ASTM D5284-93(2004)e1
(Test Method)Standard Test Method for Sequential Batch Extraction of Waste with Acidic Extraction Fluid
Standard Test Method for Sequential Batch Extraction of Waste with Acidic Extraction Fluid
SIGNIFICANCE AND USE
This test method is intended as a means for obtaining sequential extracts of a waste. The extracts may be used to estimate the release of certain constituents of the waste under the laboratory conditions described in this test method.
The pH of the extraction fluid used in this test method is to reflect the pH of acidic precipitation in the geographic region in which the waste being tested is to be disposed.
Note 1—Possible sources of information concerning the pH of precipitation in the geographic region of interest include state and federal environmental agencies, state universities, libraries, etc.
Note 2—For sequential batch extraction of waste using a nonacidic extraction fluid, see Test Method D 4793.
An intent of this test method is for the final pH of each of the extracts to reflect the interaction of the extractant with the buffering capacity of the waste.
This test method is not intended to provide extracts that are representative of the actual leachate produced from a waste in the field or to produce extracts to be used as the sole basis of engineering design.
This test method has not been demonstrated to simulate actual disposal site leaching conditions.
This test method produces extracts that are amenable to the determination of both major and minor (trace) constituents. When minor constituents are being determined, it is especially important that precautions be taken in sample storage and handling to avoid possible contamination of the samples.
This test method has been tested to determine its applicability to certain inorganic components in the waste. This test method has not been tested for applicability to organic substances, volatile matter (see Note 5), or biologically active samples.
The agitation technique, rate, liquid-to-solid ratio, and filtration conditions specified in the procedure may not be suitable for extracting all types of wastes (see Sections 7 and 8 and Appendix X1).
SCOPE
1.1 This test method provides a procedure for the sequential leaching of a waste containing at least 5 % dry solids in order to generate solutions to be used to determine the constituents leached under the specified testing conditions.
1.2 This test method calls for the shaking of a known weight of waste with acidic extraction fluid of a specified composition as well as the separation of the liquid phase for analysis. The pH of the extraction fluid is to reflect the pH of acidic precipitation in the geographic region in which the waste being tested is to be disposed. The procedure is conducted ten times in sequence on the same sample of waste, and it generates ten solutions.
1.3 This test method is intended to describe the procedure for performing sequential batch extractions only. It does not describe all types of sampling and analytical requirements that may be associated with its application.
1.4 The values stated in SI units are to be regarded as the standard.
1.5 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
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Designation:D5284–93 (Reapproved 2004)
Standard Test Method for
Sequential Batch Extraction of Waste with Acidic Extraction
Fluid
This standard is issued under the fixed designation D5284; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Reference to a research report was added in May 2004.
1. Scope D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
1.1 Thistestmethodprovidesaprocedureforthesequential
D2234 Test Methods for Collection of a Gross Sample of
leaching of a waste containing at least 5% dry solids in order
Coal
to generate solutions to be used to determine the constituents
D2777 Practice for Determination of Precision and Bias of
leached under the specified testing conditions.
Methods of Committee D-19 on Water
1.2 Thistestmethodcallsfortheshakingofaknownweight
D3370 Practices for Sampling Water
ofwastewithacidicextractionfluidofaspecifiedcomposition
D4793 Test Method for Sequential Batch Extraction of
as well as the separation of the liquid phase for analysis. The
Waste with Water
pH of the extraction fluid is to reflect the pH of acidic
precipitationinthegeographicregioninwhichthewastebeing
3. Terminology
tested is to be disposed. The procedure is conducted ten times
3.1 Definitions—For definitions of terms used in this test
in sequence on the same sample of waste, and it generates ten
method, see Terminology D1129.
solutions.
3.2 Symbols:Symbols—Variables listed in this test method
1.3 This test method is intended to describe the procedure
are defined in the individual sections in which they are
for performing sequential batch extractions only. It does not
discussed. A list of the defined variables is also provided in
describe all types of sampling and analytical requirements that
Section 11.
may be associated with its application.
