ASTM D4793-09(2017)
(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
4.1 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.
4.2 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.
4.3 This test method is not intended to simulate site-specific leaching conditions. It has not been demonstrated to simulate actual disposal site leaching conditions.
4.4 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.
4.5 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.
4.6 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.
4.7 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.
4.8 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 percent 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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health and environmental practices and determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4793 − 09 (Reapproved 2017)
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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope D420GuidetoSiteCharacterizationforEngineeringDesign
and Construction Purposes (Withdrawn 2011)
1.1 This test method is a procedure for the sequential
D653Terminology Relating to Soil, Rock, and Contained
leaching of a waste containing at least five percent solids to
Fluids
generate solutions to be used to determine the constituents
D1129Terminology Relating to Water
leached under the specified testing conditions.
D1193Specification for Reagent Water
1.2 Thistestmethodcallsfortheshakingofaknownweight
D2216TestMethodsforLaboratoryDeterminationofWater
of waste with water of a specified purity and the separation of
(Moisture) Content of Soil and Rock by Mass
theaqueousphaseforanalysis.Theprocedureisconductedten
D2234/D2234MPractice for Collection of a Gross Sample
times in sequence on the same sample of waste and generates
of Coal
ten aqueous solutions.
D2777Practice for Determination of Precision and Bias of
Applicable Test Methods of Committee D19 on Water
1.3 This test method is intended to describe the procedure
for performing sequential batch extractions only. It does not D3370Practices for Sampling Water from Closed Conduits
describe all types of sampling and analytical requirements that
3. Terminology
may be associated with its application.
3.1 Definitions:
1.4 The values stated in SI units are to be regarded as
3.1.1 For definitions of terms used in this test method, see
standard. No other units of measurement are included in this
Terminology D1129.
standard.
3.2 Symbols:
1.5 This standard does not purport to address all of the
3.2.1 Variables listed in this test method are defined in the
safety concerns, if any, associated with its use. It is the
individual sections where they are discussed.Alist of defined
responsibility of the user of this standard to establish appro-
variables is also given in Section 11.
priate safety, health and environmental practices and deter-
3.2.2 Explanation of Variables:
mine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accor-
¯
dance with internationally recognized principles on standard-
X = total mean value
t
¯
ization established in the Decision on Principles for the X = analytical mean value (calculated using data from
a
Development of International Standards, Guides and Recom- analysis of standards)
S = total standard deviation
mendations issued by the World Trade Organization Technical
tt
S = analytical standard deviation
Barriers to Trade (TBT) Committee. ta
S = estimated standard deviation due to the extraction
te
procedure
2. Referenced Documents
S = total single operator standard deviation
ot
2.1 ASTM Standards:
S = analytical single operator standard deviation
oa
D75/D75MPractice for Sampling Aggregates
S = estimated single operator standard deviation due to
oe
the extraction procedure
4. Significance and Use
This test method is under the jurisdiction ofASTM Committee D34 on Waste
Management and is the direct responsibility of Subcommittee D34.01.04 on Waste
4.1 This test method is intended as a means for obtaining
Leaching Techniques.
sequential extracts of a waste. The extracts may be used to
Current edition approved Sept. 1, 2017. Published September 2017. Originally
estimate the release of certain constituents of the waste under
approved in 1988. Last previous edition approved in 2009 as D4793–09. DOI:
10.1520/D4793-09R17.
the laboratory conditions described in this test method.
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 last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4793 − 09 (2017)
4.2 This test method is not intended to provide extracts that 5.13 Agitation Equipment, of any type that rotates the
arerepresentativeoftheactualleachateproducedfromawaste extraction vessel in an end-over-end fashion at a rate of 0.5 6
in the field or to produce extracts to be used as the sole basis 0.03 Hz, such that the axis of rotation is horizontal and it goes
of engineering design. through the center of the bottle (see Fig. 1 and the discussion
of agitation in Appendix X1).
4.3 Thistestmethodisnotintendedtosimulatesite-specific
leaching conditions. It has not been demonstrated to simulate NOTE 1—Similar devices having a different axial arrangement may be
used if equivalency can be demonstrated.
actual disposal site leaching conditions.
5.14 Pressure Filtration Assembly—A pressure filtration
4.4 An intent of this test method is that the final pH of each
device of a composition suitable to the nature of the analyses
of the extracts reflects the interaction of the extractant with the
to be performed and equipped with a 0.45 or 0.8-µm pore size
buffering capacity of the waste.
filter (see Note 7, pertaining to 9.4).
