ASTM D5233-92(2023)
(Test Method)Standard Test Method for Single Batch Extraction Method for Wastes
Standard Test Method for Single Batch Extraction Method for Wastes
SIGNIFICANCE AND USE
5.1 This test method is intended to generate an extract with a concentration of the target analyte(s) representative of the expected release under the scenario simulated, and which can be compared with concentration levels acceptable in waste disposal, treatment, or production activities.
5.2 The extraction conditions of the test method were chosen to simulate a potential disposal scenario to which the wastes may be exposed.
5.3 One intent of this test method is that the amount of acid in the extraction fluids reflects the acid available from the leachate of a specific landfill where municipal and industrial wastes were co-disposed.6
5.4 One intent of this test method is to not allow the pH of the extraction fluid to be lower than that of the leachate of a specific landfill where municipal and industrial wastes were co-disposed. Therefore, the pH of the extraction fluid was chosen with the following considerations:
(1) Not to be less than 4.93 ± 0.05 for the extraction of wastes with an acid neutralization capacity of less than the acid available in the total volume of extraction fluid used in the method (Extraction Fluid No. 1).
(2) At 2.88 ± 0.05, as defined by the pH of the acid, for the extraction of wastes with an acid neutralization capacity of more than the acid available in the extraction fluid used in the method (Extraction Fluid No. 2).
5.5 The interpretation and use of the results of this test method are limited by the assumptions of a single co-disposal scenario and by the factors affecting the composition of a landfill leachate and chemical or other differences between a selected extraction fluid and the real landfill leachate.
5.6 This test method may be affected by biological changes in the waste, and it is not designed to isolate or measure the effect of such processes.
5.7 This test method produces extracts that are amenable to the determination of both minor and major constituents. When minor constituents are being determined,...
SCOPE
1.1 This test method is applicable to the extraction of samples of treated or untreated solid wastes or sludges, or solidified waste samples, to provide an indication of the leaching potential.
1.2 This test method is intended to provide an extract for measurement of the concentration of the analytes of concern. The measured values may be compared against set or chosen acceptance levels in some applications.
1.3 If the sole application of the test method is such a pass/fail comparison and a total analysis of the waste demonstrates that individual analytes are not present in the waste, or that the chosen acceptance concentration levels could not possibly be exceeded, the test method need not be run.
1.4 If the sole application of the test method is such a pass/fail comparison and an analysis of any one of the liquid fractions of the extract indicates that the concentration of the target analyte is so high that, even after accounting for dilution from the other fractions of the extract, it would be equal to or above an acceptance concentration level, then the waste fails the test. In such a case it may not be necessary to analyze the remaining fractions of the extract.
1.5 This test method is intended to provide an extract suitable for the measurement of the concentration of analytes that will not volatilize under the conditions of the test method.
1.6 Presence of volatile analytes may be established if an analysis of the extract obtained using this test method detects the target volatile analyte. If its concentration is equal to or exceeds an acceptance level for that analyte, the waste fails the test. However, extract from this test method shall not be used to determine the concentration of volatile organic analytes.
1.7 This test method is intended to describe only the procedure for performing a batch extraction. It does not describe all of the sampling and analytical requirements that may be associate...
General Information
- Status
- Published
- Publication Date
- 31-Oct-2023
- Technical Committee
- D34 - Waste Management
- Drafting Committee
- D34.01.04 - Waste Leaching Techniques
Relations
- Effective Date
- 01-Nov-2023
- Effective Date
- 01-May-2020
- Effective Date
- 01-May-2020
Overview
ASTM D5233-92(2023) – Standard Test Method for Single Batch Extraction Method for Wastes is a widely recognized method developed by ASTM International for evaluating the leaching potential of waste materials. This standard provides a systematic batch extraction protocol designed to simulate conditions similar to those found in landfills where municipal and industrial wastes are co-disposed. By generating a solution (extract) from waste samples under controlled conditions, the method assesses the potential for contaminants to leach out and thus supports informed decisions regarding safe waste handling, treatment, and disposal.
