Designation: D 5891 – 02

Standard Test Method for

Fluid Loss of Clay Component of Geosynthetic Clay Liners1
This standard is issued under the fixed designation D 5891; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope API RP 131, Recommended Practice for Laboratory Testing

1.1 This test method covers an index method that enables of Drilling Fluids7
the evaluation of fluid loss properties of a clay mineral film API Specification 13A, 4, 14th ed. for Drilling Fluid Mate-
deposited on a filter paper from a 6 % solids slurry of clay rials7
mineral at 100-psi (-kPa) pressure as a measure of its useful- 3. Terminology
ness for permeability or hydraulic conductivity reduction in
geosynthetic clay liners (GCL). 3.1 Definitions— For definitions of terms used in this test
1.2 This test method is adapted from American Petroleum method, refer to API Standards and ASTM definitions for GCL
Institute drilling fluid specifications for bentonite. products.
1.3 Powdered clay mineral is tested as produced; granular 4. Significance and Use
clay mineral should be ground to 100 % passing a 100 mesh
U.S. Standard Sieve with a minimum of 65 % passing a 200 4.1 Clay mineral is the functional component of GCL that
mesh U.S. Standard Sieve with the whole ground product used reduces the hydraulic conductivity of industrial waste or
for testing. ground water through the liner.
1.4 The values stated in SI units are to be regarded as the 4.2 Clay mineral quality can vary significantly and effect the
standard. The values given in parentheses are for information hydraulic conductivity of the GCL composite. This test method
only. evaluates a significant property of clay mineral that relates to
1.5 This standard does not purport to address all of the performance.
safety concerns, if any, associated with its use. It is the 5. Apparatus
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 5.1 Laboratory Balance, 100 g capacity, 60.01-g accuracy
bility of regulatory limitations prior to use.2 and precision.
5.2 Weighing Paper, or small weighing dish.
2. Referenced Documents 5.3 Graduated Cylinder, 500 6 5-mL graduated TD (to
2.1 ASTM Standards: deliver) with 10-mL subdivisions, Class A volumetrically
D 1193 Specification for Reagent Water3 calibrated; 10 6 0.1-mL graduated cylinder, graduated TC (to
E 1 Specification for Thermometers4 contain) with 0.1-mL subdivisions.
E 11 Specification for Wire-Cloth Sieves for Testing Pur- 5.4 U.S. Standard Sieve, 100 mesh, 200 mesh, and auto-
poses5 mated sieve shaker.
E 691 Practice for Conducting an Interlaboratory Study to 5.5 Mortar and Pestle or Laboratory Hammer Mill, for
Determine the Precision of a Test Method5 grinding clay mineral to required particle sizing.
E 725 Test Method of Sampling Granular Carriers and 5.6 ASTM Calibration Immersion Thermometer, 0 to 105 6
Granular Pesticides6 0.5°C (see Specification E 1).
2.2 API Standards: 5.7 Mixer—11 000 6 300 rpm under load with single
sine-wave impeller approximately 25 mm (1.0 in.) in diameter8
(mounted flash side up). The impeller shall be replaced when it
1
This test method is under the jurisdiction of ASTM Committee D35 on weighs a minimum of 5.1 g, from an original weight of about
Geosynthetics and is the direct responsibility of Subcommittee D35.04 on Geosyn- 5.5 g. New blades will be weighed prior to installation in order
thetic Clay Liners. to ensure conformance to manufacturing criteria. Mixer speed
Current edition approved June 10, 2002. Published September 2002. Originally
published as D 5891–95. Last previous edition D 5891–01.
2
When bentonite is removed from a GCL product for testing, it may include
7
adhesives that can influence test results. Available from American Petroleum Institute, 1801 K St. N.W., Washington,
3
Annual Book of ASTM Standards, Vol 11.01. DC 20226.
4 8
Annual Book of ASTM Standards, Vol 14.03. For example, Sterling Multimixer Model 9B with 9B29X impeller blades
5
Annual Book of ASTM Standards, Vol 14.02. available from Fann Instrument Co., P.O. Box 4350, Houston, TX 77210, has been
6
Annual Book of ASTM Standards, Vol 04.07. found suitable for this purpose.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 D 5891 – 02
under sample loading shall be determined and documented 6.2 Specification D 1193 for reagent water, Type I, II, or III.
once every 90 days unless the manufacturer has documented
objective evidence to extend calibration time. 7. Hazards
7.1 Safety Precautions—Establish appropriate safety and
NOTE 1—Sterling Multimixer Model 9B with 9B29X impeller blades or
equivalent may be obtained from the suppliers given in Footnote 9. health practices for high-pressure equipment prior to use.
5.8 Mixing Container—Approximate dimensions are 180 8. Sampling and Selection
mm (7 in.) deep, 97-mm (313⁄16-in.) inner diameter at top, and 8.1 Conduct the sampling in accordance with Test Method
70-mm (23⁄4-in.) inner diameter at bottom.9 E 725.
NOTE 2—Mixing containers or equivalent may be obtained from the
suppliers given in Footnote 8. 9. Procedure
