ASTM D4793-93(2004)
(Test Method)Standard Test Method for Sequential Batch Extraction of Waste with Water
Standard Test Method for Sequential Batch Extraction of Waste with Water
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.
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 is not intended to simulate site-specific leaching conditions. It has not been demonstrated to simulate actual disposal site leaching conditions.
An intent of this test method is that the final pH of each of the extracts reflects the interaction of the extractant with the buffering capacity of the waste.
An intent of this test method is that the water extractions reflect conditions where the waste is the dominant factor in determining the pH of the extracts.
This test method produces extracts that are amenable to the determination of both major and minor constituents. When minor constituents are being determined, it is especially important that precautions are 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 3 in 5.15), 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, 8, and the discussion in Appendix X1).
SCOPE
1.1 This test method is a procedure for the sequential leaching of a waste containing at least five % solids 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 water of a specified purity and the separation of the aqueous phase for analysis. The procedure is conducted ten times in sequence on the same sample of waste and generates ten aqueous 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 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:D4793–93 (Reapproved 2004)
Standard Test Method for
Sequential Batch Extraction of Waste with Water
This standard is issued under the fixed designation D4793; 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.
1. Scope D2777 Practice for Determination of Precision and Bias of
Methods of Committee D-19 on Water
1.1 This test method is a procedure for the sequential
D3370 Practices for Sampling Water
leachingofawastecontainingatleastfive%solidstogenerate
solutions to be used to determine the constituents leached
3. Terminology
under the specified testing conditions.
3.1 Definitions:
1.2 Thistestmethodcallsfortheshakingofaknownweight
3.1.1 For definitions of terms used in this test method, see
of waste with water of a specified purity and the separation of
Terminology D1129.
theaqueousphaseforanalysis.Theprocedureisconductedten
3.2 Symbols:Symbols:
times in sequence on the same sample of waste and generates
3.2.1 Variables listed in this test method are defined in the
ten aqueous solutions.
individual sections where they are discussed.Alist of defined
1.3 This test method is intended to describe the procedure
variables is also given in Section 11.
for performing sequential batch extractions only. It does not
3.2.2 Explanation of Variables:
describe all types of sampling and analytical requirements that
may be associated with its application.
1.4 This standard does not purport to address all of the
¯
X = total mean value
t
safety problems, if any, associated with its use. It is the
¯
X = analytical mean value (calculated using data from
a
responsibility of the user of this standard to establish appro-
analysis of standards)
priate safety and health practices and determine the applica-
S = total standard deviation
tt
bility of regulatory limitations prior to use.
S = analytical standard deviation
ta
S = estimated standard deviation due to the extraction
te
2. Referenced Documents
procedure
2.1 ASTM Standards:
S = total single operator standard deviation
ot
D75 Practices for Sampling Aggregates S = analytical single operator standard deviation
oa
S = estimated single operator standard deviation due to
D420 Practice for Investigating and Sampling Soil and
oe
the extraction procedure
Rock for Engineering Purposes
D653 Terminology Relating to Soil, Rock, and Contained
4. Significance and Use
Fluids
4.1 This test method is intended as a means for obtaining
D1129 Terminology Relating to Water
sequential extracts of a waste. The extracts may be used to
D1193 Specification for Reagent Water
estimate the release of certain constituents of the waste under
D2216 TestMethodforLaboratoryDeterminationofWater
the laboratory conditions described in this test method.
(Moisture) Content of Soil, Rock, and Soil-Aggregate
4.2 This test method is not intended to provide extracts that
Mixtures
arerepresentativeoftheactualleachateproducedfromawaste
D2234 Test Method for Collection of a Gross Sample of
in the field or to produce extracts to be used as the sole basis
Coal
of engineering design.
4.3 Thistestmethodisnotintendedtosimulatesite-specific
This test method is under the jurisdiction ofASTM Committee D34 on Waste
leaching conditions. It has not been demonstrated to simulate
Management and is the direct responsibility of Subcommittee D34.01.04 on
actual disposal site leaching conditions.
Ancillary Topics.
Current edition approved Jan. 15, 1993. Published March 1993. Originally 4.4 An intent of this test method is that the final pH of each
published as D4793–88. Last previous edition D4793–88.
of the extracts reflects the interaction of the extractant with the
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
buffering capacity of the waste.
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.
D4793–93 (2004)
4.5 Anintentofthistestmethodisthatthewaterextractions approximately 95% of the container. Containers must have
reflect conditions where the waste is the dominant factor in water-tight closure. Containers for samples where gases may
determining the pH of the extracts. be released should be provided with a venting mechanism.
