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D. L.

K a n t r o 1

Influence of Water-Reducing Admixtures on Properties of


Cement Paste ,, A Miniature Slump Test

REFERENCE: Kantm, D. L., "Influence of Water-Reducing Admix- slump and compaction (Vebe test) with his "two-point" method
tures on Properties of Cement Paste--A Miniature Slump Test," Ce- [7], he points out that slump is directly related to yield value.
ment, Concrete. and Aggregates, CCAGDP, Vol. 2, No. 2, Winter
A need exists for a rapid method for comparing rheological
1980, pp. 95-102.
effects of the wide diversity of admixtures currently available. Cor-
ABSTRACT: A miniature slump test has been developed for the responding to the slump test (ASTM Test for Slump of Portland
evaluation of the influence of water-reducing admixtures on the Cement Concrete [C 143]) that is in common use for concrete
workability of neat portland cement pastes. Resulting paste pat areas mixes, a simple comparison test, the miniature slump test, has
rather than heights are measured, and the results are expressed as the been devised for use with neat cement pastes. Helmuth [8] points
percentage of water reduction. Relative effects of various admixtures
on a portland cement are illustrated, and influences of specific admix- out that paste, like concrete, slumps to the point where the yield
tures on different cements are also shown. Effects of different super- value is no longer exceeded. Plastic viscosities of pastes and of con-
water-reducing admixtures and combinations of ordinary and super- cretes may be quite different, but for practical considerations
water-reducing admixtures are compared. The mini-slump method has should not be as important as cessation of flow, which is deter-
also been used for the evaluation of the loss of workability (slump loss)
with time for various admixtures and admixture combinations. The mined by the yield value.. Consequently, there ought to be
simplicityof the method facilitates accurate and effective evaluation of reasonable correlation between the slump of concrete and that of
water-reducing admixtures. cement paste.
The miniature slump (mini-slump) test is rapid and can be used
KEYWORDS: cements, water-reducing agents, workability, portland with small sample size, so that many tests can be performed in a
cements few hours by one person.
Various combinations of cements and admixtures often yield
The term "workability" as applied to fresh concrete mixes has
mini-slump curves that are not simply explained. The scope of the
no precise definition. Tattersall [1] has discussed this problem in
present paper, however, does not include a discussion of such
detail and describes workability in terms of its qualitative com-
phenomena, which depend on the chemical reactions between the
ponents: "flowability," "compactability," "stability," "finishabil-
admixtures and compounds in the hydrating system.
ity," and "pumpability." Each of these components is a
rheological quantity of some complexity.
Since many of the flow properties of concrete studied in past Experimental Procedure
years depend on the cement paste component of the mix, some in-
The miniature slump cone was fabricated of Lucite ® and had
vestigators have looked instead into the rheological properties of
the following dimensions: top diameter, 19 mm (3/4 in.); bottom
neat cement pastes. Much of this work has been done with coaxial
diameter, 38 mm (1-1/2 in.); and height, 57 mm (2-1/4 in.). These
cylinder viscometers. Studies by Ish-Shalom and Greenberg [2],
dimensions are in the same proportions as the slump cone of
Dimond and Tattersall [3], Tanahashi [4], and Odler et al [5] have
ASTM Test C 143. Design details of the miniature cone are shown
dealt with fundamental theological properties such as thixotropy,
in Fig. 1.
antithixotropy, and dependence on volume concentration and solid
A wide flange serves to collect excess paste when the top surface
surface area; they also discussed various proposed models for the
of the paste is leveled to the height of the cone. The lower surface
system. Tattersall [1] has discussed these concepts and previous
of the cone is relieved so that only a 6.35-mm wall thickness re-
work done on them in detail.
mains, a design feature that prevents the lower surface from
TattersaU [6] argues that a workability function for concrete re-
impeding the flow of the paste as the cone is lifted.
quires knowledge of both yield stress and plastic viscosity. In his
Mixing was done with a Hamilton-Beach Model 4A kitchen
study of the relationship between British standard methods for
mixer and "egg-beater" type paddies. The batch size for a single
Presented at the Symposium on Nonstandard Test Methods Useful in mini-slump determination was 70 g. Since this amount was too
Determining Physical-Chemical Characteristics of Cements, held in San small for the standard mixing bowl, a 250 ML stainless steel
Diego on 12 Dec. 1979by ASTM Committee C-1 on Cement and chaired by beaker was used instead.
Albert W. Isberner of the Portland Cement Association. A mixing regimen of 2 rain mix/3 min stand/2 min mix was used
1Formerly, principal research chemist, Chemical/Physical Research
Dept., Portland Cement Assoc., 5420 Old Orchard Rd., Skokie, Ill. in most cases. This type of mixing schedule, used to avoid "brief
60077. Now, director of admixture research, Master Builders, 23700 mix set" and false set, has been discussed by Powers [9].
Chagrin Blvd., Cleveland, Ohio 44122. Member of ASTM. Subsequently, the sample was placed in the cone resting on a
© 1981 by the American Society for Testing and Materials 0149-612318010012-0095500.40
95
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96 CEMENT, CONCRETE, AND AGGREGATES