5.9 Timers, 30 min, two interval, mechanical or electrical, 9.1 Grind the clay mineral sample to greater than 100 %
precision 60.1 min. passing a 100 mesh U.S. Standard Sieve, and a minimum of
5.10 Spatula, flat blade, to dislodge clay mineral clumps 65 % passing a 200-mesh U.S. Standard Sieve with a mortar
adhering to the mixing container walls. and pestle or laboratory hammer mill as required.
5.11 Covered or Sealed Container, of 400 to 600-mL 9.2 Weigh 22.50 6 0.01 g of the whole composite of finely
capacity. ground clay mineral with “as received” moisture, typically 5 to
5.12 Ambient Temperature/Low-Pressure Filter Press, con- 10 %, onto a weighing paper. If bentonite is removed from a
forming to API RP 13B-1, Section 3.2. This filter press consists GCL product, the bentonite would be dried to less than 10 %
mainly of a cylindrical cell having an inside diameter of 76.2 moisture prior to weighing.
mm (3 in.) and a height of at least 64.0 mm (2.5 in.). This 9.3 Measure 350 6 5 mL of reagent water with the 500- mL
chamber is made of materials resistant to strongly alkaline graduated cylinder and added to the mixing cup. Place the cup
solutions, and is so fitted that a pressure medium can be on the mixer, and add the clay mineral slowly over approxi-
conveniently admitted into and bled from the top. Arrangement mately 30 s.
is also such that a sheet of 90-mm filter paper can be placed in 9.4 After stirring for 5 6 0.5 min, remove the container
the bottom of the chamber just above a suitable support. The from mixer, and scrape its sides with the spatula to dislodge
filtration area is 4580 6 60 mm2 (7.1 6 0.1 in.2). Below the any clay clinging to the container wall. Ensure that all of the
support is a drain tube for discharging the filtrate into a dislodged clay mineral clinging to the spatula is incorporated
graduated cylinder. Sealing is accomplished with gaskets, and into the suspension.
the entire assembly supported by a stand. A mini-press or 9.5 Replace the container on the mixer, and continue to stir
half-area press does not directly correlate with the results for a cumulative total stirring time of 20 6 0.1 min. The
obtained when using the above described standard-sized press. container may need to be removed from the mixer and the sides
Pressure can be applied with any nonhazardous fluid medium, scraped to dislodge any clay clinging to container walls after
either gas or liquid. Presses are equipped with pressure another 5 or 10 min of stirring.
regulators and can be obtained with portable pressure cylin- 9.6 Age the clay mineral suspension for a minimum of 16 h
ders, midget pressure cartridges, or means of utilizing hydrau- in a sealed or covered container at ambient temperature.
lic pressure. Record the initial temperature, final temperature, and actual
hydration aging time.
NOTE 3—Ambient temperature/low-pressure filter press conforming to 9.7 After aging the clay mineral suspension, shake vigor-
API RP 13B-1, Section 3.2, or equivalent, may be obtained from the ously to break its gel strength, and then pour the suspension
suppliers given in Footnote 9.
into the mixer container. Stir the suspension on the mixer for 5
5.13 Filter Paper, 90-mm, very dense, hardened with 6 0.5 min to completely disperse the clay mineral slurry.
smooth lint-free surface,10 must be used. These papers have 9.8 Assemble the dry filter cell with filter paper and gaskets,
high wet strength permitting application of high pressure and immediately after remixing the clay mineral slurry, pour it
during filtration. They also have good resistance to alkalies and into the filter cell and complete assembly of the filter cell. Place
acids. the filter cell in the filter frame and close the relief valve. Place
a 10 mL graduated cylinder under the filter cell drain tube.
6. Reagents 9.9 Set one timer for 7.5 6 0.1 min and the second timer for
6.1 Purity of Reagents—Unless otherwise indicated, refer- 30 6 0.1 min. Start both timers and adjust pressure on the fluid
ences to water shall be understood to mean reagent water loss cell to 100 6 2 psi. Starting the timers and adding 100 psi
conforming to Specification D 1193, Type I, II, or III. Such pressure should be completed in less than 15 s. Supply pressure
water is best prepared by distillation or the passage of tap water by compressed air, nitrogen, helium, or carbon dioxide.
through an ion-exchange resin. 9.10 At 7.5 6 0.1 min on the first timer, remove the
graduated cylinder and any adhering liquid on the drain tube,
and discard. Immediately place a clean dry 10-mL graduated
9
For example, Hamilton Beach Mixer Cup No. M110-D, or equivalent, has been cylinder under the drain tube, and collect the fluid for 22.5 6
found suitable for this purpose. Mixing containers supplied by Fann Instrument Co.,
P.O. Box 4350, Houston, TX 77210.
0.1 min to the end of the second timer. This corrects the fluid
10
For example, Whatman No. 50, S & S No. 576, or equivalent, have been found loss value for any initial unpredictable spurt loss from the fluid
suitable for this purpose. loss cell. Remove the graduated cylinder after the second time

