You are on page 1of 46

British Geological Survey

TECHNICAL REPORT WG/92/39


Mineralogy and Petrology Series

Industrial Minerals Laboratory Manual


DIATOMITE
S D J Inglethorpe

Mineralogy and Petrology Group


British Geological Survey
Keyworth
Nottingham
UnitedKingdom NG12 5GG
British Geological Survey

TECHNICAL REPORT WG/92/39


Mineralogy and Petrology Series

Industrial Minerals Laboratory Manual


DIATOMITE
S D J Inglethorpe

A Report prepared for the Overseas Development Administration under the


ODA/BGS Technology Development and Research Programme, Project 91/1

ODA Classzjkation:
Subsector: Others
Subject: Geoscience
Theme: Mineral resources
Project title: Minerals for Development
Reference number:R5541

Bibliographic reference:
Inglethorpe, S D J
Industrial MineralsLaboratory Manual:
Diatomite
BGS Technical Report WG/92/39

Subject index:
Industrial minerals, diatomite, laboratory techniques

Cover illustration:
SEM photomicrograph of the
Rio Chiquito DeLas Nubes diatomite, Costa Rica.
The presenceof genus Melosira sp. diatoms indicates
fresh, deep water environment. The predominanceof
whole diatoms suggests that accumulation was by
low-energy pelagic sedimentation.

0 NERC 1993

1993
Keyworth, Nottingham, British Geological Survey,
CONTENTS

Page
1. INTRODUCTION 1
2. BIOLOGY AND ECOLOGY OF DIATOMS 2
3. GEOLOGICAL, OCCURRENCE 3
4. INDUSTRIAL APPLICATIONS 6
5. LABORATORY CHARACTERISATION 9
6. LABORATORY TESTS RELATINGTO
INDUSTRIAL APPLICATIONS 15
7. CASE STUDY 22
8. CONCLUSIONS 24
REFERENCES 25

APPENDICES:
1. Preparation of diatomite for examinationby optical microscope 27
2. Measurement
gravity
of specific 28
3. Measurement of bulk density 30
4. Sample preparation and calcination 31
5. Filtration theory 33
6. Measurement of permeability and wet cake density 34
7. Determination of oil absorption values 36
Preface
Industrial mineral raw materials are essential for economic development.
Infrastructure improvement and growth of the manufacturing sector
requires a reliable supplyof good quality construction minerals and a
wide range of other industrial mineral raw materials.
Although many less developed countries have significant potential
industrial mineral resources, some continue to import these materials to
supply their industries. Indigenous resources may not be exploited (or
are exploited ineffectively) because they do not meet industrial
specifications, and facilities and expertise to carry out the necessary
evaluation and testwork are unavailable. Unlike metallic and energy
minerals, the suitability of industrial minerals generally depends on
physical behaviour, as well as on chemical and mineralogical properties.
Laboratory evaluation often involvesdetemination of a wide rangeof
inter-related propertiesand must be carried outwith knowledge of the
requirements of consuming industries. Evaluation may also include
investigation of likely processing required to enable the commodity to
meet industry specifications.
Overthelast 10 years, funding from the Overseas Development
Administration has enabled the British Geological Survey to provide
counties in the evaluationof their industrial
assistance to less developed
mineral resources. This series of laboratory manuals sets out experience
gained during this period. The manuals are intended to be practical
bench-top guidesfor use by organisations such as Geological Surveys
and Mines Departments and are not exhaustive in their coverage of every
test and specification. The following manuals have been published to
date:
Limestone
Flake Graphite
Diatomite
Kaolin
Bentonite
A complementary seriesof Exploration Guidesis also being produced.
These are intended to provide ideas and advice for geoscientists
involved in the identification and field evaluation of industrial minerals
in the developing world. The following guide has been published to
date:
Biogenic Sedimentary Rocks

A J Bloodworth
Series Editor
D J Morgan
Project Manager
1

Industrial Minerals Laboratory Manual

Diatomite

1. INTRODUCTION

Diatomite is a pale coloured, soft, light-weight rock composed


principally of the silica microfossils of aquatic unicellular algae known
as diatoms.It has a unique combination of physical and chemical
properties (high porosity, high permeability, small particle-size, large
surface area, low thermal conductivity and chemical inertness) that make
it suitable for a wide range of industrial applications. Its main uses are
as a filter-aidin the processing of liquid foodstuffs and chemical fluids,
as a raw material for the production
as a filler in plastics and paints, and
of insulation bricks.
This manual defines the petrographic, mineralogical, chemical and
physical characteristicsof diatomite and describes simple test procedures
for determining industrial specifications. Experimental results from
recent studiesin Thailand and Central America are includedas
examples. This manual is one of a series produced as partof the
BGS/ODA R&D Project Minerals for Development.

Mineralogy and Petrology Group, British Geological Survey 0 NERC 7992


2

Diatomite

2. BIOLOGY AND ECOLOGY OF DIATOMS


Diatoms are classified within the Kingdom Protista which also includes
protozoans, moulds andfungi (Brazier, 1990). They are single-celled
organisms consisting ofa softbody (cytoplasm, oil globules and
chloroplasts) enclosedby an opaline exoskeleton. The exoskeleton or
frustule is composedof two halves, the smaller half fitting inside the
larger half. Frustules are either circular (centric) or elliptical (pennate)
in
form, and are ornamented with sieve-like perforations (punctae) and
intricate rib structures (costae). Diatoms create their food by combining
carbon (obtained fiom photosynthesis of carbon dioxide) with nutrients
extracted from seawater. They form the foundation of the Oceanic food
chain as they are the staple diet of
krill (tiny shrimp-like crustaceans)
which support many marine vertebrates.
Diatoms are adapted to a wide range of aquatic environments including
marine, brackish and fresh waters. The organisms require suitable
environmental conditionsif they are to flourish including appropriate
temperature and photic conditions,a narrow salinity and acidity range,
and a stable supplyof nutrients including silica, nitrogen, phosphorus,
iron, oxygen and carbon dioxide. Diatoms inhabit the photic zoneat
depths down to 200m and thrive in cold watersin sub-polar and
temperate regions. Recent studies have used diatom assemblages as
environmental indicators in Quaternary and present-day freshwater lakes
(Abella, 1988; Stager, 1988).