4.5 Anintentofthistestmethodisthatthewaterextractions
5.15 Extraction Vessels, cylindrical, wide-mouth, of a com-
reflect conditions where the waste is the dominant factor in
position suitable to the nature of the waste and analyses to be
determining the pH of the extracts.
performed,constructedofmaterialsthatwillnotallowsorption
4.6 This test method produces extracts that are amenable to
of constituents of interest, and sturdy enough to withstand the
the determination of both major and minor constituents.When
impact of the falling sample fragments. Container size should
minor constituents are being determined, it is especially
be selected so that the sample plus extraction fluid occupy
important that precautions are taken in sample storage and
approximately 95% of the container. Containers must have
handling to avoid possible contamination of the samples.
watertightclosure.Containersforsampleswheregasesmaybe
released should be provided with a venting mechanism.
4.7 This test method has been tested to determine its
applicabilitytocertaininorganiccomponentsinthewaste.This
NOTE 2—Suitable container sizes range from 10 to 11 cm in diameter
test method has not been tested for applicability to organic
and 22 to 33 cm in height.
substances,volatilematter(seeNote3in5.15),orbiologically
active samples. NOTE 3—Venting the container has the potential to affect the concen-
tration of volatile compounds in the extracts.
4.8 The agitation technique, rate, liquid-to-solid ratio, and
5.15.1 Extraction vessels should be cleaned in a manner
filtration conditions specified in the procedure may not be
consistentwiththeanalysestobeperformed.SeeSection13of
suitable for extracting all types of wastes (see Sections 7, 8,
Practices D3370.
and the discussion in Appendix X1).
6. Reagents
5. Apparatus
6.1 Purity of Reagents—Reagent-grade chemicals shall be
5.1 Straightedge, such as a thin-edged yard stick.
used in all tests. Unless otherwise indicated, it is intended that
5.2 Impermeable Sheet, of glazed paper, oil cloth, or other
allreagentsshallconformtothespecificationsoftheAmerican
flexible material of a composition suitable to the analytes of
Chemical Society, where such specifications are available.
interest.
Other grades may be used, provided it is first ascertained that
the reagent is of sufficiently high purity to permit its use
5.3 Drying Pans or Dishes—Two per waste (for example,
without lessening the accuracy of the determination.
aluminum tins, porcelain dishes, or glass weighing pans),
suitable to the waste being tested and the instructions given in
6.2 Purity of Water—Unless otherwise indicated, references
9.2.
to water shall be understood to meanType IVreagent water at
18 to 27°C (Specification D1193). The method by which the
5.4 Drying Oven—Any thermostatically controlled drying
water is prepared, that is, distillation, ion exchange, reverse
oven capable of maintaining a steady temperature of 62°Cin
osmosis, electrodialysis, or a combination thereof, should
a range from 100 to 110°C.
remain constant throughout testing.
5.5 Desiccator, having the capacity to hold the drying pans
described in 5.3 and the crucibles described in 5.8.
7. Sampling
5.6 Laboratory Balance, capable of weighing to 0.1 g.
7.1 Obtain a representative sample of the waste to be tested
using ASTM sampling methods developed for the specific
5.7 Pipet, 10-mL capacity.
industry where available (see Practice D75/D75M, Guide
5.8 Crucibles—Two per waste, porcelain, 20-mL capacity
D420, Terminology D653, and Test Method D2234/D2234M).
each.
5.9 Analytical Balance, capable of weighing to 0.1 mg.
Reagent Chemicals, American Chemical Society Specifications, American
5.10 Large Glass Funnel.
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
5.11 Wash Bottle, 500-mL capacity.
listed by the American Chemical Society, see Annual Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
5.12 pH Meter—Any pH meter with a readability of 0.01
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
units and an accuracy of 60.05 units at 25°C is acceptable. MD.
D4793 − 09 (2017)
FIG. 1 Extractors
7.2 Where no specific methods are available, sampling 7.6 The time between collection and extraction of the
methodology for material of similar physical form shall be sample should be determined by the nature of the sample and
used. the information desired. See Practices D3370 for guidance.
