ASTM D5233-92(1999)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D 5233 – 92 (Reapproved 1999)
Standard Test Method for
Single Batch Extraction Method for Wastes
This standard is issued under the fixed designation D 5233; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope 1.9 This standard does not purport to address all of the
safety problems, if any, associated with its use. It is the
1.1 This test method is applicable to the extraction of
responsibility of the user of this standard to establish appro-
samples of treated or untreated solid wastes or sludges, or
priate safety and health practices and determine the applica-
solidified waste samples, to provide an indication of the
bility of regulatory limitations prior to use. For a specific
leaching potential.
precautionary statement, see Note 8.
1.2 This test method is intended to provide an extract for
measurement of the concentration of the analytes of concern.
2. Referenced Documents
The measured values may be compared against set or chosen
2.1 ASTM Standards:
acceptance levels in some applications.
D 75 Practices for Sampling Aggregates
1.3 If the sole application of the test method is such a
D 420 Practice for Investigating and Sampling Soil and
pass/fail comparison and a total analysis of the waste demon-
Rock for Engineering Purposes
strates that individual analytes are not present in the waste, or
D 653 Terminology Relating to Soil, Rock, and Contained
that the chosen acceptance concentration levels could not
Fluids
possibly be exceeded, the test method need not be run.
D 1129 Terminology Relating to Water
1.4 If the sole application of the test method is such a
D 1193 Specification for Reagent Water
pass/fail comparison and an analysis of any one of the liquid
D 2234 Test Method for Collection of a Gross Sample of
fractions of the extract indicates that the concentration of the
Coal
target analyte is so high that, even after accounting for dilution
D 3370 Practices for Sampling Water
from the other fractions of the extract, it would be equal to or
E 122 Practice for Choice of Sample Size to Estimate A
above an acceptance concentration level, then the waste fails
Measure of Quality for a Lot or Process
the test. In such a case it may not be necessary to analyze the
ES 16 Practice for the Generation of Environmental Data
remaining fractions of the extract.
Related to Waste Management Activities
1.5 This test method is intended to provide an extract
suitable for the measurement of the concentration of analytes
3. Terminology
that will not volatilize under the conditions of the test method.
3.1 Definitions—For definitions of terms used but not de-
1.6 Presence of volatile analytes may be established if an
fined in this test method, see Terminology D 1129.
analysis of the extract obtained using this test method detects
the target volatile analyte. If its concentration is equal to or
4. Summary of Test Method (See Fig. 1)
exceeds an acceptance level for that analyte, the waste fails the
4.1 For wastes containing less than 0.5 % dry solid material,
test. However, extract from this test method shall not be used
the filtrate of the waste, after filtration through a 0.6 to 0.8-μm
to determine the concentration of volatile organic analytes.
glass fiber filter, is defined as the method extract. Extraction of
1.7 This test method is intended to describe only the
,
8 9
the solid is not required for such wastes.
procedure for performing a batch extraction. It does not
describe all of the sampling and analytical requirements that
may be associated with the application of this test method.
Annual Book of ASTM Standards, Vol 04.03.
1.8 The values stated in either SI or inch-pound units are to
Annual Book of ASTM Standards, Vol 04.08.
be regarded as the standard. The values given in parentheses 4
Annual Book of ASTM Standards, Vol 11.01.
are for information only. Annual Book of ASTM Standards, Vol 05.05.
Annual Book of ASTM Standards, Vol 14.02.
Annual Book of ASTM Standards, Vol 11.04 (see 1991 edition).
1 8
This test method is under the jurisdiction of ASTM Committee D34 on Waste Federal Register, Vol 55, No. 61, March 29, 1990. Toxicity Characteristics
Revisions, Final Rule.
Disposal and is the direct responsibility of Subcommittee D34.01.06 on Analytical
Methods. Federal Register, Vol 55, No. 126, June 29, 1990. Toxicity Characteristic
Current edition approved March 15, 1992. Published May 1992. Revisions, Final Rule, Corrections.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 5233
FIG. 1 Method Flow Chart
4.2 For wastes containing greater than or equal to 0.5 % dry be compared with concentration levels acceptable in waste
solid material, the liquid, if any, is separated from the solid disposal, treatment, or production activities.
phase and stored for later analysis. The solid phase is extracted 5.2 The extraction conditions of the test method were
with an amount of extraction fluid equal to 20 times the weight chosen to simulate a potential disposal scenario to which the
of the solid phase. The extraction fluid used is a function of the wastes may be exposed.