1.4 The values stated in SI units are to be regarded as the
4. Significance and Use
standard.
4.1 This test method is intended as a means for obtaining
1.5 This standard does not purport to address all of the
sequential extracts of a waste. The extracts may be used to
safety problems, if any, associated with its use. It is the
estimate the release of certain constituents of the waste under
responsibility of the user of this standard to establish appro-
the laboratory conditions described in this test method.
priate safety and health practices and determine the applica-
4.2 ThepHoftheextractionfluidusedinthistestmethodis
bility of regulatory limitations prior to use.
toreflectthepHofacidicprecipitationinthegeographicregion
2. Referenced Documents in which the waste being tested is to be disposed.
2.1 ASTM Standards:
NOTE 1—PossiblesourcesofinformationconcerningthepHofprecipi-
D75 Practice for Sampling Aggregates tation in the geographic region of interest include state and federal
environmental agencies, state universities, libraries, etc.
D420 Guide to Site Characterization for Engineering, De-
NOTE 2—For sequential batch extraction of waste using a nonacidic
sign and Construction Purposes
extraction fluid, see Test Method D4793.
D653 Terminology Relating to Soil, Rock, and Contained
4.3 An intent of this test method is for the final pH of each
Fluids
of the extracts to reflect the interaction of the extractant with
the buffering capacity of the waste.
This test method is under the jurisdiction ofASTM Committee D34 on Waste
4.4 This test method is not intended to provide extracts that
Management and is the direct responsibility of Subcommittee D34.01.04 on
arerepresentativeoftheactualleachateproducedfromawaste
Ancillary Topics.
Current edition approved Feb. 1, 2004. Published April 2004. Originally
in the field or to produce extracts to be used as the sole basis
approved in 1992. Last previous edition approved in 1999 as D5284–93(1999).
of engineering design.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D5284–93 (2004)
4.5 This test method has not been demonstrated to simulate 5.20 Pressure Filtration Assembly—A pressure filtration
actual disposal site leaching conditions. device of a composition suitable to the nature of the analyses
to be performed and equipped with a 0.45 or 0.8-µm pore size
4.6 This test method produces extracts that are amenable to
filter (see Note 8).
thedeterminationofbothmajorandminor(trace)constituents.
5.21 Extraction Vessels, cylindrical, wide-mouth, of a com-
When minor constituents are being determined, it is especially
position suitable to the nature of the waste and analyses to be
important that precautions be taken in sample storage and
performed,constructedofmaterialsthatwillnotallowsorption
handling to avoid possible contamination of the samples.
of the constituents of interest, and sturdy enough to withstand
4.7 This test method has been tested to determine its
the impact of the falling sample fragments. The size of the
applicabilitytocertaininorganiccomponentsinthewaste.This
container should be selected so that the sample plus extraction
test method has not been tested for applicability to organic
fluid occupy approximately 95% of the container. The con-
substances, volatile matter (see Note 5), or biologically active
tainers must have water-tight closures. Containers for samples
samples.
in which gases may be released should be provided with
4.8 The agitation technique, rate, liquid-to-solid ratio, and
venting mechanisms.
filtration conditions specified in the procedure may not be
suitableforextractingalltypesofwastes(seeSections7and8 NOTE 4—Suitable container sizes range from 4.0 to 4.5 in. in diameter
and 8.5 to 13.0 in. in height.
and Appendix X1).
NOTE 5—The venting of the container has the potential to affect the
concentration of volatile compounds in the extracts.
5. Apparatus
5.21.1 Extraction vessels should be cleaned in a manner
5.1 Straight Edge, such as a thin-edged yardstick.
consistentwiththeanalysestobeperformed(seeSection13of
5.2 Impermeable Sheet, of glazed paper, oil cloth, or other
Practice D3370).
flexible material of a composition suitable to the analytes of
interest.