Report the length of time between sample collection and
7.3 The amount of sample to be sent to the laboratory
extraction.
shouldbesufficienttoperformthesolidscontentdetermination
as specified in 9.2 and to provide 100 g of sample on a dry
8. Sample Preparation
weight basis for each extraction.
8.1 For free-flowing particulate solid wastes, obtain a
7.4 It is important that the sample of the waste be represen-
sample of the approximate size required in the test by quarter-
tative with respect to surface area, as variations in surface area
ing the sample (Section 7) received for testing on an imper-
woulddirectlyaffecttheleachingcharacteristicsofthesample.
meable sheet of glazed paper, oil cloth, or other flexible
Waste samples should contain a representative distribution of
material as follows:
particle sizes.
8.1.1 Empty the sample container into the center of the
NOTE 4—Information on obtaining representative samples can also be
sheet.
found in Pierre Gy’s Sampling Theory and Sampling Practice,Volumes I
and II, by F. Picard, CRC Press, 1989.
8.1.2 Flatten out the sample gently with a suitable straight-
edge until it is spread uniformly to a depth at least twice the
7.5 In order to prevent sample contamination or constituent
maximum particle diameter.
loss prior to extraction, keep samples in closed containers
appropriate to the sample type and desired analysis. See 8.1.3 Remix the sample by lifting a corner of the sheet and
Practices D3370 for guidance. Record the storage conditions drawingitacross,lowdown,totheoppositecornerinamanner
and handling procedures in the report. that the material is made to roll over and over and does not
D4793 − 09 (2017)
merely slide along. Continue the operation with each corner, where:
proceeding in a clockwise direction. Repeat this operation ten
A = mass of sample after drying, g,
times.
B = original mass of sample, g, and
S = solids content, g/g.
8.1.4 Lift all four corners of the sheet towards the center
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)
S
this fact.
where:
NOTE 5—For other acceptable methods for mixing and subsampling
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 2-4 must be modified to reflect the use
laboratory, cut a representative section weighing approxi-
ofamassotherthan100g.Replace100intheseequationswith
mately 100 g for testing plus samples for determination for
the mass used. Use of a mass other than 100 g is not
solids content. Shape the sample so that the leaching solution
recommended.
will cover the material to be leached.
9.3.3 Addavolumeinmillilitres, V ,oftestwater(see6.2)
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.
...
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D4793 − 09 (Reapproved 2017)
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D420 Guide to Site Characterization for Engineering Design
and Construction Purposes (Withdrawn 2011)
1.1 This test method is a procedure for the sequential
D653 Terminology Relating to Soil, Rock, and Contained
leaching of a waste containing at least five percent solids to
Fluids
generate solutions to be used to determine the constituents
D1129 Terminology Relating to Water
leached under the specified testing conditions.
D1193 Specification for Reagent Water
1.2 This test method calls for the shaking of a known weight
D2216 Test Methods for Laboratory Determination of Water
of waste with water of a specified purity and the separation of
(Moisture) Content of Soil and Rock by Mass
the aqueous phase for analysis. The procedure is conducted ten
D2234/D2234M Practice for Collection of a Gross Sample
times in sequence on the same sample of waste and generates
of Coal
ten aqueous solutions.
D2777 Practice for Determination of Precision and Bias of
1.3 This test method is intended to describe the procedure Applicable Test Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Closed Conduits
for performing sequential batch extractions only. It does not
describe all types of sampling and analytical requirements that
3. Terminology
may be associated with its application.
3.1 Definitions:
1.4 The values stated in SI units are to be regarded as
3.1.1 For definitions of terms used in this test method, see
standard. No other units of measurement are included in this
Terminology D1129.
standard.
3.2 Symbols:
1.5 This standard does not purport to address all of the
3.2.1 Variables listed in this test method are defined in the
safety concerns, if any, associated with its use. It is the
individual sections where they are discussed. A list of defined
responsibility of the user of this standard to establish appro-
variables is also given in Section 11.
priate safety, health and environmental practices and deter-
3.2.2 Explanation of Variables:
mine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accor-
¯
dance with internationally recognized principles on standard-
X = total mean value
t
¯
ization established in the Decision on Principles for the X = analytical mean value (calculated using data from
a
Development of International Standards, Guides and Recom- analysis of standards)
S = total standard deviation
mendations issued by the World Trade Organization Technical
tt
S = analytical standard deviation
Barriers to Trade (TBT) Committee.