2
 D 5891 – 02
interval and record the volume of fluid collected. clay mineral samples were distributed to seven laboratories.
Three sets of test results were generated for each sample by
10. Calculation each of the laboratories.
10.1 Calculate the fluid loss in millilitres using Eq 1: 12.2 Test Results—The precision information is given in
Fluid loss volume 5 2~mL filtrate volume for last 22.5 min. interval! mL Table 1. The average fluid loss values ranged from 9 to 22 for
(1)

11. Report TABLE 1 Test Results

Statistic ILS Range
11.1 Report the following information:
11.1.1 Source of clay mineral, including sample identifica- Within laboratory repeatability limit, CV %r 1.8 to 4.7 %
Between laboratory reproducibility limit, CV %R 6 to 18 %
tion or lot number, 95 % confidence limit 5 to 13 %
11.1.2 Method of sampling used, Within laboratory repeatability, 2.8 CV %r
11.1.3 ASTM Test Method number used to perform the test, 95 % confidence limit 11.8 to 51 %
Between laboratory reproducibility, 2.8 CV %R
11.1.4 Any modifications to the test method or unusual
observations which may effect the test results,
11.1.5 Calculated fluid loss as millilitres to the nearest 0.1
mL, and the seven clay mineral samples tested. However, since the
11.1.6 Temperature of the slurry at the start and completion statistics were not related to the magnitude of the test result, the
of the test to the nearest 0.5°C. precision values have been presented in terms of coefficients of
varaiation, CV %.
12. Precision and Bias 12.3 Bias—The procedure in Test Method D 5891 for mea-
12.1 Interlaboratory Test Program—An interlaboratory suring the fluid loss value of the clay mineral component of
study of the test method was run in 1999. The design of the geosynthetic clay liners has no bias because the values of swell
experiment, similar to that of Practice E 691. Seven different index can be defined only in terms of this test method.

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