for some reason it is not expedient to allow time for the pat to dry.
Several diameter measurements of the pat can be made with a
calipers. An average diameter can be calculated and from this, the
area of the corresponding circle can be determined.
In the concrete slump test procedure, the decrease in height is
measured. Similar measurements are difficult with pastes because
of the small size Of the cone. The decrease in pat height is generally
great, and the differences resulting from different workabilities are
GENERAL VIEW
relatively small. The areas, on the other hand, show large dif-
ferences with different workabilities and, therefore, the pat area is
a better indicator of workability.
Larger paste mixes can be used if other test procedures are to ac-
company the mini-slump test. For the evaluation of loss of
workability with time (slump loss), a large paste batch is divided
into a predetermined number of smaller portions, depending on
the number of data points sought. The mixing regimen is the same
as that described above, except that the paste is mixed in a con-
tainer of suitable size. At the end of the second mixing period, the
paste is quickly apportioned to an appropriate number of 250 mL
stainless steel beakers that are allowed to stand covered and un-
disturbed for various lengths of time (the standing intervals); then
the samples are mixed for two more rain and placed in the mini-
slump cone.
TOP VIEW
i" £" 3 Results and Discussion

T h e D e p e n d e n c e on W a t e r / C e m e n t R a t i o

Pat areas of various portland cements with different water/ce-


r
ment ratios W / C as determined by the mini-slump method, are
I -I, given in Table 1. Each value listed is the average of two determina-
I tions. The average difference between duplicate determinations is
I ' 5% of the mean value, based on 47 pairs of measurements over a
/ range of areas from 7.4 to 103.2 cm 2 (2.7 to 16.0 in.2).
I t i~' Plots of area versus W / C are linear in the range W / C = 0.36 to
+';I I+ ,+o,o i:.l 0.45 for most cements examined. Some deviation from linearity
may occur at a higher W / C .
SIDE VIEW
Admixture Evaluation--Water Reduction
FIG. l--Mini.slump cone (1 in. = 25.4 mm).
Addition of sufficient water-reducing admixture (dissolved in
the mix water) to the cement-water mix results in a "mini-slump
Lucite sheet. As the cone was filled, a small spatula was moved area" larger than that of the admixture-free paste. The mini-slump
both laterally and vertically to aid in the escape of entrapped air area attained with the admixture corresponds to the pat area of an
bubbles. Cone filling requires less than 1 rain for all but the stiffest admixture-free paste having a higher W / C . The values of the
mixes. higher W / C can be obtained from the curve of pat area versus
At 1 rain after mixing, the cone was lifted with a motion rapid W / C for the cement. Water reduction values, in percent, are
enough for the cone to remain clear of the flowing paste, but slow calculated as
enough to avoid imparting a significant upward momentum to the
paste. The "feel" for this operation can be quickly gained from a (w/c)O - (w/c)A
lOO
few trial tests. (w/c) o
The pats of paste formed were allowed to stand until the next
day. By then, the pats were usually strong enough to be moved where superscript O refers to the W / C value of the admixture-free
from the Lucite sheet to a piece of paper. Tracings on paper were paste and superscript A refers to the W / C value of the admixture-
made of the pat perimeters and the areas of these tracings deter- containing paste where both pastes have the same mini-slump
mined with a planimeter. If the pat was too weak and tended to area. A W / C of 0.36 is convenient for the evaluation of water
break up when moved, its perimeter could be traced onto the paper reduction effects (Fig. 2). If, at the reference W / C = 0.36, the pat
from the carbonate stain left on the Lucite sheet. Although the area of a paste with admixture corresponds to that of a 0.45 W / C
shrinkage that occurred as the pat dried caused cracking through paste without admixture, 20% water reduction has occurred. The
the pat, the perimeter in contact with the plastic sheet was not af- amount of admixture required to accomplish this is designated
fected. Rapid area determinations can be made from fresh pats if A2O.