The test is applicable to both treated and untreated solid wastes, sludges, and solidified waste samples. It delivers crucial information that can be compared against regulatory or site-specific acceptance levels, helping facilities meet compliance requirements and minimize environmental risks.
Key Topics
- Purpose: The method simulates a potential disposal scenario by extracting wastes in a manner that reflects landfill leachate conditions where municipal and industrial materials are co-disposed.
- Application Scope:
- Extraction of both treated and untreated solid wastes, sludges, and solidified waste samples.
- Measurement of target analytes (non-volatile) in the resulting extract.
- Comparative assessment of measured concentrations against regulatory limits.
- Extraction Conditions:
- The extraction fluid pH mimics real landfill scenarios, being carefully selected based on the acid neutralization capacity of the waste.
- For wastes with low acid neutralization capacity: extraction fluid pH ≥ 4.93.
- For wastes with high acid neutralization capacity: extraction fluid pH ≈ 2.88.
- The extraction fluid pH mimics real landfill scenarios, being carefully selected based on the acid neutralization capacity of the waste.
- Result Interpretation: Results are specific to the single co-disposal scenario simulated and may not reflect all real-life landfill conditions. The method is not designed to simulate or measure biological transformations.
- Analyte Suitability: The extract is suitable for both major and minor constituent analysis, but is not intended for volatile organic analytes. However, detection of a volatile analyte above acceptance levels indicates a waste failure.
Applications
- Environmental Compliance: Provides data for regulatory pass/fail decisions regarding the acceptability of waste for landfilling or other disposal methods.
- Waste Characterization: Helps waste generators and treatment facilities understand the leaching behavior of their materials, supporting safer design and management practices.
- Risk Assessment: Assists in evaluating the environmental impact of specific wastes, especially within the context of landfill leachate management and groundwater protection.
- Quality Control in Waste Treatment: Used to validate the effectiveness of stabilization or solidification processes in limiting leaching of hazardous constituents.
- Due Diligence for Waste Management: Informs decision-making for waste minimization, beneficial reuse, and compliance with international, national, or local waste regulations.
Related Standards
- ASTM D75/D75M: Standard Practice for Sampling Aggregates
- ASTM D420: Guide for Site Characterization for Engineering Design and Construction
- ASTM D653: Terminology Relating to Soil, Rock, and Contained Fluids
- ASTM D1193: Specification for Reagent Water
- ASTM D2234/D2234M: Practice for Collection of a Gross Sample of Coal
- ASTM D3370: Practices for Sampling Water from Flowing Process Streams
- ASTM E122: Practice for Calculating Sample Size to Estimate Lot or Process Characteristics
- ASTM ES 16: Practice for Generation of Environmental Data Related to Waste Management
Referencing and following ASTM D5233-92(2023) ensures adherence to international standardization principles and supports global best practices in waste management and environmental monitoring. The standard is an essential tool for laboratories, landfill operators, waste generators, and environmental compliance professionals seeking reliable and comparable leachability data.