Mineralogy and Petrology Group, British Geological Survey 0 NERC 1992


3

Diatomite

3. GEOLOGICAL OCCURRENCE

At the end of their life-cycle, opaline diatom exoskeletons settle through


the water column and accumulate as ooze on the floor of the depositional
environment, a process known as pelagic sedimentation; Kadey (1983)
suggests an average sedimentation rate of 1-4mm per year. Diatomite,a
sedimentary rock, forms by dewatering and compaction of this ooze.
Diatoms first appearsin the geological record about one hundred million
years ago during the Upper Cretaceous, but most economic deposits are
of Miocene-Pleistocene age. Diatomite deposits are frequently associated
with volcanic activity,with air-fall ash, run-off waters and spring
waters providing a source of dissolved silica to replenish that extracted
by diatoms (Talliaferro, 1933). The purity of a diatomiteis chiefly
controlled by clastic and/or volcanogenic input during deposition.
Calcareous micro-organisms which co-exist with diatoms in equatorial
marine environments also affect purity.
At the present day, diatom-rich marine sediments accumulate in ocean
basins in regions associated with the upwelling of nutrients, such as the
zone of ocean current divergence in the sub-antarctic (Figure 1). Ocean
floor areas are free from strong water movements which would
introduce temgenous sediment, and are also deep enough to allow the
dissolution of calcareous microfossils. However, the extensive marine
Miocene-Pliocene deposits of California are known to have formed in a
shallow-water neritic environment. Conger (1942) suggested that
freshwater diatomite is likelyto accumulatein mountain or crater lakes,
free of sediment-bearing streams or rivers, where water inflow is by
seepage (Figure2). Most world deposits are of lacustrine origin. Marine
deposits, although less common, are generally larger in size. Gradual,
prolonged subsidenceof marine and freshwater basins is necessary to
allow development of thick accumulations of diatomite.
The effect of post-depositional processes on diatomite deposits is poorly
understood. Diagenetic alteration is likely to influence the porosity and
degree of cementation through dissolution, mobilisation and re-
precipitation of diatomaceous silica, and in extreme cases is likely to
convert diatomite to chert (Mathers, 1989). Diatomaceous ooze has been
reported to containa substantial proportion of organic matter derived
from diatom soft bodies and so is a possible sourcerocks for petroleum
deposits (Talliafen-o,1933). Conger (1942) reports that uplift and
exposure of diatomite under good drainage conditions removes organic
impurities by oxidation and leaching.

Mineralogy and Petrology Group, British Geological Survey 0 NERC 1992


4

Diatomite

.
- I
. .
.
. .. . . .. . . .. . . .
.. .. . .

Figure 1. Concentration of diatoms in surfacesedimentsofoceansat


the present day (after Brazier, 1991).

Plumes of s e d i m e n t - r i c h river water


e n t e r i n g l a k e as u n d e r , i n t e r a n d o v e r f l o w s ,
depending on d e n s i t y relative t o l a k e w a t e r

Figure 2. Sedimentological model for accumulation of diatomite in a


caldera lake environment (afterMathers,1989)

Mineralogy and Petrology Group, BritishGeological Survey 0 NERC 1992


5

Diatomite

3.1 Major economic deposits


The following countries are major producersof diatomite and are
responsible for 98% of world production:USA (approx. 33%),
France, Romania, former USSR (CIS), Spain, Denmark, Korea,
Mexico, Gemany, Italy, Iceland, Brazil (Harben, 1992). World
production for 1988 was estimated at 2 Mt. with reserves of 2000A Mt.
brief survey of some commercial depositsis made below. A more
comprehensive reviewof world production of diatomite is givenin
Anon. (1987).

3.1.1 USA

The most extensive deposits of commercial diatomite are the late


Miocene-early Pliocene marine diatomites of the Sisquoc Formation
located in the foothills of the Santa Ynez mountains south of Lompoc
valley, western Santa Barbera County, California, USA (Taylor, 1981;
Burnett, 1991). Commercial deposits over 1000 ft. thick are extracted
by the Johns-Manville Corp. and Grefco Inc. (who market M thei t e
and DicaZite range of products respectively) for filter-aid and
fiier
production. In mid-1986 Grefco also began to extract a high-quality
Miocene-Pleistocene freshwater diatomite at Lake Britton, northeast of
Burney, Shasta County, for filter-aid production.

3.1.2 Romania

Romania is the largest producer


in Europe with lacustrine deposits
located at Adamclisis Constanta, Patiragele Buxau and Minis-Arad.
Diatomite products in Romania (andin the former USSR) arealmost
exclusively consumed by the construction industry.

3.1.3 France
Carbonisation de Actifs SA (Ceca) produces high-quality filter-aid
grade diatomite from undergroundmining of a Miocene lacustrine
an opencast
deposit at Rioms-les-Montagnes. Ceca also operate
diatomite mine at St. Bauzille on the east side of the Andance
mountains. Manville de France SA are Frances second largest
producer with a mine at Murat, Cantal.

Mineralogy and Petrology Group, British Geological Survey 0 NERC 7992


6

Diatomite

4. INDUSTRIAL
APPLICATIONS
In the United Statesin 1985,66%of diatomite produced was used in
filtration, 21%for fillers, 1% for insulation and12%for miscellaneous
uses (Anon, 1987). The world market for diatomite is increasing,
although there is competition from perlite, calcined kaolin, talc, and
other forms of silica (Harben, 1992).

4.1 Industrial processing


Raw diatomiteis processed using the following methods:
Primary crushing After extraction the diatomite is crushed to
aggregate-size piecesin roller or hammer mills.
Simultarleous drying and milling Crude diatomite (typically
containing in excessof 40% moisture) is carriedby a stream of hot
gases produced byan air-blower coupled to a furnace, and is
simultaneously dried and milled.
Air-classification The filter-aid and filler markets require powdered
diatomite in different particle-size grades. These are produced by air-
classification. For example, Lompoc diatomite isair classified to
produce various gradesof calcined filter-aidswith different particle-
size characteristics.A proportion of the dried, milled, air-classified
powder is packaged and sold as natural diatomite mainly for the
filler market.
Calcination Following air classification, diatomite is calcinedat 870-
1 100C in a rotary kiln. The process transforms amorphous silica to
crystalline a-cristobalite, reduces surface area, increases mean
particle-size and increases hardness from 4.5-5.0 to 5.5-6.0 (Mohs
scale).The main purpose of calcination is to increase filter-aid
flowrate, improve the strength of fillers and increase abrasive
properties. Greater changein physical properties is obtained by
adding soda ash [Na2C03] asa flux. Calcined and flux-calcined
end-products are marketed both as filter-aids and as fillers.

4.2 Filtration

Diatomite is used as a filter-aid to process a wideofrange


industrial and
non-industrial fluids including inorganic/organic chemicals,
pharmaceuticals, beer, wine, whisky, fruit juices, vegetable juices,
fuels, oils,dry cleaning solventsand swimming pool waters.A filter-
aid is essentially a permeablebed of diatomite whose purpose
is to

Mineralogy and Petrology Group, British Geological Survey 0 NERC 1992


7

Diatomite

remove fine-grained particles from


a suspension and producea clear
filtrate at high flowrates.

4.3 Fillers

Diatomite is usedas a fillerin paints, plastics, rubber, pharmaceuticals,


toothpastes and polishes. Diatomite fillers are marketedasboth natural
grades (e.g. Celite266) and as flux-calcined grades (e.g. Celite 499,
281, White Mist). In certain applications diatomite is added to modify
the physical properties of the product and is therefore referred toa as
functional filler.
Diatomite is commonly added to paint products such as flat emulsions,
varnishes and primers because it has excellent flatting properties (i.e.
it reduce gloss and sheen), extends the hiding power (opacity) of the
primary pigment, improves adhesionof subsequent coats (good tooth)
and has good sanding properties. Moreland(1987) estimates that 15%
of the total industrial usageof diatomite is as a filler for plastics. Its
major useis as an anti-blocking agentin production of low-density
polyethylene film; diatomite is typically added 500-3000
at ppm
concentration and prevents self-adhesion of the film.