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KANTRO ON MINIATURE SLUMP TEST 97

TABLE 1--Mini-slump areas at various water~cement ratios W/C.

Mini-Slump Area,° in.2


Air Permeability Fine-
Cement ness, cm2/g 0.36 W/C 0.40 W/C 0.45 W/C 0.52 W/C

21802 4179 2.93 4.53 6.66 10.47


MCC-290 4023 3.85 6.54 8.70 16.00
21733 3986 2.84 4.16 5.87 8.74
21763 3833 3.21 4.46 7.06 12.32
21731 3738 2.67 4.95 8.10 12.37
21732 3513 2.76 4.07 6.18 8~65
MCC-274B6 3440 4.42 6.23 8.65 N.D. b
LTS-II 3436 4.78 6.28 8.72 N,D. b
LTS-18 3268 4.22 6.34 8.76 N.D. b
LTS-15 3229 2.70 4.14 6.69 N.D. b
21796 2937 5.58 7.89 10.51 13.39
al in.2 = 6.45 eva2.
bN.D. = not determined.

Mini-Slump Area Dependence on Admixture Concentration additions are given in Fig. 5 and with calcium lignosulfonate addi-
tions in Fig. 6. The A20 values are summarized in ascending order
Mini-slump area, of course, depends on the concentration of ad- in Table 2. Although the order of cements is the same for both ad-
mixture, and the nature of this dependence differs with different
mixtures, there are some distinct differences in the curves for the
types of admixtures. In some cases, there is a stiffening effect: the
various cements. For both admixtures, the LTS-15 curve rises
mini-slump area decreases at low admixture concentrations and in-
quite sharply above a threshold admixture content so that a very
creases at higher concentrations. Often there is an upper limit to
small increase in admixture content gives a large increase in mini-
the area, and hence to the amount of water reduction, reached at a
slump area, and therefore in water reduction. For LTS-11-sorbitol,
certain concentration of the admixture; greater concentrations
the maximum area is achieved at a concentration of 0.2%; there is
have no further effect. With super-water-reducing agents, the a significant decrease in area of higher concentrations.
mini-slump area increases steadily with increasing admixture con-
centration beyond the limits of practical measurement.
Results with Super- Water-Reducing Admixtures
Results with Sugars Two types of super water-reducers are currently available, the
The curves in Fig. 3 represent mini-slump areas with five dif- naphthalene-based material (N-type) and the melamine-based
ferent monosaccharide sugars. The relative water-reducing material (M-type). Some results for four commercial naph-
abilities of these compounds vary over a relatively wide range of thalene-based materials are shown in Fig. 7. The admixture con-
concentrations. Some stiffening always occurs at lower concentra- centrations are expressed as percentage added on the cement
tions. The Al0 and A20 values are indicated by those points where basis. The range of areas obtained is higher, and correspondingly
the curves intersect the dashed lines, and the dashed lines repre-
sent area levels obtained from plots such as that shown in Fig. 2.
The general retarding action of sugars is well known. Dif-
12
ferences in behavior of different sugars depend on differences in
chemical behavior, that is, calcium-complexing ability.
I0 Area for
I0 oY. w o t • r / / Area . .for
=,~=, .....
Results with Sugar Derivatives reduction -~ :~u-/. woler
A ~rr reduction
8 I0 / A5°
Various modified sugars, in both reduced and oxidized forms,
have influences similar to those of the sugars themselves. The /
g Area for
curves in Fig. 4 include those for mannitol, sorbitol, and dulcitol, 6 2 0 % water
molecules that differ only as optical isomers. Sodium gluconate, an 3 reduction
A:,O
admixture of considerable commercial importance, produces Q.
significant water reduction with relatively small quantities. 4
Other sugar derivatives must be used in larger quantities to pro-
duce the same effect. As with sugars, small structural variations in
the sugar-derivative molecules result in significant differences in 2 area (0.36 ~c)
Ao
water-reducing ability.
I I
).30 0.40 O.50 O.60
Results with Different Cements Water/cement ratio

Curves depicting mini-slump area versus admixture concentra- FIG. 2--Pat area versus W/C; results for a typical cement (1 in. 2 =

tion for different cements (all Type I compositions) with sorbitol 6.45 cm2).