ta
S = estimated standard deviation due to the extraction
te
procedure
2. Referenced Documents
S = total single operator standard deviation
2 ot
2.1 ASTM Standards:
S = analytical single operator standard deviation
oa
D75/D75M Practice for Sampling Aggregates
S = estimated single operator standard deviation due to
oe
the extraction procedure
4. Significance and Use
This test method is under the jurisdiction of ASTM Committee D34 on Waste
Management and is the direct responsibility of Subcommittee D34.01.04 on Waste
4.1 This test method is intended as a means for obtaining
Leaching Techniques.
sequential extracts of a waste. The extracts may be used to
Current edition approved Sept. 1, 2017. Published September 2017. Originally
estimate the release of certain constituents of the waste under
approved in 1988. Last previous edition approved in 2009 as D4793 – 09. DOI:
10.1520/D4793-09R17.
the laboratory conditions described in this test method.
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 last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4793 − 09 (2017)
4.2 This test method is not intended to provide extracts that 5.13 Agitation Equipment, of any type that rotates the
are representative of the actual leachate produced from a waste extraction vessel in an end-over-end fashion at a rate of 0.5 6
in the field or to produce extracts to be used as the sole basis 0.03 Hz, such that the axis of rotation is horizontal and it goes
of engineering design. through the center of the bottle (see Fig. 1 and the discussion
of agitation in Appendix X1).
4.3 This test method is not intended to simulate site-specific
leaching conditions. It has not been demonstrated to simulate
NOTE 1—Similar devices having a different axial arrangement may be
used if equivalency can be demonstrated.
actual disposal site leaching conditions.
5.14 Pressure Filtration Assembly—A pressure filtration
4.4 An intent of this test method is that the final pH of each
device of a composition suitable to the nature of the analyses
of the extracts reflects the interaction of the extractant with the
to be performed and equipped with a 0.45 or 0.8-µm pore size
buffering capacity of the waste.
filter (see Note 7, pertaining to 9.4).
4.5 An intent of this test method is that the water extractions
5.15 Extraction Vessels, cylindrical, wide-mouth, of a com-
reflect conditions where the waste is the dominant factor in
position suitable to the nature of the waste and analyses to be
determining the pH of the extracts.
performed, constructed of materials that will not allow sorption
4.6 This test method produces extracts that are amenable to
of constituents of interest, and sturdy enough to withstand the
the determination of both major and minor constituents. When
impact of the falling sample fragments. Container size should
minor constituents are being determined, it is especially
be selected so that the sample plus extraction fluid occupy
important that precautions are taken in sample storage and
approximately 95 % of the container. Containers must have
handling to avoid possible contamination of the samples.
watertight closure. Containers for samples where gases may be
released should be provided with a venting mechanism.
4.7 This test method has been tested to determine its
applicability to certain inorganic components in the waste. This
NOTE 2—Suitable container sizes range from 10 to 11 cm in diameter
test method has not been tested for applicability to organic
and 22 to 33 cm in height.
substances, volatile matter (see Note 3 in 5.15), or biologically
NOTE 3—Venting the container has the potential to affect the concen-
active samples.
tration of volatile compounds in the extracts.
4.8 The agitation technique, rate, liquid-to-solid ratio, and
5.15.1 Extraction vessels should be cleaned in a manner
filtration conditions specified in the procedure may not be
consistent with the analyses to be performed. See Section 13 of
suitable for extracting all types of wastes (see Sections 7, 8,
Practices D3370.
and the discussion in Appendix X1).
6. Reagents
5. Apparatus
6.1 Purity of Reagents—Reagent-grade chemicals shall be
5.1 Straightedge, such as a thin-edged yard stick.
used in all tests. Unless otherwise indicated, it is intended that
5.2 Impermeable Sheet, of glazed paper, oil cloth, or other
all reagents shall conform to the specifications of the American
flexible material of a composition suitable to the analytes of
Chemical Society, where such specifications are available.
interest.
Other grades may be used, provided it is first ascertained that
the reagent is of sufficiently high purity to permit its use
5.3 Drying Pans or Dishes—Two per waste (for example,
without lessening the accuracy of the determination.
aluminum tins, porcelain dishes, or glass weighing pans),
suitable to the waste being tested and the instructions given in
6.2 Purity of Water—Unless otherwise indicated, references
9.2.
to water shall be understood to mean Type IV reagent water at
18 to 27 °C (Specification D1193). The method by which the
5.4 Drying Oven—Any thermostatically controlled drying
water is prepared, that is, distillation, ion exchange, reverse
oven capable of maintaining a steady temperature of 62 °C in
osmosis, electrodialysis, or a combination thereof, should
a range from 100 to 110 °C.
remain constant throughout testing.
