Designation: D5891/D5891M − 02 (Reapproved 2016)´1

Standard Test Method for

Fluid Loss of Clay Component of Geosynthetic Clay Liners1
This standard is issued under the fixed designation D5891/D5891M; 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 (´) indicates an editorial change since the last revision or reapproval.

ε1 NOTE—Designation was changed to dual, units statement in 1.4 and units, where applicable, were corrected editorially
in January 2016.

1. Scope E1 Specification for ASTM Liquid-in-Glass Thermometers

1.1 This test method covers an index method that enables E691 Practice for Conducting an Interlaboratory Study to
the evaluation of fluid loss properties of a clay mineral film Determine the Precision of a Test Method
deposited on a filter paper from a 6 % solids slurry of clay E725 Test Method for Sampling Granular Carriers and
mineral at 100-psi (-kPa) pressure as a measure of its useful- Granular Pesticides
ness for permeability or hydraulic conductivity reduction in 2.2 API Standards:4
geosynthetic clay liners (GCL). API RP 131, Recommended Practice for Laboratory Testing
of Drilling Fluids
1.2 This test method is adapted from American Petroleum
Institute drilling fluid specifications for bentonite.
3. Terminology
1.3 Powdered clay mineral is tested as produced; granular
3.1 Definitions—For definitions of terms used in this test
clay mineral should be ground to 100 % passing a 100 mesh
method, refer to API Standards and ASTM definitions for GCL
U.S. Standard Sieve with a minimum of 65 % passing a 200
products.
mesh U.S. Standard Sieve with the whole ground product used
for testing.
4. Significance and Use
1.4 The values stated in either SI units or inch-pound units
4.1 Clay mineral is the functional component of GCL that
are to be regarded separately as standard. The values stated in
reduces the hydraulic conductivity of industrial waste or
each system may not be exact equivalents; therefore, each
ground water through the liner.
system shall be used independently of the other. Combining
values from the two systems may result in non-conformance 4.2 Clay mineral quality can vary significantly and effect the
with the standard. hydraulic conductivity of the GCL composite. This test method
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
responsibility of the user of this standard to establish appro-
5. Apparatus
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.2 5.1 Laboratory Balance, 100 g capacity, 60.01-g accuracy
and precision.
2. Referenced Documents
5.2 Weighing Paper, or small weighing dish.
2.1 ASTM Standards:3
5.3 Graduated Cylinder, 500 6 5-mL graduated TD (to
D1193 Specification for Reagent Water
deliver) with 10-mL subdivisions, Class A volumetrically
calibrated; 10 6 0.1-mL graduated cylinder, graduated TC (to
1
This test method is under the jurisdiction of ASTM Committee D35 on contain) with 0.1-mL subdivisions.
Geosynthetics and is the direct responsibility of Subcommittee D35.04 on Geosyn-
thetic Clay Liners. 5.4 U.S. Standard Sieve, 100 mesh, 200 mesh, and auto-
Current edition approved Jan. 1, 2016. Published January 2016. Originally mated sieve shaker.
approved in 1995. Last previous edition approved in 2009 as D5891 – 02(2009).
DOI: 10.1520/D5891_D5891M-02R16E01. 5.5 Mortar and Pestle or Laboratory Hammer Mill, for
2
When bentonite is removed from a GCL product for testing, it may include grinding clay mineral to required particle sizing.
adhesives that can influence test results.
3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
4
Standards volume information, refer to the standard’s Document Summary page on Available from American Petroleum Institute (API), 1220 L. St., NW,
the ASTM website. Washington, DC 20005-4070, http://www.api.org.

