 58, is presented in Fig. 3.
In addition to the undrained triaxial compression tests described pre-
viously, specimens with or without treatment were employed in repeated
loading triaxial tests. Figure 4 illustrates the sinusoidal loading pattern
35 I I I ! I l
s Specimen No. 58-2

30 ( no treatment )
/."- O"b'-.,O,,"
!
25
i
I
I
?
20 !
e~ | X----Specimen No. 58-3
if}
I ~ ( 3-ft suction )
I
9
Specimen No. 58-4
~ ( l-ft suction )
.VfV..--V"-- ~"" --V
i0
/
/~ ~ Specimen No. 58-5
( 2.5-in. suction )
~/ ..O~'"_O------O----~-...43
0 i 2 3 4 5 6 7
Axial Strain, percent
FIG. 3--Effect o f pretesting treatment on the stress-strain characteristics o f soil specimens

determined by undrained triaxial tests.
I I I I I I I I I I I I I I
'g 5
"~~~0.550"~60 I Resilient
strain
oso 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1 1
Time(onesecondpergrid)
FIG, 4--Illustration o f the pattern in stress and strain variations in a repeated loading
triaxial test (Specimen 58-17, l lO-th through l l4-th load applications).
with a frequency of one cycle in every 3 s, as used in the repeated loading

tests conducted in this study. The applied maximum deviator stress
during each test was 8 to 9 psi. The variations in the resilient and
residual strains of a specimen, due to repeated load applications, are also
illustrated in Fig. 4.
Table 3 presents a summary of all data obtained from the repeated
loading tests on specimens prepared by using the soils from Sites 57 and
58. The resilient modulus of a test specimen, as indicated in this table,
was determined by dividing the difference between maximum and mini-
mum deviator stresses by the corresponding resilient strain. Similar to the
trend of variation observed from the data presented in Table 2, the test
results of Specimens 57-7 through 57-9 and 58-10 through 58-13, as given
in Table 3, show that the resilient modulus of the specimen tested without
treatment is higher than those of treated specimens of the same soil. On
the other hand, the residual strains of the specimens tested without
treatment are lower than those of the treated specimens. In a comparison
of the data of Specimens 58-11 through 58-13 (compacted by a drop
hatmner) with those of Specimens 58-14 through 58-16 (compacted by a
kneading compactor), it is noted that while all the specimens have similar
as-molded conditions with respect to dry density and moisture content,
b~
4~
O~
0
T A B L E 3--Summary of data from repeated loading triaxial tests with 10 psi confining pressure. t'-
CD
Test Date at Number of Load Applications m
(NLA) Shown O
As-molded Condition Condition before Testing NLA = 100 NLA = 10000 m
z
Equipment Suction Level Dry Moisture Degree of Dry Moisture Degree of "U
Residual Resilient Residual Resilient
for in Pretesting Density, Content, Saturation, Density, Content, Saturation, Strain, Modulus, Strain, Modulus, m
Specimen No. Compaction Treatment lb/ft j 070 070 lb/ft ~ % 070 070 ksi 070 ksi
XI
57-7 no treatment 99.0 17.0 65 99.0 17.0 65 1.33 12.9 1.48 15.7 ~:~
57-8 drop 99.0 17.8 68 95.0 23.4 76 -4
3ft 4.80 11.0 5.05 13.7
57-9 hammer 99.0 17.6 67 95.0 23.4 76 5.15 10.6 5.28 11.7 k./Z
58-10 no treatment 98.1 24.5 91 98.1 24.5 91 0.35 24.3 0.38 30.6
58-11 drop 97.1 24.8 90 94.0 27.4 92 "11
1.55 12.1 1.70 21.6 C)
58-12 hammer 3 ft 97.2 24.8 90 93.7 27.8 93 1.70 12.9 1.80 20.5 ~0
58-13 97.0 24.8 90 93.3 27.5 91 1.90 16.0 2.15 21.0 r'-
58-14 kneading 3 ft 97.5 24.8 91 96.5 26.3 94 0.90 17.8 1.10 22.8 ~:~
58-15 97.3 24.8 91 96.5 26.2 93
58-16 compactor 0.75 16.6 0.85 24.3 I~
97.0 24.8 90 96.3 26.2 93 1.20 17.4 1.26 24.3 O
"3"1
58-17 93.5 27.5 91 93.5 27.5 91
58-18 drop 0.55 20.0 0.59 27.4
93.2 27.5 91 93.2 27.5 91 0.60 21.0 0.64 27.6 --4
0
no treat n~ent
58-19 hammer 94.0 27.5 92 94.0 27.5 92 0.80 20.5 0.93 25.8 -rl
58-20 93.2 27.5 91 93.2 27.5 91 0.63 19.1 0.65 25.0 "<
--4
N O T E - - I ft = 0.305 m, I lb/ft 3 : 157 N/m 3, 1 ksi = 6.9 x 106 N / m L m
O~
,-I
the difference in the method of compaction in preparing these two groups

of specimens results in some difference in the dry densities and moisture
contents after the pretesting treatment. The repeated loading test data are
also different between these two groups of specimens. While it is not the
intention of this paper to cover the effect on soil behavior due to the
differences in the method of compaction, the test data of Specimens 58-11
through 58-16 are presented primarily to illustrate the fact that the use of
the same suction level in pretesting treatment might result in different dry
densities and moisture contents of treated specimens if different methods
of compaction were used in specimen preparation. The discrepancies just
mentioned are evidently related to the difference in the type of soil struc-
ture in the test specimens, due to the deviation in the method of com-
paction.
Specimens 58-17 through 58-20 were prepared in such a manner that
the dry densities and moisture contents under the as-molded condition
are similar to those of Specimens 58-11 through 58-13 after the treatment
with 3 ft suction. In other words, the dry densities and moisture con-
tents of these two groups of specimens before testing are very close to
each other. In view of the fact that Specimens 58-17 through 58-20 were
tested without treatment, it is obvious that any difference in the repeated
loading test data of these two groups of specimens is due primarily to
the discrepancy with respect to the suction in the soil specimens. A com-
parison of the test data of these specimens may be made by referring to
Table 3 as well as Figs. 5 and 6. The relatively high resilient moduli and
comparatively low residual strains of Specimens 58-17 through 58-20, as
shown in the table and illustrated by the figures, are again due to the fact
that the specimens tested without treatment have a higher suction than
that of the treated specimens of similar density and moisture content.
As mentioned previously, the high suction values of the specimens tested
without treatment were determined by supplemental experiments, includ-
ing tensiometer and pressure plate extractor tests. Furthermore, it is
recognized that remolded specimens of partially saturated soils normally
would have suction levels much higher than those under the actual field
conditions. Consequently, the simulation of the field moisture condition
of a soil cannot be achieved simply by reproducing the field moisture
content of the soil. For this reason, the conditioning or pretesting treat-
ment of soil specimens by applying the desired suction is believed to be a
preferable method for the purpose of simulating field moisture condi-
tions. Information concerning the application of the developed method
for the conditioning of subgrade soil specimens prior to laboratory testing
for pavement design purposes was presented in other reports [3,4].
General Conclusion
Results from undrained triaxial tests and repeated loading tests on
0.4 i il I ' I
.... Specimen No. 58-17- 7
_o
0.6 U-
6O
-Q
"'" "''" """ "'"" ....... / Specimen No .~811"8 m
0.8 - Y ~ " 9 -...~ 0.... / / o
' ".... ""'V-- L_ Specimen No. 58-20
4J " / ~ .................Ir...... -y...... m
/ z
o 1.0 Specimen No. 58-19 "o
-,m
m
"o
g 1.2 Note: Specimens 58-11 through 58-13 were treated
~ with 3-ft suction. No treatment for
Specimens 58-17 through 58-209 -I
g 5
1.4 z
0
.N ~'--.~........ V- "--'"" .... ~ ~ - S p e c i m e n No. 58-11
m 1.6
i'-
>
0
"11
1.8
0
"11
2.0 '"~....... z._ Specimen No. 58-12
"~"~""M---..~............__-r Specimen No. 58-13 .-I
m
2.2 I I I .--I
i0 i00 1000 10,000 i00,000
Number of Load Applications
FIG. 5--Effect o f the pretesting treatment on the residual strain o f soil specimens.
30 L I I I
I Specimen No. 58-18 ~ --.--ll-----" --1---
I
b Specimen No. 58-17 - - - - "-' m ~ ", , ~ .----
.o -- ~"-" ". ~. . . . . ~ . . . .
! ~ - ~--S~e~men~o5820 O
I
C
9~ l . . - . ~ ~ me~~o. 58-19 ..... ~--- >
20 .... .. .. . . . . . ~ ,.~ ' - - - - 5
.--- = ~ =..-u-- --'"
~" ~ ~ " "- "L-.':- =-"
O
-r
I Specimen No. 58-13 ---~...~~ ~'" j'~.>--~" m
~=~ . . . . . . . . . . . . . . . X--"" v ,,__~, s - z
. . . . . . . . ...C;.~-
O
~-- Specimen No. 58-12 ..---"~.-" z
= \ . ~o---'" "" .: -- -u
>
"~ 10 { l'_~'-_L'-f_-2"~-~ -v- -4
>
Specimen No. 58-11 r-
r-
.<
09
Note: Specimens 58-11 through 58-13
w e r e treated w i t h 3-ft suction. c
-n
No treatment for Specimens >
58-17 through 58-20. -4
m
I I I 09
10 100 1000 10,000 o
i00,000 F"
09
Number of Load A p p l i c a t i o n s
~O
FIG. 6--Effectofpretestingtmatmentontheresilient modulus ofsoHspecimens. O1
partially saturated soils presented in this paper indicate that the soil water
suction in a test specimen is an important factor affecting the stress-
strain characteristics of the soil. Consequently, one of the primary re-
quirements in the preparation of specimens of a partially saturated soil
is to simulate the suction in the soil under prevalent field conditions.
To satisfy this requirement, it is necessary to include the step of con-
ditioning or pretesting treatment during the preparation of soil specimens
for laboratory testing. The method of treatment as described in this paper
is believed to be suitable for the aforementioned purpose, provided that
the desired suction level during treatment is relatively low. If extremely
high suction levels are to be maintained during treatment, apparatus and
procedures much more complicated than those reported in this paper
would be required.
Acknowledgments
The investigations in this study were conducted at the University of
South Carolina and were mostly in connection with a subgrade moisture
research project sponsored by the South Carolina State Highway Depart-
ment and the Federal Highway Administration. The authors wish to
express their appreciation to all who have assisted in the research project
and to some of the staff members in the soils department, Tippetts-
Abbett-McCarthy-Stratton Engineers and Architects, New York, for their
assistance during the preparation of this paper.
References
[1] Aitchison, G. D. and Richards, B. G. in Moisture Equilibria and Moisture Changes
in Soils Beneath Covered Areas, Butterworth, Australia, 1965.
[2] Russam, K., "Subgrade Moisture Studies by the British Road Research Laboratory,"
Highway Research Record No. 301, 1970, pp. 5-17.
[3] Chu, T. Y., Humphries, W. K., and Chen, S. N. in Proceedings, 3rd International
Conference on the Structural Design of Asphalt Pavements, 1972, pp. 53-66.
[4] Chu, T. Y. et al, "Soil Moisture as a Factor in Subgrade Evaluation," to be published
in Conference Proceedings, American Society of Civil Engineers Pavement Design
Specialty Conference, 1975.
[5] Kansas State Highway Commission, "Design of Flexible Pavements Using the
Triaxial Compression Test," Bulletin 8, Highway Research Board, 1947.
[6] McDowell, C., "Road Test Findings Utilized in Analysis of Texas Triaxial Method of
Pavement Design," The AASHO Road Test, Proceedings of a Conference held May
1962, St. Louis, Mo., Special Report 73, Highway Research Board, 1962.
[7] Seed, H. B., Chan, C. K., and Lee, C. E. in Proceedings, 1962 International
Conference on Structural Design of Asphalt Pavements, University of Michigan,
Ann Arbor, Mich., 1963, pp. 611-636.
[8] Monismith, C. L., Seed, H. B., Mitry, F. G., and C'han, C. K. in Proceedings,
Second International Conference on the Structural Design of Asphalt Pavements,
1968, pp. 109-140.
[9] Escario, V. in Proceedings, Second International Research and Engineering Conference
on Expansive Clay Soils, 1969, pp. 207-217.
[10| Alpah, I. in Proceedings, 4th Imernational Conference Soil Mechanics and Founda-
tions Engineering, Vol. I, 1957, p. 3.
[11] Burland, J. B., Moisture Equilibria and Moisture Changes in Soils Beneath Covered
Areas, Butterworths, Australia, 1965, p. 270.
[12] Aitchison, G. D. and Richards, B. D. in Proceedings, Second International Research
and Engineering Conference on Expansive Clay Soils, 1969, pp. 66-84.
[13] Hunt, J. E. in Special Procedures for Testing Soil and Rock for Engineering Pur-
poses, A S T M STP 479, American Society for Testing and Materials, 1970, pp. 192-197.
[14] Croney, D., Coleman, J. D., and Black, W. P. M., "Movement and Distribution of
Water in Relation to Highway Design and Performance," Special Report 40, Highway
Research Board, 1958, pp. 226-252.
[15] Aitchison, G. D. et al in Moisture Equilibria and Moisture Changes in Soils Beneath
Covered Area, Butterworths, Australia, 1965, p. 7.
[16] Chu, T. Y. and Mou, C. H. in Proceedings, Third International Conference on
Expansive Soils, 1973, pp. 177-185.
[17] Taylor, S. A., Evans, D. D., and Kemper, W. D., "Evaluating Soil Water," Bulletin
426, Agricultural Experiment Station, Utah State University, Logan, 1961, pp. 29-33.
R. T. Donaghe' and F. C. Townsend'
Scalping and Replacement Effects

on the Compaction Characteristics
of Earth-Rock Mixtures
REFERENCE: Donaghe, R. T. and Townsend, F. C., "Scalping and Replacement

Effects on the Compaction Characteristics of Earth-Rock Mixtures," Soil Specimen
ABSTRACT: This investigation examines the validity of a scalping and replacement

procedure used by many laboratories to determine compaction characteristics of
earth-rock mixtures containing oversized particles. Two commonly used methods of
computing densities of full-sized specimens, based upon results from tests performed
on minus No. 4 fractions of the actual total sample, were examined. Compaction
tests were performed on full-scale and scalped and replaced specimens, in which
both gravel and fines content were varied. The test results indicate that the scalping
and replacement procedure results in significantly lower maximum dry unit weights
and higher optimum water content than are obtained for full-scale specimens. The
use of the theoretical methods provided better approximations of experimental
results on full-scale specimens having gravel contents up to 70 percent than did
the relationships developed using the scalping and replacement procedure. For gravel
contents above 70 percent, better approximations were obtained using the scalping
and replacement procedure.
KEY WORDS: soils, compaction, density, moisture content, earth-rock mixtures
L a b o r a t o r y tests t o d e t e r m i n e c o m p a c t i o n characteristics o f e a r t h - r o c k
m i x t u r e s for use in field c o n t r o l h a v e b e e n subject t o q u e s t i o n for m a n y
years. D u e t o l i m i t a t i o n s o f e q u i p m e n t size, l a b o r a t o r y tests a r e g e n e r a l l y
p e r f o r m e d o n s m a l l s p e c i m e n s , thus p l a c i n g a limit o n t h e m a x i m u m
d i a m e t e r o f t h e particles w h i c h c a n b e used in the specimens. M a n y
l a b o r a t o r i e s , i n c l u d i n g t h o s e o f t h e C o r p s o f Engineers, scalp o v e r s i z e d
particles o f full-scale s p e c i m e n s a n d r e p l a c e t h e particles with an equal
p e r c e n t a g e , b y weight, o f smaller p a n i c l e s , a s s u m i n g t h a t results f r o m
tests p e r f o r m e d in small m o l d s o n such m a t e r i a l are c o m p a r a b l e to t h o s e
U.S. Army civil engineering technician and research engineer, respectively, Soils Research
Facility, Waterways Experiment Station, Vicksburg, Miss. 39180.
248
Downloaded/printed
DONAGHE AND TOWNSEND ON SCALPING AND REPLACEMENT 249
obtained from tests performed on full-scale specimens in large molds)

Other laboratories perform compaction tests on the minus No. 4 fraction
of soils in small molds and then apply theoretical correction factors,
based on the influence of gravel on compaction characteristics, to com-
pute densities of the full-scale specimens containing gravel. In both cases,
however, various investigators have found that additional modifications
have to be made in the small-scale test results in order to obtain agree-
ment with the results of tests on full-scale specimens.
The objectives of this investigation were to determine the validity of
the Corps of Engineers scalping and replacement procedure and to
evaluate theoretical methods of computing dry unit weights of full-scale
specimens, using results from tests performed on minus No. 4 fractions
of the total specimen.
These objectives were achieved by comparing compaction curves for
full-scale specimens (3 in. maximum particle size) and scalped and
replaced specimens ( 90 in. maximum particle size), determined by using
a mechanical compactor with 18 and 6-in.-diameter molds, respectively.
Additional comparisons involved compaction curves for scalped and
replaced specimens ( 90 in. maximum particle size), determined by using
a hand-held hammer with the 6-in.-diameter mold. Companion compac-
tion curves on the minus No. 4 fraction of the full-scale material were
determined by using a hand-held hammer and 4-in.-diameter mold.
Effects investigated are given in Table 1.
Procedure
Equipment
A mechanical compactor, manufactured by Howard Company and
equipped with 5.5 and 24.7-1b rammers, having face diameters of 2.0
and 6.0 in., respectively, was used to perform the testing. Large-scale
tests were performed using an 18-in.-diameter mold and 24.7Ab rammer,
while small-scale tests were performed using a 6-in.-diameter mold and
5.5-1b rammer. A special harness for suspending the 18-in.-diameter mold
and specimen from a forklift was rigged with an electronic load cell,
sensitive to within 0.1 lb, to obtain the specimen-plus-mold weights. A
photograph of the compactor, the 24.7-1b rammer, the 18-in.-diameter
mold, and the weighing harness is shown in Fig. 1.3 All other weights
ZThe Corps of Engineers scalping and replacement procedure for materials containing
particles larger than 2 in. for compactingin a 12-in.-diametermoldis givenin the appendix.
3The 12-in.-diameter mold shown with the weighing harness was not used in this in-
vestigation.
ol
0
T A B L E l--Summary o f compaction data.
co
O
M a x Dry Optimum I-"
Type o f Gravel Fines Unit Weight Water
Compactor Mold Dia, Max Particle Content, Content, ),a, w,
rn
Effect Investigated Used in. Size 070 070 lb/ft 3 07o
Equipment size mechanical 6 No. 4 sieve 0 25 130.9 8.6 ill

18 z
133.9 6.9
6 90 40 25 131.1 7.9
18 134.1 7.3 11
t'"u
Removal and replacement o f
coarse particles mechanical 18 90 40 25 134.1 7.3
3b ---i
138.0 5.9
Gravel content (large-scale tests) mechanical 18 No. 4 sieve 0 25 133.9 6.9 z
3b 10 135.0 6.7 -11
20 136.1 6.1 O
30 137.2 5.7 i--
40 138.0 5.9
50 137.1 5.8 0
60 134.9 5.2
100 112.0 ...C
Gravel content (small-scale tests) mechanical 0

6 No. 4 sieve 0 25 130.9 8.6
a/~a 10 133.5 7.7
20 132.5 8.1 -4
m
30 132.3 8.1 .--t
40 131.1 7.9
50 131.9 7.8
60 129.5 9.5
100 C
103.6
Gravel content (small-scale tests) hand-held No. 4 sieve 0 25 132.6 8.0
3Aa 10 132.5 7.8
20 131.8 7.9
30 132.0 7.9 O
40 z
132.0 7.9
50 129.3 8.0
60 32
128.5 9.2 m
100 101.2 ...c
Fines content (large-scale tests) mechanical 18 3b 40 15 141.8 4.9 Z
o
25 138.0 5.9
.-I
35 133.3 7.5 0
Fines content (small-scale tests) mechanical 6 90 40 15 134.8 7.4 z
25 131.1 7.9
m
35 126.6 9.4 Z
a Scalped and replaced material. 0

b Full-scale material. z
cSingle-point test performed on dry material.
r'-
z
o
m
"10
r'-
m
m
z
..-t
bO
...g
FIO. l--Howard mechanical compactor with 12 and 18-in.-diameter molds and load
cell harness f o r weighing.
were obtained by using a scale, having a sensitivity of 0.01 lb. Calibration

data for the molds were:
Nominal
Mold
Inside
Diameter, Area, Height, Volume, Weight,
in. ft2 in. ft 3 lb
6 0.196 4.582 0.075 6.21

18 1.767 18.005 2.651 321.40
Equipment used for tests with the hand-held hammer conformed to that
used for standard compaction tests performed by the Corps of Engineers
[1]4 and is similar to that specified in ASTM Tests for Moisture-Density
Relations of Soils, Using 5.5-1b Rammer and 12-in. Drop (D 698-70),
except the rammer is equipped with a sliding weight instead of a guide-
sleeve.
Material
The materials tested in this investigation consisted of a subrounded to
subangular washed gravel, having a maximum particle size of 3 in., a
subrounded to subangular concrete mortar sand, and a clay (CL), com-
bined according to the gradations given in Figs. 2 and 3. Classification
data for the clay and sand are given in Fig. 4.
Batches for specimens were prepared by thoroughly mixing a pre-
determined amount of sand and CL material mixture (minus No. 4
material) with a measured quantity of water, using either a commercial
kitchen mixer or a pugmill (specimens tested in 4 and 6-in.-diameter
molds were mixed with the kitchen mixer). The resulting minus No. 4
material was then stored in airtight containers and allowed to cure for a
period of at least 16 h. The plus No. 4 material for each batch was
prepared by combining the air-dry portion (by weight) of material required
for each sieve and then storing the resulting material in containers filled
with water. Immediately prior to compaction, the cured minus No. 4 frac-
tion was mixed with the saturated surface-dry aggregate. Each layer was
hatched separately to prevent any variations in grading between layers.
.O
t~
r
0
r-
"IJ
m
o_
m
z
"u
:I1
m
-o
"in
-t
r-
0.'n
-t
m
FIG. 4 - - G r a i n size distribution c u r v e s a n d classification data, C L material a n d sand.
Testing Procedure
Table 2 lists pertinent data concerning the rammer sizes and the com-
paction procedure. All specimens were compacted in three layers, using
compactive efforts made approximately equal to the standard effort
(12 300 ft. lb/ft 3) by adjusting the number of blows.
Test Results and Discussion