4.6 This test method produces extracts that are amenable to
NOTE 2—Suitable container sizes range from 4.0 to 4.5 in. (102 to 114
the determination of both major and minor constituents. When
mm) in diameter and 8.5 to 13.0 in. (216 to 330 mm) in height.
minor constituents are being determined, it is especially
NOTE 3—The venting of the container has the potential to affect the
important that precautions are taken in sample storage and
concentration of volatile compounds in the extracts.
handling to avoid possible contamination of the samples.
5.15.1 Extraction vessels should be cleaned in a manner
4.7 This test method has been tested to determine its
consistent with the analyses to be performed. See Practices
applicabilitytocertaininorganiccomponentsinthewaste.This
D3370, Section 13.
test method has not been tested for applicability to organic
substances,volatilematter(seeNote3in5.15),orbiologically
6. Reagents
active samples.
6.1 Purity of Reagents—Reagent grade chemicals shall be
4.8 The agitation technique, rate, liquid-to-solid ratio, and
used in all tests. Unless otherwise indicated, it is intended that
filtration conditions specified in the procedure may not be
allreagentsshallconformtothespecificationsoftheAmerican
suitable for extracting all types of wastes (see Sections 7, 8,
Chemical Society, where such specifications are available.
and the discussion in Appendix X1).
Other grades may be used, provided it is first ascertained that
the reagent is of sufficiently high purity to permit its use
5. Apparatus
without lessening the accuracy of the determination.
5.1 Straightedge (such as a thin-edged yard stick).
6.2 Purity of Water—Unlessotherwiseindicated,references
5.2 Impermeable Sheet, of glazed paper, oil cloth, or other
to water shall be understood to mean Type IV reagent water at
flexible material of a composition suitable to the analytes of
18 to 27°C (Specification D1193). The method by which the
interest.
water is prepared, that is, distillation, ion exchange, reverse
5.3 Drying Pans or Dishes—Two per waste (for example,
osmosis, electrodialysis, or a combination thereof, should
aluminum tins, porcelain dishes, or glass weighing pans),
remain constant throughout testing.
suitable to the waste being tested and the instructions given in
9.2.
7. Sampling
5.4 Drying Oven—Any thermostatically controlled drying
7.1 Obtain a representative sample of the waste to be tested
oven capable of maintaining a steady temperature of 62°C in
using ASTM sampling methods developed for the specific
a range from 100 to 110°C.
industry where available (see Practices D75 and D420,
5.5 Desiccator, having the capacity to hold the drying pans
Terminology D653, and Test Method D2234).
described in 5.3 and the crucibles described in 5.8.
7.2 Where no specific methods are available, sampling
5.6 Laboratory Balance, capable of weighing to 0.1 g.
methodology for material of similar physical form shall be
5.7 Pipet, 10-mL capacity.
used.
5.8 Crucibles—Two per waste, porcelain, 20-mL capacity
7.3 The amount of sample to be sent to the laboratory
each.
shouldbesufficienttoperformthesolidscontentdetermination
5.9 Analytical Balance, capable of weighing to 0.1 mg.
as specified in 9.2 and to provide 100 g of sample on a dry
5.10 Large Glass Funnel.
weight basis for each extraction.
5.11 Wash Bottle, 500-mL capacity.
7.4 It is important that the sample of the waste be represen-
5.12 pH Meter—Any pH meter with a readability of 0.01
tative with respect to surface area, as variations in surface area
units and an accuracy of 60.05 units at 25°C is acceptable.
woulddirectlyaffecttheleachingcharacteristicsofthesample.
5.13 Agitation Equipment, of any type that rotates the
Waste samples should contain a representative distribution of
extractionvesselinanend-over-endfashionatarateof30 62
particle sizes.
r/min such that the axis of rotation is horizontal and it goes
NOTE 4—Information on obtaining representative samples can also be
through the center of the bottle, (see Fig. 1 and the discussion
found in Pierre Gy’s Sampling Theory and Sampling Practice, Volumes I
of agitation in Appendix X1).
and II, by F. Picard, CRC Press, 1989.
NOTE 1—Similar devices having a different axial arrangement may be
7.5 In order to prevent sample contamination or constituent
used if equivalency can be demonstrated.
loss prior to extraction, keep samples in closed containers
5.14 Pressure Filtration Assembly—A pressure filtration
appropriate to the sample type and desired analysis. See
device of a composition suitable to the nature of the analyses
Practices D3370 for guidance. Record the storage conditions
to be performed and equipped with a 0.45 or 0.8-µm pore-size
and handling procedures in the report.
filter (see Note 7, pertaining to 9.4).
5.15 Extraction Vessels, cylindrical, wide-mouth, of a com-
position suitable to the nature of the waste and analyses to be
“ReagentChemicals,AmericanChemicalSocietySpecifications,”Am.Chemi-
performed,constructedofmaterialsthatwillnotallowsorption
cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by
of constituents of interest, and sturdy enough to withstand the
theAmericanChemicalSociety,see“ReagentChemicalsandStandards,”byJoseph
impact of the falling sample fragments. Container size should
Rosin, D. Van Nostrand Co., Inc., New York, NY, and the “United States
be selected so that the sample plus extraction fluid occupy Pharmacopeia.”
