ASTM D5233-92(2009)
(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
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.
The extraction conditions of the test method were chosen to simulate a potential disposal scenario to which the wastes may be exposed.
One intent of this test method is that the amount of acid in the extraction fluids reflect the acid available from the leachate of a specific landfill where municipal and industrial wastes were co-disposed.
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).
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.
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.
This test method produces extracts that are amenable to the determination of both minor and major constituents. When minor constituents are being determined, it is especially important that pr...
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 associated with...
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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: D5233 − 92 (Reapproved 2009)
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 problems, 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 and health practices and determine the applica-
measurement of the concentration of the analytes of concern.
bility of regulatory limitations prior to use. For a specific
The measured values may be compared against set or chosen
precautionary statement, see Note 8.
acceptance levels in some applications.
1.3 If the sole application of the test method is such a
2. Referenced Documents
pass/fail comparison and a total analysis of the waste demon-
2.1 ASTM Standards:
strates that individual analytes are not present in the waste, or
D75 Practice for Sampling Aggregates
that the chosen acceptance concentration levels could not
D420 Guide to Site Characterization for Engineering Design
possibly be exceeded, the test method need not be run.
and Construction Purposes (Withdrawn 2011)
1.4 If the sole application of the test method is such a
D653 Terminology Relating to Soil, Rock, and Contained
pass/fail comparison and an analysis of any one of the liquid
Fluids
fractions of the extract indicates that the concentration of the
D1129 Terminology Relating to Water
target analyte is so high that, even after accounting for dilution
D1193 Specification for Reagent Water
from the other fractions of the extract, it would be equal to or
D2234/D2234M Practice for Collection of a Gross Sample
above an acceptance concentration level, then the waste fails
of Coal
the test. In such a case it may not be necessary to analyze the
D3370 Practices for Sampling Water from Closed Conduits
remaining fractions of the extract.
E122 Practice for Calculating Sample Size to Estimate,With
Specified Precision, the Average for a Characteristic of a
1.5 This test method is intended to provide an extract
Lot or Process
suitable for the measurement of the concentration of analytes
ES 16 Practice for the Generation of Environmental Data
that will not volatilize under the conditions of the test method.
Related to Waste Management Activites
1.6 Presence of volatile analytes may be established if an
analysis of the extract obtained using this test method detects
3. Terminology
the target volatile analyte. If its concentration is equal to or
3.1 Definitions—For definitions of terms used but not de-
exceeds an acceptance level for that analyte, the waste fails the
fined in this test method, see Terminology D1129.
test. However, extract from this test method shall not be used
to determine the concentration of volatile organic analytes.
4. Summary of Test Method (See Fig. 1)
1.7 This test method is intended to describe only the
4.1 Forwastescontaininglessthan0.5 %drysolidmaterial,
procedure for performing a batch extraction. It does not
the filtrate of the waste, after filtration through a 0.6 to 0.8-µm
describe all of the sampling and analytical requirements that
may be associated with the application of this test method.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This test method is under the jurisdiction of ASTM Committee D34 on Waste contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Management and is the direct responsibility of Subcommittee D34.01.04 on Waste Standards volume information, refer to the standard’s Document Summary page on
Leaching Techniques. the ASTM website.
Current edition approved Sept. 1, 2009. Published November 2009. Originally The last approved version of this historical standard is referenced on
approved in 1992. Last previous edition approved in 2004 as D5233–1992 (2004). www.astm.org.
DOI: 10.1520/D5233-92R09. 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 (2009)
FIG. 1 Method Flow Chart
glass fiber filter, is defined as the method extract. Extraction of the liquid extract is separated from the solid phase by filtration
5,6
the solid is not required for such wastes. through a 0.6 to 0.8-µm glass fiber filter.
4.2 For wastes containing greater than or equal to 0.5 % dry 4.3 If compatible (that is, multiple phases will not form
solid material, the liquid, if any, is separated from the solid upon combination), the initial liquid phase of the waste is
phase and stored for later analysis.The solid phase is extracted added to the liquid extract, and these are analyzed together. If
with an amount of extraction fluid equal to 20 times the weight incompatible, the liquids are analyzed separately and the
of the solid phase.The extraction fluid used is a function of the results are combined mathematically to yield a volume-
alkalinity of the solid phase of the waste. Following extraction, weighted average concentration.