4.4 Insulation,absorbentpowders and granules


The Danish companies Skamol and Damolin produce insulation bricks
from a raw material known as moler- a natural mixture of
diatomaceous silica and20-25%plastic clay (Griffiths,1990).
Insulation bricks are produced as follows:(1) crude moler is fed from a
hopper to a primary crusher and reduced to a particle-sizeof 2-3 mm;
(2) up to 50% pinewood sawdustis added to increasethe porosityof the
final product through gases generated during firing;(3) the
moler/sawdust blend is then mixed with steam to improve plasticity,
extruded and wire cut into lengths;
(4) these green bricks are dried at
90C for 2-5 days and then fired.
Moler isalso used to produce kiln-dried absorbent powders/granules
(uses: industrial absorption, animal feed, pesticides, cat litter) and
calcined powders (uses: explosives, seed coating, chemicals industry).
It is likely that current uses for moler were developed because it is not
1983).
sufficiently pure for filtration and filler applications (Lefond,

4.5 Miscellaneous
Diatomite is also used asa mild abrasive (toothpaste and metal polish)
anti-caking agentin fertilizer prills, pozzolana/concrete additive to

Mineralogy and Petrology Group, British GeologicalSurvey 0 NERC 1992


8
. .

Diatomite

improves plasticand hardened properties, stabilising agent in


explosives, chromatography support media, pitch controlin paper
manufacture, andas a catalyst carrier (for nickel catalyst
in vegetable oil
hydrogenation, for vanadium in sulphuric acid manufactureand for
phosphoric acidin petroleum refining).

Mineralogy and Petrology Group, British Geological Survey 0 NERC 1992


9
. -

Diatomite

5. LABORATORYCHARACTERISATION

This section describes the mineralogical, chemical and physical


properties of diatomite. Appropriate methods for the laboratory
assessment of diatomite are outlinedin Figure 3. Diatomite has
distinctive chemical and physical characteristics, including high silica
content in combination witha low SG. An optical or scanning electron
microscope is usually required to detect the presence of diatoms, and
XRD analysis is necessary to identify diatomaceous silica (opal A).

5.1 Chemistry

The prime criterion for judging potential industrial is uses


chemical
composition. Typical chemical analyses of diatomites used by industry
are shownin Table 1. Diatomites used in filtration and filler applications
generally contain>85% silica. Theune& Bellet (1988) define maximum
levels for several chemical constituents of filter-aids: (1) 4 % CaO to
prevent turbidity in beer filtration resulting from oxalic acid formation
and precipitationof tartaric acid crystalsin the filterbed during wine
filtration; (2) <1.5% Fe203 to prevent formation of deleterious iron
tannates in wine filtration; and(3) d o 0 ppm solublesalts to prevent
chemical contamination of foodstuff liquors.
The British Standard Specifications for paint extenders
(BS 17951976)
lists two chemical categories for diatomite fillers: 70-80% silica (Si02)
for type1 diatomite fders, and a minimum of 80% silica for the type
2 classlfication. In contrast, diatomite extracted
in Denmark for
production of insulation bricks and
kiln-dridcalcined powders and
granules hasa relatively low silica, high alumina and iron.

5.2 Mineralogy

The type of silica present


in diatomite is a hydrous form of opaline silica
which contains between3-8% structural water. Several types of opaline
silica were defined by Jones & Segnit (1 97l), principally by their
different X-ray diffraction(XRD) characteristics. These include opal C
CT (disordered cristobalite/
(well-ordered a-cristobalite); opal
tridymite); and opalA (poorly-ordered, almost amorphous). Diatomiteis
composed of biogenic opalA silica which is indicated from XRD
analysis bya broad peak in the vicinityof the a-cristobalite spacing at
4.05 A (Figure 4).The qualitative mineral content of diatomite also can
be determined byXRD analysis. Common impurities include quartzsilt
and sand, volcanic ashand pumice, clay minerals, carbonate minerals,
iron oxides/oxyhydroxides, hydrothermal minerals (e.g. alunite group)
and organic matter.

Mineralogy and PetrologyGroup, British Geological Survey 0 NERC 1992


I INITIAL CHARACTERISATION I

TESTS RELATING TO P O K E

I
. ........... ............................................... ......................... ............ .... ... ... ..... ... ... ... ... ...... ... .. .... . .. . .. . .. . . . . . .. . .. .. .... .. ..... .. .. .. .. .. .. . .
. . .
I FILLERS FOR PLASTICS AND PAINTS I

Figure 3. Laboratory evaluation of diatomite


11

Diatomite

0.84 -
0.01 -
02 e cO-K a
1 I

0.0 40.0
10-0 30.0 20.0 sD.0

Figure 4. Whole-rock XRD trace of a high-purityfreshwater


diatomitefrom Burney, California. Thebroadhump in the vicinity
of the a-cristobalite peak (4.05 A) is typical of opal A type silica.

Figure 5. SEM photomicrograph of the Rio Chiquito De Las Nubes


diatomite, Costa Rica. Thepresence of genusMelosira sp. diatoms
indicates a fresh, deep water environment. The predominance of
whole diatomssuggests that accumulationwas by low-energy
pelagic
sedimentation.

Mineralogy and Petrology Group, British Geological Survey0 NERC 1992


12

Diatomite

5.3 Microscopy

Diatoms are microfossils andso are not generally visible to the naked
eye although larger diatoms(30-40 pm) maybe resolved by a hand-
lens. Optical or scanning electron microscope (SEM) methods are
therefore usually necessary to identify their presence.
Inspection by binocular microscopeis a useful rudimentary method for
investigating the micropalaeontology and particle morphology of larger
diatoms, andfor estimating the proportions
of coarse-grained mineral
impurities (quartz, feldspar, heavy minerals etc.) present.
A preparation
procedure for diatomite prior to binocular microscopyis given in
Appendix 1.
Secondary electron modeSEM analysis is carried out on fragments of
rock coated under vacuum with gold or carbon. It is a high-resolution
method (conventionally used for detailed petrographic work) capable of
providing comprehensive dataon the morphology of diatoms and their
micropalaeontology. Semi-quantitative chemical analysis of individual
mineral grains can generallybe determined usingan energy dispersive
detector. A high Sflow Al spectra is typicalof diatom particles.An
SEM photomicrograph of a diatomite from Costa Rica is shown in
Figure 5.
Diatomite composed predominantlyof whole diatomsis likely to have
accumulated by pelagic sedimentation in a relatively low-energy
environment. However,if a large proportionof diatom fragmentsis
present this suggest a relatively high-energy environment where attrition
resulted from sediment transport and reworking. Micropalaeontological
in a
studies of diatom taxa can reveal whether a deposit was formed
freshwater, brackish or marine environment, and whether deposition
occurred in deep or shallow water.