5.5 Desiccator, having the capacity to hold the drying pans
described in 5.3 and the crucibles described in 5.8.
7. Sampling
5.6 Laboratory Balance, capable of weighing to 0.1 g.
7.1 Obtain a representative sample of the waste to be tested
using ASTM sampling methods developed for the specific
5.7 Pipet, 10-mL capacity.
industry where available (see Practice D75/D75M, Guide
5.8 Crucibles—Two per waste, porcelain, 20-mL capacity
D420, Terminology D653, and Test Method D2234/D2234M).
each.
5.9 Analytical Balance, capable of weighing to 0.1 mg.
5.10 Large Glass Funnel. Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
5.11 Wash Bottle, 500-mL capacity.
listed by the American Chemical Society, see Annual Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
5.12 pH Meter—Any pH meter with a readability of 0.01
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
units and an accuracy of 60.05 units at 25 °C is acceptable. MD.
D4793 − 09 (2017)
FIG. 1 Extractors
7.2 Where no specific methods are available, sampling 7.6 The time between collection and extraction of the
methodology for material of similar physical form shall be sample should be determined by the nature of the sample and
used. the information desired. See Practices D3370 for guidance.
Report the length of time between sample collection and
7.3 The amount of sample to be sent to the laboratory
extraction.
should be sufficient to perform the solids content determination
as specified in 9.2 and to provide 100 g of sample on a dry
8. Sample Preparation
weight basis for each extraction.
8.1 For free-flowing particulate solid wastes, obtain a
7.4 It is important that the sample of the waste be represen-
sample of the approximate size required in the test by quarter-
tative with respect to surface area, as variations in surface area
ing the sample (Section 7) received for testing on an imper-
would directly affect the leaching characteristics of the sample.
meable sheet of glazed paper, oil cloth, or other flexible
Waste samples should contain a representative distribution of
material as follows:
particle sizes.
8.1.1 Empty the sample container into the center of the
NOTE 4—Information on obtaining representative samples can also be
sheet.
found in Pierre Gy’s Sampling Theory and Sampling Practice, Volumes I
and II, by F. Picard, CRC Press, 1989.
8.1.2 Flatten out the sample gently with a suitable straight-
edge until it is spread uniformly to a depth at least twice the
7.5 In order to prevent sample contamination or constituent
maximum particle diameter.
loss prior to extraction, keep samples in closed containers
appropriate to the sample type and desired analysis. See 8.1.3 Remix the sample by lifting a corner of the sheet and
Practices D3370 for guidance. Record the storage conditions drawing it across, low down, to the opposite corner in a manner
and handling procedures in the report. that the material is made to roll over and over and does not
D4793 − 09 (2017)
merely slide along. Continue the operation with each corner, where:
proceeding in a clockwise direction. Repeat this operation ten
A = mass of sample after drying, g,
times.
B = original mass of sample, g, and
8.1.4 Lift all four corners of the sheet towards the center S = solids content, g/g.
and, holding all four corners together, raise the entire sheet into
Average the two values obtained. Record the solids content.
the air to form a pocket for the sample.
9.3 Extraction Procedure—If the entire procedure cannot be
8.1.5 Repeat 8.1.2.
conducted without interruption, at least the first four extraction
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 Determine the mass of the extraction vessel to be used
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 Add 100 g (weighed to 60.1 g) of solid waste on a dry
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)
S
this fact.
where:
NOTE 5—For other acceptable methods for mixing and subsampling
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 2-4 must be modified to reflect the use
laboratory, cut a representative section weighing approxi-
of a mass other than 100 g. Replace 100 in these equations with
mately 100 g for testing plus samples for determination for
the mass used. Use of a mass other than 100 g is not
solids content. Shape the sample so that the leaching solution
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 t
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4793 − 09 D4793 − 09 (Reapproved 2017)
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method is a procedure for the sequential leaching of a waste containing at least five %percent 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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety problems,concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appropriate safety safety, health and healthenvironmental practices and
determine the applicability of regulatory limitations prior to use.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D75D75/D75M Practice for Sampling Aggregates
D420 Guide to Site Characterization for Engineering Design and Construction Purposes (Withdrawn 2011)
D653 Terminology Relating to Soil, Rock, and Contained Fluids
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2216 Test Methods for Laboratory Determination of Water (Moisture) Content of Soil and Rock by Mass
D2234/D2234M Practice for Collection of a Gross Sample of Coal
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Closed Conduits
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this test method, see Terminology D1129.