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ASTM D5233-92(2023) - Standard Test Method for Single Batch Extraction Method for Wastes
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Frequently Asked Questions
ASTM D5233-92(2023) is a standard published by ASTM International. Its full title is "Standard Test Method for Single Batch Extraction Method for Wastes". This standard covers: SIGNIFICANCE AND USE 5.1 This test method is intended to generate an extract with a concentration of the target analyte(s) representative of the expected release under the scenario simulated, and which can be compared with concentration levels acceptable in waste disposal, treatment, or production activities. 5.2 The extraction conditions of the test method were chosen to simulate a potential disposal scenario to which the wastes may be exposed. 5.3 One intent of this test method is that the amount of acid in the extraction fluids reflects the acid available from the leachate of a specific landfill where municipal and industrial wastes were co-disposed.6 5.4 One intent of this test method is to not allow the pH of the extraction fluid to be lower than that of the leachate of a specific landfill where municipal and industrial wastes were co-disposed. Therefore, the pH of the extraction fluid was chosen with the following considerations: (1) Not to be less than 4.93 ± 0.05 for the extraction of wastes with an acid neutralization capacity of less than the acid available in the total volume of extraction fluid used in the method (Extraction Fluid No. 1). (2) At 2.88 ± 0.05, as defined by the pH of the acid, for the extraction of wastes with an acid neutralization capacity of more than the acid available in the extraction fluid used in the method (Extraction Fluid No. 2). 5.5 The interpretation and use of the results of this test method are limited by the assumptions of a single co-disposal scenario and by the factors affecting the composition of a landfill leachate and chemical or other differences between a selected extraction fluid and the real landfill leachate. 5.6 This test method may be affected by biological changes in the waste, and it is not designed to isolate or measure the effect of such processes. 5.7 This test method produces extracts that are amenable to the determination of both minor and major constituents. When minor constituents are being determined,... SCOPE 1.1 This test method is applicable to the extraction of samples of treated or untreated solid wastes or sludges, or solidified waste samples, to provide an indication of the leaching potential. 1.2 This test method is intended to provide an extract for measurement of the concentration of the analytes of concern. The measured values may be compared against set or chosen acceptance levels in some applications. 1.3 If the sole application of the test method is such a pass/fail comparison and a total analysis of the waste demonstrates that individual analytes are not present in the waste, or that the chosen acceptance concentration levels could not possibly be exceeded, the test method need not be run. 1.4 If the sole application of the test method is such a pass/fail comparison and an analysis of any one of the liquid fractions of the extract indicates that the concentration of the target analyte is so high that, even after accounting for dilution from the other fractions of the extract, it would be equal to or above an acceptance concentration level, then the waste fails the test. In such a case it may not be necessary to analyze the remaining fractions of the extract. 1.5 This test method is intended to provide an extract suitable for the measurement of the concentration of analytes that will not volatilize under the conditions of the test method. 1.6 Presence of volatile analytes may be established if an analysis of the extract obtained using this test method detects the target volatile analyte. If its concentration is equal to or exceeds an acceptance level for that analyte, the waste fails the test. However, extract from this test method shall not be used to determine the concentration of volatile organic analytes. 1.7 This test method is intended to describe only the procedure for performing a batch extraction. It does not describe all of the sampling and analytical requirements that may be associate...
SIGNIFICANCE AND USE 5.1 This test method is intended to generate an extract with a concentration of the target analyte(s) representative of the expected release under the scenario simulated, and which can be compared with concentration levels acceptable in waste disposal, treatment, or production activities. 5.2 The extraction conditions of the test method were chosen to simulate a potential disposal scenario to which the wastes may be exposed. 5.3 One intent of this test method is that the amount of acid in the extraction fluids reflects the acid available from the leachate of a specific landfill where municipal and industrial wastes were co-disposed.6 5.4 One intent of this test method is to not allow the pH of the extraction fluid to be lower than that of the leachate of a specific landfill where municipal and industrial wastes were co-disposed. Therefore, the pH of the extraction fluid was chosen with the following considerations: (1) Not to be less than 4.93 ± 0.05 for the extraction of wastes with an acid neutralization capacity of less than the acid available in the total volume of extraction fluid used in the method (Extraction Fluid No. 1). (2) At 2.88 ± 0.05, as defined by the pH of the acid, for the extraction of wastes with an acid neutralization capacity of more than the acid available in the extraction fluid used in the method (Extraction Fluid No. 2). 5.5 The interpretation and use of the results of this test method are limited by the assumptions of a single co-disposal scenario and by the factors affecting the composition of a landfill leachate and chemical or other differences between a selected extraction fluid and the real landfill leachate. 5.6 This test method may be affected by biological changes in the waste, and it is not designed to isolate or measure the effect of such processes. 5.7 This test method produces extracts that are amenable to the determination of both minor and major constituents. When minor constituents are being determined,... SCOPE 1.1 This test method is applicable to the extraction of samples of treated or untreated solid wastes or sludges, or solidified waste samples, to provide an indication of the leaching potential. 1.2 This test method is intended to provide an extract for measurement of the concentration of the analytes of concern. The measured values may be compared against set or chosen acceptance levels in some applications. 1.3 If the sole application of the test method is such a pass/fail comparison and a total analysis of the waste demonstrates that individual analytes are not present in the waste, or that the chosen acceptance concentration levels could not possibly be exceeded, the test method need not be run. 1.4 If the sole application of the test method is such a pass/fail comparison and an analysis of any one of the liquid fractions of the extract indicates that the concentration of the target analyte is so high that, even after accounting for dilution from the other fractions of the extract, it would be equal to or above an acceptance concentration level, then the waste fails the test. In such a case it may not be necessary to analyze the remaining fractions of the extract. 1.5 This test method is intended to provide an extract suitable for the measurement of the concentration of analytes that will not volatilize under the conditions of the test method. 1.6 Presence of volatile analytes may be established if an analysis of the extract obtained using this test method detects the target volatile analyte. If its concentration is equal to or exceeds an acceptance level for that analyte, the waste fails the test. However, extract from this test method shall not be used to determine the concentration of volatile organic analytes. 1.7 This test method is intended to describe only the procedure for performing a batch extraction. It does not describe all of the sampling and analytical requirements that may be associate...