5.4 Physical properties

k e diatomite is composed essentially of diatoms and diatom fragments


in the size range 63-2 pm, but the presenceof mineral impurities can
>63 pm fractionof the
alter particle-size distribution. The substantial
Nan Jo diatomite (Table2) is due to cementation of particles by goethite,
and its largeQ pm fraction is a resultof a high clay mineral content.
Pure diatomite hasan SG value of 2.0-2.1, >80% porosity (total void
volume) and a bulk density between 0.2-0.4 gJcm3. The presenceof
mineral impurities increasesSG and bulk density values and lowers
porosity. SG is generally the most reliable indicator of purity, since
bulk density and porosity areboth influenced by particle-size

Mineralogy and Petrology Group, British Geological Survey0 NERC 1992


13

Diatomite

distribution as wellas mineral content. Proceduresfor the determination


2 and 3.
of specific gravity and bulk density are given in Appendices
High-purity diatomites are typically white, buff or greyin colour (in the
as illustrated by the Burney diatomite
natural state and after calcination)
(Table 3). The colourof calcined diatomite is particularly affected by
iron content; for example, the low brightness values of calcined Lorna
Camastro diatomite are due to a pink colouration imparted by hematite
(formed from thermal decompositionof alunite-group minerals).
Addition of a soda ash flux may improve the colour of the calcined
product. A procedure for sample preparation and calcination of diatomite
for physical propertytesting is given in Appendix4.

Table 1. Chemicalcomposition of naturaldiatomites.

(A) (C) @)
Element (%) CeliteNatural
Bumey 266 Skamol
Damolin

91.39 86.9 68-80 74


0.10 0.18 NA 1.o
1.97 3.1 8-10 11
0.48 1.1 5-7 7.O
0.002 NA NA NA
0.04 0.65 1-1.5 2.0
0.5 1 0.4 1 1-3.5 1.o
NA 0.5
0.07 3 o.88 3 2-3 1.5
0.00 0.15 NA NA
4.18 3.8 0.5-3.5 1.o

(A) Burney diatomitefrom Shasta County, CA, USA, extracted for filter-aid production
by Grefco Inc. (BGS
analysis.)
(B) Johns-Manville diatomite paint filler @emmers
& Kranich, 1986).
(C)& (D)Dansk Moler Industriand Skamol-Skarrehenge Moler-vaerk technical literature.

Mineralogy and Petrology Group, British Geological Survey0 NERC 1992


14
. .

Diatomite

Table 2. Physicalproperties of diatomite (BGS data).

(1)> 63 Cun (%I 0.8 1.2 18.2 0 0


63-10
(2) (%) 9.9 5.0 3.3 7.0 24.0
(3) 1 0 - 2 p (%) 68.5 21.7 19.6 88.0 66.5
(4) 2 lun (%I 20.8 72.1 58.9 5.0 9 .o
(5) Graphic mean(w) 4.8 1.5 1.5 5.3 6.8
(9Bulk density (g/cm3) 0.298 0.250 0.245 0.296 0.407
(7) SG 2.0 1 NA 2.26 NA NA
(8) Porosity (%) 85 NA 89 79 NA
(9) Surface area (m2/g) 13.1 59.8 NA 3.4 4.7

(A) Burney diatomite, Shasta County, CA, USA. High purity: extracted by Grefco Inc. for
fiter-&d production.
-
(B) Loma Comastro, diatomite,NE of Liberia, Costa Rica. Impure: 22% clay mineral content plus alunite-
group minerals (Inglethorpe, 1990).
(C) Nan Jo diatomite, Lampang,Thailand. Impure: 3040% clay mineral content plus 12% quartz and 6%
goethite (Inglethorpe,1991).
(D)& (E) show values for samples calcinedat 1100C for 1hour.
(1)-(4) Particle-size distributionby wet sieving and sedimentation.
( 5 ) Mean particle-size of e63 p n fraction.
(6)-(9) Values fordry powdered samples.

Table 3. Brightnessvalues of natural and calcineddiatomites


~ ~~ ~ ~ ~~

602 filter 603filter 605 fiiter 606 filter


Yellow
Yellow-green
Blue-green Blue
Sample (4700 A) (4900 A) (5500 A) (4800 A)

Burney 69.8 69.1 74.2 72.1


Bumey, calcined 66.1 66.0 78.6 73.4
Loma Camastro 74.7 75.6 78.8 78.1
Loma Camastro, 30.2
calcined 32.4 46.0 36.6

Mineralogy and Petrology Group, British Geological Survey0 NERC 7992


15

Diatomite

6. LABORATORYTESTSRELATING TO INDUSTRIAL
APPLICATIONS

6.1 Filtration

as a - a thin bed of
Diatomite filter-aids have two functions: (1) precoat
diatomite used to filter fluids by removing suspended particles,(2)and
as a bodyfeed - diatomite added to the fluid to maintain the porosityof
the filter.A schematic diagram ofan industrial filtration processis
shown in Figure 6.
The Brewing Research Foundation(BRF) Surrey, England, has
developed a modelof filtration characteristics usingpermeability and
mean hydraulic radius as the principal parameters (Reed and
Picksley, 1987; Picksley and Reed, 1989). These two properties control
flowrate and clarity respectively . These are key properties
referred to by manufacturers and consuming industries.An outline of
5.
filtration theory is given in Appendix
Permeability is defined as the ability of a granular materialallowto the
passage of a fluid, andis the property which determines the rate of
flow of a fluid through a filter-aid. Manufacturers and consuming
industries often refer to permeability in terms of flowrate or relative
flowrate. Mean hydraulic radius is the average void size within a filter-
aid andis ameasure of cut-off size- the smallest size of particle that
the filter-aid is able to remove from suspension. In industry this
property is often referredto as clarification ability or filtrate clarity.

6.1 .I Filtration properties

The physical propertiesof diatomite filter-aids are summarised in Table


all the
4. In a preliminary investigation,it is not practical to determine
parameters given in Table4. Permeability and wet cake density will give
a good indication of likely filtration performance. Parameters such as
mean hydraulic radiusand effective void volume are useful theoretical
concepts (Appendix5) but are not essential to a preliminary
investigation of diatomite forfilter aids. Table4 shows that increasing
the particle-sizeof a filter-aid raisesflowmte by increasing
permeability, and lessens clarity by increasing mean hydraulic radius.
Procedures for the determination
of permeability and wet density values
of calcined diatomites are given in Appendix6. Theune & Bellet (1988)
9.03
state that calcined diatomite filter-aids have permeability values
pm* and wet density values (the density of a filter-aid precoat) between
0.35-0.5 gJcm3. The authors suggest that high permeability values are
required for fast flowrates, and that low wet density values are

Mineralogy and Petrology Group, British GeologicalSurvey 0 NERC 1992


16

Diatomite

necessary to provide porosity for the retention


of particles removedfrom
fluid during filtration.
as
Total void volumeis calculated fromSG and wet density values
follows:

Total void volume(% porosity)= [1-(wet density/SG)]* 100/1


Permeability canbe measured with simple experimental apparatus using
Darcys Law:
Permeability (13)[pm2] = p U L * 1012
AP
p = viscosity of water at20 O C
U = superficial velocity= (volumetric flowrate [m3/s] / cross-sectional
area [m*])
AI? = pressure drop across bed
L = depth of bed [m]
Diatomite shouldbe prepared for thesetests using the preparation and
in Appendix 4. During the test only
calcination procedure described
volumetric flowrate(U) and depthof bed (L) are recorded, as the other
parameters are constant. The apparatus usedcany to out permeability
and wet density determinationsis illustrated in Figure 7. Procedures for
particle size measurementof mineral powders are given elsewhere in
this series of manuals.