3.2 Symbols:
3.2.1 Variables listed in this test method are defined in the individual sections where they are discussed. A list of defined
variables is also given in Section 11.
3.2.2 Explanation of Variables:
This test method is under the jurisdiction of ASTM Committee D34 on Waste Management and is the direct responsibility of Subcommittee D34.01.04 on Waste Leaching
Techniques.
Current edition approved July 1, 2009Sept. 1, 2017. Published October 2009September 2017. Originally approved in 1988. Last previous edition approved in 20042009
as D4793 – 93 (2004).D4793 – 09. DOI: 10.1520/D4793-09.10.1520/D4793-09R17.
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.
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4793 − 09 (2017)
X¯ = total mean value
t
X¯ = analytical mean value (calculated using data from analysis of standards)
a
S = total standard deviation
tt
S = analytical standard deviation
ta
S = estimated standard deviation due to the extraction procedure
te
S = total single operator standard deviation
ot
S = analytical single operator standard deviation
oa
S = estimated single operator standard deviation due to the extraction procedure
oe
4. Significance and Use
4.1 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.
4.2 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.
4.3 This test method is not intended to simulate site-specific leaching conditions. It has not been demonstrated to simulate actual
disposal site leaching conditions.
4.4 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.
4.5 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.
4.6 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.
4.7 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.
4.8 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).
5. Apparatus
5.1 Straightedge, (suchsuch as a thin-edged yard stick).stick.
5.2 Impermeable Sheet, of glazed paper, oil cloth, or other flexible material of a composition suitable to the analytes of interest.
5.3 Drying Pans or Dishes—Two per waste (for example, aluminum tins, porcelain dishes, or glass weighing pans), suitable to
the waste being tested and the instructions given in 9.2.
5.4 Drying Oven—Any thermostatically controlled drying oven capable of maintaining a steady temperature of 62°C62 °C in
a range from 100 to 110°C.110 °C.
5.5 Desiccator, having the capacity to hold the drying pans described in 5.3 and the crucibles described in 5.8.
5.6 Laboratory Balance, capable of weighing to 0.1 g.
5.7 Pipet, 10-mL capacity.
5.8 Crucibles—Two per waste, porcelain, 20-mL capacity each.
5.9 Analytical Balance, capable of weighing to 0.1 mg.
5.10 Large Glass Funnel.
5.11 Wash Bottle, 500-mL capacity.
5.12 pH Meter—Any pH meter with a readability of 0.01 units and an accuracy of 60.05 units at 25°C25 °C is acceptable.
5.13 Agitation Equipment, of any type that rotates the extraction vessel in an end-over-end fashion at a rate of 0.5 6 0.03 Hz,
such that the axis of rotation is horizontal and it goes through the center of the bottle,bottle (see Fig. 1 and the discussion of
agitation in Appendix X1).
NOTE 1—Similar devices having a different axial arrangement may be used if equivalency can be demonstrated.
5.14 Pressure Filtration Assembly—A pressure filtration 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 pore size filter (see Note 7, pertaining to 9.4).
5.15 Extraction Vessels, cylindrical, wide-mouth, of a composition suitable to the nature of the waste and analyses to be
performed, constructed of materials that will not allow sorption of constituents of interest, and sturdy enough to withstand the
D4793 − 09 (2017)
FIG. 1 Extractors
impact of the falling sample fragments. Container size should be selected so that the sample plus extraction fluid occupy
approximately 95 % of the container. Containers must have water-tightwatertight closure. Containers for samples where gases may
be released should be provided with a venting mechanism.
NOTE 2—Suitable container sizes range from 10 to 11 cm in diameter and 22 to 33 cm in height.
NOTE 3—Venting the container has the potential to affect the concentration of volatile compounds in the extracts.
5.15.1 Extraction vessels should be cleaned in a manner consistent with the analyses to be performed. See Section 13 of
Practices D3370, Section 13.