ASTM D5233-92(2023) is classified under the following ICS (International Classification for Standards) categories: 13.030.40 - Installations and equipment for waste disposal and treatment. The ICS classification helps identify the subject area and facilitates finding related standards.
ASTM D5233-92(2023) has the following relationships with other standards: It is inter standard links to ASTM D5233-92(2017), ASTM D1129-13(2020)e2, ASTM D1129-13(2020)e1. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
ASTM D5233-92(2023) is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
Standards Content (Sample)
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: D5233 − 92 (Reapproved 2023)
Standard Test Method for
Single Batch Extraction Method for Wastes
This standard is issued under the fixed designation D5233; 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 1.8 The values stated in either SI or inch-pound units are to
be regarded as the standard. The values given in parentheses
1.1 This test method is applicable to the extraction of
are for information only.
samples of treated or untreated solid wastes or sludges, or
1.9 This standard does not purport to address all of the
solidified waste samples, to provide an indication of the
safety concerns, if any, associated with its use. It is the
leaching potential.
responsibility of the user of this standard to establish appro-
1.2 This test method is intended to provide an extract for
priate safety, health, and environmental practices and deter-
measurement of the concentration of the analytes of concern.
mine the applicability of regulatory limitations prior to use.
The measured values may be compared against set or chosen
For a specific precautionary statement, see Note 8.
acceptance levels in some applications.
1.10 This international standard was developed in accor-
1.3 If the sole application of the test method is such a
dance with internationally recognized principles on standard-
pass/fail comparison and a total analysis of the waste demon-
ization established in the Decision on Principles for the
strates that individual analytes are not present in the waste, or
Development of International Standards, Guides and Recom-
that the chosen acceptance concentration levels could not
mendations issued by the World Trade Organization Technical
possibly be exceeded, the test method need not be run.
Barriers to Trade (TBT) Committee.
1.4 If the sole application of the test method is such a
2. Referenced Documents
pass/fail comparison and an analysis of any one of the liquid
fractions of the extract indicates that the concentration of the 2.1 ASTM Standards:
target analyte is so high that, even after accounting for dilution D75/D75M Practice for Sampling Aggregates
from the other fractions of the extract, it would be equal to or D420 Guide for Site Characterization for Engineering De-
above an acceptance concentration level, then the waste fails sign and Construction Purposes
the test. In such a case it may not be necessary to analyze the D653 Terminology Relating to Soil, Rock, and Contained
remaining fractions of the extract. Fluids
D1129 Terminology Relating to Water
1.5 This test method is intended to provide an extract
D1193 Specification for Reagent Water
suitable for the measurement of the concentration of analytes
D2234/D2234M Practice for Collection of a Gross Sample
that will not volatilize under the conditions of the test method.
of Coal
1.6 Presence of volatile analytes may be established if an
D3370 Practices for Sampling Water from Flowing Process
analysis of the extract obtained using this test method detects
Streams
the target volatile analyte. If its concentration is equal to or
E122 Practice for Calculating Sample Size to Estimate, With
exceeds an acceptance level for that analyte, the waste fails the
Specified Precision, the Average for a Characteristic of a
test. However, extract from this test method shall not be used
Lot or Process
to determine the concentration of volatile organic analytes.