5. Significance and Use
Federal Register, Vol 55, No. 61, March 29, 1990. Toxicity Characteristics
5.1 This test method is intended to generate an extract with
Revisions, Final Rule.
6 a concentration of the target analyte(s) representative of the
Federal Register, Vol 55, No. 126, June 29, 1990. Toxicity Characteristic
Revisions, Final Rule, Corrections. expected release under the scenario simulated, and which can
D5233 − 92 (2009)
be compared with concentration levels acceptable in waste 6. Apparatus and Materials
disposal, treatment, or production activities.
6.1 Agitation Apparatus, capable of rotating the extraction
vessel in an end-over-end fashion (see Fig. 2), at 30 6 2 r/min,
5.2 The extraction conditions of the test method were
such that the axis of rotation is horizontal and passes through
chosen to simulate a potential disposal scenario to which the
the center of the bottle.
wastes may be exposed.
NOTE 1—Similar devices may be used having a different axle arrange-
5.3 One intent of this test method is that the amount of acid
ment if equivalency can be demonstrated.
in the extraction fluids reflect the acid available from the
6.2 Extraction Vessel—Suitable vessels include cylindri-
leachate of a specific landfill where municipal and industrial
cally shaped, minimum 2-L size, with capacity sufficient to
wastes were co-disposed.
holdthesampleandtheextractionfluid.Head-spaceisallowed
5.4 One intent of this test method is to not allow the pH of
in this vessel. The extraction bottles may be constructed from
the extraction fluid to be lower than that of the leachate of a
various plastic materials, depending on the analytes of interest
specific landfill where municipal and industrial wastes were
and the nature of the waste. Plastic bottles, other than
co-disposed. Therefore, the pH of the extraction fluid was
polytetrafluoroethylene, shall not be used if organics are to be
chosen with the following considerations:
investigated.Thebottlesshouldbesturdy,inordertowithstand
(1) Not to be less than 4.93 6 0.05 for the extraction of
the impact of the falling sample fragments, and shall have a
wasteswithanacidneutralizationcapacityoflessthantheacid
leak-free seal. The use of polytetrafluoroethylene tape is
available in the total volume of extraction fluid used in the
recommended to ensure a tight seal. Due to their potential for
method (Extraction Fluid No. 1).
breakage, the use of glass bottles is not recommended.
(2) At2.88 60.05,asdefinedbythepHoftheacid,forthe
NOTE 2—Suitable bottles range from 4.0 to 4.5 in. (102 to 114 mm) in
extraction of wastes with an acid neutralization capacity of
diameter and from 8.5 to 13.0 in. (216 to 330 mm) in height.
more than the acid available in the extraction fluid used in the
6.3 Filtration Device—It is recommended that all filtrations
method (Extraction Fluid No. 2).
be performed in a hood. Wastes should be filtered using
5.5 The interpretation and use of the results of this test
positive-pressure filtration using a pre-purified grade inert gas
method are limited by the assumptions of a single co-disposal
such as nitrogen.
scenario and by the factors affecting the composition of a
6.3.1 Filter Holder, capable of supporting a glass fiber filter
landfill leachate and chemical or other differences between a
and able to withstand the pressure needed to accomplish
selected extraction fluid and the real landfill leachate.
separation (maximum 50 psi or 345 kPa). These devices shall
5.6 This test method may be affected by biological changes have a minimum internal volume of 300 mL and shall be
in the waste, and it is not designed to isolate or measure the equipped to accommodate a minimum filter size of 47 mm.
effect of such processes. (Filter holders having an internal capacity of 2.2 L and
equipped to accommodate a 142-mm diameter filter are rec-
5.7 This test method produces extracts that are amenable to
ommended.)
the determination of both minor and major constituents. When
6.3.1.1 Materials of Construction—Filtration devices shall
minor constituents are being determined, it is especially
be made of inert materials that will not leach or adsorb the
important that precautions be taken in sample storage and
analytesofconcern.Glass,polytetrafluoroethylene,ortype316
handling to avoid possible contamination of the samples.
stainless steel equipment may be used when both organic and
5.8 The agitation technique, rate, liquid-to-solid ratio, and
inorganic analytes are of concern. Devices made of high-
filtrationconditionsspecifiedinthemethodmaynotbesuitable density polyethylene (HDPE), polypropylene (PP), or polyvi-
for extracting all types of wastes.
nylchloride (PVC) may be used when only inorganics are of
concern.