6. Reagents
6.1 Purity of Reagents—Reagent grade Reagent-grade chemicals shall be used in all tests. Unless otherwise indicated, it is
intended that all reagents shall conform to the specifications of the American Chemical Society, where such specifications are
available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high purity to permit its use
without lessening the accuracy of the determination.
6.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean Type IV reagent water at 18
to 27°C27 °C (Specification D1193). The method by which the water is prepared, that is, distillation, ion exchange, reverse
osmosis, electrodialysis, or a combination thereof, should remain constant throughout testing.
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed by
the American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
D4793 − 09 (2017)
7. Sampling
7.1 Obtain a representative sample of the waste to be tested using ASTM sampling methods developed for the specific industry
where available (see PracticesPractice D75D75/D75M and, Guide D420, Terminology D653, and Test Method D2234/D2234M).
7.2 Where no specific methods are available, sampling methodology for material of similar physical form shall be used.
7.3 The amount of sample to be sent to the laboratory should be sufficient to perform the solids content determination as
specified in 9.2 and to provide 100 g of sample on a dry weight basis for each extraction.
7.4 It is important that the sample of the waste be representative with respect to surface area, as variations in surface area would
directly affect the leaching characteristics of the sample. Waste samples should contain a representative distribution of particle
sizes.
NOTE 4—Information on obtaining representative samples can also be found in Pierre Gy’s Sampling Theory and Sampling Practice, Volumes I and
II, by F. Picard, CRC Press, 1989.
7.5 In order to prevent sample contamination or constituent loss prior to extraction, keep samples in closed containers
appropriate to the sample type and desired analysis. See Practices D3370 for guidance. Record the storage conditions and handling
procedures in the report.
7.6 The time between collection and extraction of the sample should be determined by the nature of the sample and the
information desired. See Practices D3370 for guidance. Report the length of time between sample collection and extraction.
8. Sample Preparation
8.1 For free-flowing particulate solid wastes, obtain a sample of the approximate size required in the test by quartering the
sample (Section 7) received for testing on an impermeable sheet of glazed paper, oil cloth, or other flexible material as follows:
8.1.1 Empty the sample container into the center of the sheet.
8.1.2 Flatten out the sample gently with a suitable straightedge until it is spread uniformly to a depth at least twice the maximum
particle diameter.
8.1.3 Remix the sample by lifting a corner of the sheet and drawing it across, low down, to the opposite corner in a manner
that the material is made to roll over and over and does not merely slide along. Continue the operation with each corner, proceeding
in a clockwise direction. Repeat this operation ten times.
8.1.4 Lift all four corners of the sheet towards the center and, holding all four corners together, raise the entire sheet into the
air to form a pocket for the sample.
8.1.5 Repeat 8.1.2.
8.1.6 With a straightedge (such as a thin-edged yard stick), one at least as long as the flattened mound of sample, gently divide
the sample into quarters. Make an effort to avoid using pressure on the straightedge sufficient to cause damage to the particles.
8.1.7 Discard alternate quarters.
8.1.8 If further reduction of sample size is necessary, repeat 8.1.3 – 8.1.7. Use a sample size to give 100 g of solid for each
extraction. Provide additional samples for determination of solids content. If smaller samples are used in the test, report this fact.
NOTE 5—For other acceptable methods for mixing and subsampling free-flowing solid particulate wastes, see Pierre Gy’s Sampling Theory and
Sampling Practice, Volumes I and II, by F. Picard, CRC Press, 1989. The method of subsampling should be determined by the physical properties of the
waste, analytes of interest, and equipment available.
8.2 For field-cored solid wastes or castings produced in the laboratory, cut a representative section weighing approximately 100
g for testing plus samples for determination for solids content. Shape the sample so that the leaching solution will cover the
material to be leached.
8.3 For multiphasic wastes, mix thoroughly to ensure that a representative sample will be withdrawn. Take samples for
determination of solids content at the same time as the test samples.
9. Procedure
9.1 Record the physical description of the sample to be tested, including particle size so far as it is known.
9.2 Solids Content—Determine the solids content of two separate portions of the sample as follows:
9.2.1 Dry to a constant weight at 104 6 2°C2 °C two dishes or pans of size suitable to the solid waste being tested. Cool in
a desiccator and weigh. Record the values to 60.1 g.
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 physical
form of the waste tested. Use a minimum of 50 g, but use larger samples where particles larger than 10 mm in average diamet
...
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