ES 16 Practice for the Generation of Environmental Data
Related to Waste Management Activites
1.7 This test method is intended to describe only the
procedure for performing a batch extraction. It does not
3. Terminology
describe all of the sampling and analytical requirements that
may be associated with the application of this test method.
3.1 Definitions—For definitions of terms used but not de-
fined in this test method, see Terminology D1129.
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 For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Leaching Techniques. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved Nov. 1, 2023. Published November 2023. Originally Standards volume information, refer to the standard’s Document Summary page on
approved in 1992. Last previous edition approved in 2017 as D5233 – 92 (2017). the ASTM website.
DOI: 10.1520/D5233-92R23. Annual Book of ASTM Standards, Vol 11.04 (see 1991 edition).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5233 − 92 (2023)
4. Summary of Test Method (See Fig. 1) 4.3 If compatible (that is, multiple phases will not form
upon combination), the initial liquid phase of the waste is
4.1 For wastes containing <0.5 % dry solid material, the
added to the liquid extract, and these are analyzed together. If
filtrate of the waste, after filtration through a 0.6 to 0.8 μm
incompatible, the liquids are analyzed separately and the
glass fiber filter, is defined as the method extract. Extraction of
4,5 results are combined mathematically to yield a volume-
the solid is not required for such wastes.
weighted average concentration.
4.2 For wastes containing ≥0.5 % dry solid material, the
liquid, if any, is separated from the solid phase and stored for
5. Significance and Use
later analysis. The solid phase is extracted with an amount of
5.1 This test method is intended to generate an extract with
extraction fluid equal to 20 times the weight of the solid phase.
a concentration of the target analyte(s) representative of the
The extraction fluid used is a function of the alkalinity of the
expected release under the scenario simulated, and which can
solid phase of the waste. Following extraction, the liquid
be compared with concentration levels acceptable in waste
extract is separated from the solid phase by filtration through a
disposal, treatment, or production activities.
0.6 to 0.8 μm glass fiber filter.
5.2 The extraction conditions of the test method were
chosen to simulate a potential disposal scenario to which the
wastes may be exposed.
Federal Register, Vol 55, No. 61, March 29, 1990. Toxicity Characteristics
5.3 One intent of this test method is that the amount of acid
Revisions, Final Rule.
in the extraction fluids reflects the acid available from the
Federal Register, Vol 55, No. 126, June 29, 1990. Toxicity Characteristic
Revisions, Final Rule, Corrections.
FIG. 1 Method Flow Chart
D5233 − 92 (2023)
leachate of a specific landfill where municipal and industrial
wastes were co-disposed.
5.4 One intent of this test method is to not allow the pH of
the extraction fluid to be lower than that of the leachate of a
specific landfill where municipal and industrial wastes were
co-disposed. Therefore, the pH of the extraction fluid was
chosen with the following considerations:
(1) Not to be less than 4.93 6 0.05 for the extraction of
wastes with an acid neutralization capacity of less than the acid
available in the total volume of extraction fluid used in the
method (Extraction Fluid No. 1).
FIG. 2 Rotary Agitation Apparatus
(2) At 2.88 6 0.05, as defined by the pH of the acid, for the
extraction of wastes with an acid neutralization capacity of
more than the acid available in the extraction fluid used in the
6.2 Extraction Vessel—Suitable vessels include cylindri-
method (Extraction Fluid No. 2).
cally shaped, minimum 2 L size, with capacity sufficient to
hold the sample and the extraction fluid. Headspace is allowed
5.5 The interpretation and use of the results of this test
in this vessel. The extraction bottles may be constructed from
method are limited by the assumptions of a single co-disposal
various plastic materials, depending on the analytes of interest
scenario and by the factors affecting the composition of a
and the nature of the waste. Plastic bottles, other than
landfill leachate and chemical or other differences between a
polytetrafluoroethylene, shall not be used if organics are to be
selected extraction fluid and the real landfill leachate.