Mineralogy and Petrology Group, British Geological Survey 0 NERC 1992


17
. ..

Diatomite

diatomite particle

- liquor particle

Liquor + bodyfeed

Precoat

Filtrate M

Glossarv:

Filter septum - a wire mesh or cloth screen upon which precoatis deposited
Precoat - a thin permeable bed of diatomite particles deposited on fiter septum prior to filtration
Filtration - process for removing suspended particles from a liquor
liquor - industrial fluid containing particles in suspension
Body feed - diatomite added to the liquor to maintain flowrate by increasing porosity of the
filter-cake.
Filter-cake - a layer comprised of diatomite and liquor particles which builds up on the ofsurface
the precoat during filtration
Filtrate - clear liquor that has passed
through the precoat
Flowrate - volume of filtrate that passes through precoat with respect
to time
Clarity - amount/or lack of particles present in filtrate

Figure 6. Schematic diagram of an industrial filtrationprocess

Mineralogy and Petrology Group, British Geological Survey0 NERC 1992


18
, .. ...... .. . .~ . , . ..;. . . .. ,.. . ... . ~ - . .. . ,

Diatomite

Table 4. Filtrationproperties of diatomitefilter-aids (BGS experimentaldataandtechnical


literature).

Flowrate Clarity
Mean Wet Total Effective Mean
particle void Measured
void cake hydraulic
permeability radius volume
volume
density size SG
Product m21 [PI [g/cm31 [%I [%I [WI
~~ ~~~ ~

Dicalite 215 0.02 # NA NA NA NA 5.8 2.25


Bumey 0.04 NA 0.42 79 NA 5.3 2.01
Superaid 0.04 # NA 0.352 84 NA 5.9 2.25
FPlW 0.069 0 0.3 0 NA NA 17 0 NA NA
Celite 578 0.07 * NA NA 83 * 27 * 7.1 * NA
FP4 0.20 0 0.5 0 NA NA 25 0 NA NA
Standard Supercel 0.22 0 0.7 0 NA 86 * 35 * 6.8 * NA
speedflow 0.22 # NA 0.368 # 84 NA 7.5 2.25 #I
Hyflo Supercel 1.62 * NA NA 86 * 58 * 10.7 * NA

Nan Jo (ax) 0.02 NA 0.59 73 NA 2.1 3.1 7

0 Reed & Freeman (1991).


* Reed & Picksley (1987).
# Manufacturersdata.

Mineralogy and Petrology Group, British Geological Survey 0 NERC 1992


19

Diatomite

Figure 7. Laboratory filtration apparatus. Components are connected in seriesto a filter-


pump as follows:(1) conical flask, (2) vacuum regulator unit, (3) bleed valve, (4) vacuum
meterand (5) filtration unit.

Mineralogy and Petrology Group, British Geological Survey 0 NERC 1992


20

Diatomite

6.2. Fillers

General characteristicsof fillers that influence usage include


colour
oil absorption
surface wetting and bonding properties
chemicalresistance
strength/iability.
The physical properties of diatomite fillers summarised
are in Table 5;
chemical specifications are discussed in section 5.1. Remmers and
Krannich (1986) cite high oil absorption, high silica content andlow
bulk density as important properties of diatomite fillers for paint. A
procedure for determination of oil absorption by diatomiteis given in
Appendix 7.

Table 5. Physicalpropertyspecifications of diatomitefillers for paintsandplastics.

Celite:
supmoss* White 0.1 NA NA NA NA 120 9-10 1.48 NA 0.7-3.5 NA NA
Silver Frost K 5 * White trace NA NA NA NA 115 9-10 1.48 NA 0.7-3.5 NA NA
White Mist* White trace NA NA NA NA 160 9-10 1.48 NA 0.7-3.5 NA NA
266# Grey 0.5 96 92 NA 16 135 6.5 1.42 0.128 NA NA NA
499# trace
White 82 99 NA 1 105 9.5 1.48 0.136 NA NA NA
28 1# White 1.5 96 68 NA 3 110 9.5 1.48 0.136 NA NA NA

Type 1 diatomite* / 15 70 10 / / 60-100 6.5-10 / / / 1 15


Type 2 diatomite* / 5 75 20 5 / 60-100 6.5-10 / / / 1 1

* Moreland (1987).
#Remmers
I &h i c h (1986).
5 BS 1795 (1976).

Mineralogy and Petrology Group, British Geological Survey0 NERC 1992


21

Diatomite

6.3. Insulation bricks, absorbent powders and


granules
Insulation bricks are produced from a Danish clay-rich diatomite known
as moler which is characterised
by a lowSi02 content and high levels
of Fe2O3 and A1203 compared to other commercial diatomites (Tablel).
The physical specifications for insulation bricks are based on bulk
density, porosity, cold crushing strength and thermal conductivity
(Table 6).
The heat resistant properties (or low thermal conductivity) of diatomite
bricks resultfrom their high porosity (or low bulk density).
The Danish
company Skamol produce seven types of insulation brick (with a
temperature resistanceof 900-950C) classified on the basisof bulk
density; low bulk density bricks have good heat resistance but only
moderate strength whereas high bulk density bricks have better strength
but lower heat resistance. The main usesof these products arein kiln
and furnace applications.

Table 6. Typicalphysicalproperties of diatomiteinsulationbricks.

ROTOL HTpoR(450)

Bulk density (kg/m3) 800 450


Porosity (%) 66 81
Cold crushing strength (kg/cm2) 100 8
Modulus of rupture (kglcm2) 20 NA
Thermal conductivity (kcal/m hr C) 0.17-0.2 1 0.09-0.16
~~ ~

Data source: Skamol-Skarrehenge Moler-vaerk technical literature.


(Thermal conductivity valuesquoted are for temperature range200-80O0C.)

Mineralogy and Petrology Group, British Geological Survey0 NERC 1992


22
,. . .

Diatomite

7. CASE STUDY

7.1 Diatomite, Thailand


A 20 kg sample of diatomite was collected from Nan Jo quarry, Mae
Tha, Lampang Province, Thailand. A laboratory study was planned to
define the chemistry, mineralogy, petrography and physical properties
of the diatomite, examine mineral processing techniques to reduce levels
of mineral impurities, and evaluate the sample as a potential industrial
raw material for filter-aid production (Inglethorpe, 1991).
A flowsheet
summarizing the laboratory investigation ofthis material is shown in
Figure 8.
Nan Jo quarry is situated to the south
of Lampang. Diatomiteis
currently extracted for useby the local paper-making industry. The
geological map ofthis area is the Department of Mineral Resources
(DMR) Changwat Lampang 1:250000 scale sheet. The diatomite
sequence is partof the MaeMo Group which consistsof freshwater
sandstone, shale, carbonaceous shale and lignite beds of
Miocene-Pliocene age. The sample examined in this study was collected
from the basalbed of the 10 m high north face of the quarry.
Results indicated thatthe Nan Jo diatomite contains30-40% clay
minerals, 12% quartz and6% goethite. These impuritiesare probablyof
detrital origin. The sample was depositedin a relatively high-energy
freshwater environment. Attrition during sediment transport reduced
whole diatoms to 10-1 pm size fragments. The sample has aSi02 low
and high A 1 2 0 3 and Fe2O3 content compared to diatomites utilised by
industry. Mineral processing trials were not effective
in upgrading the
sample.
The filtration performance of the Nan Jo diatomite is poor. Calcined
samples are of low permeability (0.02 prnz), high filter-cake density
(0.57-0.61 g/cm3) and small average particle-size (2.5-3.7 pm). The
iron oxide content ofthis material is above levels acceptable for the
processing of foodstuffs. The sampleis therefore unlikely tobe suitable
for use in filter-aid applications. However, the chemistry and
mineralogy of the Nan Jo sample aresimilar to commercially-mined
diatomites usedin the production of insulation bricks.