D4793–93 (2004)
FIG. 1 Extractors
7.6 The time between collection and extraction of the 8.1.1 Empty the sample container into the center of the
sample should be determined by the nature of the sample and
sheet.
the information desired. See Practices D3370 for guidance.
8.1.2 Flatten out the sample gently with a suitable straight-
Report the length of time between sample collection and
edge until it is spread uniformly to a depth at least twice the
extraction.
maximum particle diameter.
8. Sample Preparation
8.1.3 Remix the sample by lifting a corner of the sheet and
drawingitacross,lowdown,totheoppositecornerinamanner
8.1 For free-flowing particulate solid wastes, obtain a
that the material is made to roll over and over and does not
sample of the approximate size required in the test by quarter-
merely slide along. Continue the operation with each corner,
ing the sample (Section 7) received for testing on an imper-
meable sheet of glazed paper, oil cloth, or other flexible proceeding in a clockwise direction. Repeat this operation ten
times.
material as follows:
D4793–93 (2004)
8.1.4 Lift all four corners of the sheet towards the center
S = solids content, g/g.
and,holdingallfourcornerstogether,raisetheentiresheetinto
Average the two values obtained. Record the solids content.
the air to form a pocket for the sample.
9.3 ExtractionProcedure—Iftheentireprocedurecannotbe
8.1.5 Repeat 8.1.2.
conductedwithoutinterruption,atleastthefirstfourextraction
8.1.6 With a straightedge (such as a thin-edged yard stick),
sequences must be conducted without interruption.
one at least as long as the flattened mound of sample, gently
9.3.1 Determinethemassoftheextractionvesseltobeused
divide the sample into quarters. Make an effort to avoid using
in the extraction procedure to the nearest 0.1 g. Record the
pressure on the straightedge sufficient to cause damage to the
mass of the extraction vessel, M . Use one extraction vessel
v1
particles.
per waste throughout the sequence of extractions.
8.1.7 Discard alternate quarters.
9.3.2 Add100g(weighedto 60.1g)ofsolidwasteonadry
8.1.8 If further reduction of sample size is necessary, repeat
weight basis to the extraction vessel. Calculate the amount of
8.1.3-8.1.7. Use a sample size to give 100 g of solid for each
waste as received to add using the following equation:
extraction. Provide additional samples for determination of
solids content. If smaller samples are used in the test, report
M 5 (2)
this fact.
S
NOTE 5—For other acceptable methods for mixing and subsampling
where:
free-flowing solid particulate wastes, see Pierre Gy’s Sampling Theory
M = mass of waste as received to add to the extraction
and Sampling Practice, Volumes I and II, by F. Picard, CRC Press, 1989.
vessel to give 100 g (weighed to 60.1 g) of solid
The method of subsampling should be determined by the physical
waste.
properties of the waste, analytes of interest, and equipment available.
9.3.2.1 If a mass of solid waste on a dry weight basis other
8.2 For field-cored solid wastes or castings produced in the
than 100 g is used, (Eq 2) through (4) must be modified to
laboratory, cut a representative section weighing approxi-
reflecttheuseofamassotherthan100g.Replace100inthese
mately 100 g for testing plus samples for determination for
equations with the mass used. Use of a mass other than 100 g
solids content. Shape the sample so that the leaching solution
is not recommended.
will cover the material to be leached.
9.3.3 Add a volume in millilitres, V , of test water (see 6.2)
vl
8.3 For multiphasic wastes, mix thoroughly to ensure that a
to the extraction vessel determined using the following equa-
representative sample will be withdrawn. Take samples for
tions:
determination of solids content at the same time as the test
M 5 M 2100 (3)
samples.
sw
9. Procedure
where:
9.1 Record the physical description of the sample to be
M = mass of moisture in the sample added to the
sw
tested, including particle size so far as it is known.
extraction vessel, g.
9.2 Solids Content—Determine the solids content of two
V 5 ~20! ~100! 2 M . (4)
v sw
separate portions of the sample as follows:
9.2.1 Dry to a constant weight at 104 6 2°C two dishes or
9.3.4 Agitate continuously for 18 6 0.25 h at 18 to 27°C.
pans of size suitable to the solid waste being tested. Cool in a
Record the agitation time and temperature.
desiccator and weigh. Record the values to 60.1 g.
9.3.5 Open the extraction vessel. Observe and record any
9.2.2 Put an appropriately sized portion of sample of the
waste to be tested into each pan. Scale the weight used to the visible physical change
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