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98 CEMENT, CONCRETE, AND AGGREGATES

12 .... i " I.... I I I I ........I I ......... ! ....

Ribose
I0 Fructose
/ / xylose

8
/ / ,ro0,0 1 I-
/ / . /
<x 6
E
/--S . . . .

,,I ,,I I I I ..... I I. . . . I . . . . . I ....


0 0,2 0,4 0.6 O,8 1.0

% Admixture, cement t~sis

FIG. 3--lnfluence of dlfferent sugars on mini-slump area; cement Sample MCC.2741t,


with W/C = 0.3611 in. 2 = 6.~5 cm2).

....... I ...... ! ! i J t ! '1 i ....


,21 Ascorbic Dulcito| Monnitol
acid"~i~_.. / Sorbitoi
io Sodium f 7 " / /
/
,,ooo,o - / _ - - ,,o
% 8

6
- -F z . . . . . ,o
.L
.E 4

j t I I .... I I I,, I .....


O 0,2 0.4 0.6 0,8 .0
% Admixture, cement basis

FIG. 4--Influenee of different sugar derivatives on mini.slump area; cement Sample


MCC-274B. with W/C = 0.36 (1 in. 2 = 6.45 cm 2 ).

the amounts of water reduction are greater. No apparent flattening and with mixtures in which 10, 20, and 30% by weight of the super
of the curve occurs over the concentration range investigated; in water-reducer was replaced by sodium gluconate (90:10, 80:20,
fact, no significant difference in results is apparent, when expressed 70:30). The curves indicate that to produce a given water reduc-
in percentage of solids on the cement basis, to distinguish among tion, lower total amounts of the mixtures are required than of the
the four N-type admixture preparations. super water-reducer by itself. For example, 0.49% by weight of the
Corresponding curves of mini-slump area versus admixture con- 80:20 mixture is required for 30% water reduction while 0.61% of
centration for N-type and M-type admixtures are shown in Fig. 8. the super water-reducer alone is required. The 0.49% includes
The two curves are similar but not superimposed. A larger amount 0.39% of the super water-reducer and 0.10% sodium gluconate.
of the M-type admixture is required for a given water reduction. Thus, for 30% water reduction, 0.22% (0.61-0.39) of the N-type
admixture is replaced by 0.10% sodium gluconate. The inversion
of the relative positions of the 70:30 and 80:20 curves suggests that
there is an optimum ratio for minimum total admixture.
Results W i t h T w o - C o m p o n e n t A d m i x t u r e s
Results for other cements vary somewhat in amount of total ad-
Water-reducing capabilities of mixtures of conventional and mixture compared to the amount of N-type super water-reducer re-
super-water-reducing admixtures, added in the mix water, have quired for a given water reduction. Generally, however, a part of
been examined by the mini-slump method. The curves in Fig. 9 the N-type super water-reducer can be replaced by sodium
were obtained with an N-type super water-reducer alone (100:0), glueonate without loss of water-reduction capability.

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KANTRO ON MINIATURE SLUMP TEST 99

12 I I I I 1 I ! 1 I

I0

/
~, 8
.=_
/
/ \
i
"r.
"\/ / \
2 LTS-15

I I I I I I I t
0 0.2 0.4 0.6 0.8 1.0
% Admixture, cement b a s i s

FIG. 5--Influence of sorbitol on different cements with W/C = 0.36 (I in. e = 6.45
cm2).

14 I I I ! I I 1 t I

12

|0

/ ~ ~ MCC-274B

)! /
6
I

4
"--/ /

I I I I ,I I I I I
0 0.2 0.4 0.6 0.8 1.0
°/o Admixture, cemeot basis

FIG. 6--Influence of calcium lignosulfate on different cements, with W/C = 0.36


(1 in. 2 = 6.45 cm2).