Results of the compaction tests are summarized in Table 1 and pre-
sented graphically in Figs. 5 through 15.
Effects of Equipment
Figure 5 presents results of tests performed, using both large- and
small-scale equipment, on scalped and replaced specimens and minus
No. 4 sieve specimens, having gravel contents of 40 and 0 percent, with
25 percent fines. The data indicate that, for both gradations, maximum
dry unit weight and optimtun water content varied with the different
sizes of equipment used. Optimum water contents of the 0 and 40 per-
cent gravel specimens were decreased by 1.7 and 0.6 percent, respectively,
when the 18-in.-diameter mold and 24.7-1b rammer were used in place of
the 6-in.-diameter mold and 5.5-1b rammer. The maximum dry unit
weight of both materials was increased by 3.0 lb/fP for the same change
in sizes of equipment. This difference in maximum dry unit weight falls
within a range comparable to that determined by previous investigators
[2-4], who indicated that the variation in densities determined using
various mold sizes was limited to not more than 4 lb/ft 3. Since only
limited testing was performed to determine the effects of variation in
equipment size, no attempt was made to correct other test results for
these effects. When comparisons which involve both large- and small-
scale test results are made, however, it appears safe to assume that dif-
ferences in densities due to varying the size of equipment used are
limitied to not more than 4 lb/ft 3.
Effect of Removal and Replacement of Oversize Particles

Figure 6 shows compaction curves and data for the tests performed on
the scalped and replaced specimen having 40 percent gravel and 25
percent fines and on the corresponding full-scale specimen, both of which
were tested using large-scale equipment. The curves indicate that, in this
case, scalping and replacing oversize particles results in a lower maximum
dry unit weight and a higher optimum water content. The 3.9 lb/fP de-
crease in maximum dry unit weight due to scalping and replacement of
Ol
Oo
t,D
__q
I'-
fD
"O
m
o
m
z
TABLE 2--Compaction tests using hand-heM sliding weight rammer and Howard mechanical compactor.
m
"o
Rammer a Blows per Coverage
Complete
Mold Compactive Dia of Blows Coverage Along At -t
Dia, Effort, Weight, Circular Drop, No. of per of Circumfer- Center of z
in. ft'lb/ft ~ lb Face, in. in. Layers Layer Mold Area enceof Mold Specimen
"11
O
:lJ
6 12 420 5.5 2 12 3 56 2 24 4
18 12 299 24.7 6 24 3 220 7 24 b 6c t--
t~
aCompaction equipment used: hand and mechanical compaction: 6-in.-dia mold, mechanical compaction: 18-in.-dia mold. O
:D
bPius 6 on last coverage.
Cplus 4 on last coverage.
O
-<
.--I
m
(D
-4
O
T E S T GRADATIONS
4SIEVE 0PENINGS=I = SIEVE NUMBERS
3 3/4 4 10 40 200
I00 0
-I i\ i !~---o~ cr
8 O -I 20
Z
E
F-
60
-I
-I
I
I "i\[ i \ U
-I I I
7 I I
~4o I ' ~ '
6o
-I
Q. j w
2 0 rl I I ~ BO Q.-
I 1 I
I I I
i' I I I I00
GRAVEL : ! : SAND : ]: FINES~
140
135
Q.
40%Gr(18"MO V'LD~~.~
~~
I.-
:I:
,,:}
bJ
I--
,25 I
O~Gr( ~ xll
c}
1,9.0 - GRAVEL CONTENT, % ( F i = 25%)

I 0 40
6" M O L D 18" M O L D 6" M O L D 18" M O L D
O P T W, % 8.6 6.9 7.9 7.3

M A X . "Xd, P C F 130.9 133.9 131.1 134.1
115 I I I I .I
2 4 6 8 10 12
WATER CONTENT p ~
FIG. 5--Compaction curves f o r tests to determine effect o f varying mold diameter.
TEST GRADATIONS
~51EVE 0PENINGS;I : SIEVE NUMBERS P

3 3/4 4 I0 40 200
I00 i I 0
\~ .
ki \ ,,..--3/4", MAXl,
80 20m
Z
,"~,..\ ,I ,l r~.
k,-
I-
60 _, ~. M~.~~..~; 4o <
I U
Z -I
t-
4o -I
6o z
l,J
D_
20 I i so
I I
,) I
4 GRAVEL L 9 SAND " -- I ~ FINES~
1 4 0 --
3"MAX(FULL. ~ ~ n
SCALESPECIMEN)~ ~l~ N)O0
135
5~
O.
~" 130
h- ANDREPLACEDSPECIMEN)
I
0
NOTE: T E S T S P E R F O R M E O USING 18*IN.-O~AM M O L D .

)-
Z 125
MAX. P A R T I C L E
120 SIZE, IN,
::]/4 3
OPT W, % 7.3 5.9

MAX. ~Xd. P C F 134,1 138.0
115 I I I I I
4 6 8 l0 )2
WATER C O N T E N T t ='7o
FIG. 6--Compaction curves for tests to determine effect of removal and replacement
of oversize particles.
oversize particles compares to a difference of 2.2 lb/ft 3 obtained for a

material from DeGray Dam (48 percent gravel, 26 percent fines) tested
in a pervious Corps of Engineers investigation [5] and a difference of 4
lb/ft 3 obtained for a material containing 59 percent gravel and 14 percent
fines, tested in an investigation by the South Atlantic Division Laboratory
of the Corps of Engineers [4]. It should be pointed up that results of
comparable tests on specimens having gravel contents other than 40 per-
cent would probably not indicate the same differences due to scalping
and replacement.
Effects of Gravel Content

Full-Scale Specimens--Figure 7 presents compaction curves and data
for large-scale tests performed on specimens having gravel contents rang-
ing from 0 to 100 percent and a maximum particle size of 3 in. (except, of
course, for the 0-gravel material). The fines content (minus No. 200 sieve
material) of each specimen, except for that of the 100-percent gravel ma-
terial, was maintained at 25 percent. The maximum dry unit weight versus
gravel content curve for the tests on full-scale samples (Fig. 8) shows that
the maximum dry unit weight increased as the gravel content varied from
0 to 40 percent and then decreased with increasing gravel content above
40 percent. The increase in density between gravel content of 0 and 40
percent was 4.1 lb/ft 3. It is common knowledge that a threshold or opti-
mum gravel content exists, past which, particle interference produces
lower densities. However, other investigators have not shown optimum
gravel content as low as 40 percent or such small increases in density with
increasing gravel content in the range from zero to optimum. Holtz and
Lowitz [6], for example, showed a 17 lb/ft 3 increase in maximum dry unit
weight for a comparable increase in gravel content (0 to 40 percent) and
an optimum gravel content of between 60 and 70 percent in tests conducted
on a clayey gravel (liquid limit = 49, plasticity index = 28). However, in
their tests, as well as in those of other previous investigators [2,3] the
fines content varied significantly because the gradation of the minus No.
4 fraction remained unchanged with the addition of various amounts of
gravel. It is thought that this may account for the difference in results be-
tween those obtained for this investigation and those obtained previously.
As will be shown in the following paragraphs, fines content has a greater
effect on maximum dry unit weight than does gravel content. The opti-
mum water content versus gravel content curve for full-scale specimens
(Fig. 8) shows that, except for a small increase in optimum water content
occurring for gravel contents slightly above the optimum gravel content,
optimum water content decreases with increasing gravel content.
Scalped and Replaced Specimens--Figures 9 and 10 present compaction
curves and test data for the small-scale tests, using the hand-held rammer
TEST GRADATIONS
~SIEVE 0PENINGS~i = SIEVE NUMBERS--
3 3/4 4 10 40 200
100 0
~ I I
- ~ , 10~
8O 20
uJ
or I I
Z c,-' ~ \ \ i I <
E 60 -i-,, ,-, G;~\\'N I 4O O
u
Z Gr" II"
~4o o 6o ~"
I
20 -I o 80 a_
I I
I I l
-I "N I I I I00
SAND I= FINES~
140
50% Gr ~
135
40% Gr
U
~'0130 20~7o Gr
60% Gr
I-
'0
t.o
I'-
Z t25 NOTE: TESTS PERFORMED USING 18-1N. DIAM MOLDI AND
MECHANICAL COMPACTOR,
GRAVELCONTENT,%
120 0 10 20 30 40 50 60 1O0
OPT W, % 6.9 6.7 6,1 5.7 5.9 5.8 5.2 -*

MAX. ~d' PCF 133.9 135.0 136.1 137.2 138.0 137.1 134.9 112.0
* SINGLE POINT TEST PERFORMED ON DRY MATERIAL.
115 I I I [ I
2 4 6 8 i0 12
WATER CONTENT~ 07o
FIG. 7--Compaction curves for tests performed on full-scale specimens having variable
gravel contents.
P
M A X I M U M DRY U N I T WEIGHT )'dMAx~PCF OPTIMUM WATER C O N T E N T ~ aTo
5' : F,
O O O O
O -r
/
rrl
z
o
z
rm~ m
OO z
o
0
Z z
m z_ r-
ffJ
(31- 0
O~ >
~0 o,.2 r'-
"1
1-~ - 0
z
0-I 0
~0
z
o
m
"u
r'-
0
m
m
z
.-t
(~
TEST GRADATIONS
~SIFVE OPENINGS- t " SIEVE NUMBERS

3 3/4 4 I0 40 200
IO0
L! "~'o~ I
9'o~ c - . \
I
I
~c
8O -I
I 20~C.""~ I
~ I
'20
YO~. i uJ
ol
,o;:.%,,",,i
-I n,
I
E 6O -I 4o ~
I--
Z -I U
p-
I
~ 4o -I 6o ~
Q. II w
20 I I I 80 a.
I I I
I I I
I I I
I00
GRAVEL SAND I~ FINES~
140
NOTE: TESTS PERFORMED USING 6-1N.-DIAM MOLD,
135
%
a_
;~130 -
z 20%G r ~ ~
o
w
30%Gr~
F-
Z 125-
40%G~50%Gr~
a
%Gr
GRAVEL CONTENT, %
120
0 10 20 30 40 50 60 100
OPT W, % 8.6 7.7 8.1 8.1 7.9 7,8 9.5 -*
MAX. ~/d' PCP 130.9 ~33,5 f32.5 132,3 131.1 131.9 129.5 103.6
" SINGLE POINT TEST PERFORMED ON D R Y M A T E R I A L .
115 I i I I I
2 4 6 8 I0 I?_..
WATER CONTENT; ~
FIG. 9--Compaction curves f o r small-scale tests performed on specimens having scalped

and replaced coarse particles with variable gravel contents by mechanical compactor.
TEST GRADATIONS
"SIEVE OPENINGS=[ : SIEVE NUMBERS
3 3/4 4 I0 40 200
I00 o
o~__' I
8O t
I
LI
l
~ I
I
20 ac
uJ
Z I
~- 60 -I
I-
Z
I c~i , t--
~4o -I G 6o ,.z,
5
0. %,
20 I ~T I I ao ~-
I I I
,, I
I
I
F
100
I.
i
GRAVEL _- 1T_ - SAND = I = FINES~
140 --
NOTE: TESTS PERFORMED USING 6-1N.-DIAM MOLD.
135 --
I,i_
u
o_
~130
p-
"r
L~ 20% Gr
b
bJ
z 125 sos o,~,i~ /
a
ii,,~"'t- 60% Gr
GRAVEL CONTENT, %
120
0 10 20 30 40 50 60 100
OPT W, % 8.0 7.8 7.9 7.9 7.9 8.0 9.2 --*
MAX. ~d' PCF 132.6 132.5 131.8 132.0 132.0 129.3 128.5 101.2
SINGLE POINT TEST PERFORMED ON D R Y M A T E R I A L .
115 I I I I I
2 4 6 8 I0 12
WATER CONTENT/ 07o
FIG. l O--Compaction curves for small-scale tests performed on specimens having scalped
and replaced coarse particles with variable gravel contents by hand-held compactor.
and mechanical compactor, performed on scalped and replaced specimens

having a maximum particle size of 3/4 in. (except, of course, for the
0-gravel material) and gravel content ranging from 0 to 100 percent. The
fines content of each specimen (except for the 100-percent gravel material)
was maintained at 25 percent. Figure 8 shows no significant difference in
optimum water content and maximum dry unit weight between tests per-
formed using mechanical and hand-held rammers. Figure 8 also shows
that the threshold gravel content at which particle interference begins to
produce lower maximum dry unit weights is between 10 and 20 percent
for the scalped and replaced specimens, as compared to the value of 40
percent for the full-scale specimens. This finding, that the more poorly
graded gravel fraction resulting from the scalping and replacement pro-
cedure significantly lowers the optimum gravel content, is contrary to that
of Holtz and Lowitz [6], who indicated that the optimum gravel content is
only slightly decreased for a poorly graded gravel fraction in small-scale
tests. However, as mentioned previously, their results reflect effects due
to both gravel and fines variation, and it may be possible that the increase
in maximum dry unit weight values with increasing gravel content for
their tests was due to the decrease in fines content, rather than to increased
gravel content. When comparing the compaction results in Fig. 8, it should
be remembered that differences in maximum dry unit weight between the
scalped and replaced and the full-scale specimens reflect effects due to
equipment size, in addition to the effects of the scalping and replacement
procedure. The optimum water content versus gravel content curves for
the scalped and replaced specimens (Fig. 8) show that, unlike that for the
full-scale specimens, there was no significant change in optimum water
content with increasing gravel content up to 50 percent. In this range (0 to
50 percent), optimum water content values for the full-scale specimens de-
creased from 6.9 to 5.8 percent, while those of the scalped and replaced
specimens averaged 7.9 percent. The higher optimum water content values
for the scalped and replaced specimens were apparently caused by the
interference of the gravel on the compaction of the fines.
Effect of Fines Content

Full-Scale Specimens--Compaction curves and data for full-scale speci-
mens having fines contents (percent by weight passing the No. 200 sieve)
of 15, 25, and 35 percent and a maximum particle size of 3 in. are given
in Fig. 11. The gravel content of each sample was 40 percent. The data
show that, as the fines content increased from 15 to 35 percent, the maxi-
mum dry unit weight decreased, and the optimum water content increased.
The influence of fines on compaction characteristics was much greater
than that of gravel. A change in gravel content from 0 to 40 percent re-
suited in an increase in maximum dry unit weight o f 4.1 lb/ft 3 and a de-
crease in o p t i m u m water content o f 1.2 percent, whereas a change in fines
content from 15 to 35 percent resulted in a 8.5 lb/ft ~ decrease in maxi-
TEST GRADATIONS
~SIEVE OPENINGS'I 9 SIEVE NUMBERS--
3 3/4 4 10 40 200
|00 \ I , I I I
\ I I i
I I I I
I I I
8O ' ' I 20
~ L i i I ,
Z
L~ 60
Z Fi t---
~4o 6o ~
13.
',~ ~ ~; ~.~
2O i I
I I
I I I00
GRAVEL - SAND = I= FINES~
1 4 5 --
NOTE: TESTS PERFORMED USING 18-1N.-DIAM MOLD.
140 --
Lt_
u
0-
0%
I--
~ 13e_
125 -- FINES CONTENT,

( G r : 40%)
15'7, 25% 35%
OPT W, % 4.9 5.9 7.5

MAX. "7"d, P C F 141.8 138.0 133.3
J20 I I I I I
2 4 6 8 I0 12
WATER CONTE NT, eTo
FIG. l l--Compaction curves for large-scale tests performed on full-scale specimens

having variable fines contents.
mum dry unit weight and a 2.6 percent increase in optimtnn water con-
tent.
Scalped and Replaced Specimens--Compaction curves and test data for
small-scale tests on scalped and replaced specimens having 3A in. maxi-
mum particle sizes with fines contents of 15, 25, and 35 percent are
given in Fig. 12. The gravel content of each specimen was 40 percent.
These results, summarized in Fig. 13, show that the effect of fines con-
tent in the small-scale tests is similar to that in the large-scale tests. In
the small-scale tests, an increase in fines content from 15" to 35 percent
decreased the maximum dry unit weight 8.2 lb/fP and increased the
optimum water content 2.0 percentage points. By comparison, for the
same variation in fines content for the large-scale tests, the maximum dry
unit weight decreased 8.5 lb/ft 3, and the optimum water content in-
creased 2.6 percentage points. As in the case of tests performed to deter-
mine effects of varying gravel contents, the higher optimum water con-
tent values obtained for scalped and replaced specimens was probably
caused by a lower compactive effort being applied to the fines as a
result of interference of the gravel. The differences in maximum dry unit
weight between the scalped and replaced and the full-scale specimens,
indicated by the curves in Fig. 13, are due to the scalping and replacement
procedure and the effects of variation in equipment size.
Applicability of Theoretical Equations and the Scalping and

Replacement Procedure
Various theoretical equations have been derived to compute the total
density of a material containing oversize particles, based on densities
obtained from small-scale tests without replacement.
(a) The most commonly used equation, presented by several investiga-
tors, including Shockley [7], is as follows
yfOmyw
y~ = X 100 (i)
YsP~ + G.,ywP~
where
ya = calculated dry unit weight of total sample,
Yi = dry unit weight of finer fraction (from compaction tests on
scalped material),
G m = bulk specific gravity of coarser fraction (oversize material),
yw -- unit weight of water, and
Pi and Pc -- percent of fine and coarse material by weight of the sam-
ple.
TEST GRADATIONS
!
*SIEVE OPENINGS~'{ " ~ SIEVE NUMBERS
3 3/4 4 I0 40 200
I00 , I 0
'
I i
I i
n- 8O I I
2 0 ~c
td I !
Z cc
t,. 60 4o o~
j- U
z I I I I
I.-
,, ', 6o z
G. : I ~ ~ 25% F i
i
2O "1 I I 1 so
I 5%
J I I IO0
L
[,4 GRAVEL -I : SAND = I ~ FINES~
140
NOTE: TESTS PERFORMED USrNG 6-1N.-DIAM MOLD.
135
~" 130
%
t~
I-
Z 12~
o
o
FINES CONTENT, %
120 --
( G r = 40%)
15% 25% 36%

OPT W, % 7.4 7.9 9.4
MAX. "Xd, P C F 134.8 131.1 126.6
115 I I I I I
2 4 6 B I0 IZ
WATER CONTENT I '='7o
FIG. 12--Compaction curves f o r small-scale tests performed on specimens having

scalped and replaced coarse particles with variable fines contents.
12
/
~ I0
I--
Z
SCALPED AND REPLACED
SPECIMENS (6-1N,-DIAM MOLD)~
~ 8
/
/
/
o
J
"~ FULL-SC~LE SPECIMENS
I0 20 30 40 50
145
t,_ 1 4 0
Q.
\
\
N
\.
I- 1 3 5
-.... \
I-
Z
D
4
X
~[ 1 2 5
1,20
t0 20 30 40 50
FINES CONTENT~ 070 ( G r = 4 0 ~
FIG. 13--Optimum water content and maximum dry unit weight versus fines content for
full-scale and scalped and replaced specimens.
The equation is based on the assumption that the coarser particles simply
replace the finer material, with the density of the finer material remaining
constant. Generally, Yi is considered to be the density of minus No. 4
material. However, its value can be based upon other sizes. For example,
calculations can be made for plus 90 material, if the density of the
minus 90 material is known. In this case, P~ amd Pc are the percentages
of material finer and coarser than 90 in., respectively. The equation
makes no allowances for the interference of the coarser particles to the
compaction of the finer fraction at higher gravel contents. The gravel
content at which interference is initiated is referred to as the limiting
gravel content and is the gravel content at which a theoretical curve,
based on Eq 1, corrected for equipment effects, and the experimental
curve, begin to diverge. Tests performed by the U.S. Bureau of Reclama-
tion [8] have shown that, for poorly graded fractions, such as may result
from the scalping and replacement procedure, the limiting gravel content
may be less than 10 percent, while for well-graded coarse fractions, such
as might occur when the maximum particle size is increased to that of a
full-scale sample, the limiting gravel content may be as high as 35 to 40
percent.
(b) The FAA [9] uses the following equation to account for oversized
particles
PyYs + 0.9 PcGmyw

yd= (2)
100
where the terms are the same as those defined in Eq 1. The equation is
simply the weighted average of the densities of the finer and coarser
fractions, based on the percent by weight of each in the total sample. A
factor of 0.9 is used to account for the coarser particles interfering with
the compaction of the fine fraction.
Table 3 lists test data for small-scale tests conducted on minus No. 4
fractions of the full-scale samples, using a hand-held rammer and 4-in.-
diameter mold. These tests were conducted to provide input data for the
preceding equations. Figure 14 shows relationships between dry unit
weight and gravel content, developed using results of these tests with Eqs
1 and 2, along with experimental values obtained for the full-scale and
the scalped and replaced samples. As may be seen, the curves show that,
for gravel contents in the range from 0 to 50 percent, the use of Eq 1,
with results of tests performed on finer fractions, provides a better ap-
proximation of experimental results than does Eq 2 or the relationship
developed from tests performed on scalped and replaced samples. The
curve based on Eq 1 almost coincides with the experimental curve up to
the limiting gravel content of approximately 35 percent. The curve based
on Eq 2, on the other hand, indicates significantly lower maximum dry
TABLE3--Compaction tests performed on minus No. 4 fractions of full-scale specimens.
MinusNo. 4 Fractionsof Full-ScaleSpecimens