5.9 This test method is intended to extract the samples in
6.4 Filters, made of borosilicate glass fiber, containing no
their original physical state as is, without any size reduction.
binder materials, and having an effective pore size of 0.6 to
However, the sample/extractor interaction is expected to cor-
relate with the environmental conditions to which a waste may
be exposed.
5.10 The extraction conditions defined by this test method
are expected to yield steady-state concentrations, determined
by the extraction liquid-to-solid ratio and the duration of the
extraction, which may or may not agree with the concentration
of an equilibrium.
Kimmel, T. A., and Friedman, D. A., “Model Assumptions and Rationale
BehindtheDevelopmentofEPIII,” ASTM STP886,J.K.Petros,etal,Eds.,ASTM,
Philadelphia, PA, 1986, pp. 36–53.
Federal Register, Vol 53, No. 100, May 24, 1988. Proposed Cage Modification
of TCLP. FIG. 2 Rotary Agitation Apparatus
D5233 − 92 (2009)
0.8µ m. Pre-filters must not be used. When inorganic analytes 7.6 Glacial Acetic Acid (CH COOH), ACS reagent grade.
are of concern, the filter shall be acid washed prior to use by
7.7 Extraction Fluids—Several batches or multiple volumes
rinsing with 1 N nitric acid followed by three consecutive
of extraction fluids should be prepared in accordance with the
rinses with Type II reagent water as defined in Specification
number of extractions. The volume needed for an individual
D1193. (A minimum of 1 L per rinse is recommended.) Glass
extractionisapproximately2L.Theextractionfluidsshouldbe
fiber filters are fragile and should be handled with care.
monitored frequently for impurities. The pH should be exam-
6.5 pH Meter, with a readability of 0.01 unit and an inedpriortoextractiontoensurethatthesefluidsweremadeup
accuracy of 60.05 unit at 25°C. accurately. If impurities are found or the pH is not within the
specifications, the fluid shall be discarded and fresh extraction
6.6 Laboratory Balance, accurate to within 60.01 g. (All
fluid prepared.
weight measurements are to be within6 0.1 g.)
7.7.1 Extraction Fluid No. 1—Add 5.7 mL glacial acetic
6.7 Beakers or Erlenmeyer Flasks, glass 500-mL, and 2-L.
acid to 500 mL of reagent water, add 64.3 mL of 1 N NaOH,
and dilute to a volume of 1 L.When correctly prepared, the pH
6.8 Watch-Glass, with an appropriate diameter to cover the
beaker or Erlenmeyer flask. of this fluid will be 4.93 6 0.05.
7.7.2 Extraction Fluid No. 2—Dilute 5.7 mL glacial acetic
6.9 Magnetic Stirrer.
acid with reagent water to a volume of 1 L. When correctly
6.10 Mold, cylindrical, made of inert, non-adsorbing and
prepared, the pH of this fluid will be 2.88 6 0.05.
non-contaminating material for casting of laboratory samples.
8. Sampling
6.11 Straightedge, made of stainless steel.
8.1 If representative samples of the waste must be tested,
6.12 Impermeable Sheet or Glazed Paper.
use ASTM Sampling methods developed for the specific
6.13 Volumetric Flask, 1-L size.
industry where available (see Practices D75, D420, D3370,
6.14 Drying Oven—Any thermostatically controlled drying
Terminology D653, and Method D2234/D2234M).
oven capable of maintaining a temperature between 85 and
8.2 All samples shall be collected using an appropriate
115°C within 65°C.
sampling plan to ensure sample integrity and representative-
6.15 Graduated Pipet, readable to 0.1 mL.
ness (see Practice E122).
6.16 Hot Plate, equipped for agitation and temperature
8.3 Where no specific methods are available, sampling
control capable of maintaining a 50 6 3°C temperature.
methodology for materials of similar physical form shall be
used.
6.17 Graduated Measuring Cylinder, with a precision of
63%.
8.4 It is important that the sample of the waste be represen-
tative with respect to surface area, as variations in surface area
7. Reagents
would directly affect the extraction characteristics of the
7.1 Purity of Reagents—Reagent grade chemicals shall be sample. Waste samples should contain a representative distri-
used in all tests. Unless otherwise indicated, it is intended that bution of particle sizes.
all reagents shall conform to the specifications of the Commit-
NOTE 3—Information on obtaining representative samples can also be
t
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