6. Reagents
5.3 Drying Pans or Dishes (for example, aluminum tins,
6.1 Purity of Reagents—Reagent grade chemicals shall be
porcelain dishes, glass weighing pans), two per waste, suitable
used in all tests. Unless otherwise indicated, it is intended that
to the waste being tested and the instructions given in 9.2.
all reagents shall conform to the specifications of the Commit-
5.4 Drying Oven—Any thermostatically controlled drying
tee onAnalytical Reagents of theAmerican Chemical Society,
oven capable of maintaining a steady temperature of 62°C in
where such specifications are available. Other grades may be
a range of 100 to 110°C.
used, provided it is first ascertained that the reagent is of
5.5 Desiccator, having a capacity to hold the drying pans
sufficiently high purity to permit its use without lessening the
described in 5.3 and the crucibles described in 5.16.
accuracy of the determination.
5.6 Laboratory Balance, capable of weighing to 0.1 g. 6.2 PurityofWater—Unlessotherwiseindicated,references
to water shall be understood to mean Type IV reagent water at
5.7 Erlenmeyer Flask, 2-L capacity, equipped with a mag-
18 to 27°C conforming to Specification D1193. The method
netic stir bar.
by which the water is prepared, that is, distillation, ion
5.8 Magnetic Stir Plate.
exchange, reverse osmosis, electrodialysis, or a combination
5.9 Graduated Cylinder, 1 or 2-L capacity.
thereof, should remain constant throughout testing.
5.10 Pipet, 1-mL capacity.
6.3 Sulfuric Acid/Nitric Acid Solution—A 60/40 weight
5.11 Volumetric Flask, 1-L capacity.
percent (wt%) mixture prepared using 95 to 98 wt% sulfuric
5.12 Pipet, 10-mL capacity. (Various other sized pipets,
acid and 69 to 71 wt% nitric acid. (See 9.3 for instructions on
including micropipets, may be necessary for 9.3.2.)
the preparation of this solution.)
5.13 pH Meter—Any pH meter with a readability of 0.01
7. Sampling
units and an accuracy of 60.05 units at 25°C.
5.14 Carboy-type Container, with spigot, 20 to 50-Lcapac- 7.1 Obtain a representative sample of the waste to be tested
ity,ofacompositionsuitabletothenatureoftheanalysestobe byusing,whereavailable,ASTMsamplingmethodsdeveloped
performed (see Practices D3370). for the specific industry (see Practice D75, Guide D420,
Terminology D653, and Test Method D2234).
5.15 Large Glass Funnel.
7.2 Sampling methodology for materials of similar physical
5.16 Crucibles, porcelain, 20-mL capacity each, two per
form shall be used where no specific methods are available.
waste.
7.3 The amount of sample to be sent to the laboratory
5.17 Analytical Balance, capable of weighing to 0.1 mg.
shouldbesufficienttoperformthesolidscontentdetermination
5.18 Wash Bottle, 500-mL capacity.
5.19 Agitation Equipment, of any type that rotates the
extraction vessel in an end-over-end fashion at a rate of 30 6
Reagent Chemicals, American Chemical Society Specifications, American
2r/minsuchthattheaxis of rotation is horizontal anditpasses
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
through the center of the bottle (see Fig. 1 andAppendix X1).
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
NOTE 3—Similar devices having a different axial arrangement may be
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
used if equivalency can be demonstrated. MD.
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D5284–93 (2004)
FIG. 1 Extractors
as specified in 9.2, and to provide 100 g of sample on a dry 7.6 The time between collection and extraction of the
weight basis for each extraction. sample should be determined by the nature of the sample and
7.4 It is important that the sample of the waste be represen- the information desired. See Practices D3370 for guidance.
tative with respect to surface area, as variations in surface area Report the length of time between sample collection and
woulddirectlyaffecttheleachingcharacteristicsofthesample. extraction.