Having VariableGravelContents
Gravel content, 070 10 20 30 40 50 60
Optimum w, 070 8.2 8.6 9.3 9.8 10.5 11.9
Max Ya,lb/ft~ 132.0 13L0 128.5 127.0 124.8 119.3
MinusNo. 4 Fractionsof Full-ScaleSpecimens
Having VariableFinesContents
Fines content, % 15 25 35
Optimum w, ~ 8.1 9.8 11.7
Max )'a, lb/ft~ 132.1 127.0 121.5
unit weight values than those indicated by the experimental curve for
gravel content in this same range (from 0 to 50 percent). At a gravel con-
tent of 40 percent, for example, the value computed using Eq 2 is 3.8
lb/fP less than the corresponding experimental value. Thus, it appears
that the use of results from tests performed on minus No. 4 fractions
of full-scale samples and Eq 1 would provide the most suitable means
of predicting densities of full-scale samples having gravel contents below
about 50 percent.
By comparison, results of the previous Corps of Engineers study [5] on
full-scale and scalped and replaced samples of a clayey sandy gravel
from DeGray Dam, having a gravel content of 54 percent, showed that
the scalping and replacing procedure gave slightly better estimates of the
full-scale maximum dry unit weights than did Eq 1. The maximum dry
unit weight of the full-size sample was 127.9 lb/fP, and the maximum dry
unit weight of the small-scale test on scalped and replaced material
underestimated this density by 4.3 lb/fP. On the other hand, Eq 1 over-
estimated the full-size maximum dry unit weight by 4.9 lb/fP. Most of
the error associated with Eq 1 is attributed to the increased particle
interference, which occurs at higher gravel content. In the case of Eq 2,
which considers particle interference through a correction factor of 0.9,
excellent agreement was obtained between the calculated maximum dry
unit weight, 128.1 lb/fP, and the observed value, 127.9 lb/fP. This agree-
ment by Eq 2, as opposed to the overestimation of Eq 1, indicates that
particle interference must be accounted for at higher gravel contents.
Relationships between fines content and maximum dry unit weight,
developed using Eqs 1 and 2, with results from tests performed on minus
No. 4 fractions of the full-scale samples, are given in Fig. 15. Also in-
cluded are experimental relationships developed from tests performed on
the full-scale and the scalped and replaced samples. These curves show
that, for tests in which the fines content is varied while maintaining the
170
1 T
EQUATIONS APPLIED TO DATA
GIVEN IN FIG. T A B L E GM = 2.58
160
/
THEORETICAL CURVE BASED ON /
SHOCKLEY'IS EQUATION (EQ I ) . . . . ~ /
b 150
THEORETICAL CURVE BASED 4/"
ON EAA EQUATION (EQ 2)~..~ /
/
. ~ 140
0
t-- q
1:30
o
g
120
-- - - EXPERINENTAL CURVE N N I
SCALPED AND REPLACED SPECIMENS~'~ ~ I
(6-1N,-DIAM M O L D ) ~ ~ - ~ \ I
IlO
I00
0 20 40 ~0 80 I O0
GRAVEL CONTENT.=, ~
FIG. 14--Experimental and theoretical relationships between maximum dry unit weight
and gravel content.
gravel content constant (40 percent), Eq 1 once again provides a better

approximation of experimental results than does Eq 2 or the relationship
developed from results of tests performed on scalped and replaced
samples. It is of interest to note that, since Eq 1 provides the best agree-
ment with the full-scale experimental curve, the threshold gravel content
at which particle interference produces lower maximum dry unit weights
(optimum gravel content) may not have been affected by varying the fines
content.
145
b
r
X
,,{
140
"%, ~~
.~
/= ~ r /
f
~----THEORETICAL CURVE BASED ON
SHOCKLEY'SEQUATION (EQ l)
I-
3: ~'X~
0
~
\~EXPERIMENTAL CURVE FULL-SCALE
\ P E CIMEN5 (78.1N-DIAM MOLD)
1:35
Z
x~
~b.~---THEORETICAL CURVE BASED ON

e~ ~ FAA EQUATION (EQ 2)
EXPERIMENTAL CURVE, SCALPED AND

EPLACED SPECIMENS (6.1N.-DIAM MOLs
~z5 6
I0 20 30 40 50 60
FINES CONTENT, '~o
FIG. 15--Experimental and theoretical relationships between maximum dry unit weight
and fines content.
Conclusions
The results of this program of tests performed on blended earth-rock
material indicate the following conclusions.
(a) Maximum dry unit weight and optimum water content vary with
sizes of equipment used. When the mold diameter is increased from 6
to 18 in. and the rammer weight is increased from 5.5 to 24.7 lb, the
maximum dry unit weight of specimens containing 0 and 40 percent gravel
with 25 percent fines is increased by 3.0 lb/ft 3. For the same increase in
equipment size, the optimum water content for the specimen containing
no gravel is decreased by 1.7 percent, while that of the specimen
containing 40 percent gravel is decreased by 0.6 percent.
(b) The scalping and replacement procedure results in a lower maximum
dry unit weight and a higher optimum water content than obtained when
testing the full-scale specimen. In the case of tests performed using an 18-
in.-diameter mold on a full-scale and a scalped and replaced sample
having 40 percent gravel and 25 percent fines, the maximum dry unit
weight and optimum water content of the scalped and replaced sample is
3.9 lb/ft 3 lower and 1.4 percent higher, respectively, than the correspon-
ding values for the full-scale sample.
(c) For tests in which the gravel content is varied while maintaining
the fines content constant, the optimum gravel content, that is, gravel
content producing the highest density, is decreased from 40 percent to

between 10 and 20 percent by the scalping and replacement procedure.
Thus, in the range of gravel contents from between 10 and 20 percent to
40 percent, the difference between maximum dry unit weights determined
for fuU-scale and for scalped and replaced specimens increases with
increasing gravel contents.
(d) When the fines content is varied from 15 to 35 percent while
maintaining the gravel content constant, maximum dry unit weights and
optimum water contents of the full-scale and the scalped and replaced
samples vary similarly.
(e) The influence of fines content on compaction characteristics is much
greater Shan that of gravel content. A change in gravel content from 0
to 40 percent resulted in a difference in maximum dry unit weight of
4.1 lb/ft 3 and a difference in optimum water content of 1.0 percent,
whereas a change in fines content from 15 to 35 percent resuked in an
8.5 lb/ft 3 difference in maximum dry unit weight and a 2.6 percent
difference in optimum water content.
(10 For gravel contents ranging up to 50 percent, the Eqs 1 and 2 pro-
vide better approximations of experimental results than do the relation-
ships developed using the Corps of Engineers scalping and replacement
procedure. In this range, Eq 1 provides a better estimate of actual results
than does Eq 2. For gravel contents above 50 percent, Eq 2 produces the
best agreement for gravel content in the range from 50 to 60 percent.
Acknowledgments
The tests described and the resulting data presented herein, unless
otherwise noted, were obtained from research conducted by the Water-
ways Experiment Station for the Civil Works Investigation Studies Pro-
gram sponsored by the Office, Chief of Engineers. Permission to publish
this information was granted by the Chief of Engineers. W. J. Hughes
was the principal engineering technical assisting in the laboratory pro-
gram. Additional personnel assisting in performing tests were Isaac
Smith, Jr., Mose Ellis, and R. L. January.
APPENDIX
The scalping and replacement procedure as outlined in Ref 1 follows:
(a) Spread the material to be tested in flat pans and air dry the entire sample.
Other means, such as ovens and heat lamps, may be used to accelerate drying if
the maximum drying temperature is 60 ~
(b) Reduce all aggregates, or lumps formed during drying, of fine-grained
material to particles finer than the No. 4 sieve. With a wire brush or other means,
remove all fine-grained material that may be clinging to rock sizes, taking care not
to lose the fine-grained material.
(c) Separate all the material, using a set of sieves ranging from the largest
particle size in the sample to the No. 4 sieve. The total sample must be processed
to determine the as-received gradation.
(d) Place the material retained on each sieve and that passing the No. 4 sieve
in separate containers, weigh the contents of each, and compute the percent of
the total sample retained on each sieve as follows:
070 retained = dry weight of material retained on sieve

x 10007o
dry weight of total sample
(e) If 10 percent or less of a field sample is retained on the 2-in. sieve, the
partides larger than this size should be discarded, and replacement is not necessary.
(]) If more than 10 percent of a field sample is retained on the 2-in. sieve, it will
be necessary to remove the plus 2-in. sizes, and replace them with an equal weight
of material between the 2-in. and No. 4 sieve sizes. The gradation of the replace-
ment material must be the same relative gradation as that of the total sample
between the 2-in. and the No. 4 sieve sizes. The percent passing the No. 4 sieve
remains constant and is equal to the percent passing the No. 4 sieve for the total
as-received sample. For each sieve between the 2-in. and the No. 4 sizes, the per-
cent required to replace the plus 2-in. sizes is computed as follows
replacement O7o = total 070 of __2-in. sizes x

070 retained on one sieve s
total ~ between 2-in. and No. 4 sieve
For each sieve, add the "replacement 070" to the "~ retained" on that sieve
initially. This gives the percent by weight of a test specimen required for each
sieve size in order to reconstitute a specimen with the +2-in. sizes replaced with
sizes ranging from the 2-in. to the No. 4 sizes.
References
[1] "Engineering and Design: Laboratory Soils Testing," Engineer Manual EM 1110-2-1906,
Office, Chief of Engineers, Department of the Army, Washington, D.C., Nov. 1970.
[2] Ziegler, E. J., "Effect of Material Retained on the Number 4 Sieve on the Compaction
Test of Soil," Proceedings, Highway Research Board, Vol. 28, 1948.
[3] Cunny, R. W. and Strohm, W. E., Jr., "Compaction Tests on Gravelly Soils with
Cohesive Soil Matrix," Miscellaneous Paper No. 3-676, U.S. Army Engineer Water-
ways Experiment Station, Vicksburg, Miss., Oct. 1964.
[4] "Procedures and Equipment for Determining the Maximum Standard Compaction
Density of Granular Material (6 and 12 in. Diameter Molds)," U.S. Army Engineer
Division Laboratory, South Atlantic, March 1968.
[5] Donaghe, R. T. and Townsend, F. C., "Compaction Characteristics of Earth-Rock
Mixtures, Report 1, Vicksburg Silty Clay and DeGray Dam Clayey Sandy Gravel,"
Miscellaneous Paper No. S-73-25, U.S. Army Engineer Waterways Experiment Station,
Vicksburg, Miss., May 1973.
[6] Holtz, W. G. and Lowitz, C. A., "Compaction Characteristics of Gravelly Soils,"
Earth Laboratory Report No. 509, U.S. Bureau of Reclamation, Sept. 1957.
[71 Shockley, W. G., "Correction of Unit Weight and Moisture Content for Soils Con-
taining Gravel Sizes," Technical Data Sheet No. 2, U.S. Army Engineer Waterways
Experiment Station, June 1948..
[8] U.S. Bureau of Reclamation, "Research on Compaction Control Testing of Gravelly
Soils," Earth Research Program, EM 662, 8 Aug. 1963.
5Any sieve between 2 in. and No. 4 sieve sizes.
[9] Mainfort, R. C. and Lawton, W. L., "Laboratory Compaction Tests of Coarse-Graded

Pavement and Embankment Materials," Proceedings, Highway Research Board, Vol.
32, 1953.
P. Y. L e e I
Study of Irregular
Compaction Curves
REFERENCE: Lee, P. Y., "Study of Irregular Compaction Curves," Soil Specimen

ABSTRACT: Curves of dry density versus moisture content, as yielded by the

standard ASTM compaction tests, usually show a single maximum, but some soils
exhibit compaction curves with irregular shapes. This study examines some of the
influences of soil preparation on these irregular compaction curves. When a surface
tension reducing agent, such as aerosol-AY, is added to the water in soil specimen
preparation, the shape of the irregular compaction curve will be altered. This
effect is regarded as a verification of the effects of negative pore water pressure on
the irregular compaction curve. In repeated compaction tests, it is economical and
convenient to reuse the soil specimens. The results of liquid and plastic limit tests
reveal approximatdy the same values in new and reused specimens. However, the
reused soil specimens reveal a predominantly higher density in the zone of lower
water content in an irregular compaction curve.
KEY WORDS: soils, tests, compaction, clays, surface tension, soil mechanics,
density, clay minerals, water content
Many soils are too weak and unstable to perform adequately as good
engineering materials. Despite their inadequacies, many of these materials
must be used in engineering construction because it is not economically
feasible to bypass or replace them. To correct their deficiencies, such
soils must be stabilized. Various methods of stabilization are currently
used, but the most common and most useful method is that of soil com-
paction. The compaction process involves optimizing the water content
so that maximum density is reached, thereby providing the greatest
stability. For most soils commonly encountered in earth construction,
there is a single peak in the dry density versus moisture content relation-
ship (Fig. 1). In contrast to this, some soils yield compaction curves with
two peaks or a curve that is oddly shaped (Fig. 2). An acceptable and
l Associate professor, Department of Civil Engineering, Tulane University, New Orleans,
La. 70118.
278
Downloaded/printed
LEE ON IRREGULAR COMPACTION CURVES 279
m .
I I I I | ! i ! -
r~
~z
I I I I
MOISTURE CONTENT - % MOISTURE CONTENT - %
FIG. 1--Typical single peak compaction curve. FIG. 2--Irregular compaction curves.
experimentally demonstrable explanation for these irregularly shaped

curves has not been given; attempts have been made to rationalize the
phenomena. Because of the limitied research on the subject, the existing
theories of compaction have not been extended to explain these irregular
curves.
The compaction process itself is only partially understood; it has been
known for some time, however, that water plays an extremely important
role, especially with fine-grained cohesive soils. The effect of water on
the common single peak compaction curve is included in some of the
basic theories of compaction; however, the scope of this discussion in-
dudes only a limited explanation of the effect of water on irregular com-
paction curves.
Therefore, a laboratory investigation was designed to analyze the
irregularly shaped compaction curves in detail. Of the four compaction
theories proposed previously, Proctor's capillarity and lubrication theory
[1], 2 Hogentogler's viscous water theory [2], Lambe's physico-chemical
theory [3], and Olson's effective stress theory [4], none has been extended
to explain the complete irregular compaction curve; all have been de-
veloped for a single peak compaction curve. Several shapes have since
been observed to which the preceding theories have not been applied
[4-7]. Olson noted this deficiency when he stated that the effective stress
theory can only be applied to the peak at the higher water content. Olson
presented a tentative explanation for his having double peaked curves in
limited experiments on the kneading compaction of an ill!tic clay. For the
first peak at the lower water content in the double peak compaction
curve, O]son reasoned that, when the soil is dry, high surface friction is
2The italic numbers in brackets refer to the list o f references appended to this paper.
present, resulting in high shear strength and a low dry density. As water is
added, the effect is one of lubrication, thereby increasing the dry density.
At this point, water menisci begin to form, tending to increase the soil
strength by providing more particle contact area. The balance point
between lubrication and the formation of water menisci then occurs at
the low-water-content peak point. Additional water results in more
menisci, causing an increase in effective stress and a decrease in dry
density because less particle interference is required to resist the applied
pressure. When all the possible menisci have developed, the minimum
point between the two compaction peaks is reached. Olson then reasoned
that additional water reduces the pressure differential across the menisci,
at which point, the effective stress considerations should begin to apply.
With only limited data available, Olson proposed that the double peak
curve could only form in soils containing a dominant percentage of plate-
shaped collodal particles. Additional research in this area included work
of Lee and Suedkamp [5] on characteristics of irregularly shaped com-
paction curves. They investigated 34 different soils possessing a wide
range of characteristics and identified the compaction curve for each. By
mixing different portions of commercially available soils, they were able
to obtain a large variety of soil characteristics in their specimens. The
compaction curve for each specimen was then produced by ASTM Tests
for Moisture-Density Relations of Soils, Using 5.5-1b Rammer and 12-in.
Drop (D 698-70). They found that specimens with a liquid limit between
30 and 70 usually yielded the typical single peak compaction curve. Speci-
mens with a liquid limit of less than 30 and greater than 70 usually pro-
duced irregularly shaped curves. There are only a few exceptions to this
rule which was probably caused by the mineral constituents of the specific
specimens. The classification breakdown is shown in Fig. 3. Olson's
hypothesis is logically appealing; hence, the first objective of this investi-
gation was to examine the influence of negative pore pressure on the
irregularly shaped compaction curve by using a surface tension reducing
agent, together with water.
It has long been suspected that there is a difference on moisture-
density curves between values obtained by reusing the same portion of
soil repeatedly and values obtained by using a new batch of soil for each
point on the compaction curve. Concerning this viewpoint, Nelson and
Sowers [8] concluded from a series of tests that the single peak compac-
tion curve produced by reusing the same specimen of soil appears to have
a slightly greater maximum dry density than the single peak compaction
curve produced by using separate batches of soil for each test. It should
be noted that their investigations were limited to examination of the single
peak compaction curve. Therefore, an investigation of the characteristics
of irregularly shaped compaction curves was deemed desirable.
16
I I I I I I I .~
UPPER REGION OF / -I
14 _
12 _
10
m REGION OF TYPICAL
SINGLE PEAK CURVES / O
- i/4o -
~ow~o,o~o~ ,V ! o~
-~'~ ~y'~ ~it 0
I zq~o _
V
/ / ~IZ?~ i [] O,R~GU,.,T
~~-
/ 9 u~ ~ n~PiCAL -
V , J ,'1 i i t i
0 2 4 6 8 l0 12 14 16
~/ LIQUID LIMIT
FIG. 3--A classification of compaction curves [5].
Laboratory Investigation
Soil Specimens
To adequately investigate the influence of the soil preparation on the
irregularly shaped curves, it was necessary to compare several discrete
types of curves. For this reason, a particular selection of soil specimens
was necessary in order to include soils with a wide variance of character-
istics, especially in compaction curves. The approximate compaction
curves were needed as a starting point; therefore, full use was made of
the paper but Lee and Suedkamp on irregularly shaped curves. Noting
their classification scheme of soils according to compaction curve charac-
teristics, and knowing that the compaction curve for each soil had been
identified, it was possible to make a good selection of appropriate soils
for investigation. A few of these were soils found in nature, while
others were laboratory combinations of kaolinite, montmorillonite, illite,
quartz, and felspar, so that the percentages of each mineral could be
known. Selection of minerals provided a good analogy to natural soils
and provided maximum information about the constitution of the soil
specimens. Several specimens were selected, both natural and combined,
for this investigation, and their composition is given in Table 1.
TABLE 1--Selected soil specimens.
Montmoril-
Specimen lonite, b Illinite, c Kaolinite, d Liquid Plasticity
No. Sand, a % % % Limit Index
1 100 0 0 0 0 NP
2 75 0 0 25 13 NP
3 0 0 100 0 51 21
4 75 0 25 0 17 NP
5 25 50 25 0 172 142
6 Pierre shale (natural soil) 110 66
7 Pierre bentonite (natural soil) 310 244
apure sand obtainedlocally.

bBentoniteobtained from Baroid Divisionof Natural Lead Co., Houston, Tex.
CGrundite obtained from GreenRefractioneryCo., Morris, Ill.
d Clay Hydrite--121obtainedfrom Thompson-HaywardChemicalCo., Kansas City, Kans.
Testing Procedure and Test Apparatus

In the compaction process, a variety of factors influence test results to
various degree. These parameters include the type and magnitude of com-
paction effort, size and shape of the mold, type of support for the mold,
depth o f compacted soil, and soil preparation methods. In an effort to
provide a good degree of comparison and of conlxol, standard procedures
were specified for soil compaction, namely Standard American Associa-
tion o f State Highway Officials (AASHO) Designation T99, also known
as ASTM Tests for Moisture-Density Relations of Soils, Using 5.5-1b
Rammer and 12-in. Drop (D 698-70). In this method, soil passing a No. 4
sieve (4.76 mm) is compacted in a 4-in. (10.16-cm) diameter mold by
dropping a 5.5-1b (2.5-kg) hammer from a height of 12 in. (30.5 cm), 25
times per layer, for 3 layers in the 6-in. (15.2-cm) high mold.
In preparation for each test, the soils were air dried and pulverized to
pass a No. 4 sieve, mixed with water in increments of two or three
percent. Each sample was stored in a leakproof plastic bag. A batch of
samples was sealed in a large plastic bag and stored in a moisture control
room for at least 24 h.
Aerosol-AY (100 percent) was used to reduce the surface tension of
the water by 55 percent. This was accomplished by mixing two percent
Aerosol-AY, by weight, with water.
Discussion of Test Results
Reduction o f Surface Tension o f Water by Aerosol

Pore pressure is decreased as the water content is increased. This
phenomenon is directly related to the surface tension of the water, since
LEE O N I R R E G U L A R COMPACTION CURVES 283
surface tension causes water menisci to form and they act as a bond
between the soil particles. This tends to cause more interparticle friction
and a lower dry density, thus causing the depression noted between the
two peaks in the double peak compaction curve. However, if Aerosol-AY,
a commercial surface tension reducing agent, is introduced in the water,
the shape of the double peak curve should be altered. This was found to
be the case.
Aerosol-AY was introduced into the water, causing a 55 percent reduc-
tion in surface tension and notable changes in the shapes of the double
peak compaction curves (Figs. 4-7). In each test, the double-peak curve
was replaced by a single peak compaction curve or one closely resembling
it. Since capillary pressure is directly related to surface tension, the
results of these tests verify the fact that pore pressure, or negative pore
pressure caused by surface tension, is the dominant factor in the formula-
tion of the double-peak compaction curve.
l-] - A E R O S O L TREATED
O - STANDARD TEST
130 m
I25 m
~z
rr
120
Z
115
I I I I I i
5 10 i5
MOISTURE CONTENT, PER CENT
FIG. 4--Double peak curve showing effects of aerosol, Specimen 2.
Influence of Reusing Soil Specimens