Loss of Workability Effects of delayed addition of an N-type admixture on worka-


bility of cement pastes with high and low amounts of tricalcium
Use of super water-reducers to enhance concrete workability aluminate are shown in Fig. 11. In the delayed addition procedure,
results in loss in that workability with time. The mini-slump 80% of the mixing water was added to the cement; after the first
method provides a useful tool for the study of this slump loss prob- 2-rain stirring period and the 3-min standing period, the remaining
lem. Loss in area as a function of time is shown in Fig. 10 for super 20% of the mixing water with admixture dissolved in it was also
water-reducers at various concentrations. Reference data for an added to the cement-water mixture. The amounts of admixture
admixture-free paste of the same cement at 0.45 W / C are also in- used were enough to produce approximately 10% water reduction
cluded and show no decrease during the first hour of hydration. in each case, when added without delay. Much greater initial
Although all mini-slump area losses were quite large, at higher workability occurred with delayed addition and although there was
concentrations some water reduction remained after 1 h. At lower significant loss with time, after 1 h the pastes still had mini-slump
admixture concentrations, by 1 h the mini-slump area had re- values corresponding to a water reduction greater than 20%.
turned to the value of the admixture-free paste. Substitution of sodium gluc0nate for a part of an N-type super-

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100 CEMENT, CONCRETE, AND AGGREGATES

TABLE 2--A2o values for different 18 I I I ............ I I I I


cements % by weight of cement. 70/30

A20 Calcium t6
/
Cement A2o Sorbito! Lignosulfonate !
LTS-11 0.13 0.09 14
/
LTS-18 0.16 0.21
LTS-15 0.18 0.27
MCC-274B 0.27 0.31 t2 0/0

.c
10
16 l I I

~ 8
14 f

I-I
AIO
A30
42 -

AO
iO

A2O
~ B

_f
g. Aio
6 I ! I I ....... t ,, I |
0 0.2 0.4 0.6 0.8
4 AO Total admixture, %, cement basis

FIG. 9--Influence of mixtures of one N-type super water-reducer and


sodium gluconate on cement Sample 21731, with W / C = 0.36 (1 in. 2 =
6.45 cruZ).
l I I I
0 .2 .4 .6 .8
% Admixture,cementb o s i s

FIG. 7--Influence of four commercial naphthalene.based materials


super-water-reducing admixtures; cement Sample 21731, with W / C =
0.36 (1 in. 2 = 6.45 cm2). 14 I I I ............. i..........................1....... I I
A30
12
14 I I
I ....I ....... I ........ I ...... ~ ~ --0,60%
type M 0.36 W/C

12

c' ~ No admix~ t e ~ * ~ A20


N- type 8
I0
M-type - - ~
%
E 6 ----
~s
,,° 4 . _ . . . . . .
6
c
\ \,o.oo% type, o . , , . , c
AO 2 ~0.55% type M 036w/c -
~'-0.55% type MO~6w/c
I I I ,, I.......... I,,, I I
" 0 15 30 45 60
Standing interval, minutes
I I I i I I
0.2 O.4 0.6 0.8 FIG. tO--Mini-slump area versus time for cement Sample 21731 con-
Admixture concentratiOn, %, solids, cement basis taining super-water-reducing admixtures and for admixture-free paste of
the same cement (1 in. 2 = 6.45 cm2).
FIG. 8--Influence of N-type and M-type super water-reducers; cement
Sample 21731, with W / C = 0.36 (1 in. 2 = 6,45 cm2).

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KANTRO ON MINIATURE SLUMP TEST 101