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

1
 D5891/D5891M − 02 (2016)´1
5.6 ASTM Calibration Immersion Thermometer, 0 to 105 6 5.13 Filter Paper, 90-mm, very dense, hardened with
0.5°C (see Specification E1). smooth lint-free surface, must be used.7 These papers have
high wet strength permitting application of high pressure
5.7 Mixer—11 000 6 300 rpm under load with single
during filtration. They also have good resistance to alkalies and
sine-wave impeller approximately 25 mm [1.0 in.] in diameter acids.
(mounted flash side up).5 The impeller shall be replaced when
it weighs a minimum of 5.1 g, from an original weight of about 6. Reagents
5.5 g. New blades will be weighed prior to installation in order
6.1 Purity of Reagents—Unless otherwise indicated, refer-
to ensure conformance to manufacturing criteria. Mixer speed
ences to water shall be understood to mean reagent water
under sample loading shall be determined and documented
conforming to Specification D1193, Type I, II, or III. Such
once every 90 days unless the manufacturer has documented
water is best prepared by distillation or the passage of tap water
objective evidence to extend calibration time.
through an ion-exchange resin.
NOTE 1—Sterling Multimixer Model 9B with 9B29X impeller blades or 6.2 Specification D1193 for reagent water, Type I, II, or III.
equivalent may be obtained from the suppliers given in Footnote 6.
5.8 Mixing Container—Approximate dimensions are 7. Hazards
180 mm [7 in.] deep, 97-mm [313⁄16-in.] inner diameter at top, 7.1 Safety Precautions—Establish appropriate safety and
and 70-mm [23⁄4-in.] inner diameter at bottom.6 health practices for high-pressure equipment prior to use.
NOTE 2—Mixing containers or equivalent may be obtained from the
8. Sampling and Selection
suppliers given in Footnote 5.
8.1 Conduct the sampling in accordance with Test Method
5.9 Timers, 30 min, two interval, mechanical or electrical,
E725.
precision 60.1 min.
5.10 Spatula, flat blade, to dislodge clay mineral clumps 9. Procedure
adhering to the mixing container walls. 9.1 Grind the clay mineral sample to greater than 100 %
5.11 Covered or Sealed Container, of 400- to 600-mL passing a 100 mesh U.S. Standard Sieve, and a minimum of
capacity. 65 % passing a 200-mesh U.S. Standard Sieve with a mortar
and pestle or laboratory hammer mill as required.
5.12 Ambient Temperature/Low-Pressure Filter Press, con- 9.2 Weigh 22.50 6 0.01 g of the whole composite of finely
forming to API RP 131, Section 3.2. This filter press consists ground clay mineral with “as received” moisture, typically 5 to
mainly of a cylindrical cell having an inside diameter of 10 %, onto a weighing paper. If bentonite is removed from a
76.2 mm [3 in.] and a height of at least 64.0 mm [2.5 in.]. This GCL product, the bentonite would be dried to less than 10 %
chamber is made of materials resistant to strongly alkaline moisture prior to weighing.
solutions, and is so fitted that a pressure medium can be
conveniently admitted into and bled from the top. Arrangement 9.3 Measure 350 6 5 mL of reagent water with the 500-mL
is also such that a sheet of 90-mm filter paper can be placed in graduated cylinder and added to the mixing cup. Place the cup
the bottom of the chamber just above a suitable support. The on the mixer, and add the clay mineral slowly over approxi-
filtration area is 4580 6 60 mm2 [7.1 6 0.1 in2]. Below the mately 30 s.
support is a drain tube for discharging the filtrate into a 9.4 After stirring for 5 6 0.5 min, remove the container
graduated cylinder. Sealing is accomplished with gaskets, and from mixer, and scrape its sides with the spatula to dislodge
the entire assembly supported by a stand. A mini-press or any clay clinging to the container wall. Ensure that all of the
half-area press does not directly correlate with the results dislodged clay mineral clinging to the spatula is incorporated
obtained when using the above described standard-sized press. into the suspension.
Pressure can be applied with any nonhazardous fluid medium, 9.5 Replace the container on the mixer, and continue to stir
either gas or liquid. Presses are equipped with pressure for a cumulative total stirring time of 20 6 0.1 min. The
regulators and can be obtained with portable pressure container may need to be removed from the mixer and the sides
cylinders, midget pressure cartridges, or means of utilizing scraped to dislodge any clay clinging to container walls after
hydraulic pressure. another 5 or 10 min of stirring.
NOTE 3—Ambient temperature/low-pressure filter press conforming to 9.6 Age the clay mineral suspension for a minimum of 16 h
API RP 131, Section 3.2, or equivalent, may be obtained from the in a sealed or covered container at ambient temperature.
suppliers given in Footnote 6. Record the initial temperature, final temperature, and actual
hydration aging time.
9.7 After aging the clay mineral suspension, shake vigor-
5
For example, Sterling Multimixer Model 9B with 9B29X impeller blades ously to break its gel strength, and then pour the suspension
available from Fann Instrument Co., P.O. Box 4350, Houston, TX 77210, has been
found suitable for this purpose.
6
For example, Hamilton Beach Mixer Cup No. M110-D, or equivalent, has been
7
found suitable for this purpose. Mixing containers supplied by Fann Instrument Co., For example, Whatman No. 50, S & S No. 576, or equivalent, have been found
P.O. Box 4350, Houston, TX 77210. suitable for this purpose.