investigated. The bottles should be sturdy in order to withstand
5.6 This test method may be affected by biological changes
the impact of the falling sample fragments, and shall have a
in the waste, and it is not designed to isolate or measure the
leak-free seal. The use of polytetrafluoroethylene tape is
effect of such processes.
recommended to ensure a tight seal. Due to their potential for
5.7 This test method produces extracts that are amenable to
breakage, the use of glass bottles is not recommended.
the determination of both minor and major constituents. When
NOTE 2—Suitable bottles range from 4.0 to 4.5 in. (102 to 114 mm) in
minor constituents are being determined, it is especially
diameter and from 8.5 to 13.0 in. (216 to 330 mm) in height.
important that precautions be taken in sample storage and
6.3 Filtration Device—It is recommended that all filtrations
handling to avoid possible contamination of the samples.
be performed in a hood. Wastes should be filtered using
5.8 The agitation technique, rate, liquid-to-solid ratio, and
positive-pressure filtration using a pre-purified grade inert gas
filtration conditions specified in the method may not be suitable
such as nitrogen.
for extracting all types of wastes.
6.3.1 Filter Holder, capable of supporting a glass fiber filter
and able to withstand the pressure needed to accomplish
5.9 This test method is intended to extract the samples in
separation (maximum 50 psi or 345 kPa). These devices shall
their original physical state as is, without any size reduction.
have a minimum internal volume of 300 mL and shall be
However, the sample/extractor interaction is expected to cor-
equipped to accommodate a minimum filter size of 47 mm.
relate with the environmental conditions to which a waste may
(Filter holders having an internal capacity of 2.2 L and
be exposed.
equipped to accommodate a 142 mm diameter filter are
5.10 The extraction conditions defined by this test method
recommended.)
are expected to yield steady-state concentrations, determined
6.3.1.1 Materials of Construction—Filtration devices shall
by the extraction liquid-to-solid ratio and the duration of the
be made of inert materials that will not leach or adsorb the
extraction, which may or may not agree with the concentration
analytes of concern. Glass, polytetrafluoroethylene, or type 316
of an equilibrium.
stainless steel equipment may be used when both organic and
inorganic analytes are of concern. Devices made of high-
6. Apparatus and Materials
density polyethylene (HDPE), polypropylene (PP), or polyvi-
6.1 Agitation Apparatus, capable of rotating the extraction
nylchloride (PVC) may be used when only inorganics are of
vessel in an end-over-end fashion (see Fig. 2), at 30 6 2 r/min,
concern.
such that the axis of rotation is horizontal and passes through
6.4 Filters, made of borosilicate glass fiber, containing no
the center of the bottle.
binder materials, and having an effective pore size of 0.6 to
NOTE 1—Similar devices may be used having a different axle arrange- 0.8 μm. Pre-filters must not be used. When inorganic analytes
ment if equivalency can be demonstrated.
are of concern, the filter shall be acid washed prior to use by
rinsing with 1 N nitric acid followed by three consecutive
rinses with Type II reagent water as defined in Specification
D1193. (A minimum of 1 L per rinse is recommended.) Glass
Kimmel, T. A., and Friedman, D. A., “Model Assumptions and Rationale
Behind the Development of EP III,” ASTM STP 886, J. K. Petros, et al., Eds., fiber filters are fragile and should be handled with care.
ASTM, West Conshohocken, PA, 1986, pp. 36–53.
6.5 pH Meter, with a readability of 0.01 unit and an
Federal Register, Vol 53, No. 100, May 24, 1988. Proposed Cage Modification
of TCLP. accuracy of 60.05 unit at 25 °C.
D5233 − 92 (2023)
6.6 Laboratory Balance, accurate to within 60.01 g. (All accurately. If impurities are found or the pH is not within the
weight measurements are to be within 60.1 g.) specifications, the fluid shall be discarded and fresh extraction
fluid prepared.