It is economical and convenient to reuse soil specimens; however, it is
impossible to thoroughly break up the air-dried aggregations of soil in the
reused specimen into individual particles showing the same grain-size
distribution as a new specimen, particularly in cohesive soils. In the corn-
[] - A E R O S O L TREATED
O- STANDARD TEST
t2S
120
A o
u~
~ [15 []
z
110
S l0 lS
MOISTURE CONTENT, PER CENT
I"I - AEROSOL TREATED
O - STANDARD TEST
85 L
~0
A
Q
75
70 m
I I I I I I
10 20 30 40 50 60
MOISTURE CONTENT, PER C E N T
- AEROSOL TREATED
O - STANDARD TEST
85
80
75
73
I I I,, I I
10 20 30 40 50 60
MOISTURE CONTENT, PER C E N T
FIG. 7--1rregular curve showing effects of aerosol.
paction tests, reused specimens usually gave results different from that of
new specimens.
For the cohesive soils (Figs. 8,9), the significant differences in the shape
of compaction curves between the new and reused specimens are located
on the zone of low-water content. The results of liquid-limit and plastic-
limit tests reveal approximately the same values in new and reused speci-
mens, except that the liquid limit of Specimen 5 was found to be slightly
greater for the reused specimen than the new one. As indicated in Table 1,
these new specimens were combinations of known minerals obtained from
commercial sources. These commercial soil minerals were very uniform
products. According to the results of sieve analysis, however, the grain-
size distribution of new specimens appeared to be much more uniform,
containing many more fine particles than the reused specimens. As
Michaels [9] has pointed up, dried and pulverized clay consists of packets
of many tightly bonded clay particles. The packets do not tend to stick
to each other, and the dry soil lacks cohesion, behaving more like
granular particles. If this theory is true, the higher density of reused
clay at lower water contents is predominantly due to the reduction of
the shear strength caused by the decrease of cohesion between the soil
particles and the nonuniform grain-size distribution. In addition, air-dried
cohesive soil, having been exposed to the air for a long time, usually
retains a small portion of water which is distributed evenly around the
STANDARD TEST
105 TEMPERATURE - 80 ~
" - - ~ ' ~ A [] - NEW SPECIMEN
~ J
SPECIMEN
100
95
Z
90
0 5 10 15 20 25 30
M O I S T U R E CONTENT, PERCENT
FIG. 8--Shape ofcompaction curves for test using new specimen compared with test
reusing the soil, Specimen 5.
STANDARD TEST
TEMPERATURE - 80 ~
~] - N E W SPECIMEN
110
O - REUSED SPECIMEN
tO0
C3
90
0 5 10 15 20 25 30
MOISTURE CONTENT, PERCENT
FIG. 9--Shape o f compaction curves for test using new specimen compared with test
reusing the soil, Specimen 3.
soil particles. It seems difficult for the new specimen, on the other hand,
to have an even distribution of water if mixed with a small amount of
water. The intraparticle lubrication effect, therefore, is greater in the
reused specimen corresponding to a higher dry density. As more water
is added, the effects of packets tend to disappear, and both specimens
should have a more even distribution of water content. As a result, the
dry density attains the same normal value.
In pure sand, shown in Fig. 10, the reused specimen appeared to have
a higher dry density in the portion between the zero water content and
STANDARD TEST
TEMPERATURE - 80~
[] - NE~V SPECIMEN
110
O - REUSED SPECIMEN
] 00
v~
z 95
90
I I .,, I I I t
1S
5 10
MOISTURE CONTENT, PERCENT
FIG. lO--Shape o f compaction curves f o r test using n e w specimen compared with test
reusing the soil.
optimum point (water content from 0 to 8 percent), but there was no

significant variation close to and beyond the optimum point. It was found
that the particle distribution curve from the sieve analysis exhibited
identical shapes for both specimens. However, the percentage passing was
slightly higher on the distribution curve of sieve analysis for the reused
specimen. Therefore, it could be theorized that the difference of dry
density between reused sand and new sand is attributable to the different
grain-size distribution.
Conclusions
On the basis o f this series of laboratory tests, the following conclusions
are suggested:
1. Reused specimens of cohesive clay obtain predominantly higher

densities, in the region of lower water content, as compared to new speci-
mens. The existence of packets of many tightly bonded clay particles in
reused clay and the uneven distribution of water in new clay may have
affected this phenomenon.
2. When a surface tension reducing agent, such as Aerosol-AY, is
added to the water in a soil, the shape of the double peak compaction
curve will be altered. Surface tension has been shown to cause reduction
in pore pressure due to capillarity, thus causing the depression between
the two peaks. However, when the surface tension of the water is re-
duced considerably, the double peak curves are replaced by single peak
curves or by curves closely resembling single peak curves. This is verifica-
tion of the direct relationship between surface tension and pore pressure,
or, more exactly, negative pore pressure.
Ackno wledgment
The financial support provided by the National Science Foundation is
gratefully acknowledged.
References
[1] Proctor, R. R. in Engineering New Record, McGraw-Hill, New York, Vol. III, 1933,
p. 245.
[2l Hogentogler, C. A. in Proceedings, Highway Research Board, National Research
Council, 1936, pp. 309-316.
[3] Lambe, T. W., Transactions, American Society of Civil Engineers, Vol. 125, 1960,
pp. 682-706.
[4 ] Olson, T. E., Journal of Soil Mechanics and Foundation Division, Proceedings, Ameri-
can Sodety of Civil Engineers, Vol. 89, No. SM2, 1963, pp. 27-45.
[5] Lee, P. Y. and Suedkamp, R. J., "Characteristics of Irregularly Shaped Compaction
Curves," Highway Research Record 381, 1972, pp. 1-9.
[6] Lee, P. Y. and Hsu, D. C., "Temperature Effect on Irregularly Shaped Compaction
Curves of Soils," Highway Research Record 438, 1973, pp. 16-20.
[7] Johnson, A. W. and Sallberg, J. R., "Factors Influencing Compaction Test Results,"
Bulletin No. 319, Highway Research Board, National Research Council, 1962, pp. 1-146.
[8] Nelson, G. H. and Sowers, G. F., "Effect of Re-using Soil on Moisture-Density
Curves," Proceedings, No. 29, Highway Research Board, 1949, pp. 482--487.
[9] Michaels, A. S., Discussion of "Physico-t3aemical Properties of Soils: Soil-Water
System," by I. Th. Rosenqvist, Proceedings, Paper 2010, American Society of Civil
Engineers, April 1959.
J. E. Gillott'
Importance of Specimen Preparation

in Microscopy
REFERENCE: Gillott, J. E., "Importance of Specimen Preparation in Microscopy,"

Soil Specimen Preparation for Laboratory Testing, ASTM STP 599, American
Society for Testing and Materials, 1976, pp. 289-307.
ABSTRACT: Samples must be representative and specimen preparation must intro-

duce ,'is few changes as possible if microscopic information is to be significant in
characterization and classification of soils and rocks and in interpretation of their
engineering behavior. Soils and recent sediments are damaged most easily, and
specimen preparation is most complex for these materials. Air drying may cause
shrinkage and distortion; freeze drying and drying by the critical point method pro-
vide partial solutions. Even so, differences in the procedure followed in the removal
or replacement of water can cause marked differences in appearance of specimens
examined on the electron and optical microscopes. Sectioning and surface exposure
may also introduce artifacts. Soil specimens for fabric study commonly are fractured
when frozen, since cutting may not be used generally. The use of ion bombard-
ment in metal coating and as an etch method is discussed, and the possibility of
improving specimen preparation procedures by combining an etch technique with
freeze drying is outlined.
KEY WORDS: soils, rocks, microscopy, water replacement, freeze drying, ion beams
ion bombardment
Engineers examine soils and rocks microscopically to understand their

behavior and properties better and to place classifications on a more
scientific foundation. The most commonly used instruments are the opti-
cal microscope, the transmission electron microscope, and the scanning
electron microscope. X-ray diffraction procedures are used widely in all
areas of microstructural analysis but will not be described in this paper
dealing with microscopic methods.
Laboratory preparation varies with the information sought and the
technique employed. Fabric studies may involve drying or water replace-
ment, fracture, or sectioning and replication, or coating. Information to
~Professor, Department of Civil Engineering, University of Calgary, Calgary, Alta.,

Canada.
289
Downloaded/printed
do with size distribution and morphology of minerals often involves speci-

men disaggregation and dispersion.
Users of the optical microscope had less success in interpreting soil
structure than was achieved in the related field of petrology because clay,
often the most important constituent in soil, is too fine grained to be re-
solved satisfactorily by light optics. Nonetheless, useful information to do
with both overall fabric relations and composition of silt- and sand-sized
minerals can be obtained. Light will pass through a standard thin section
(',,30 /am) of most soils, and slides are made by a modification of the
procedure used for the rocks.
Specimens examined on the transmission electron microscope may be
individual particles, replicas, or ultrathin sections. The microtome has
been employed to make sections from soils, supported by impregnating
agents, but practical difficulties limit the method to a few select clays, and
replicas or dispersed particles are examined, more commonly.
The specimen is deposited on a metal disk containing a fine grid, which
may range from 200 to 1000 meshes to the inch, depending on the appli-
cation. Special supports are available also or can be made for particular
uses. The grid is coated with collodion, formvar, carbon, or other material,
evaporated under vacuum. In general, evaporated films give the best re-
suits.
In the scanning electron microscope, there is a reflection geometry
between the beam incident on the specimen and the image-forming beam,
so the electrons do not have to pass through the material, and this simpli-
fies specimen preparation.
Dried materials are needed for replication and for direct viewing on the
electron microscope because the specimen has to be placed in the high
vacuum system where water molecules would evaporate and collide with
the electrons and cause a loss of resolution. Air drying may be inadequate
because many soils shrink markedly, and fabric relations may be changed;
it is also possible that the morphology of thin clay minerals may be af-
fected. Drying shrinkage results from an increase in surface free energy of
the material and a rise in the capillary potential or soil moisture suction;
moisture migration is a common accompaniment. Sometimes, water is
replaced before optical thin sections are made, and this is also sometimes
done in connection with studies involving the electron microscope.
The method by which the surface of the soil or rock is exposed requires
consideration when a replica is to be prepared or when the specimen is to
be viewed on the scanning electron microscope. In the latter case, even
though the reflection geometry makes possible the examination of thick
materials, the information is derived from only a very thin layer because
of the low penetrating power of the electron beam. Indeed this fact may
sometimes be used to an advantage. If the accelerating potential is reduced,
the depth of penetration of the electron beam is reduced also, so the
GILLO'I-I" ON SPECIMEN PREPARATION IN MICROSCOPY 291
image-forming electrons originate near the surface. When there are thin,
platy, or elongate particles projecting into voids or above the surface of
the specimen, the image formed at low kilovoltage reveals greater surface
detail. At higher kilovoltage, electrons which form the image may originate
from both surfaces of platy minerals if the primary beam passes through
the thin particle (Fig. la and b).
Most soils deform more readily than rocks at low stress levels and dilate
when unloaded. Relief of pressure may be accompanied also by exsolution
of gas from pore liquids. Such changes may distort the fabric, and the
collection of specimens for fabric study should be carried out so as to
reduce these effects to a minimum. Even though special core samplers are
used, it is still probable that they sometimes cause fabric damage, particu-
larly near the edges. Bulk specimens are more satisfactory, but collection
is not always possible. The field orientation should be recorded, and the
specimen coated or packaged to prevent drying.
Microscopic Methods
The polarizing microscope is the standard version of the light (optical)
microscope used for examination of materials such as rocks and soils. By
about 1880, inherent limitations of glass lenses, which gave rise to chromatic
aberration, spherical aberration, coma, astigmatism, distortion, etc., had
been corrected almost completely, and, by 1931, when the electron micro-
scope was invented, the optical microscope was not very inferior to the
modem instrument. Today, as in 1931, performance of the light microscope
is limited by resolution, which prevents formation of images which show
detail in the range less than 0.2 ~an. Spacings which are smaller than
about one third the wavelength of the wave motion do not cause diffrac-
tion. Since diffraction is involved in image formation, it follows that
detail less than about 2000 A may not be observed, even theoretically,
when light optics are used, since the wavelength range of the visible spec-
trum is 4000 to 7600 A. Practical limitations commonly make for unsatis-
factory viewing of mineralogical materials in the micrometer size range.
In practice, little more than general orientation can be deduced from clay
soil sections of standard thickness (~30/am). Many other techniques, such
as phase contrast and ultraviolet microscopy, are now available but have
received scant attention in this field, and details of the morphology of
minerals in the clay size range and fabric relations in fine grained rocks
and clay soils are obtained generally by observations on transmission or
scanning electron microscopes.
When it was realized that electrons have the properties of waves as well
as particles, and electron diffraction was established, the production of
an electron microscope became a possibility. The wavelength of the elec-
tron beam is related to the accelerating potential, and, at 60 kV, it is about
University of British Columbia Library pursuant to License Agreement. No further reproductions author
FIG. 1--Scanning electron micrographs of rocks and soils.
0.05 ~,. As the resolution of a microscope is directly proportional to the

wavelength of the radiation used to form the image, it is evident that it
GILLOTI" ON SPECIMEN PREPARATION IN MICROSCOPY 293
should be possible to observe much f'mer detail with an electron microscope

than with a light microscope. The correctness of these ideas was demon-
strated with the first electron microscopes. Electron lenses suffer from
similar defects to glass lenses, but electron optics is a much younger sci-
ence than light optics, and electron lenses are not nearly so well corrected
as are glass lenses. Even so, detail as fine as about 1.5 A can be resolved
with transmission electron microscopy and lattice spacings of about 2 A
observed, mainly because of the very short wavelength of the electron
beam. The approximate resolving power of the unaided eye, optical, and
electron microscopes, in relation to the wavelength of the electromagnetic
spectrum and particle size range of fine sediments, is shown in Fig. 2.
At the present time, there are two major classes of electron micro-
scope--the transmission instrument and the scanning dectron microscope.
In the transmission microscope, the beam passes through the specimen or
a replica, whereas a reflection arrangement is employed in the scanning
microscope. It is also possible to employ reflection methods with the
transmission microscope. Recently, scanning transmission electron micro-
scopes, which combine the features of both instruments, have become
available commercially. High voltage microscopes, which may be operated
at a potential of the order of one million volts, are also available; among
other advantages, the greater penetrating power of the beam makes it
possible to examine thicker specimens.
The versatility of the electron microscope has been increased greatly by
a variety of analytical attachments. The facility to record general poly-
crystalline or selected area electron diffraction pattern was one of the first.
Mineralogical and structural analysis is thus possible from areas as small
as 250 A with some transmission instruments. Attachments to the scanning
electron microscope now make possible elemental analysis by energy
dispersive and wavelength dispersive X-ray spectrometric techniques from
areas of 1/am or less. Light elements below about atomic number eight are
difficult to detect because of the low X-ray yield. These elements may be
picked up by Auger electron analysis [1]2 and by measurement of energy
loss of electrons transmitted through very thin specimens. Observation in
the cathodoluminescence mode and use of auxiliary devices, such as the
hot-cold stage, deformation stage, etc., give additional information
(Fig. 3).
Specimen Preparation for Fabric Analysis

Fabric refers to the orientation and arrangement of particles--individ-
ual crystals or more or less cemented agglomerations of crystalline and
noncrystalline material--and voids. The word microstructure is sometimes
The italic numbers in brackets refer to the list of references appended to this paper.
VISIBLE
)'-RAYS X-RAYS ULTRAVIOLET INFRARED MICROWAVES RADIO
/ELECTROMAGNETIC
I I I I I I ------ L, SPECTRUM
I0-10 I0-8 I0- 6 I0" 4 I0-2 I WAVELENGTH
(METRES)
(1~) (I/J.m)
[_ ELECTRON I " OPTICAL i~ UNAIDED ~ ( LIMIT OF
MICROSCOPE MICROSCOPE EYE L RESOLUTION
S~)IL CLASSIFICATION
CLAY SILT SAND GRAVEL
--- I 1 I M. I . T .
2/J.m 60Fro 2 rnm
CLAYS AND SILTS SANDS GRAVELS

A.S.T.M.
75p.m 4.75 mm
( 5 0 % OR MORE PASSES
No. 2 0 0 SIEVE )
FIG. 2--Resolving power relative to soil particle size range and wavelength of electro-
magnetic spectrum.
ELECTRON BEAM
SECONDARY ELECTRON BACK- SCATTERED

IMAGE ELECTRON IMAGE
LUMINESCENCE ~
ENERGY
DISPERSIVE
TENSILE/COMPRESSIVE IS/SHE, c IME N'/ A HOT/COLD

r
LWAVE - LENGTH
STAGE DISPERSIVE
9 ~r r t t ~ , ' ," J STAGE
SCANNING T P,ANSMISSION
FIG. 3--1maging and accessory techniques in scanning electron microscopy.
used similarly, but, in soil engineering, this term also implies consider-
ation of the bond between the particles and their interactions in the soil-
water system, as well as fabric relations. Optical and electron microscopes
have been the instruments used most commonly in fabric investigations,
though X-ray diffraction and radiography have been employed also. In
some studies, more than one technique has been used to analyze the fabric
of similar specimens [2 ]. Fabric has also been analyzed by measurement
of sound propagation [3 ], thermal conductivity [4], and dielectric proper-
ties [5 ]. In these cases, the anisotropic or isotropic nature of the specimen,
with respect to the physical property measured, reveals indirectly the
presence or absence of preferred orientation among the mineral particles.
Specimen preparation techniques differ, depending on the method of
fabric analysis, but moisture removal or replacement from poorly lithified
materials and exposure of the surface for examination present problems
common to most microscopic methods of fabric study.
GILLOTT ON SPECIMEN PREPARATION IN MICROSCOPY 295
Drying
Air Drying--Spedmens may be air dried if shrinkage on drying is not
regarded as detrimental to the fabric information to be obtained. It is evi-
dent that drying shrinkage will effect the greatest changes in fabric when
the specimen is weak and the environment in which it is found is not sub-
ject to wetting and drying cycles. For example, air-dried sensitive soils
often show a relatively dense fabric when compared with the more open
fabric of the same area when the specimen is frozen on a cold stage (Fig.
1c and d). Displacement of minerals is also readily apparent if. a com-
parison is made between these two photographs; this is not to imply that
the frozen soil is undisturbed, since freezing is accompanied by volume
change, which may well cause fabric disturbance.
Replacement of the water (surface tension 72.75 x 10- 3 N/m at 20~
by another more volatile liquid, such as ethyl alcohol (22.75 x 10 -3 N/m)
or acetone (23.70 x 10-3 N/m), should reduce drying shrinkage. As
with other replacement techniques, fabric damage due to fluid migration
is a possibility.
Freeze DryingmFreeze drying reduces shrinkage and distortion of the
specimen because ice is removed by sublimation. The surface energy of
the solid-vapor interface is commonly higher than that of the liquid-vapor
interface, but no meniscus forms in pores and capillary spaces. Since ice is
much less mobile than liquid water, fluid migration into finer pores is
largely prevented as moisture is removed. The method, however, has cer-
tain drawbacks.
When the specimen is frozen, the conversion of liquid water to ice one
in larger void spaces will be accompanied by an increase in specific vol-
ume of about 9 percent. So specimen dilation at the outset may induce
fabric change.
Moisture movements within the specimen, on freezing, have been at-
tributed to at least three causes. First, the unfrozen solutions will become
more concentrated, and differences in concentration may arise because ice
already formed will be composed of fresh water. So moisture will migrate
to reestablish equilibrium in solution concentration and also to feed grow-
ing ice crystals. Vapor pressure gradients are thought to be another cause
of moisture movements. Water held close to surfaces remains unfrozen
because its freezing point is depressed. As it is metastable, however, its
vapor pressure is high, relative to that of ice elsewhere in the system. So
desorption takes place, and the water migrates towards the ice in response
to the gradient [6, 7].
Fabric changes have also been attributed to the tendency of crystals to
expel impurities to grain boundaries [8] and to grain growth of ice crystals
during freezing [9, 10]. Small crystals are probably less damaging in these
regards, so the use of ice nucleators, such as amino acids [11], and clathrate
hydrate formers, such as chloroform and ether [12], should be considered.
Theoretical considerations show that the possibilities of fabric damage