Mineralogy and Petrology Group, British Geological Survey 0 NERC 1992


23

Diatomite

PETROGRAPHY:

- Optical
II

microscopy
I(II
( ) ............................................ ...... ... . ..
..............

i.i:. Polished'
ii;;~insectio"i,:i:i
.. .....................
. ... .... ... ... ... .. . . . .. ... ... .. .
.:<
(T)
(>
. ...
.....
......
: ....:
. .
,-Sample,,.
.... ... .... .. .. .. . . .. ... .. .. .. .....
...
. . . . .
:.: : . .: .. ... ' .. .: . . .. : .
.. . . .. . . . .. .. . .. ... .. .:::
. .
'
: j:j
. .
. ...
. . .......... ............. ....... .... .......... .. ..... ......... . .
. .. .... .. ... ... ......... .... .. .... ......... .
.................
.. ...... . . . . . .;:. ...Rock-chip ;.::i.i;
.. . .. .. . .. .. . .. .. . .. .. . ..
':
.............. .... .... .. .... ... ... ..... ......... .
.... ... .. .... .. ........... ...... ...... ... . .
.. ... .. . .. . .. ... ... .. . .. . .. . ..
I- .
I I
...............

PETROGRAPHY:

- secondary electron mode

-Electron probe micro-analysis scanning electron microscopy

(EPMA) element maps Crushed to


(SEW

.
Dispersed Sub-sampled
toMilled
in deionised
I I
r
by
water rime-splitting

e2 pm fraction Gently
separated & disaggregated
dried to c63 pm (,,,,powderI:J
.. .. .. .. .. .. .. .. .. .. ....... .. .. .
- Whole-rock major-element

chemistry
Calcined - Whole-rock X-ray diffraction
at 1 100C
for 1 hour (XRD) analysis

MINERALOGY:
I

I
-Clay fraction
I
I
XRD analysis
I
PHYSICAL PROPERTY TESTS:

- Permeability
- Wet-cake densiiy
- Total void volume
- SG
- Bulk density

- Particle-size analysis

Figure 8. Flowsheet showing laboratory proceduresusedto


investigate the Nan Jo diatomite.

Mineralogy and Petrology Group, British GeologicalSurvey 0 NERC 1992


24

Diatomite

8. CONCLUSIONS
Diatomite is a pale coloured light-weight rock composed principally of
the silica microfossils of aquatic unicellular algae
known as diatoms.Its
main uses are as a filter-aid to remove fine particles
from industrial
in plastics and paints. Diatomiteis also added to a
fluids, and as a filler
range of insulation products to improve their thermal resistance.
The type of silica presentin diatomite is apoorly-ordered opalA type
which is recognised from a broad X-ray diffraction at 4.0581. Pure
peak
diatomite is characterised by high silica content(>85%), high porosity
(>80%),low SG (2.0-2.1), low bulk density (0.2-0.4 9/cm3), and fine-
particle size (typically63-2 pm).
Diatomite used in industrial filtration ofishigh chemical puritywith low
calcium, low iron and low soluble salts content. The key property
controlling filtration performance is permeability (porosity, wet cake
density and particle-size are also important filtration characteristics).
Diatomite fillers for paints and plastics are also chemicallyaspure,
elements such as iron adversely affect colour. Key specifications for
good whiteness, highoil absorption and a fine-
filler applications are
grained, narrow particle-size distribution. Danish moler diatomite is
used in insulation bricks and absorbent powders and granules. Its high
A1203 and Fez03 content precludes its use in filter-aids, paints and
plastics.

Mineralogy and Petrology Group, British Geological Survey0 NERC 1992


25

Diatomite

REFERENCES
Abella, S E B (1988) The effects of Mt. Manzama ashfall on the
Limml. Oceanogr.
planktonic diatom community of Lake Washington.
33(6), 1376-1385.
Anon. (1987) Diatomite.Ind. Miner. 236, 22-39.
Brazier, M D (1990) Microfossils. George Allen& Unwin, London: 39-
44.
BS 1795: 1976. for Extendersfor Paints.
British Standard Specifications
Brit. Standards Inst. Publ.
Burnett, J L (1991) Diatoms- the forageof the sea. Calif. Geol. 44(4),
75-81
Conger, P S (1942) Accumulationof diatomaceous deposits.J . Sed.
Petrol. 12(2), 55-66.
Ind. Miner. 279,50-
Griffiths, J (1990) Denmarks industrial minerals.
55.
Haben, P W (1992) Industrial Minerals Handybook.Metal Bulletin
PLC, London: p 27.
Inglethorpe, S D J (1990) Mineralogical composition and filtration
properties of a sample of diatomite from Loma Camastro, Costa Rica.
Rep. Brit. Geol. Sum. WG/90/13R.
from Nan Jo
Inglethorpe, S D J (1991) Evaluation of a diatomite sample
quarry, Lampang Province, Thailand.Rep. Brit. Geol. Sum.
WG/91/32R.
Jones, J B & Segnitt, E R (1971) The natureof opal: (i) Nomenclature
and Classification. J . Geol. SOC.of Austr. 18 (l),57-68.
Moreland (1987) in Handbook of Fillersfor Plastics. (Katz, H S &
Milewski, J V Eds.) Van Norstrand ReinholdCo., New York.
Lefond, S J (1983)Industrial Mineralsand Rocks (5th Edn.). AIMMPE
publication.
Mathers, S J (1989) CostaKcan diatomite: a review of existing
knowledge and future potential.Rev. Geol. Amer. Central. 10,3-17.
Picksley, M & Reed, R J R (1989) Characteristicsof Filter-aids. J. Inst.
Brewing. 95(3). 169-179.

Mineraloav and Petroloav Grow. British Geoloaical Survev 0 NERC 1992


26

Diatomite

Reed, RJ R & Freeman, G J (1991) Filter-aid fundamentals- selection


J. Znst.
of clarification characteristicsby use of mean hydraulic radius.
Brewing. In press.
Reed, R J R & Picksley, M A (1987) The determinationof the true
filtration characteristicsof diatomaceous earth.J. American Sociew
Brewing Chemists. 45 (2), 48-53.
Remmers, T E& Krannich, M A (1986) Pigment Handbook: Vol. 1
Properties and Economics, 2nd Edn.
Lewis, P A(4). John Wiley&
Sons.
Stager, J C(1988) Environmental changes atLake Cheshi, Zambia
since 40 000 years B.P. Quat. Research.29,54-65.
Talliaferro, N L (1933) The relationof volcanism to diatomaceousand
associated siliceous sediments.Geological Science[Univ Calif. Publ.].
23, 1-55.
Taylor, G C (198 1) Californias diatomite industry.Calif.Geol.
34(9),183-192.
Theme, C & Bellet, J (1988) Aptitude of diatomaceous orefor filter aid
processing Proc. 8th Znd. Min. Con$ 223-229.