Waste samples should contain a representative distribution of
particle sizes. 8. Sample Preparation
8.1 For free-flowing particulate solid wastes, obtain a
NOTE 6—Information on obtaining representative samples can also be
found in Pierre Gy’s Sampling Theory and Sampling Practice.
sample of the approximate size required in the test by quarter-
ing the sample (Section 7) received for testing on an imper-
7.5 In order to prevent sample contamination or constituent
meable sheet of glazed paper, oil cloth, or other flexible
loss prior to extraction, keep the samples in closed containers
material having a composition suitable to the analytes of
appropriate to sample type and desired analysis. See Practices
interest, as follows:
D3370 for guidance. Record the storage conditions and
8.1.1 Empty the sample container into the center of the
handling procedures in the report.
sheet.
8.1.2 Gently flatten the sample out with a suitable straight-
edge until it is spread uniformly to a depth at least twice the
Pitard, F., Pierre Gy’s Sampling Theory and Sampling Practice, Vols I and II,
CRC Press, 1989. maximum particle diameter.
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D5284–93 (2004)
8.1.3 Remix the sample by lifting a corner of the sheet and 9.2.5 Repeatthestepsgivenin9.2.3and9.2.4untilconstant
drawing it low across to the opposite corner in such a manner container-sample masses are obtained. Discard the dried
that the material is made to roll over and over and does not
samples following completion of this step.
merely slide along. Continue the operation with each corner,
9.2.6 Calculate the solids content of the sample from the
proceeding in a clockwise direction. Repeat this operation ten
data obtained in 9.2.1, 9.2.2, and 9.2.4 as follows:
times.
S 5 A/B (1)
8.1.4 Liftallfourcornersofthesheettowardthecenterand,
holding all four corners together, raise the entire sheet into the
where:
air to form a pocket for the sample.
A = mass of sample after drying, g,
8.1.5 Repeat the procedure described in 8.1.2 to flatten the B = original mass of sample, g, and
sample out. S = solids content, g/g.
8.1.6 Withastraightedge(suchasathin-edgedyardstick)at
Average the two values obtained. Record the solids content.
least as long as the flattened mound of sample, gently divide
9.3 Preparation of Extraction Fluid—Prepare a 60/40 wt%
thesampleintoquarters.Makeanefforttoavoidusingpressure
mixture of sulfuric acid/nitric acid. Cautiously mix 60 g of
on the straightedge sufficient to cause damage to the particles.
concentratedsulfuricacidwith40gofconcentratednitricacid.
8.1.7 Discard the alternate quarters.
The preparation of this mixture should be performed in a
8.1.8 If further reduction of the sample size is necessary,
laboratory fume hood.
repeatthestepsgivenin8.1.3through8.1.7.Useasamplesize
9.3.1 Using the 60/40 sulfuric acid/nitric acid mixture,
to provide 100 g of solid on a dry weight basis for each
prepare a second solution by diluting 1.0 mL of the 60/40
extraction. Provide additional samples for the determination of
mixture to 1000 mL using water and a 1-L volumetric flask.
solids content (see 9.2). Use of a sample size other than 100 g
9.3.2 Using the 1/1000 solution prepared in 9.3.1, prepare
of solid on a dry weight basis for extraction is not recom-
the extraction fluid having the desired pH 6 0.05 (see 4.2)by
mended; however, if a different sample size is used, report this
pipetingavolumeofthe1/1000solutioninto2000mLofwater
fact.
with mixing until the desired pH 6 0.05 is achieved. A
NOTE 7—For other acceptable methods of mixing and subsampling
recommended method for preparing the extraction fluid is to
free-flowing solid particulate wastes, see Pierre Gy’s Sampling Theory
5 add 2000 mLof water to a 2-Lerlenmeyer flask equipped with
and Sampling Practice. The method of subsampling should be deter-
a magnetic stir bar. Place the erlenmeyer flask on a magnetic
mined by the physical properties of the waste, analytes of interest, and
equipment available.
stirplate,andaddthe1/1000solutiontotheflaskwithstirring.
Shake the mixture vigorously, and measure its pH once the
8.2
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