on freeze drying are reduced if ice #ass, rather than crystalline ice, is
formed. For example, there is no tendency for material to be concentrated
at ice grain boundaries, since they do not exist in glass, and the volume
increase on solidification of the water is reduced. Glass formation is
favored by rapid cooling, by high viscosity near the freezing point, and by
depression of the freezing point. Direct immersion in liquid nitrogen (N2)
( - 196~ appears to cause rapid freezing, but the rate of cooling is less
than required because of the formation of an insulating envelope of gas
surrounding the specimen. This pitfall can be avoided if the specimen is
immersed in propane, isopentane, or Freon 22, supercooled in liquid N2.
These compounds have a low freezing point, so they are liquids at very
low temperatures. In addition, they have a relatively high boiling point,
so they are not vaporized as readily by heat from the specimen as is N2;
therefore, cooling is more efficient. That cooling rate and drying proce-
dure can affect fabric is underlined by the remarkable differences in ap-
pearance of flocculated Wyoming bentonite when air dried and when
freeze dried, following freezing by direct immersion in liquid N2 and by
immersion in supercooled Freon 22 (Fig. 4a, b, and c).
An increase in viscosity to favor ice glass formation has been used
experimentally by biologists. They have introduced glycerol, dimethyl
sulfoxide, ammonium acetate, polyvinyl pyrrolidone, and sucrose into
tissue fluids with some success. The tendency to moisture migration, due
to vapor pressure gradients, should be reduced also because of the smaller
difference in vapor pressure between the liquid and solid phases. The
vapor pressure of the solution is reduced by the low vapor pressure solutes,
while that of the solid is raised, since ice glass has a higher vapor pressure
than crystalline ice.
Even when ice glass is formed successfully in the specimen, there is a
considerable possibility that it will devitrify and recrystallize during
sublimation. It has been reported that this occurs at about - 130~ [13],
which is close to the recrystallization temperature--a temperature of
about half of the melting point, in degrees Kelvin, at which many materials
recrystallize. However, the rate of sublimination is extremely slow, owing
to the low vapor pressure of ice below this temperature. Replacement of
water by a liquid such as amyl acetate, which solidifies in the vitreous
state more readily than water, and which has a relatively high vapor pres-
sure below the freezing point, may be advantageous. The possibility of
fabric damage, due to flow of fluids during water replacement, is again a
consideration. Another partial solution is to freeze-etch the specimen. A
surface layer of ice is sublimated at a very low temperature (~,, - 1 0 0 ~
by passing a metal surface at an even lower temperature (~ - 196~ the
temperature of liquid N2) close to the specimen. The temperature gradient
leads to rapid sublimation of the ice from the surface layer of the specimen.
GILLO'I-I" ON SPECIMEN PREPARATION IN MICROSCOPY 297
FIG. 4--Scanning electron and optical micrographs showing effects of specimen pre-
treatment.
Thus the surface, which is replicated for examination on the transmission

electron microscope or examined directly on the scanning electron micro-
scope, is dried under very favorable conditions. The bulk of the ice from the
remainder of the specimen is removed generally by sublimation at a higher
temperature.
If a hot-cold stage is available, the specimen may be examined on the
scanning electron microscope in the frozen state. Reasonably good micro-
graphs may be taken up to about x 2000 magnification without the need
to metallize the specimen. Frost sometimes forms on the surface and ob-
scures detail. It may be removed by sublimation in the microscope if the
temperature is raised slightly for a short time.
Critical Point Drying--Critical point drying involves raising the temper-

ature and pressure of the liquid phase to values above those of the critical
point at which the physical properties of a liquid and its vapor become
the same. At this point, the interface vanishes, so surface tension forces
cease to exist. The critical point of water is at a temperature of 374~
and at a pressure of 2.25 • 107 N/m 2, so the specimen has to be placed
in a strong container to withstand the pressure. The critical point occurs
at lower values of temperature and pressure for other fluids. In the case
of liquid carbon dioxide, it is at 31 ~ and 73.97 x 105 N/m s, and for
ethyl alcohol, it is at 243~ and 65.26 x lff N / m s. Various authors
have used the method, either evaporating the water itself or replacing
this by another liquid and removing the new fluid subsequently, under
supercritical conditions [14-17].
Supercritical water is known to be chemically reactive, but water
replacement involves the same problems associated with fluid flow, as
discussed previously. Exsolution of gas from pore fluids, osmotic effects,
and pressure buildup, due to inadequate permeability of the specimen
during fluid expansion, are other possible causes of fabric damage. Sur-
face interactions between pore fluids and soil minerals will cause the
critical point to deviate from that of the bulk liquid, so drying by this
method should be carried out at temperatures and pressures above those
of the published values for the critical point for the water or replacement
liquid.
Surface Exposure
Surface exposure requires care in the preparation of specimens for
either scanning electron microscopy or transmission electron microscopy.
Cutting should not be used generally, since it is a shearing action which
may orient platy or elongate minerals, though it may be possible to
reduce or overcome this problem by impregnation. Specimens which are
to be freeze dried are generally fractured when frozen, the technique

being termed freeze fracturing. Air dried soils and specimens dried by
the critical point method are fractured generally after drying. Air dried
soil is often hard and brittle, but critical point dried material may be very
fragile, and loose particles are liable to fall on the surface and obscure
the true fabric. Some particles of this sort can be removed by a jet of
compressed clean air or gas. If the specimen is sufficiently strong, it
may be peeled with adhesive tape [18].
A plane of failure may be predetermined to some extent by notching
the specimen, but the fracture will propagate along a surface of weakness,
so it may not be completely representative. Conversely, careful study of
fracture surfaces [19] can give information regarding crystal orientation,
defects and the distribution of impurities, particularly when these are
concentrated at grain boundaries. Electron fractography has given useful
information in the study of metals and other materials.
Preparation of Optical Thin Sections

When the optical microscope is used to study fabric, thin sections of
soils are made by a modification of the method employed routinely for
making thin sections of rocks. The water in the soil is either removed or
replaced before the thin section is made. If the water is removed, it is
common practice to support the specimen by impregnation with a suitable
resin before sectioning. Often, the water is replaced by Carbowax 6000
[20]. This replacement is often accompanied by volumetric change, the
amount of which depends on the void ratio, but which is nonetheless
much smaller than that caused by air drying of a water-containing speci-
men [21]. Carbowax crystallizes on slow cooling, and the spherulites may
sometimes be seen superimposed on the original fabric of the soil. Rate
of cooling affects the size of the spherulites markedly (Fig. 4d, e and ./)
and ultrarapid cooling in Freon 22 surrounded by liquid N2 largely over-
comes the problem of spherulite formation in soil specimens [22]. Since
Carbowax 6000 is water-soluble, the thin section is made by dry grinding
or by grinding in an organic liquid such as kerosene.
Specimen Preparation for Analysis of Particle Size and Shape

Individual clay mineral particles may be examined on the electron
microscope. On the transmission instrument, agglomerations show few
distinguishing features because the electron beam fails to pass through the
specimen. Also, overheating is more probable, due to absorption of the
electron beam and accompanying interactions in the specimen. Phase
changes, fusion, and evaporation or sublimation of the specimen, and
destruction of the support film may result. On the other hand, when
clay minerals are too thin ( •50 A), contrast becomes inadequate for the
clear observation of detail; shadow casting generally solves this problem.
Disaggregation is carried out in water by hand grinding, by use of a
homogenizer, ultrasonic vibrator, or other methods. The simplest pro-
cedure is to allow a drop of the suspension to evaporate on the specimen
grid, which has been previously coated with a support film. This tech-
nique often gives unsatisfactory results because the particles agglomerate
during drying, though this tendency can be reduced by use of a dispersing
agent. As with bulk clays, droplets containing suspended clay may be
freeze dried or dried by the critical point method. The droplet is usually
placed on a support grid, prior to freezing and drying. Association of
smectites freeze dried from droplet suspension has been described [9,23],
and marked differences in fabric underline heavily the importance of
specimen preparation (Fig. 4a, b, and c).
Various methods of spray drying have been employed also. An atomi-
zer or nebulizer is used to produce a mist of clay particles in water
droplets, which are collected on the support grid. The suspension placed
in the nebulizer may contain a dispersing agent, or the solution may be
designed to gel during drying to prevent reaggregation of the clay
minerals [24]. Other modifications have included use of an electrostatic
precipitator [25] and paper extraction thimble [26] to improve the ef-
ficiency with which the clay is recovered. The mist may be dried by
passing it down an electrically heated tube.
Another technique is to disaggregate the specimen in amyl acetate and
make a smear between two glass slides. When dry, this may be shadowed
and backed by collodion or evaporated carbon before being floated off
on distilled water, scooped up, and placed on the specimen grid. Electro-
deposition [27] and replica techniques for study of dispersions have been
employed also. Particle shape and size distribution information can, of
course, be obtained from bulk specimens, and this method has some
advantages, since disaggregation is sometimes accompanied by breakup of
particles, so that shape and size distribution are affected.
Ion Bombardment
Etch techniques have increased the information obtained by micro-
scopic examination of rocks, metals, and other materials, but have been
little used in the study of soils because, until recently, there were no dry
techniques available. It has been known for over a hundred years that ion
bombardment of solid surfaces is accompanied by physical and chemical
interactions (Fig. 5). The ejection of atoms from the solid is termed
sputtering and is thought to result from a transfer of momentum, due
to a series of collisions between the incoming ion and the atoms of the
target. Recently, the effect has been used as a means of etching. The
ION BOMBARDMENT
NEUTRAL ATOMS r t RADIATION
REFLECTEDNNEU~I ~f~ ECONDARY ELECTRONS
(~ //1~~
ION IMPLANTS - - ~ t ~ S p ECi M EN " ~ HEAT
,
ARTIFACTS
I
ETCH PATTERN
,
SPUTTERCOATING
DUETO LOW YIELD DUE TO GRAINBOUNDARIES, METAL DEPOSITED
COMPONENTS,CONTAMINATION,COMPOSITIONDIFFERENCES, FROM NUMEROUS
DEFECTS, ETC. CRYSTALORIENTATION-SELECTIVE DIRECTIONSAND
EROSIONOF DENSEATOMICPLANES IMPLANTED
FIG. 5--Results and uses of ion bombardment.
rate at which the surface is eroded depends upon the nature of the solid,
the crystal orientation, and structure, and on the energy, angle of inci-
dence, and nature of the incident ions. Various methods have been used
to neutralize the positive charge which builds up on the surface of in-
sulators. These have included an electron beam [28], a Langmuir probe
[29], and imposition of a high frequency field [30]. Much recent work
has been stimulated by interest in ion pumping, surface reactions, the
nature of interatomic forces, ion implantation of semiconductors, and
film preparation in microelectronic circuitry. There are extensive reviews
of the principles [31-34].
Ceramics, fibers, biological materials, and metals have been sputter
etched, and thin foils for observation on the transmission electron
microscope have been prepared by this technique. Limitations arise
because of differences in the rate at which the surface is eroded, so
that artifacts results. Conical shapes are often produced, due to the
presence of variable yield components and to effects of original topog-
raphy which determine the local angle of incidence of the ion beam and
so influence rate of sputtering. Such problems are reduced by rotation of
the specimen.
The effects of topography may also be reduced by polishing rocks
before they are etched. In some limestones, grain boundaries between
dolomite (rhombic crystals ~30 /am) and matrix (calcite as irregular
crystals r~2 to 10 gin and clay) were etched selectively, and circular pits
were visible in the polished surface after bombardment with argon ions
in a r-f field. As a method of revealing fabric detail, the overall result
of ion etching has, so far, been somewhat disappointing in comparison

with acid etching. Nonetheless, in some areas the disturbed polished
layer was removed, and the structure of the f'me matrix was revealed.
The detail made visible by ion etching a polished limestone may be com-
pared with that seen in the same polished limestone after acid etching
(Fig 1 e and f ) . Contrary to present experience, other workers have
reported that, in some metals, hillocks form at grain boundaries and also
in other areas where atoms are relatively protected from collision chains,
as at the point of emergence of dislocations extending perpendicularly
below the sputtered surface.
Equipment for ion etching is available as an attachment to the scanning
electron microscope, so that the effects of sputtering can be observed on
a before and after basis. The metal coating is, however, removed by the
ion beam, so a loss of resolution is common in the observation of non-
conductors. Other commercial equipment is available, which operates as
an independent unit.
Replication, Shadowing, and Coating

A replica is a thin film, relatively transparent to electrons, which
reproduces the surface features of the specimen reasonably faithfully.
Replicas are made because the electron beam has a very low penetrating
power which depends upon the accelerating potential and the atomic
number of the atoms in the specimen. At 50 to 100 kV, the beam will
generally only pass through specimens which are between 1000 and 2000
A in thickness. Thus, replicas provide a relatively simple alternative to
ultrathin sectioning of bulk specimens and, in the study of disaggregated
material, avoid many problems caused by agglomeration of particles.
The best replicas are made by vacuum evaporation. Carbon commonly
is deposited to a thickness of about 100 A, from a direction normal to
the surface (Fig. 6). The carbon replica may be backed by polystyrene,
and the clay specimen removed in water and by dissolution with hydro-
fluoric acid. The polystyrene is dissolved in ethylene dichloride, the
replica washed by being floated on several dishes of distilled water, and
mounted on the specimen support grid.
Replicas may also be made of plastics, formvar, or collodion applied
as a liquid or plastic. This procedure is generally not well suited to clays,
as the liquid flows into pore spaces, and true surface features become
hard to recognize. Also, plastic often has to be pressed against the
surface to obtain the required intimacy of contact for good replication,
and pressure is obviously undesirable for weak or friable specimens.
Replicas made by vacuum evaporation are more suitable. Both one and
two stage replicas are used, and positive or negative impressions of the
surface may be made.
APPARATUS
CHAMBEREVACUATEII"~ ~ECTRIC ARC
Ii' L INDICATOR
HEAVY META "~'~"~ dl
SHADOWING- [ ~ " ~ ~ CARBONREPLICA
"~SAMPLE
|
| I I
REPLICATION WITH
I I I (~) EVAPORATED CARBON
(~) REPLICATION WITH POST-SHADOWING) ~. l !
EVAPORATED CARBON WITH H E A V Y / ~ ~. ~ ,~
PRE-SRADOWING/; ,~ METAL / ~ ~ ~ r CARBON
W,TH HEAVY J'~ ~ -~. ~ REPLICA
METAL J ~/ ~ ~~ ~~ ' ~ ~ CARBON
REPLICA
FIG. 6--Shadow casting and replication for examination on transmission electron

microscope.
Contrast in the electron image results largely from differences in

scattering power of different parts of the specimen or replica. This may
result from surface roughness in the object, which causes different parts
of the surface to present orientations to the beam, which range from
normal to near parallel; hence, the thickness which the electrons must
traverse varies. However shadowing at 20 to 45 deg by a heavy metal
such as platinum or gold/palladium of either the specimen or replica is
a more reliable method of ensuring that contrast is adequate (Fig. 6). The
metal is deposited generally to a thickness of about 10 A. In addition,
the height or shape of surface features may be derived if the shadowing
angle is known and shadow lengths are measured. Details of the pro-
cedures for shadow casting and replication have been published [35-37].
In the scanning electron microscope, nonconductors such as rocks and
clay soils rapidly acquire a charge which causes a serious loss of resolu-
tion. Charge buildup is prevented by the deposition of a conductive
layer on the specimen surface. Metal coating is carried out commonly
in a vacuum chamber by evaporation of a suitable metal from an elec-
trically-heated filament (Fig. 7).
Sputtering may be used also (Fig. 5). This method often gives a
superior coating to that obtained by the more conventional thermal
evaporation technique. Problems due to charging are reduced greatly,
and this advantage is particularly noticeable when the specimens are
porous or have an irregular topography, as is the case in fabric studies
of many clay soils. The better coating results in part, probably, from
APPARATUS
~ ~ PLANETARY ROTATION
OF SAMPLES
EVACUATED CHAMBER
EVAPORATED METAL
COATING
STEPS HIGHER THAN COATING THICKNESS AND RE-ENTRANT ANGLES

TEND TO BREAK CONTINUITY ANO IMPAIR EFFICIENCY OF CONDUCTIVE
LAYER
BREAK IN COATING EVAPORATED METAL

COATING
ED
ATING
FIG. 7--Metalizing specimens for examination on scanning electron microscope.
the higher energies with which the sputtered atoms reach the specimen,
where they form a better bond to the surface being coated. Another
factor is thought to arise from the relatively poor vacuum in the system.
This leads to collisions between the gas and metal atoms being deposited,
which consequently arrive at the specimen from numerous angles so
surfaces not directly in line of sight with the source receive a metal
coating.
Discussion
It is now accepted widely that constituents in the micrometre and sub-
micrometre size range and crystal imperfections play an important and
often decisive role in the engineering behavior of soils and rocks. The
detail accessible to microscopic observation has been extended almost
to the angstrom range. Attachments available to existing microscopes
have made them almost as much a miniature laboratory as an instrument
for observing fine detail. There is every indication that this trend will
continue. If the information is to be meaningful, the specimen must be
representative, and specimen preparation must introduce as few artifacts
as possible.
The scanning electron microscope makes it possible to resolve detail
well beyond that accessible to observation by means of the optical micro-
scope; its introduction has also simplified specimen preparation for robust
specimens. The preparation of fragile soils and sediments is, however,
still relatively complex, though the problems are well understood. All
present techniques have limitations, but procedures most likely to give
satisfactory results are established.
It is best to examine specimens for fabric analysis on both the optical
and electron microscopes. The optical instrument often gives an overview
of general fabric relations, and the presence of such features as preferred
orientation are generally more easy to detect than on the electron micro-
scope. Relative disposition of minerals, contact relations, authigenic
crystal growth, morphology of minerals, and surface texture of sediment
grains are observed best on the electron microscope.
The preparation of optical thin sections is a well established technique
and is normally no problem, unless weak soils or sediments are to be
sectioned. Moisture removal or replacement and impregnation are then
required. Specimens for observation on the electron microscope have to
be dried. In fabric studies of soils not thought to have dried in nature,
this is accomplished best by the critical point method or by freeze drying;
freeze etching is desirable. It is probable that ice~glass forms only very
close to the surface of soils, even when cooling is ultrarapid. A fracture
most probably passes through parts of a frozen specimen where there is
crystalline ice; so, it is improbable that the surface exposed by freeze
fracture ever contained ice glass. For this reason, a procedure such as ion
beam etching should make it possible to improve specimen preparation
technique. Observation on the scanning electron microscope of the corner
of a rectangular specimen discloses fabric relations on three orthogonal
surfaces. Ice glass could be formed close to the three surfaces of such a
specimen and dried by freeze etching. A specimen of soil is readily cut
to this shape, but the surfaces would not be representative because of
the disturbance of the minerals caused by the shearing action of cutting.
If the disturbed layer can be removed by ion bombardment or other etch
technique and without production of new artifacts, three representative
surfaces of a specimen, which has been dried under very favorable
conditions, could be viewed.
When the higher resolution of the transmission electron microscope
is required, replica techniques offer a more convenient procedure than
ultrathin sectioning (Fig. 8). Specimen preparation for analysis of particle
shape or size, or single crystal electron diffraction, may be carried out
by one of the numerous techniques of dispersion (Fig. 9).
Conclusions
The preparation of robust specimens for microscopic examination
presents few problems generally and may be carried out by routine pro-
SAMPLE
FREEZE / FRACTURE/DRY REPLACE WATER

OR
CRITICAL po INT DRy / F RACTURE~,,,,,,,,,,,~ (CARBOWAX6000)
I IMPREGNATE~ I
SECTION
r I I
I
METAL COAT
I ] OPT,CAL
MICROSCOPE
SEM REPLICA IMPREGNATE
I
TEM
'
ULTRA THIN SECTION
I
TEM
FIG. 8--Specimen treatment prior to microscopic examination of soil fabric.
SAMPLE
I
DISPERSE
I
DRY
I
OPTICAL
J i
METALIZE
I
MICROSCOPE I I I
SEM REPLICA TEM
I
TEM
SEM" SCANNING ELECTRON MICROSCOPE
TEM: TRANSMISSION ELECTRON MICROSCOPE
FIG. 9--Specimen treatment prior to microscopic examination of particle shape and

size of soil minerals.
cedures. When the specimen may be distorted by drying shrinkage, more

elaborate techniques of specimen preparation are required. While the
problems are fairly well identified, present methods provide only a partial
solution. Technical developments in the next few years may lead to
improvements. Significant improvements in microscopic methods are to
be expected from new and more versatile auxiliary stages.
Acknowledgments
I wish to express my sincere thanks for technical assistance to Howard