6.7 Beakers or Erlenmeyer Flasks, glass, 500 mL and 2 L.
7.7.1 Extraction Fluid No. 1—Add 5.7 mL glacial acetic
6.8 Watch Glass, with an appropriate diameter to cover the
acid to 500 mL of reagent water, add 64.3 mL of 1 N NaOH,
beaker or Erlenmeyer flask.
and dilute to a volume of 1 L. When correctly prepared, the pH
of this fluid will be 4.93 6 0.05.
6.9 Magnetic Stirrer.
7.7.2 Extraction Fluid No. 2—Dilute 5.7 mL glacial acetic
6.10 Mold, cylindrical, made of inert, non-adsorbing and
acid with reagent water to a volume of 1 L. When correctly
non-contaminating material for casting of laboratory samples.
prepared, the pH of this fluid will be 2.88 6 0.05.
6.11 Straightedge, made of stainless steel.
8. Sampling
6.12 Impermeable Sheet or Glazed Paper.
8.1 If representative samples of the waste must be tested,
6.13 Volumetric Flask, 1 L size.
use ASTM sampling methods developed for the specific
6.14 Drying Oven—Any thermostatically controlled drying
industry where available (see Practices D75/D75M and D3370,
oven capable of maintaining a temperature between 85 and
Guide D420, Terminology D653, and Practice D2234/
115 °C within 65 °C.
D2234M).
6.15 Graduated Pipet, readable to 0.1 mL.
8.2 All samples shall be collected using an appropriate
sampling plan to ensure sample integrity and representative-
6.16 Hot Plate, equipped for agitation and temperature
ness (see Practice E122).
control capable of maintaining a 50 6 3 °C temperature.
8.3 Where no specific methods are available, sampling
6.17 Graduated Measuring Cylinder, with a precision of
methodology for materials of similar physical form shall be
63 %.
used.
7. Reagents
8.4 It is important that the sample of the waste be represen-
7.1 Purity of Reagents—Reagent grade chemicals shall be
tative with respect to surface area, as variations in surface area
used in all tests. Unless otherwise indicated, it is intended that
would directly affect the extraction characteristics of the
all reagents shall conform to the specifications of the Commit-
sample. Waste samples should contain a representative distri-
tee on Analytical Reagents of the American Chemical Society,
bution of particle sizes.
where such specifications are available. Other grades may be
NOTE 3—Information on obtaining representative samples can also be
used, provided it is first ascertained that the reagent is of 9
found in Pierre Gy’s Sampling Theory and Practice.
sufficiently high purity to permit its use without lessening the
8.5 Approximately 100 g of solid phase samples are re-
accuracy of the determination.
quired for each extraction. Preliminary evaluation also requires
7.2 Purity of Water—Reagent water is defined as water in
100 g of solid phase sample. A larger sample size may be
which an interfering analyte is not observed at or above the
required, depending on the solids content of the waste sample
method detection limit of the analyte(s) of interest. Type II of
(percent solids; see 10.2.9).
Specification D1193 or equivalent meets the definition of
8.6 Enough extract should be generated such that the
reagent water.
volume will be sufficient to support all of the analyses required.
7.3 Hydrochloric Acid (HCl), 1 N, made from ACS reagent
If the volume of extract generated by the performance of a
grade.
single extraction will not be sufficient to perform all of the
analyses to be conducted, it is recommended that more than
7.4 Nitric Acid (HNO ), 1 N, made from ACS reagent grade.
one extraction be performed and that the extracts from each
7.5 Sodium Hydroxide (NaOH), 1 N, made from ACS
extraction be combined and then aliquoted for analysis.
reagent grade.
8.7 For the evaluation of solidified or stabilized wastes, or
7.6 Glacial Acetic Acid (CH COOH), ACS reagent grade.
both, samples may be cast in the form of a cylinder that will fit
7.7 Extraction Fluids—Several batches or multiple volumes
into the extraction apparatus. Such cylinders may be used for
of extraction fluids should be prepared in accordance with the
the evaluation. The casting may be allowed to cure for 30 days
number of extractions. The volume needed for an individual
before the extraction procedure is performed. For other mono-
extraction is approximately 2 L. The extraction fluids should be
lithic materials, a coring may be produced that will fit into the
monitored frequently for impurities. The pH should be exam-
extraction apparatus. Waste materials to which these casting
ined prior to extraction to ensure that these fluids were made up
and coring procedures apply include concrete materials, rock,
wood, slag, and so forth.