Mineralogy and PetrologyGroup, British Geological Survey 0 NERC 7 992


27

Diatomite

Appendix 1: Preparation of diatomitefor examination


by opticalmicroscope

Use this technique to positively identify the presence of diatoms in a


sample. Stages5 to 8 are optional.
CAUTION: Handle CC4 with care. Stages5-8 should be carried out
in a fume cupboard,and safety glasses and protective gloves should
also be worn.

Apparatus and chemicals


dishPetri 5 litre
bucket
Plastic
Hard
bristled
scrubbing
brush
Small
glass
funnel
45 pm/325 mesh sieve (20 cm diameter) Fast filter paper
rod Stirring beaker Glass
Small stoppered vial/container
Carbon tetrachloride(CC4)

Method
1. Immerse samplein bucket of water and gently scrub using hard-
bristled scrubbing brush to liberate microfossils.
2. S t r a h resulting suspension through 45
a pm (325 mesh) sieve.
3. Transfer >45 pm residue into an evaporatingdish and dry at
55OC.
5. Place dried sample residue in a beaker and add carbon
tetrachloride (CC4, SG 1.58) at 2-3 times the sample volume.
6. Stir using a cleandry glass rod. Diatoms should float to the
surface if present.
7. and to air-dry.
Decant float into a fiiter-lined funnel allow
8. Repeat stages 5-7 if necessary.
9. Sprinkle a thin layer of dried diatoms onto a petri dish backed
with black paper.
10. a binocular microscope.
Illuminate and examine using

Survey 0 NERC 1992


Mineralogy and Petrology Group, British Geological
28

Diatomite

Appendix 2: Measurement of specificgravity

This procedure is used to determine the specific gravity of small mineral


fragments or powdered minerals.

Apparatus/materials
Balance (0.01g readability)
Drying oven (105C)
Pycnometer bottlewith stopper
Aluminium dish ors m a l l evaporating basin
Distilled water

Method
1. Weigh out approximately 10g of powdered sample into an
in 105OC oven
aluminium dish/small evaporating basin and place
overnight.
2. The following morning, place a clean pycnometer bottle
with
stopper in oven at 105C for one hour.
3. Accurately weigh the pycnometer bottle with stopper to the
nearest 0.01 g. Note reading as A = ..... g.
4. Remove stopper from pycnometer bottle and add approximately
log of dry mineral powder. Replace stopper and weigh bottle
0.0 1 g. Note reading as B = .... g.
plus contents to the nearest
5. Remove stopper and carefully add distilled water to the bottle to
cover sample until pycnometer bottle is three quartersfull.
Gently agitate bottle(in an ultrasonic bath,if available).
Continue agitation until sample is thoroughly wetted all and
trapped air has been dispelled.
6. After agitation add more water to the pycnometer bottle until
water levelis justbelow the brim. Replace stopper until both the
in stopper are full
bottle and fine capillary opening of water.
7. Thoroughly dry outside of pycnometer bottle and weigh bottle
plus contents. Note reading as C= .... g.

8. Thoroughly rinse out pycnometer bottle and then repeat steps 5-


7 but with water only filling the bottle. Note reading Das= ....
g*

Mineralogy and Petrology Group, British Geological Survey 0 NERC 1992


29
. .

Diatomite

Appendix 2 (continued)

Calculation
Specific Gravity (SG) = B-A
(B+D)-(A+C)

Mineralogy and Petrology Group, British Geological Survey0 NERC 1992


30

Diatomite

Appendix 3: Measurement of bulk density


This methodis used to determine a nominal bulk density value
for
powdered minerals.

Apparatus/materials
Balance (0.01 g readability)
Drying oven(105OC)
Aluminium dish orsmall evaporating basin
Measuring cylinder(10/20/50 ml)

Method
1. Weigh out in excess of 10 g powdered sample into an aluminium
dish/small evaporating basin and place in105OC
a oven
overnight.
2. Placeweighingboatonbalanceandtareweight.Weighout
10.00 g (+ 0.01 g) of sample.
3. Transfersamplefromweighingboattomeasuringcylinder (10,
20, or 50 ml size as appropriate).
4. Gentlytampmeasuringcylinderbygentlyknockingbaseof
this action 10 times. Record
cylinder against flat surface. Repeat
volume of sample asV = .... ml.

Calculation
Bulk density (BD) [g/cm3] = 1O[g]/V [ d l

Mineralogy and Petrology Group, British Geological Survey 0 NERC 7992


31

Diatomite

Appendix 4: Sample preparation and calcination


.. ..I

. ..
This is a procedure for the preparation
of diatomite powders and
1.

calcined diatomite powders for physical property testing.

Apparatus
Dust
masks
Balance (0.1
readability)
g
Dryingoven (55C) Laboratory
mufflefurnace
Jaw crusher
Roller mill (or large automatic/manual mortar and pestle)
63 pm (240 BS mesh size)20 cm diameter metal sieve,
(preferably usedin conjunction with vibratory or vacuum-assisted
sieving apparatus)
Furnace crucibles, tongs, heat-resistant gloves, heat-resistant face shield

Method
1. Dry a portion of the asreceived sample in a 55C oven overnight.
2. Coarsely crush to 4mm diameter in size using a small jaw-
crusher if available. (Note:this coarsely-crushed diatomite may
be used as stock material for bulk chemical and XRD analyses.)
Sub-sample by riffle splitting or coning-and-quartering.
4. Gentlygrindthecoarsely-crushedsub-sample,preferablyusing
- a roller mill at a narrow gap setting. Alternatively, gently grind
for approximately5 minutes using a pestle and mortar.
5. Screengroundsampleona 63 pm aperture metal sieve.
Vibratory or vacuum-assisted sieves are most effective. Weigh
c63 pm sieve undersize obtained and transfer to sample bag.
6. Re-grindany >63 pmsieveoversizebyrepeatingsteps 4-5.
7. The <63 pm sieve undersize material obtained can be used as
powdered diatomitein physical property tests.
63 a
Note: pure diatomites are soft and friable and easily pass through
pm sieve. However, diatomites containing clay minerals or iron oxides
of these sample
are often more cemented, and a significant proportion
4-5
will remainin the >63 pm fraction even after repeating stages
several times.In these cases, the>63 pm material remaining should be
weighed and retained for reference.