Johnson, Lorna Moffat, Peter Gifford, and Bob Fitch. Financial support
from the National Research Council of Canada and the Defence Research
Board of Canada is acknowledged.
References
[1] MacDonald, N. C., Marcus, H. L., and Palmburg, P. W., Proceedings, O. Johari,
Ed., 3rd Annual Scanning Electron Microscopy Symposium, liT Research Institute,
Chicago, Ill., 1970, p. 25.
[2] Gillott, J. E., Journal o f Engineering Geology, Vol. 4, No. 2, April 1970, pp. 133-153.
[3] Kaarsberg, E. A., Journal of Geology, Vol. 67, No. 4, 1959, pp. 447-472.
[4] Penner, E. in International Clay Conference, Vol. 1, I. T. Rosenquist and P. Graft-
Peterson, Eds., Pergamon, London, 1963, pp. 365-376.
[5] Winkelmolen, A. M., American Association Petroleum Geol~,ists Bulletin, Vol. 56,
No. 11, 1972, pp. 2150-2159.
[6] Weiser, C. J., Science, Vol. 169, 1970, pp. 1269-1278.
[7] Litvan, G. G., Cryobiology, Vol. 9, 1972, pp. 182-191.
[8] Lincoln, J. and Tettenhorst, R., Clays and Clay Minerals, Vol. 19, 1971, pp. 103-107.
[9] Hoffman, U., Scharrer, E., Czerch, W., Friihauf, K., and Burck, W., Berichte der
Deutscher Keramischen Gesellschaft, Vol. 39, 1962, pp. 125-130.
[10] Borst, R. L., Journal o f Petroleum Technology, Oct. 1971, pp. 1193-1201.
[11] Garten, V. A. and Head, R. B., Nature, Vol. 205, No. 4967, 1965, pp. 160-162.
[12] Tracey, M. V., Proceedings, Royal Society, Vol. 171, 1968, pp. 59-65.
[13] Meryman, H. T. and Kafig, E., "The Study of Frozen Specimens, Ice Crystals and
Ice Crystal Growth by Electron Microscopy," Research Report NM 000 018.01.09,
Naval Medical Research Institute, Bethesda, Md., 1955, pp. 529-544.
[14] Anderson, T. F., Proceedings, 2nd International Conference on Electron Microscopy,
1950, pp. 567-576.
[15] Horridge, G. A. and Tamm, S. L., Science, Vol. 163, 1969, pp. 817-818.
[16] Gillott, J. E., Journal of Sedimentary Petrology, Vol. 39, No. 1, 1969, pp. 90-105.
[17] Gillott, J. E., Clay in Engineering Geology, Elsevier, New York, 1968, pp. 296.
[18] Sides, G. and Barden, L., Canadian Geotechnical Journal, Vol. 8, 1971, pp. 392-399.
[19] Zapffe, C. A., Worden, C. O., and Zapffe, C., American Mineralogist, Vol. 36, 1951,
pp. 202-232.
[20] Mitchell, J. K., Proceedings, Highway Research Board, Vol. 35, 1956, pp. 693-713.
[21] Quigley, R. M. and Thompson, C. D., Canadian Geotechnical Journal, Vol. III, 1966,
pp. 61-73.
[22] Gillott, J. E., Clays and Clay Minerals, Vol. 22, 1974, pp. 199-200.
[23] Bates, T. F., "Selected Electron Micrographs of Clays," Circular No. 51, College of
Mineral Industries, Pennsylvania State University, University Park, Pa.
[24] Schofield, F., British Journal o f Applied Physics, Vol. 2, 1951, pp. 18-19.
[25] Jonas, E. C. and Kuykendall, J. R., Clay Minerals, Vol. 6, 1966, pp. 232-235.
[26] Hughes, R. and Bohor, B., American Mineralogist, Vol. 55, Sept.-Oct. 1970, pp. 1780-
1786.
[27] Mering, J., Oberlin, A., and Villiere, J., Bulletin Societie Francaise Mineralogie et
Cristallographie, Vol. 79, 1956, pp. 515-522.
[28] Akishin, A. I., Vasil'ev, S. S., and Isaev, L. N., Bulletin o f the Academy of Sciences
o f the U.S.S.R., Physical Series, Vol. 26, 1963, p. 1379.
[29] Jorgenson, G. V. and Wehner, G. K., Journal of Applied Physics, Vol. 36, 1965,
p. 2672.
[30] Anderson, G. S., Mayer, W. N., and Wehner, G. K., Journal of Applied Physics,
Vol. 33, 1962, p. 2991.
[31] Tsong, I. S. T. and Barber, D. J., Journal o f Materials Science, Vol. 8, 1973, pp. 123-
135.
[32] Holland, L. and Priestland, C. R. D., Vacuum, Vol. 22, No. 4, 1972, pp. 133-141.
[33] Carter, G. and Colligon, J. S. in Ion Bombardment o f Solids, Heinemann, London,
1968, p. 446.
[34] Davidse, P. D., Vacuum, Vol. 17, No. 3, 1966, pp. 139-145.
[35] Comer, J. J. and Turley, J. W., Journal o f Applied Physics, Vol. 26, 1955, pp. 346-
350.
[36] Techniques for Electron Microscopy, Kay, D., Ed., BlackweU, Oxford, 1965.
[37] The Electron-Optical Investigation of Clays, Mineralogical Society, Gard, J. A., Ed.,
London, 1971.
A . L Johnson' a n d R. P. M o s t o n 2
Use of Ultrasonic Energy for

Disaggregation of Soil Samples
REFERENCE: Johnson, A. I. and Moston, R. P., "Use of Ultrasonic Energy for

Disaggregation of Soil Samples," Soil Specimen Preparation for Laboratory Testing,
ASTM STP 599, American Society for Testing and Materials, 1976, pp. 308-319.
ABSTRACT: A method for faster and more nearly complete dispersion of soil
samples for particle size analysis now appears feasible. Using agitation by ultra-
sonic energy, disaggregation and dispersion appeared to be as thorough in 10 min
as by mechanical preparation through a sieve with 0.0625-mm openings. The ultra-
sonic agitation appeared to cause no deleterious effect, on the primary particle
sizes. The time and effort required to obtain high quality dispersion is much less
for ultrasonic than for mechanical techniques, especially for heavy soils.
KEY WORDS: particle size, nondestructive tests, soil properties, ultrasonics, soils,
tests
A s o n e p h a s e o f r e s e a r c h o n l a n d subsidence in C a l i f o r n i a , a p p r o x i -
m a t e l y 500 u n d i s t u r b e d s a m p l e s were t a k e n f r o m d e p t h s as great as 2000
ft in t h e S a n J o a q u i n a n d S a n t a C l a r a Valley [1-3]. 3 T h e p a r t i c l e size
d i s t r i b u t i o n f o r these s a m p l e s was a n a l y z e d in the G e o l o g i c a l S u r v e y ' s
H y d r o l o g i c L a b o r a t o r y in D e n v e r , C o l o r a d o [4]. Because t h e m e c h a n i c a l
d i s a g g r e g a t i o n o f these s a m p l e s was t i m e c o n s u m i n g , u l t r a s o n i c e n e r g y
w a s s t u d i e d to f i n d a faster a n d s i m p l e r m e t h o d f o r t h e d i s a g g r e g a t i o n
a n d s u b s e q u e n t d i s p e r s i o n o f t h e f i n e - t e x t u r e d samples. This p a p e r ,
b r i e f l y describing s o m e results o f this s t u d y , shows t h a t ultrasonic e n e r g y
p r o v i d e s a m u c h faster a n d m o r e c o m p l e t e d i s a g g r e g a t i o n a n d d i s p e r s i o n
o f the f i n e - t e x t u r e d soils.
Ultrasonic Equipment
In t h e f o l l o w i n g discussion o f u l t r a s o n i c energy o r s o u n d , sonic s o u n d

1Assistant chief, Office of Water Data Coordination, U.S. Geological Survey, National
Center, Reston, Va. 22092
2District materials engineer, Colorado Division of Highways, Grand Junction, Colo.
308
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JOHNSON AND MOSTON ON USE OF ULTRASONIC ENERGY 309
(range of sounds audible to the human ear) is considered to be greater

than 18 to 20 kHz. All sound waves above the audible range are con-
sidered ultrasonic. The use of ultrasonic energy for the testing and pro-
cessing of a wide variety of materials has invaded virtually every phase
of science and industry [5,6]. One wide-spread use has been the ultra-
sonic cleaning of parts. Ultrasonic cleaning equipment was adapted to soil
dispersion during this study.
Energy required for ultrasonic cleaning is produced when mechanical
vibrations in the cleaning liquid, induced by the high-intensity sound
waves, cause "cavitation." Cavitation, or cold boiling, is established in
liquids when the amplitude of an applied sound pressure is sufficient
to cause continuous rupture of the entrapped air bubbles. Rod [7] states
that the forces developed in the immediate locale of such collapsing
bubbles are on the order of several hundred atraospheres of pressure,
even though only a small fraction of this high pressure is required to initi-
ate the process. If such cavitation is developed and aggregations of
solids--such as clay particles, for examplemare immersed in the liquid,
the individual solids (clay particles) are separated by the large forces
associated with the cavitation.
Because cavitation is induced in liquids under the action of a sufficiently
intense sound source, the effectiveness is dependent upon the applied
power. However, the cavitation does not increase linearly with applied
power because of a scattering effect. Thus, there is a point beyond which
an increase in power is no longer economical. For example, more than
ten times the power needed at 10 kHz is required to cavitate water at 400
kHz. The number of ultrasonic transducers and the power used for any
particular ultrasonic cleaning application will be determined, at least in
part, by the operating frequency proposed for use in the equipment.
Because cavitation is less effective as the frequency of sound rises, low
frequencies are generally superior for cleaning purposes. However, slight
changes in frequency (20 to 40 kHz, for example) have little effect, and
frequencies of 40 kHz or more are usually used because of the human
discomfort caused by sound of less frequency.
Two main types of acoustic transducers are used to transform electric-
driving energy into sound energy--the magnostrictive and the piezoelectric
types. The magnostrictive-type transducer, in simple form, is nothing
more than a bar magnet, usually in the form of a stack of thin sheets of
nickel or a nickel alloy, which has a large change in dimensions per unit
change in applied current. If the bar is wound with a few turns of wire
and electric current is allowed to flow through this wire, the bar is
magnetized and becomes shorter, and, when the current ceases to flow,
the bar becomes longer again. Thus, if the current through the coil is
varied at the resonant frequency of the bar, it can be made to oscillate
regularly, and cavitation is developed at the liquid-transducer interface.
For well-designed magnostrictive-type transducers operating at about 30

kHz, approximately 70 percent o f the electrical driving force results in
effective sound energy, and the remainder is lost as heat.
With piezoelectric-type transducers, the oscillations required to create
cavitation are obtained by impressing opposite and alternating electric
charges (positive and negative) on the top and b o t t o m faces o f slabs of
crystalline materials such as quartz, barium titanate, and certain ferro-
ceramics. H e n r y [5] states that, as often as several million times per
second, the slab becomes thicker when the upper face is made positive
and the lower face negative and becomes thinner when the charges are
reversed. Behaving much as a piston, the upper face o f the crystal is
driven at its resonant frequency and transmits its vibrations to the liquid
in the cleaning chamber. Those piezoelectric materials which deliver the
greatest acoustic output per unit of input voltage are generally the least
stable electrically and mechanically; quartz is probably the most stable.
Because o f lower internal losses, piezoelectric-type transducers (although
more fragile) are probably more suitable than magnostrictive-type trans-
ducers for applications requiring frequencies above 100 kHz.
Ultrasonic cleaning equipment, such as m a y be used for soil dispersion,
consists of two main units: (1) an electronic signal generator, and (2) a
fluid container with one or more attached acoustic transducers. A sec-
ondary fluid container, such as a beaker o f glass or metal, is used inside
the primary fluid container to hold the soil or rock sample. Water is
used in both the primary and secondary liquid container to provide the
most efficient medium for transmission o f the ultrasonic energy. The
ultrasonic cleaning apparatus used in the present investigation is described
in Table I. This equipment was generously loaned to the study by m a n u -
facttlrers and by other offices o f the Geological Survey.
TABLE 1--Test data for ultrasonic equipment.
Signal Generator Transducers

Power Operating Power
Equipment Output, Temperatures, Input, Frequency,
Designation W ~ W Type kHz
A 125 to 500 125 125 to 500 barium titanate 38
B 35 to 140 unknown 20 to 80 barium titanate 90
C 60 to 240 83 60 to 240 barium titanate 40
D 50 to 200 130 to 150 50 to 200 magnostrictive 20
E 40 to 120 110 40 to 120 piezoelectric 40
ceramic
F 50 to 200 150 50 to 200 barium titanate 40
Testing Methods
The accuracy of any particle size analysis is dependent primarily on
the effectiveness of the disaggregation and dispersion methods used to
separate the soil sample into its fundamental particles. However, this
analysis must be done without deleterious effects to the soil particles, such
as the fracturing of any of the fundamental particles. The present study
was initiated to determine the speed and effectiveness of disaggregation
and dispersion of soil samples in water by the use of ultrasonic energy.
With the standard procedure (ASTM Particle Size Analysis of Soils
(D 422-72)) for determining particle size distribution, a soil sample is
disaggregated and dispersed by: (1) mechanical manipulation, (2) agitation
by shaking or stirring, and (3) chemical deflocculation. The mechanical
manipulation is normally done by a mortar and rubber-covered pestle--
taking as long as several hours to work a sample of suitable size down
through a sieve with 0.0625-mm openings. For the study reported in this
paper, the mechanical manipulation was followed with dispersion of the
sample by at least 8 h soaking in distilled water and 8 h agitation by
shaking in a reciprocating shaker. A chemical deflocculating agent,
sodium hexametaphosphate, was added prior to shaking to assist in
separation of the individual particles.
To evaluate characteristics of different ultrasonic equipment, a number
of 50-g samples of soil, passing through a sieve with 2-mm openings,
were obtained by splitting a large soil sample. Each 50-g sample was
placed in a 500-ml beaker containing 190 ml of water and 10 ml of
sodium hexametaphosphate and was stirred with a stirring rod. The
beaker was placed immediately in the liquid container of the ultrasonic
cleaning equipment being tested and was subjected to ultrasonic agitation
for a period of 10 to 30 min. Following the ultrasonic agitation, the
particle size distribution of the soil was determined by the standard
methods for sieve analysis and hydrometer analysis. Sample splits were
tested in a number of different ultrasonic cleaners ranging in frequency
and power, as shown in Table I.
To compare the results of the ultrasonic method of disaggregation and
dispersion with those of the more orthodox methods, particle size analyses
were made also on the same soils but prepared by the conventional
procedure of mechanical disaggregation and chemical deflocculation.
Some sample splits were also analyzed without use of deflocculent. The
mechanical disaggregation with the mortar and pestle was varied some-
what by preparing one sample split to pass through a sieve with 2.0-mm
openings (No. 10), a second sample split to pass through a sieve with
0.420-mm openings (No. 40), and a third sample split to pass through a
sieve with 0.0625-mm openings (No. 230). These sample splits were
analyzed by the ASTM standard sieve and hydrometer procedures,
mentioned previously, to obtain their particle size distribution. Duplicate

sample splits were also treated to ultrasonic agitation and analyzed
similarly (Table 2). The results of some of these analyses are shown in
Figs. 1, 2, and 3, for one of the samples tested.
P A R T I C L E * S I Z E DIAMETER IN ~,AILLIMETERS
CLAY S I Z E S SILT SIZES SAND S I Z E S

V. line Fbne ~%d bum Coarse V.Co~rse
''" 79.2 20.0 0.6 0.2

83.5 16.3 0.2
F I G . l--Graph showing distribution of particles after mechanical and ultrasonic disag-

gregation o f clay samples passing No. 10 sieve.
Summary
The disaggregation of the silt- and clay-size particles appeared to be
essentially complete after only 10 rain of ultrasonic agitation, even though
the samples had been prepared only down to 2-mm size. Microscopic
examination of the soil suspensions demonstrated that many of the ag-
gregations of smaller particles (Fig. 4) resulting from purely mechanical
TABLE 2--Results of various mechanical and ultrasonic disaggregation on samples

of four different textures.
Sonic
Disaggregation Silt Content, Clay Content," Velocity,
Treatment ~ ~ kHz
Bonny Loess
P10, mechanical 70.6 13.6 ...
P40, mechanical 73.8 12.2 ...
P230, mechanical 74.8 12.0
P10, ultrasonic, 5 min 74.1 10.1 56"
P10, ultrasonic, 10 min 72.9 12.3 56
PI0, ultrasonic, 20 rain 69.7 16.5 56
PI 0, ultrasonic, 30 min 68.0 17.6 58
PI0, ultrasonic, 15 min 71.8 13.8 55
P40, ultrasonic, 15 min 70.2 14.2 54
P230, ultrasonic, 15 min 69.4 16.4 54
Clay
P10, mechanical 20.0 79.2 ...
P40, mechanical 20.2 79.2 ...
P10, ultrasonic, 5 min 18.1 81.5 '60"
P10, ultrasonic, 10 min 16.3 83.5 6O
P10, ultrasonic, 30 min 18.3 81.5 60
P10, ultrasonic, 15 min 18.1 81.5 60
P40, ultrasonic, 15 min 16.3 83.5 60
P230, ultrasonic, 15 min 16.5 83.5 60
Sandy Silt
PIG mechanical 38.9 14.0 ...
P40 mechanical 41.0 14.6 ...
P230 mechanical 40.5 14.0
PI0 ultrasonic, 5 rain 41.9 12.0 60
P10 ultrasonic, 10 rain 41.0 14.0 58
P10 ultrasonic, 15 rain 41.4 14.0 60
P I 0 ultrasonic, 20 rain 40.5 14.0 60
P10 ultrasonic, 30 min 41.3 14.3 60
P10. ultrasonic, 15 rain 41.4 14.0 60
P40, ultrasonic, 15 min 41.0 14.6 62
P230, ultrasonic, 15 min 41.6 13.8 62
Very Fine Sand
PI0, mechanical 17.8 3.2
P10, ultrasonic, 5 min 16.8 3.2 56
P230, ultrasonic, 15 rain 18.4 3.2 58
I00 I|
20 ~ Ln ~--~_
I '16 m
II
5 mln |
1
// ii
7C
b / ,
ta 60
n~
~ 5r,
~, 3G
I0
I
u
o o. o
P A R T I C L E - S I Z E D I A M E T E R IN M I L L I M E T E R S
CLAY SIZES SILT SIZES SAND S I Z E S
< ~0~4 ~m 0.004 - 0.0~,25 ~ .0625-.125 .125-~25 .25-.5 .S-I I-2

81.5 18.i 0.2 0.2
-- 83.5 16.3 0.2
___ 83.0 16.8
F I G . 2--Graph showing effect of ultrasonic agitation of various periods of clay samples

passing No. 10 sieve.
disaggregation, were separated (Fig. 5) when treated with sodium hexa-

metophosphate. Comparison of Figs. 5 and 6 shows that disaggregation
by ultrasonic action for only a short period of time provides disaggrega-
tion equivalent to that received from a much longer mechanical prepara-
tion. Microscopic examination of the soil suspensions also indicated that
good quality disaggregation was obtained by ultrasonic action, without
any apparent deleterious effect on the fundamental particles. There is,
however, some indication that ultrasonic vibration of distilled water will
cause the formation of nitric acid, thus lowering the pH of the soil
suspension [8]. A lowered pH could reduce the efficiency of the defloccu-
lation process. Continuing research on the ultrasonic method, therefore,
l-^
o r o o
c~ ~ c~ c5 c~ c~
PARTICLE-SIZE D I A M E T E R IN M I L L I M E T E R S
CLAY SIZES SILT SIZES SAND SIZES

V. line Fine Medlum Co0rse V.Coorse
• 0.004 mm 0.00~t - 0-0625 mm .0625..125 .125-_25 .25..5 .5-1 1.2
16.4 69.4 4.6 2.2 4,5 2.8 0.2

~r 14 o2 70.2 5.0 2.0 4.8 3.4 004
13.8 7l .8 5.2 2~0 4.4 2.4 004
FIG. 3--Graphs showing effects o f ultrasonic agitation o f 15 min on loess samples pre-
pared through various sieves.
should include more study to determine if this factor is critical within the
range of agitation time.
Disaggregation by purely mechanical means and chemical defloccula-
tion, even when the sample was prepared to pass a 0.0625-mm sieve, does
not appear to be any more complete for most type soils than that done
by ultrasonic energy. Analyses of samples prepared by this method pro-
vided as much as 20 percent fewer clay-size particles than did analyses
using samples disaggregated and dispersed by ultrasonic energy. A clay
sample prepared only to 2.0-ram size provided 4.3 percent fewer clay-size
particles than obtained by the ultrasonic method (Fig. 1). Figure 2 shows
that a clay sample provided maximum clay content after 10 min disag-
FIG. 4--Photomicrograph of clay samples following mechanical preparation, passing

No. 40 sieve, with no deflocculating agent (X880).
FIG. 5--Photomicrograph of clay sample following mechanical preparation, passing No.