I I ! I I I I water-reducing agent results in increased area (Fig. 12). Cement


MCC-287 contains a low amount of tricalcium aluminate, and
although a relatively low percentage of the N-type admixture pro-
duces a large pat area, further gains are obtained by replacement
of 10% of the N-type super water-reducer with sodium gluconate.
High CSA 0 , 4 0 % , deloyed
30 Cement 21731 contains a larger amount of tricalcium aluminate
than does cement MCC-287. Replacement of 30% of the super
water-reducer with sodium gluconate results in a doubling of the
initial pat area, and even after 1 h the pat area of the sodium
gluconate sample is significantly greater than the initial area of the
o unsubstituted ease.
E
.2=
,k
~ oyed
Relationship to Concrete S l u m p Data
Relationships between results of the mini-slump test and those
of the concrete slump method were examined by Perenchio et al
10
[10]. The authors point out that by using the mini-slump pro-
cedure, it is possible to identify separate effects that are not readily
differentiated with concrete mix data. However, the major effects
|, observed by the mini-slump technique do in fact correspond to ef-
High CaA 0 . 4 0 * / .
fects observed with concretes.
I I I I I I
o 15 30 45 60 The greater sensitivity of the mini-slump procedure results from
$tonding time, minutes the greater concentration of the paste in the test specimen.
Dosages determined by the mini-slump method are less than those
FIG. ll--Effect of delayed addition, N-type super-water-reducing ad- required for comparable water reductions in concrete. The mini-
mixture, on loss of workability in a cement with high tricalcium aliminate slump method does, however, permit evaluation of admixture ef-
(CaA) content (Sample 21795) and in a cement with low tricalcium fects that, when combined with only a few tests with concrete, can
aluminate content (Sample 21796) (1 in. 2 = 6.45 cm2).
be translated into terms applicable to the concrete. One factor that
must be studied is the proportional increase in admixture dosage
required in concrete applications [10].
720 I I I I I ! I

Conclusions
18 MCC-287 0.30% 9 / I type N/No gluconote
A miniature slump test has been developed for neat portland ce-
ment pastes. Comparative tests for admixture requirement can be
16 made and loss in workability with time can be followed by means of
this new procedure. The mini-slump method for cement pastes is
14 much more sensitive than the slump test for concretes, but the
gross effects observed correlate with corresponding concrete
N
results.

Acknowledgment

~
i
¢
,o

e ~ onote
Part of the work reported here was supported by a grant from
the Federal Highway Administration. The author expresses his ap-
preciation to David R. Gnaedinger for his valuable laboratory
assistance.

#21731 0 . 4 0 % type N
Relerenees

[1] Tattersall, G. H., "The Workability of Concrete," Publication No.


11.008, Viewpoint Publications, Cement and Concrete Association,
Wexham Springs, Slough, U.K., 1976.
[2] Ish-Shalom, M. and Greenberg, S. A., in Proceedings of the 4th In-
ternational Symposium on the Chemistry of Cement, Monograph 43,
I } I I I I Vol. II, National Bureau of Standards, Washington, D.C., 1960, pp.
0 15 50 45 60 731-744.
[3] Dimond, C. R. and Tattersall, G. H., in Hydraulic Cement Pastes:
Standing time, minutes
Their Structure and Properties, Publication No. 15.121, Cement and
Concrete Association, Wexham Springs, Slough, U.K., 1976.
FIG. 12--Effect of substituting sodium gluconate for N-type water- [4] Tanahashi, I., Architectural Institute of Japan, Transactions, Vol.
reducing admixture on workability (1 in. 2 = 6. 45 cm2). 269, July 1978, pp. 19-30.

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102 CEMENT,CONCRETE, AND AGGREGATES

[5] Odler, I., Becker, T., and Weiss, B., II Cemento, Vol. 3, July-Sept. the Chemistry of Cement, Communications, Vol. III, Ciments,
1978, pp. 303-310. Betons, Platres, Chaux, Paris, 1980, pp. VI-0-1-30.
[6] Tattersall, G. H., in Fresh Concrete--Important Properties and [9] Powers, T. C., Properties of Fresh Concrete, John Wiley and Sons,
Their Measurement, Vol. 1, International Union of Testing and Inc., New York, 1968, pp. 441-442.
Research Laboratories for Materials and Structures (RILEM), Leeds, [I0] Perenchio, W. F., Whiting, D. A., and Kantro, D. L., in Proceedings
U.K. 1973, pp. 2.2-1-2.2-33. of the CANMET-ACI Symposium on Superplasticizers in Concrete,
[7] Tattersall, G. H., Magazine of Concrete Research, Vol. 28, No. 96, Vol. I, CANMET, Dept. of Energy, Mines and Resources, Ottawa,
Sept. 1976, pp. 143-147. Canada, 1978, pp. 295-323 and Appendix pp. 315-323.
[8] Helmuth, R. A., in Proceedings of the 7th International Congress on

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