Mineralogy and Petrology Group, British Geological Survey0 NERC 1992


32

Diatomite

Appendix 4 (continued)

Calcination method
1. Re-heat laboratorymufflefurnacetollOOC.
2. Weighoutapproximately 100 g ofpowdereddiatomiteand
g. Transfer sample toa furnace
record weight to nearest 0.1
crucible.
3. Place crucible in furnaceandcalcinesamplefor 1 hour.
4. After 1hour, remove crucible from furnace, place on heat
resistant surface andallow to cool.
5. After cooling, record weight of sample to nearest 0.1 g.
6. Repeatsteps4-6 of samplepreparationmethodtoobtain
powdered calcined diatomite.

Caution: Dust masks shouldbe worn throughout both procedures.


Protective heat-resistant clothing (lab coat, gloves, face shield) should
be worn at all stages of handling material to andfrom furnace.

Mineralogy and Petrology Group, British Geological Survey 0 NERC 1992


33

Diatomite

Appendix 5: Filtration theory


Diatomite porosity (total void volume) two has separate components:
(1) the internal porosityof particles, and(2) the external porosity
between particles (effective porosity). Permeability be can
calculated
theoretically from total void volume(et) as follows (Reed and Picksley,
1987):

o= (Ed3
5(6/d)2 (1 -
d = mean particlediameter
Permeability values obtained from equation1 are far higher than
by modifying this equation closer agreementis
experimental values, but
obtained:

De =
5(6/d$ (I - &e)
de = effective mean particle diameter

= [(l-Ee)/(l - &dl113
In equation 2, effective permeability(Be) is calculated using only
external porosity(E, - effective void volume).E, can be determined
experimentally (6is calculated using equation3). The model definedby
equations 2-3 suggests thatthe flowrate of diatomite filter-aidsis
primarily controlledby their external porosity, and that flow through the
internal porosityof the filter-aid is neghgible. Because of the positive
correlation between% external porosity and particle-size, filter-aids with
a coarse particle size distribution should have higher permeability values
than thosewith a f i e particle-size distribution.This is confirmed by
experimental findings.
Mean hydraulic radius(m) can be calculated from effective void volume
and effective permeability using the following equation:

Mineralogy and Petrology Group, British Geological Survey 0 NERC 1992


34
1 .. .

Diatomite

Appendix 6: Measurement of permeability and wet


cake density

This test is used to assess the filtration performance of calcined


diatomite. Samples shouldbe prepared using the procedure given in
Appendix 4. Permeability and wet cake density values should be
compared with data quoted by Theune and Bellet (1988) (see Section
6.2.1).

Apparatus
Balance (0.1 g readability)
Vacuum
gauge
regulator
(optional)
Vacuum
Filter-pump
5-10 m of Tygon/rubber vacuum tubing l O O m l glass beaker
rulerStainless
steel rod
stirring
Glass
Fastfilterdiscs(orfastfilterpaper)Stopwatch
11Nalgene filtration unit
(or sintered glass funnel + 11measuring cylinder)

Method
1. 0:l g and tare.
Place beaker on balance. Record weight to within

2. Add 10g (k 0.1 g) of calcined powdered diatomiteto beakerand


record weight.
3. While constantly stirring, add the minimum amount of water for
the sample toflow smoothly.
4. Turn on the filter-pump and place filter disc/paper
on perforated
septum/sintered glass of filter unit/funnel and moisten.
5. Stir diatomite slurry and transfer to filter unit/fimnel
form
to a
smooth even cakeon surface.
6. Dry beaker in oven at55. After drylng place on balance and
record weight of remaining diatomite.

7. 15-20 Hg)
Set vacuum pressure to a constant value (typically
an air-
for duration of test, using either a vacuum regulator or
bleed valve.
8. Simultaneously start stopwatch and add water to filter
unit/hnnel, and record volumeof filtrate at1 minute intervals
between 0-15 minutes.

Mineralogy and Petrology Group, British Geological Survey 0 NERC 1992


35
.._

Diatomite

Appendix 6 (continued)

9. Stoprecordingvolume of filtrate after 15 minute reading


10. Allow remaining water to drain through apparatus until surface
of diatomite cakeis dry.
11. Record depth of diatomite cake to within 0.5 mm using the steel
ruler (average several depth readingsif necessary).

Calculations

Permeability
6.1.):
Permeability is calculated using Darcys Law (See section
Permeability (f3)[pm2]
= p u L * 1012
AP
p = viscosity of water at 20 OC = 0.0010019 [kg/m/s]
U = superficial velocity= (volumetric flowrate [m3/s]/
cross-sectional area [m2])
volumetric flowrate [m3/s]= volume of filtrate after 15 minutes
[m3/s]/ (time= 900 [SI)
cross-sectional area= n; (0.5d)2 [m2]
AP = pressure drop across bed (15 inches Hg = 50663 [Nm3])
L = depth of diatomite cake [ml\
Wet-cake density
1. Subtract weight recordedin step 7 from that recorded in step2.
This value equals thedry weight of diatomite usedin the test (m).
2. Wet density of the diatomitew) can the be calculated as follows:
WD [g/cm3]= massof diatomite / volume of diatomite cake
-
- m
n; (0.5d)21

m = dry weight of diatomite [g]


d = diameter of filter [cm]
1= depth of diatomite cake [cm]

Survey 0 NERC 7992


Mineralogy and Petrology Group, British Geological
36

Diatomite

Appendix 7: Determination of oil absorption values


This methodis used for testing the oil absorption
of pigments for paints
BS 3483: Part B7
(adapted from British Standards Institute method
British Standard method for testing pigments for paints).

Apparatusheagents
Balance (0.1g readability)
Refined linseed oil
Ground glass plate (typically 300 mm by 400 mm)
Small palette knifewith tapered steel blade (typically140-150long by
20-25 mm wide)
10 ml capacity burette,0.1 ml graduations

Method
1. Weigh out approximatelyl g of dry powdered sample and record
value to nearest0. lg. Note reading asM = ..... g. Fill burette to
zero meniscus with linseed oil.
2. Transfer sample to glass plate.
3. Add linseed oil slowly(4-5 drops at a time) from the burette. After
each additionrub the oil into the sample using the palette
Me.
Initially, oil added will be absorbed rapidly.
4. Continue additionsof oil as in step 3 until a stageis reached when
conglomeratesof oil and sampleare formed,i.e. prolonged
mixing is required for absorptionof oil.
5. From this point, continue to add oil one drop
at a time and follow
each addition by thoroughly rubbing with the palette knife.
6. Cease the addition of oil when
a pasteof smooth consistency has
formed. This paste should just spread without cracking or
crumbling and should only loosely adhere to glass plate.
7. Read burette to0.1 ml to record volumeof oil added. Note value
as V = .... ml.
8. be 20-25 minutes.
The time takento complete the operation should
The operator should mix theoil and samplewith maximum effort.
If necessary, determine the oil absorption value
of a known
reference sample for comparison.

Mineralogy and Petrology Group, British Geological Survey 0 NERC 1992


37

Diatomite

Appendix 7 (continued)

Calculation of oil absorption value

Mass/mass basis:
mass oil absorption per lOOg of sample [g/lOOg] = 93V/M

Volume/mass basis:
volume oil absorption value per lOOg of sample [ml/lOOg] = lOOV/M

ml or g [/lOOg]
Quote results to the nearest

Mineralogy and PetrologyGroup, British GeologicalSurvey 0 NERC 1992

You might also like