40 sieve, treated with sodium hexametaphosphate and shaken 8 h ~880 ).
FIG. 6--Photomicrograph of clay sample following mechanical preparation, passing

No. 40 sieve, treated with hexametaphosphate, and ultrasonically agitated for 30 min (X880).
gregation by ultrasonic energy. A silt (loess) sample gave 2.6 percent

more clay-size partices, using ultrasonic treatment on material prepared
through the No. 230 (0.0625-mm) sieve, than when using material pre-
pared through the No. 10 (2.0-mm) sieve (Fig. 3). Although these may
not seem to be greatly significant differences, the important point is that
considerably less time and effort were spent preparing the sample by the
ultrasonic technique. The authors believe ultrasonic disaggregation has
considerable potential and further research on the method is recom-
mended.
References
[1] Poland, J. F. and Davis, G. H., Transaction, American Geophysical Union, Vol. 37,
No. 3, 1956, pp. 287-296.
[2] "Progress Report on Land Subsidence Investigations in the San Joaquin Valley,
California, Through 1957," Inter-Agency Committee on Land Subsidence in the San
Joaquin Valley, Sacramento, Calif., 1958.
[3] Poland, J. F. and Green, J. H., "Subsidence in the Santa Clara Valley, California--A
Progress Report," U.S. Geological Survey Water-Supply Paper 1619-C, 1962.
[4] Johnson, A. I., Moston, R. P., and Morris, D. A., "Physical and Hydrologic Properties
of Water-Bearing Deposits in Subsiding Areas in Central California," Professional
Paper 497-A, U.S. Geological Survey, 1968.
[5] Henry, G. E., Scientific American, Vol. 190, No. 9, 1954, pp. 54--63.
[6] Goldman, Richard, Ultrasonic Technology, Reinhold, New York, 1962.
[7] Rod, R. L.,Research and Engineering, Vol. 1, No. 2, Sept. 1955, pp. 18-23.
[8] Akiya, Schichiro and Okui, Seiichi, Journal, Pharmaceutical Society of Japan, Vol. 67,
1947, pp. 233-235.
P. V. Lade' and H. Nejadi-Babadai I
Soil Drying by Microwave Oven
REFERENCE: Lade, P. V. and Nejadi-Babadai, H., "Soil Drying by Microwave

Oven," Soil Specimen Preparation for Laboratory Testing, ASTM STP 599, Ameri-
can Society for Testing and Materials, 1976, pp. 320-340.
ABSTRACT: An investigation of the usefulness of the microwave oven for water

content determination and for drying of soil before testing was performed. Soils
ranging from highly plastic clays to clean sand were used. The influences of initial
water content, amount of soil, and soil type on the drying time were investigated.
Differences between water content determined using a microwave oven and a
conventional oven decreased with decreasing plasticity of the soils. The micro-
wave oven can be used for quick drying of soil, but accurate determinations of
water content may only be achieved for nonplastic soils such as coarse silts, sands,
and gravels. The change in classification according to the Atterberg limits was
taken as a measure of the effects of heating by microwaves. The plasticity and
swelling potential of the soils decreased after preheating in the microwave oven, and
these effects are comparable to the effects of drying the soils in a conventional oven
at high temperatures.
KEY WORDS: Atterberg limits, clays, tests, moisture, soil mechanics, temperature,
soils, plastic properties
The microwave oven presents definite potential advantages over the

conventional oven when used for soil drying. Substantial time savings and
low purchase price render the microwave oven very attractive for use in
water content determination and for drying of soil before testing. How-
ever, due to the nature of the action of the microwaves and the sensitivity
of clay minerals to drying temperature, the amount of water driven off
in the microwave oven may not correspond to that evaporated in a con-
ventional oven at a given temperature. Due to the complex heating
process by microwaves, only practical experience can demonstrate the
effects of microwave heating. Therefore, a systematic investigation of the
usefulness of the microwave oven for soil drying and water content deter-
mination and the possible effect of microwave heating on the soil
behavior was performed.
~Assistant professor of engineering and applied science and former graduate student,
respectively, University of California, Los Angeles, Calif. 90024
320
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Copyright 9 1976 byby ASTM International www.astm.org
LADE AND NEJADI-BABADAI ON MICROWAVE OVEN DRYING 321
Heating with Microwaves
Process oYHeating with Microwaves

In the process of heating with microwaves, electric field energy is con-
verted into heat through frictional action between molecules of the
material in the electric field [1].2 This process is best understood from
consideration of the action of dipole molecules in an electric field. Some
molecules such as water molecules, are natural dipoles, that is, the centers
of the positive and the negative charges do not coincide but are separated
by a small distance. In the absence of an electric field, the dipole mole-
cules in a material are in thermal equilibrium, that is, they oscillate about
their position of rest as a result of thermal agitation. However, if an
external electric field is imposed, the dipole molecules will rotate to align
themselves in the direction of the field. Due to frictional resistance of
the material, the molecules will be impeded in their rotation, and a finite
time is required for their alignment. Thus, the response of a dipole
molecule in an electric field is of a viscous nature.
If the direction of the electric field is alternated at sufficiently high
frequency, the energy lost, due to molecular friction in the material,
becomes significant. Thus, energy is converted to heat through the fric-
tional action at high frequencies of the alternating electric field. The
energy converted into heat increases in proportion to the frequency, f,
and the square of the electric field strength, E
Pheat = C X f X E2 (1)
where C is a constant which depends on the dielectric constant of the

material.
The penetration depth of the electromagnetic waves decreases greatly
with increasing frequency [1]. Limits are therefore set to the heat treat-
ment with microwaves because of the diminished penetration depth
experienced at the high frequencies which are most favorable for effective
heating. Thus, it can happen that the waves do not reach the nucleus of
large volumes of material. However, due to heat transfer from the surface
to the interior of the material, heating with microwaves will still have an
effect at distances greater than the microwave penetration depth. Further
limitations to the effectiveness of microwave heating are posed by the
reflection of a portion of the waves at the surface of the material
and by damping of the waves on penetration into the material [2].
The dielectric constant of a soil, upon which the constant C in Eq 1
depends, decreases with increasing frequency, a phenomenon referred to
as dielectric dispersion [3]. The dielectric constant also decreases with
2The italic n u m b e r s in brackets refer to the list o f references appended to this paper.
decreasing water content; and the type o f clay, the clay content, and the
temperature also affect the dielectric dispersion. Due to the influence of
various factors on the dielectric constant, the effectiveness of heating with
microwaves can only be explored through practical experience.
It should be noted that only materials which are able to absorb the
microwaves, as explained previously, can be heated by the microwaves.
Metal objects reflect the microwaves, and materials such as glass, paper,
and some plastic objects let the microwaves pass through them without
affecting the molecules of which they are formed.
Microwave Oven
The microwave oven used for this investigation was purchased for
approximately $180 (March 1974). It had a rated power requirement of
0.97 k W and, like most microwave ovens, was set to operate at a fre-
quency o f 2450 M H z .
Effects of Heating Clay Mineral Systems

Because the temperatures generated within soil specimens in a micro-
wave oven are difficult to control, an appreciation of the potential value
o f a microwave oven for drying soil must include considerations of the
possible harmful effects which uncontrolled temperatures m a y have on
the soil.
The effects of heating on the physico-chemical behavior o f clay mineral
systems have been studied to great extent, and various techniques and
measures of the changes in this behavior have been employed. The altera-
tion o f the engineering properties of clays and clayey soils, when heated,
has often been expressed in terms of the changes in the values of the
liquid, plastic, and shrinkage limits.
Grim [4] writes that
when clays are heated to increasingly high temperatures, they first lose
their pore water and then their adsorbed water. As the adsorbed water is
lost, the flat plane surfaces tend to come together. Apparently the com-
plete collapse of the particles makes it extremely difficult for water to
again penetrate to me adsorbing surfaces. As a consequence, heating
clays to temperatures of the order of 100 to 300~ tends to substantially
reduce their plastic character when they are again mixed with water.
When the clay minerals are heated to temperatures of the order of 500 ~C
and above, they lose their hydroxyl water with a consequent change in
the crystalline structure, and, as a further consequence, the shape of the
particles and the character of the surface change. The result is likely to
be development of a substantially nonplastic material.
Grim [4] summarizes further: ' ' I n the case of the expanding clay minerals,
temperatures in the order of 100 to 300~ cause the loss of the ability to
swell again. The loss of swelling potential is related to the complete loss
of interlayer water."
The loss of water from clays, which occurs with increasing drying
temperature, may be quite substantial and results in apparent increasing
water content [5]. As the clays are heated at increasingly high tempera-
tures, water is lost in irregular amounts and dehydration curves, typical
for each type of clay, are obtained [4].
It has often been reported that heating prior to determination of the
plasticity of a soil results in lower values of the liquid limit and the
plastic limit [5-10]. The results of tests performed by Radhakrishnan et
al [10] on black cotton soils showed that these soils became nonplastic,
and the clay-size fraction was reduced in the 500 to 700~ range. At even
higher temperatures, the soils became friable and sandy, and consistency
limit tests could not be performed.
The effect of partial or complete dehydration on the subsequent swell-
ing of clay soils, when mixed with water, has also been studied to some
extent [4,10--12]. It has been found that the shrinkage limit values
generally increase with increasing preheating temperature, thus indicating
decreases in the ability of the soils to swell.
Drying by Micro waves

An investigation of the use of a microwave oven for quick determina-
tion of the water content of soils was performed by Ryley [13]. On the
basis of the tests performed for this investigation, it was concluded that
the microwave drying method results i n water content analyses accurate
to within 0.4 percent for most soils. The specimens dried within 10 to 15
min, but it was concluded that the drying method is unsuitable for soils
containing gypsum or materials with high carbon content.
Preliminary Investigations
Preliminary investigations concerning the choice of soil container and
the uniformity of the microwave radiation within the oven were per-
formed prior to any testing of soils.
Since microwaves are unable to penetrate metal objects such as alu-
minum soil drying cans used in the conventional oven, a number of con-
tainer types were tested in the microwave oven in order to select a suitable
soil container. The criteria used for selecting a suitable soil container
were that it (1) does not impede the microwaves noticeably, (2) does not
burn or deform, and (3) does not experience any loss in weight. Experi-
ments were devised to test the ability of various types of containers to
meet these three criteria [14]. As a result of this investigation, glass
beakers were selected as the most suitable containers to be used for soil
drying in the microwave oven.
Although microwave ovens are designed to produce uniform radiation,
an investigation of the distribution of the microwave radiation was per-
formed. Glass beakers were filled with 100 ml o f cold water and, in turn,
placed at nine different points in the oven, and the time to reach boiling
o f the water was noted for each point. The microwave radiation was
found to be only slightly nonuniform. During all subsequent testing, the
glass beaker with soil to be heated was placed in the center of the oven.
Determination of Water Content
Soils Tested
Soil types ranging from highly plastic clays to clean sand were used in
the investigation o f the applicability of the microwave oven to soil drying
and water content determinations. Some o f the characteristics o f all the
soils tested are given in Table 1. Liquid limits, plastic limits, and shrink-
age limits were determined according to the standard procedures [15,16].
A conventional forced draft oven, which was set at 105 ~ was used for
this purpose. A comprehensive range o f plasticity was covered, and all
soils tested were inorganic.
Due to the already well-documented sensitivity of clay minerals to dry-
ing temperature [4-12], the main effort was concentrated on the clay
types. Seven o f the clays were obtained in form of air-dry powder. The
two marine clays were obtained in the form o f wet specimens.
Factors Influencing Drying Time in a Microwave Oven

Due to the sensitivity of clay minerals to drying temperature, the water
content of a soil has been defined as that corresponding to drying the
soil at 105~ (or 110 _+ 5~ according to the ASTM Test for Laboratory
Determination of Moisture Content of Soil (D 2216-71)) until no further
weight loss occurs. Unfortunately, the temperature to which the soil is
heated in the microwave oven is difficult to measure, but the heating
process can be continued until a final constant weight is obtained. There-
fore, only experiments will show whether the water content determined
using the microwave oven corresponds to those determined using a con-
ventional oven.
The following factors emerge as being important in considerations
regarding the usefulness of the microwave oven for water content deter-
minations:
1. Influence of initial water content on drying time.
2. Influence o f amount of soil on drying time.
r-
o
m
z
o
z
m
t._
TABLE 1 - - - C h a r a c t e r i s t i c s o f soils tested. ~"
Black NBC-1 NBC-23 Antelope ~,

Hills Dixie Bond Marine Marine Haley Grundite Valley Ottawa ~
Characteristic Bentonite Bentonite Clay Clay Clay Clay H-Soil M-Soil L-Soil Silty Sand Sand Sand "'0
Liquid limit 514 98 147 151 57 55 48 30 24 . . . . . . . . . O

Plastic limit 45 44 41 48 27 24 24 20 23 . . . . . . . . . Z
Plasticity index 469 54 106 103 30 31 24 10 1 . . . . . . . . .
Shrinkage limit 9.2 a 12.7a . . . . . . . . . 11.7 12.7 16.5 20.2 . . . . . . . . .
Gravel, % (>2 mm) . . . . . . . . . . . . . . . . . . . . . . . . . . . 9 25
Sand, 070 (0.06 to 2.0 ram) 5 3 8 76 73 i~ 20
. . . . . . . . . . . . . . . . . . O
Silt, ~ (0.002 to 0.06 mm) . . . . . 40-28 40-28 .., 48 51 76 80 13 2 ...
Clay, ~ (<2 ~m) 1(~ tO0 60-72 60-72 100 52 44 21 12 2 . . . . . . ~.
<
aThese values are believed to be slightly too high. m
O
<
Fn
Z
0
.<
CO
O'l
3. Influence of soil type on drying time.

4. Comparison of water content determined using microwave oven and
conventional oven at 105 ~
The effects of each of these factors have been investigated, and the results
are presented in the following paragraphs.
Effects of Initial Water Content and Soil Type

Clays--Batches of clay powder were thoroughly mixed with water to
produce wet soil with uniform but different water content. A specimen of
100 g of wet soil was placed in the microwave oven and dried. The glass
beaker with the specimen was periodically taken out of the oven, covered
with a lid, weighed, and put into the oven for further drying. This pro-
cedure was continued until no loss in weight was registered between two
consecutive weighings. The water content was calculated after each weigh-
ing, assuming that the soil weight at that time was the correct dry weight.
The change in apparent water content with drying time is shown in Fig.
1 for one of the seven clays and clayey silts tested. Data for the other
soils were similar. The soil specimens were found to dry relatively slowly
in the beginning, and the highest rate of drying occurred after 2 to 5 min
of exposure to microwave radiation. It has been found that soil which is
wet on the surface reflects the microwaves better and therefore absorbs
less energy than dry soil [2]. Thus, the heating process is relatively slow
until the surface of the initially wet soil specimen has been dried out to
some extent. The soil specimens with the higher water content dried
slower initially than those with the lower water content, which is in accord
with the findings regarding microwave reflection from wet surfaces [2].
All soil specimens, which weighed 100 g, initially dried to constant
weight in about 20 min. However, the soils with high plasticity and high
initial water content tended to require slightly longer time for complete
drying than the soils having low plasticity and low initial water content.
Control specimens were dried for 24 h in a conventional oven, at
105 ~ All control specimens were taken from the same batches of soil
as the specimens dried in the microwave oven. The water contents deter-
mined from the specimens dried at 105 ~ are also shown on Fig. 1 for
Haley clay. It may be seen that the microwave heating, in all cases,
resulted in removal of slightly more water from the soil than that evap-
orated by conventional heating at 105 ~
For Haley clay, the difference in water content varied from 1.3 to 2.4
percent, depending on the initial water content. Table 2 shows the water
contents from the microwave oven and the conventional oven, and the
differences between these water contents for different types of soil. It
may be seen that the differences in water contents increase with decreas-
ing initial water content for all the clays and clayey silts tested. This may
200 I I I I I I I q
MICROWAVE OVEN: 148.6 %

160 CONVENTIONAL OVEN: 147.3%qi ~ V
121.2 o-~
~
120
I'-
Z
bJ
t,'- ~ A
86., a 5 A
oZ,._) 80 zx-"--- - ' 65.3 %
609% 1
hi
o - o " -~ ~ o
4O
0 I I I I I I I
0 5 I0 15 20 25 50 55 40
DRYING TIME (rain)
FIG. l--Drying curves for lO0-g specimens of Haley clay with different initial water
contents.
be explained as follows: For the same amount of wet soil, the amount of
solid material increases with decreasing water content. Assuming that the
amount of absorbed and hydroxyl water increases with the amount of
solid material, the water available for removal by microwave heating (but
not for removal by conventional heating at 105 ~ increases with decreas-
ing water content. Therefore, the difference between water contents
determined from the two different heating processes increases with
decreasing water content.
The data presented in Table 2 indicate that drying of clayey soils in
the microwave oven corresponds to drying in a conventional oven at
temperatures higher than 105 ~ Increasing the drying temperature results
in removal of adsorbed water and some hydroxyl water. Highly plastic
clays can adsorb more water to the surfaces of the particles than low
plastic silts. The difference in water contents, as determined by micro-
wave oven and conventional oven, is therefore greater for the highly
plastic bentonites than for the low plastic L-soil.
Sands--The results of tests on Antelope Valley sand, with negligible

amount of particles smaller than 2/~m and on silty sand with 2 percent
clay (< 2/~m) are also shown in Table 2. It may be seen that the differ-
ences between the water contents determined by the microwave oven and
by the conventional oven were only 0.5 and 0.2 percent, respectively.
Thus, very little additional water was removed by the microwave heating,
and this little water was most likely associated with the clay minerals
TABLE 2--Comparison o f water contents for lO0-g specimens with different initial
water contents dried in the microwave oven and the conventional oven.
Difference
Water Content Water Content Between
Determined Using Determined Using Water Contents,
Type of Soil Microwave Oven, % Conventional Oven, % %
926.1 906.5 19.6

Black Hills bentonite 692.7 660.8 31.9
659.0 603.0 56.0
138.4 127.3 11.1
Dixie Bond bentonite 130.3 116.6 13.7
84.1 70.1 14.0
148.6 147.3 1.3
121.2 119.8 1.4
Haley clay 88.3 86.1 2.2
63.3 60.9 2.4
97.8 96.3 1.5
61.5 59.8 1.7
Grundite clay 54.1 52.2 1.9
40.8 38.4 2.4
56.2 55.1 1.1
H-soil 50.4 49.0 1.4
41.6 40.1 1.5
43.0 42.7 0.3
M-soil 31.2 30.5 0.7
30.4 29.3 1.1
41.6 40.7 0.9
L-soil 33.5 32.4 1. I
27.9 26.5 1.4
Antelope Valley sand 11.6 11.1 0.5
Silty sand 15.3 15.1 0.2
Ottawa sand 8.0 8.0 0.0
present in the soils. Tests on clean Ottawa sand, consisting o f quartz

grains, resulted in exactly the same water content determined by the two
methods of heating, which also supports the hypothesis that only clay
minerals are sensitive to the drying process in the microwave oven.
Effects of Amount of Soil and Soil Type

Batches o f soil with uniform water content were prepared as follows.
Air-dry powder was mixed with water to produce a uniform lean mix,
with water content above the liquid limit. This liquid soil was then con-
solidated in a large double draining consolidometer to produce a cylinder
of soil with uniform water content. Specimens ranging in weight from 10
to 500 g were cut from the soil cylinder and dried in the microwave oven,
according to the procedure outlined previously. Control specimens were

dried for 24 h in the conventional oven at 105 ~ for comparison of water
contents.
Typical drying curves are shown in Fig. 2 for soil specimens of different
sizes. The same characteristic shape was observed in all cases, regardless
of the weight of soil. The larger specimens required longer drying times.
This increase in drying time with increasing amount of wet soil may be ex-
plained as follows: the initial microwave penetration is impeded because a
portion of the waves is reflected from the wet surface of the soil, and the
penetration depth of the microwaves is limited, as explained previously.
The loss in weight from equally wet specimens is therefore initially pro-
portional to the surface area of the specimens. For specimens with the
same shape, the ratio between volume and surface area is proportional to
the linear dimensions of the specimens. Therefore, the amount of water
being driven off, relative to the volume of the specimen, is smaller for a
large specimen than for a small specimen, and the initial slopes of the
drying curves consequently decrease with increasing amount of wet soil.
The time required for complete drying of the soil specimens in the
microwave oven increased with amount of wet soil. Complete drying of
the small specimens (10 g) was accomplished within 10 to 20 min. The
highly plastic clays with high initial water content tended to require longer
time for complete drying than less plastic soils with low water content.
The difference is drying time between the high and low plastic soils was
more pronounced for the large specimens (500 g), for which the drying
times ranged from about 20 min to 1 h.
The water contents obtained from the two different drying methods and
the differences in water content are listed in Table 3 for the seven types of
clay soil tested. The difference in water content for each type of soil is
seen to decrease with increasing amount of wet soil. This may be explained
by the limited penetration depth of the microwaves. Thus, for large
volumes of soil, the microwaves may not reach the interior of the speci-
men, and the drying of the soil in the middle is accomplished through
heat transfer from the surface. It was noticed that a specimen, which was
first dried in the microwave oven, then cooled down in the desiccator, and
again heated by microwaves, does not heat up to the same high tempera-
ture as the initially wet specimen. Therefore, after the outer shell of a
specimen had dried, the heat generation by microwaves and the heat
transfer to the interior of the specimen decreased. Some of the more
strongly held water molecules, which could not be reached by the micro-
waves, may therefore not have evaporated from the large specimens. The
difference between the two water contents therefore decreased with in-
creasing specimen size. However, this effect is somewhat obscured by a
tendency of the large specimens to crack, due to high vapor pressures
generated inside the specimens by the rapid heating process in the micro-
wave oven.
70 I t 1 I I , r f
oE/ g L
/
g
~ 3o
~ 20
0 I I I L I I
0 5 I0 15 20 25 30 35 40
DRYING TIME (mi n)
FIG. 2--Drying curves for specimens o f Haley clay showing influence of amount o f soil.
Effects of Microwave Heating on Soil Characteristics

Due to the nature of the microwave heating process, the temperature to
which the soil is heated in the microwave oven is difficult to measure.
However, the change in the soil classification according to the Atterberg
limits may be taken as a measure of the effects of heating by microwaves.
Liquid limit, plastic limit, and shrinkage limit tests were performed on
clays and clayey silts which, in powder form, first had been either (1)
dried in the microwave oven for 20 min, (2) dried in the conventional
oven at 105 ~ for 24 h, or (3) left in initial air-dry condition before test-
ing. All water content determinations, subsequent to these treatments,
were made using the conventional oven.
The results from the liquid limit and plastic limit tests are presented on
plasticity charts in Fig. 3 for soils of low plasticity and in Fig. 4 for highly
plastic clays. Liquid limits, plastic limits, and plasticity indices all de-
creased. Clay soils predried in the microwave oven gave the greatest
changes, and those predried in the conventional oven gave intermediate
changes, as compared to the values obtained from only air-dried soil. This
sequence is referred to hereafter as M-C-A. The most extreme reductions
in plasticity occurred for the highly plastic Black Hills bentonite, and the
smallest reductions occurred for the low plastic L-soil. The general trend
indicated on the plasticity charts is to change the soil classification in the
order M-C-A along the A-line towards the silt region. The same trend has
TABLE 3--Comparison o f water contents f o r specimens with the s a m e initial water

content and different wet weights dried in the m i c r o w a v e oven and the
conventional oven.
Water Content Water Content