8 8.8 Quality control measures may require additional
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not samples.
listed by the American Chemical Society, see Analar 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, Pitard, F., Pierre Gy’s Sampling Theory and Practice, Volumes I and II, CRC
MD. Press, 1989.
D5233 − 92 (2023)
9. Sample Handling and Preparation or their portions for metallic analyte determinations should be
acidified with nitric acid to pH <2 unless precipitation occurs.
9.1 For free-flowing particulate solid wastes, obtain a
To minimize losses, filtrates or extracts or their portions for
sample in accordance with the requirements of Section 8 by
organic contaminant determinations shall not be allowed to
quartering the sample received for testing on an impermeable
make contact with the atmosphere (that is, headspace).
sheet of glazed paper or other flexible non-contaminating
material as follows: 9.7 Sample maximum holding times (days) are given in
9.1.1 Empty the sample container into the center of the Table 1.
sheet.
9.1.2 Flatten out the sample gently with a suitable straight-
10. Preliminary Evaluations and Pre-Extraction
edge until it is spread uniformly to a depth at least twice the Procedures
maximum particle diameter.
10.1 Perform preliminary method evaluations on a mini-
9.1.3 Remix the sample by lifting a corner of the sheet and
mum 100 g aliquot of waste. This aliquot may not undergo the
drawing low across to the opposite corner in the manner that
actual extraction. These preliminary evaluations include the
the material is made to roll over and over and does not merely
determination of the following: (1) percent solids, (2) whether
slide along. Return that corner to its original position. Continue
the waste contains dry solids in excess of 0.5 %, and (3) which
the operation with each corner, proceeding in a clockwise
of the two extraction fluids is to be used for extraction of the
direction. Repeat this cycle ten times.
waste.
9.1.4 Lift all four corners of the sheet toward the center and,
10.2 Preliminary Determination of Percent Solids—Percent
holding all four corners together, raise the entire sheet into the
solids is defined as that fraction of the waste sample (as a
air to form a pocket for the sample.
percent of the total sample w/w) from which no liquid may be
9.1.5 Repeat 9.1.2.
forced out by an applied pressure as described below.
9.1.6 Gently divide the sample into quarters with a
10.2.1 If the waste will obviously yield no free liquid when
straightedge, one at least as long as the flattened mound of
subjected to pressure filtration of this method (that is, 100 %
sample. Make an effort to avoid using pressure on the straight-
solids), proceed to 10.4.
edge sufficient to cause damage to the particles.
9.1.7 Discard alternate quarters.
NOTE 4—Some materials may look like dry solids but may release
9.1.8 If further reduction of the sample volume is necessary,
liquids under pressure, for example, adsorbents, filter cakes, paint, and
other sludges. If uncertain, proceed to the filtration step (10.2.2).
repeat 9.1.3 – 9.1.7. Use a sample volume to give 100 g of solid
for each extraction. Provide additional samples for the prelimi-
10.2.2 If the sample is liquid or multi-phasic, liquid/solid
nary evaluation.
separation to make a preliminary evaluation of percent solids is
required. This involves the filtration device described in 6.3,
9.2 For field-cored solid wastes or castings produced in the
and the procedure is outlined in 10.2.3 – 10.2.9.
laboratory, cut a representative section weighing approxi-
10.2.3 Pre-weigh the filter and the container that will
mately 100 g for each extraction plus the preliminary evalua-
receive the filtrate.
tion. Take samples for the preliminary evaluation at the same
10.2.4 Assemble the filter holder and filter following the
time as the test samples.
manufacturer’s instructions. Place the filter on the support
9.2.1 If necessary, shape the sample so that its largest
screen and secure.
dimension would not exceed the radius of the extraction bottle.
10.2.
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