2
 D5891/D5891M − 02 (2016)´1
into the mixer container. Stir the suspension on the mixer for 11.1.4 Any modifications to the test method or unusual
5 6 0.5 min to completely disperse the clay mineral slurry. observations which may effect the test results,
9.8 Assemble the dry filter cell with filter paper and gaskets, 11.1.5 Calculated fluid loss as millilitres to the nearest
and immediately after remixing the clay mineral slurry, pour it 0.1 mL, and
into the filter cell and complete assembly of the filter cell. Place 11.1.6 Temperature of the slurry at the start and completion
the filter cell in the filter frame and close the relief valve. Place of the test to the nearest 0.5°C.
a 10 mL graduated cylinder under the filter cell drain tube. 12. Precision and Bias
9.9 Set one timer for 7.5 6 0.1 min and the second timer for 12.1 Interlaboratory Test Program—An interlaboratory
30 6 0.1 min. Start both timers and adjust pressure on the fluid study of the test method was run in 1999. The design of the
loss cell to 100 6 2 psi. Starting the timers and adding 100 psi experiment, similar to that of Practice E691. Seven different
pressure should be completed in less than 15 s. Supply pressure clay mineral samples were distributed to seven laboratories.
by compressed air, nitrogen, helium, or carbon dioxide. Three sets of test results were generated for each sample by
9.10 At 7.5 6 0.1 min on the first timer, remove the each of the laboratories.
graduated cylinder and any adhering liquid on the drain tube, 12.2 Test Results—The precision information is given in
and discard. Immediately place a clean dry 10-mL graduated Table 1. The average fluid loss values ranged from 9 to 22 for
cylinder under the drain tube, and collect the fluid for 22.5 6 the seven clay mineral samples tested. However, since the
0.1 min to the end of the second timer. This corrects the fluid statistics were not related to the magnitude of the test result, the
loss value for any initial unpredictable spurt loss from the fluid precision values have been presented in terms of coefficients of
loss cell. Remove the graduated cylinder after the second time varaiation, CV %.
interval and record the volume of fluid collected.
12.3 Bias—The procedure in Test Method D5891/D5891M
10. Calculation for measuring the fluid loss value of the clay mineral compo-
10.1 Calculate the fluid loss in millilitres using Eq 1: nent of geosynthetic clay liners has no bias because the values
of swell index can be defined only in terms of this test method.
Fluid loss volume 5 2 ~ mL filtrate volume for last 22.5 min. interval! mL
(1)
TABLE 1 Test Results
11. Report Statistic ILS Range
Within laboratory repeatability limit, CV %r 1.8 to 4.7 %
11.1 Report the following information: Between laboratory reproducibility limit, CV %R 6 to 18 %
11.1.1 Source of clay mineral, including sample identifica- 95 % confidence limit 5 to 13 %
tion or lot number, Within laboratory repeatability, 2.8 CV %r
95 % confidence limit 11.8 to 51 %
11.1.2 Method of sampling used, Between laboratory reproducibility, 2.8 CV %R
11.1.3 ASTM Test Method number used to perform the test,

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