Determined Determined
Using Micro- Using Con- Difference
Initial Amount wave Oven, ventional Oven, Between Water
Type of Soil of Wet Soil, g e/0 07o Contents, %
10 746.3 44.3
Black Hills bentonite 50 735.6 33.6
200 728.4 702.0 26.4
500 709.0 7.0
10 81.4 7.6
50 80.7 6.9
Dixie Bond bentonite 73.8
200 80.5 6.7
500 80.1 6.3
10 66.7 3.6
Haley clay 50 64.5 63.1 1.4
250 64.0 0.9
500 64.0 0.9
10 41.1 1.4
Grundite clay 50 40.2 39.7 0.5
200 40.0 0.3
500 40.0 0.3
10 35.4 1.7
H-soil 50 34.8 33.7 1.1
200 34.3 0.6
500 34.0 0.3
10 27.3 1.3
M-soil 50 26.9 26.0 0.9
250 26.5 0.5
500 26.4 0.4
10 27.7 1.2
L-soil 50 27.4 26.5 0.9
200 27.5 1.0
500 26.9 0.4
been observed for soils being heated conventionally to increasingly high

temperatures, [4, 6-10]. These observations indicate that drying of clayey
soils in a microwave oven corresponds to drying in a conventional oven at
temperatures higher than 105 ~ However, the temperature corresponding
to the microwave heating is most likely different for different types of clay
mineral. The loss of plasticity has been attributed to irreversible loss of
adsorbed water and to breakdown of the crystalline structure of the clay
minerals, due to loss of hydroxyl water [4] and fusion of the flat surfaces
of the clay mineral particles [10]. This produces larger soil particles, with
properties closer to those of silt.
[ i I I I I I
40 o AIR-DRY SOIL
z~ SOIL HEATED IN CONVENTIONAL OVEN
a SOIL HEATED IN MICROWAVE OVEN
x 30
la.i
t:3
>.-
20
o_ io M-
o t /~ L- SOIL I l I
0 I0 20 30 40 50 60 70
LIQUID L.IMIT
F I G . 3--Plasticity chart showing reduction in plasticity after heat treatment in con-
ventional oven and microwave oven f o r soils o f low plasticity.
6O i I I E [ I I I I I
t
sO0 I o AIR-DRY SOIL //o I
BLACKHILLS A SOIL HEATED IN CONVENTIONAL / , , ~
BENTON,TE /0 OVEN ///A-, I
4oo / /- [] SOIL HEATED IN M I C R O W A V E / / I
x I / / OVEN BOND
40-
zo | / / _ ~ GRUNDITE ///- BENTONITE I
~ 3o-
Boo
I0-
0 J ~ I I I I I
0 I0 20 30 40 50 60 70 80 90 I O0
LIQUID LIMIT
FIG. 4--Plasticity chart showing reduction in plasticity after heat treatment in con-
ventional oven and microwave oven f o r highly plastic clays.
The shrinkage limits were found to increase in the order A-C-M, thus
indicating a reduction in swelling potential of the soils having initially
been heated in the two ovens. Similar reductions in swelling potential have
been observed for soils which have been heated to high temperatures
[4, 10--121.
Liquid limit and plastic limit tests were performed on the two marine
days, designated NBC-1 and NBC-23. These soils were only available in
wet condition and were not predried. Half of each specimen tested was
dried in the microwave oven, and the other half was dried in the conven-
tional oven. The results of the Atterberg limit tests are listed in Table 4.
Both liquid limits and plastic limits were found to be higher for the speci-
mens dried in the microwave oven than those obtained from soil drying in
the conventional oven. These results are in agreement with the other data
described herein. Thus, it is concluded that, if the microwave oven is used
for soil drying, values of liquid and plastic limits will be determined to be
too high.
Summary and Conclusions

This paper presents the results of an investigation of the usefulness of
the microwave oven for water content determination and soil drying before
testing. Twelve different soils, ranging from highly plastic clays to clean
sand, were used in the investigation. All soils were inorganic, and the main
effort was concentrated on drying of different clay types.
The influences of initial water content, amount of soil, and soil type on
the drying time were investigated. Typically, the time for complete drying
varied from about 10 min for 10 g to about 45 min for 500 g of wet soil.
Highly plastic clays with high water content tended to require longer time,
whereas low plastic soils with low water content dried completely in shorter
time.
The water contents determined using the microwave oven were higher
for all soils containing clay minerals than those determined for the same
soils, using the conventional oven at 105~ The greatest difference in
these water contents was observed for small volumes of highly plastic
clays. The difference decreased with increasing volume, increasing initial
water content, and decreasing plasticity. Typically, the difference in water
content varied from 0.3 to 1.5 percent for low to medium plastic soils to
14 percent for very highly plastic clays. Negligible or no difference was
observed for silty sand and clean sand.
The change in soil classification, according to the Atterberg limits, was
taken as a measure of the effects of heating by microwaves. The liquid limit,
the plastic limit, and the plasticity index were found to decrease for all the
soils when they had been preheated in the microwave oven. The largest re-
ductions in these limits occurred for the highly plastic days, and the
TABLE 4--Liquid and plastic limits for marine clays determined using the
microwave oven and the conventional oven.
Determined Using Determined Using

Type of Soil Limit Microwave Oven Conventional Oven
NBC-I LL 165 147

PL 46 41
NBC-23 LL 173 151
PL 55 48
smallest reductions were observed for the low plastic soils. The shrinkage
limits tended to increase after preheating in the microwave oven, thus in-
dicating a reduction in swelling potential of the soils. The effects of pre-
heating a plastic soil in the microwave oven are comparable to the effects
of drying the soil in a conventional oven at high temperatures.
It may be concluded that the microwave oven can be used for quick
drying of soil, but the characteristics of plastic soils will change. Although
accurate determinations of water content may only be achieved for non-
plastic soils such as coarse silts, sands, and gravels, the error encountered
for plastic soils may be acceptable for many purposes. Thus, the micro-
wave oven may be useful for rapid determinations of approximate water
content of clay soils and for research purposes, when control specimens
show no difference in water content. However, it is not recommended to
use this oven on a routine basis until the magnitude of the possible error
has been established for the type of soil to be dried.
Acknowledgment
The writers express their appreciation to the National Science Founda-
tion which provided support for this study under Grant GK 37445. K. L.
Lee of the University of California at Los Angeles provided valuable ad-
vice for the preparation of the manuscript.
References
[1] Piischner, H., Heating with Microwaves, Centrex Publishing Co., Eindhoven, The
Netherlands, 1966.
[2] Waite, W. P., Cook, K. R., and Bryan, B. B., "Broad Spectrum Microwave Systems
for Remotely Measuring Soil Moisture Content," Publication No. 18, Water Resources
Research Center, University of Arkansas, Fayetteville, 1973.
[3] Arulanandan, K., Basu, R., and Scharlin, R. J., Highway Research Record, No. 426,
1973, pp. 23-32.
[4] Grim, R. E., Applied Clay Minerology, McGraw-Hill, New York, 1962.
[5] Lambe, T. W., "How Dry is a 'Dry' Soil?", Proceedings, Highway Research Board,
1949, pp. 491-496.
[6] Casagrande, A., Public Roads, Vol. 13, 1939, pp. 121-130.
[7] Chandrasekharan, E. C., Boominathan, S., Sadayan, E., and Narayanaswamy Setty,
K. R., Proceedings, International Conference on Effects of Temperature and Heat on
Engineering Behavior of Soils, Special Report 103, Highway Research Board, 1969,
pp. 161-172.
[8] Laguros, J. G., Proceedings, International Conference on Effects of Temperature and
Heat on Engineering Behavior of Soils, Special Report 103, Highway Research Board,
1969, pp. 186-193.
[9] Lambe, T. W., and Martin, R. T., Proceedings, Highway Research Board, Vol. 34,
1955, pp. 566-582.
[10] Radhakrishnan, N., Katti, R. K., and Hussain, M., Proceedings, Third Asian Regional
Conference on Soil Mechanics and Foundation Engineering, Vol. I, Haifa, 1967,
pp. 111-115.
[11] Aylmore, L. A. G., Quirk, J. P., and Sills, I. D., Proceedings, International Conference
on Effects of Temperature and Heat on Engineering Behavior of Soils, Special Report
103, Highway Research Board, 1969, pp. 31-38.
[12] Leonards, G. A., Foundation Engineering, McGraw-Hill, New York, 1962.
[13] Ryley, M. D., "The Use of a Microwave Oven for the Rapid Determination of Moisture
Content of Soils," Report LR 280, Road Research Laboratory, Berkshire, England,
1969.
[14] Lade, P. V., and Nejadi-Babadai, H., "Characteristics of Soil Drying by Microwave
Oven," Report No. UCLA-ENG-7476, School of Engineering and Applied Science,
University of California, Los Angeles, Oct. 1974.
[15] Lambe, T. W., Soil Testing for Engineers, Wiley, New York, 1951.
[16] "Laboratory Soils Testing," Engineer Manual EM 1110-2-1906, Office of the Chief of
Engineers, Department of the Army, Washington, D. C., 1970.
DISCUSSION
P. A . Gilbert ~ a n d M. M . A l - H u s s a i n i I (written d i s c u s s i o n ) - - T h e au-

t h o r s have p r e s e n t e d v a l u a b l e a n d interesting i n f o r m a t i o n o n soil d r y i n g
in a m i c r o w a v e oven. I n a r e c e n t study, 2 t h e W a t e r w a y s E x p e r i m e n t Sta-
tion (WES) conducted a number of water content determinations on vari-
o u s t y p e s o f soil, o f which t h e p e r t i n e n t characteristics a r e p r e s e n t e d in
T a b l e 5. B o t h c o n v e n t i o n a l a n d m i c r o w a v e ovens were u s e d in the test
p r o g r a m , a n d the results are p r e s e n t e d in T a b l e 6. T h e s t u d y shows t h a t ,
while m i c r o w a v e e n e r g y o f f e r s a r a p i d m e t h o d f o r d r y i n g soil, it s h o u l d
b e used with c a u t i o n since m i c r o w a v e e x p o s u r e t i m e g r e a t l y influences t h e
r e s u l t i n g water c o n t e n t . I n all tests c o n d u c t e d , the s t a n d a r d d e v i a t i o n in
water c o n t e n t , as o b t a i n e d b y the t w o m e t h o d s , was less t h a n 0.5 p e r c e n t .
T h e c o n s i s t e n c y a n d r e l i a b i l i t y o f the results d e p e n d o n a c c u r a t e k n o w -
~Civil engineer and research civil engineer, respectively, Soils and Pavements Laboratory,
U.S. Army Engineer Waterways Experiment Station, Vicksburg, Miss. 39180.
2Gilbert, P. A., "Feasibility Study--Microwave Oven Used for Rapid Determination of
Soil Water Contents," WES MP 3-478, U.S. Army Engineer Waterways Experiment Station,
Vicksburg, Miss. 39180.
TABLE 5--Description o f materials tested.
Atterberg Limits, %
Identification LL b pL c PI d Description
Long Lake clay (CH) 71 23 48 fat dark brown, alluvial soil com-
posed of silt and clay-size par-
tides of montmorillonite with
some quartz and illite; ex-
tremely sticky and plastic when
wet
Vicksburg buckshot
clay (CH) 56 22 34 similar to Long Lake clay
Vicksburg silty clay
(CH) 34 22 12 fine-grained loessial deposits.
Minus 2 fraction is about 9 per-
cent of total specimen and is
predominately montmorillonite
EABPL a gray clay
(CH) 79 26 53 inorganic gray clay from
Atchafalaya River Basin, La.
Aquagel(CH) 679 36 643 commercial bentonite drilling
mud, approximately 95 percent
montmor_illonite
Brazilian clay (CH) 96 38 58 dark red clay with mottles of
whitish clay, approximately 17
percent iron oxides, specific
gravity G, = 3.12
DeGray Dam fines
(GC) 37 14 23 clayey sandy gravel; only minus
No. 4 material tested
Reid Bedford
sand (SP) NP e NP NP fine, uniform quartz sand with
some feldspar from Mississippi
River near Vicksburz. Miss.
EABPL a peat (Pt) fibrous organic material from
Atchafalaya River Basin, La.
QEABPL = East Atchafalaya Basin Protection Levee.

bLL = liquid limit.
cpL = plastic limit.
dpI = plasticity index.
eNp = nonplastic.
TABLE 6--Summary o f water contents measured by conventional and microwave ovens and microwave
oven drying times for various soils.
I'-
Water Content, Percent O

m
Time in Wet Weight of
Conventional Microwave b Microwave Microwave Oven z
Material (actual) (predicted) Difference Oven, s c Specimen, g o
z
Long Lake clay 52.20 52.09 0.11 1240 574.69
Vicksburg buckshot clay 49.19 49.33 - 0.14 966 463.14
Vicksburg silty clay 17.13 17.09 0.04 1054 989.28
16.48 16.54 - 0.06 682 501.36
14.21 14.19 0.02 600 357.60 o
EABPL a gray clay 141.35 142.09 - 0.74 980 282.53
58.39 59.79 - 1.40 1247 653.95 O
Z
Aquagel 274.32 275.06 - 0.74 1302 349.88
373.04 374.16 - 1.12 1451 346.60
Brazilian clay 47.22 47.05 0.17 913 387.86
O
44.74 44.21 0.53 1225 599.00
DeGray Dam fines 10.60 10.55 0.05 795 709.28 <
m
Reid Bedford sand 5.13 5.08 0.05 620 471.20
O
5.54 5.53 0.01 754 733.50 <
m
EABPL a peat 220.25 ignited . .. 1551 470.53 z
ID
aEABPL = East Atchafalaya Basin Protection Levee. .-n
..<
bWater content determined from Eq 11 using conventional oven water contents and experimental water con -
tent-drying time data.

c Time required for water loss equivalent to water loss in conventional oven.
ledge o f exposure time. The exposure time required in the microwave

oven to produce water contents comparable to those obtained in a con-
ventional oven can be expressed as follows
4.2Mw[(0.2/w + 1)(100 - to) + 539]

T=
P
where
T = time in microwave oven, s,
Mw = mass o f water present in soil-water mixture, g,
w = water content of soil specimen,
to = initial temperature o f soil-water mixture, and
P = power output of oven, W.
This governing equation indicates that an estimate o f the specimen water
content is required. This is not a serious limitation since a duplicate speci-
men can be incrementally dried in the microwave oven to obtain a water
content estimate as input into the equation. The results o f the investiga-
tion indicate that microwave ovens are not suitable for drying soils with
high organic content or soils containing gypsum. In addition, microwave
energy must be used with care when drying soils with high metallic con-
tent, such as iron ore and bauxite. The WES study also pointed up the
difficulties involved in the simultaneous drying o f multiple specimens.
These difficulties were grave enough that this procedure is not recom-
mended. The use of metallic tare cans or plates should be avoided, as they
shield their contents from microwaves. Glass vessels should be used as
specimen containers since they are transparent to microwaves. The study
showed that drying time in a microwave oven is influenced by the amount
of water present in a soil-water mixture and is not significantly affected
by the amount, type, or plasticity of the soil. The WES study did not
show any evidence o f the effect o f wet surface on drying time; therefore,
it is doubtful that there is any significant reflection of microwave from
wet surfaces.
The authors have shown that the water content reached a constant
value after about 20 min of drying time. On the other hand, tests at WES
show that, while this is indeed the case for sand and silt (Fig. 5), it is not
true with clay (Fig. 6), for which water content continued to increase with
increasing drying time. The authors indicated correctly that, the larger the
volume o f specimen, the closer the value o f water content obtained by the
conventional and microwave ovens. For this reason, WES tests have been
conducted on specimens o f not less than 250 g, which should be the lower
limit for any successful water content determination in the microwave
oven. A difference in water content of 14 to 56 percent for certain plastic
soils, as indicated by the authors, is unusually high, which may indicate
that the soils may have been overheated by the microwave oven.
.50
~.o ....-.o
I-
Z 40
El
O
n"
El
n
30
Z
El
I-
Z
0 2.0 L EGEN D
O
nr"
I.i.I OB R A Z I L I A N CLAY
ix V I C K S B U R G B U C K S H O T C L A Y
I0
I1~, 9 C O N V E N T I O N A L OVEN
WATER C O N T E N T
0 200 400 600 800 1000 1200 1400 l iO0

T I M E IN OVEN;, S
FIG. 5 - - T i m e in microwave oven versus water content o f clay.
z 6
--o
4
z LEGEND
~
Z # OREIDBEDFORDS A N D
8 2 . [] REID BEDFORD S A N D
9 C O N V E N T I O N A L OVEN
WATER C O N T E N T
~ o
0 200 400 600 800 I DO0 1200 1400 1600
T I M E IN OVEN~ S
FIG. 6 - - T i m e in microwave oven versus water content o f sand.
It is vital that normal safety precautions be observed when using micro-

wave ovens, since microwaves are a form of radiation energy and should
be treated as such; also, microwaves affect heart pacers and other sustain-
ing devices at substantial distances.
P. V. Lade and H. Nejadi-Babadai (authors" closure)--The authors
appreciate the discussion and the additional information provided by Gil-
bert and AI-Hussaini. The authors agree that the exposure time required
in the microwave oven is critical for correct determination of water con-
tent of plastic soils due to the sensitivity of clay minerals to drying tern-
perature. Since the temperatures generated by the microwaves in the soil

specimen are difficult if not impossible to control, a fairly precise esti-
mate of microwave exposure time may substitute the condition used for
the conventional oven that drying should continue until no further weight
loss occurs. An estimate of exposure time is complicated by nonuniform
temperature distribution in the specimen and, therefore, by influence of
most of the factors mentioned in the paper. Gilbert and A1-Hussaini pre-
sent a formula for estimating the microwave exposure time on the basis of
the mass of water present in the soil water mixture, the initial water con-
tent, the initial temperature of the specimen, and the power output of the
oven. The microwave oven used for the present study had a power output
of 400 W. Whereas the trend indicated by this formula appears to be cor-
rect, the drying times calculated for the clays tested in the present study
are 30 to 40 percent too short, resulting in water contents which are too
small compared to those obtained from the conventional oven. However,
it is possible that only part of the power output is effective in heating the
soil specimen, and the formula for exposure time, therefore, may be
better than indicated by the calculations.
Microwave reflection from wet soil surfaces has been studied previously
([2] of the paper), and it is influenced by the complex dielectric constant
and, therefore, the water content of the wet soil. The microwave reflec-
tion was offered as an explanation for the shape of the initial parts of the
drying curves. However, the reflection may not have significant effects on
the time for complete drying, as pointed up by Gilbert and AI-Hussaini.
The ability of clays to adsorb water increases with increasing plasticity.
Since the clays in the present study were dried until no further weight loss
occurred, the adsorbed water and some of the hydroxyl water was re-
moved due to temperatures higher than 105 ~ generated by the micro-
waves. Thus, the clays were overheated in the microwave oven, as sug-
gested by Gilbert and AI-Hussaini, and this resulted in the rather high
differences in water content for the highly plastic clays.
The results of the studies performed at the U.S. Army Engineer Water-
ways Experiment Station and at the University of California at Los An-
geles serve to indicate the problems and the complexity involved in using a
microwave oven for water content determination.

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SOIL SPECIM EN

ASTM SPECIAL TECHNICAL PUBLICATION 599

List Price $35.00

Printed in Bahimore, Md.

Field Testing and Instrumentation of Rock, STP 554 (1974), $18.75,

Analytical Methods Developed for Application to Lunar Sample Analysis,

Effect of Water Saturation History on the Strength of

Four Factors Influencing Observed Rock Properties--

Trimming Device for Obtaining Direct Shear Specimens from

Effects of Specimen Type on the Residual Strength of Clays and

Effects of Storage and Extrusion on Sample Properties--

Temperature-Controlled Humid Storage Room--

Effect of Storage and Reconsolidation on the Properties of

Pore Water Extraction and the Effect of Sample Storage on the

Variation in Atterberg Limits of Soils Due to Hydration

Effect of Specimen Preparation Method on Grain Arrangement

A Technique for the Preparation of Specimens of Loose

Shrinkage of Soil Specimens During Preparation for

Compaction and Preparation of Soil Specimens for

Laboratory Preparation of Specimens for Simulating Field

Scalping and Replacement Effects on the Compaction

Study of Irregular Compaction Curves--P. Y. LEE 278

Importance of Specimen Preparation in Microscopy--

Use of Ultrasonic Energy for Disaggregation of Soil

Soil Drying by Microwave Oven--P. V. LADEAND

A laboratory test run on an inappropriate specimen is often worse

TABLE 1--ASTM standards and relevant papers.

This ASTM special technical publication contains a group o f sympo-

Effect of Water Saturation History

It is well known [1-5] 3 that the strength of rock depends, in large

through a regulator, on the saturation fluid contained in the vessel (A),

Cambrian Cemented Sandstone (Potsdam Group)

Ordovician Sublithographic Limestone (Trenton Group, Tdtreauville

Specimens f o r Tensile Splitting (diametral compression) Tests

TABLE l--Groups of specimens prepared by different methods

From saturated samples (S):

Specimensfor Triaxial Compression Tests

C opyri ght by ASTM Int ' l ( a l l r i g h t s r e s e r v e d ) ; W e d De c 2 2 1 4 : 0 0 : 0 0 E S T 2 0 1 0

Group AOC--The specimens in this group were as in group AOSC,

Triaxial Compression Tests

Check o f Pore Pressure Distribution in Triaxial Specimens

Effect o f Specimen Preparation History on the Results o f Tension

ksi ' MPo /

Test with opplied

t,~176 Specimen:Cemented sondstone~

FIG. 4--Results of triaxial compression tests with Potsdam sandstone.

the overconsolidation effect seems to affect much less the modulus of

Effect of Specimen Preparation History on the Results of Triaxial Tests

the effect of preparation history on the failure behavior of rocks under

Initml conditions: S or A -~...._....~ A

LEGEND= 5~ number of tests (160psi) =standard

I- -300 ~z 9 A/0SC (sea water) .

=- 3o-L2oo/ I" ~ o _ ~ ~ ~''

FIG. 7--Effect of mode of saturation on triaxial compression strengths of Trenton limestone

Mode of Saturation n ol ult psi s 070 W , 070 n Ol ult, psi s ~0 W , 070

AOS 24 43 100 2.9 0.22 24 50 500 3.1 0.28 Z

Effect o f Type o f Pore Fluid on the Results o f Triaxial Tests

Effect o f the Time o f Saturation on the Water Content

Four Factors Influencing Observed

The U. S. Bureau o f Mines has measured numerous rock properties for

specimen handling procedures. The order of factor presentation does not

Discussion of Critical Factors

T A B L E 1--Strength and Young "s modulus o f shale as a function o f relative humidity.