alkalinity of the solid phase of the waste. Following extraction, 5.3 One intent of this test method is that the amount of acid
the liquid extract is separated from the solid phase by filtration in the extraction fluids reflect the acid available from the
through a 0.6 to 0.8-μm glass fiber filter. leachate of a specific landfill where municipal and industrial
4.3 If compatible (that is, multiple phases will not form wastes were co-disposed.
upon combination), the initial liquid phase of the waste is 5.4 One intent of this test method is to not allow the pH of
added to the liquid extract, and these are analyzed together. If the extraction fluid to be lower than that of the leachate of a
incompatible, the liquids are analyzed separately and the specific landfill where municipal and industrial wastes were
results are combined mathematically to yield a volume- co-disposed. Therefore, the pH of the extraction fluid was
weighted average concentration. chosen with the following considerations:
5. Significance and Use
5.1 This test method is intended to generate an extract with
Kimmel, T. A., and Friedman, D. A., “Model Assumptions and Rationale
a concentration of the target analyte(s) representative of the
Behind the Development of EP III,” ASTM STP 886, J. K. Petros, et al, Eds., ASTM,
expected release under the scenario simulated, and which can Philadelphia, PA, 1986, pp. 36–53.
D 5233
(1) Not to be less than 4.93 6 0.05 for the extraction of 6.2 Extraction Vessel—Suitable vessels include cylindri-
wastes with an acid neutralization capacity of less than the acid cally shaped, minimum 2-L size, with capacity sufficient to
available in the total volume of extraction fluid used in the hold the sample and the extraction fluid. Head-space is allowed
method (Extraction Fluid No. 1). in this vessel. The extraction bottles may be constructed from
(2) At 2.88 6 0.05, as defined by the pH of the acid, for the various plastic materials, depending on the analytes of interest
extraction of wastes with an acid neutralization capacity of and the nature of the waste. Plastic bottles, other than polytet-
more than the acid available in the extraction fluid used in the rafluoroethylene, shall not be used if organics are to be
method (Extraction Fluid No. 2). investigated. The bottles should be sturdy, in order to withstand
5.5 The interpretation and use of the results of this test the impact of the falling sample fragments, and shall have a
method are limited by the assumptions of a single co-disposal leak-free seal. The use of polytetrafluoroethylene tape is
scenario and by the factors affecting the composition of a recommended to ensure a tight seal. Due to their potential for
landfill leachate and chemical or other differences between a breakage, the use of glass bottles is not recommended.
selected extraction fluid and the real landfill leachate.
NOTE 2—Suitable bottles range from 4.0 to 4.5 in. (102 to 114 mm) in
5.6 This test method may be affected by biological changes
diameter and from 8.5 to 13.0 in. (216 to 330 mm) in height.
in the waste, and it is not designed to isolate or measure the
6.3 Filtration Device—It is recommended that all filtrations
effect of such processes.
be performed in a hood. Wastes should be filtered using
5.7 This test method produces extracts that are amenable to
positive-pressure filtration using a pre-purified grade inert gas
the determination of both minor and major constituents. When
such as nitrogen.
minor constituents are being determined, it is especially
6.3.1 Filter Holder, capable of supporting a glass fiber filter
important that precautions be taken in sample storage and
and able to withstand the pressure needed to accomplish
handling to avoid possible contamination of the samples.
separation (maximum 50 psi or 345 kPa). These devices shall
5.8 The agitation technique, rate, liquid-to-solid ratio, and
have a minimum internal volume of 300 mL and shall be
filtration conditions specified in the method may not be suitable
equipped to accommodate a minimum filter size of 47 mm.
for extracting all types of wastes.
(Filter holders having an internal capacity of 2.2 L and
5.9 This test method is intended to extract the samples in
equipped to accommodate a 142-mm diameter filter are rec-
their original physical state as is, without any size reduction.
ommended.)
However, the sample/extractor interaction is expected to cor-
6.3.1.1 Materials of Construction—Filtration devices shall
relate with the environmental conditions to which a waste may
be made of inert materials that will not leach or adsorb the
be exposed.
analytes of concern. Glass, polytetrafluoroethylene, or type 316
5.10 The extraction conditions defined by this test method
stainless steel equipment may be used when both organic and
are expected to yield steady-state concentrations, determined
inorganic analytes are of concern. Devices made of high-
by the extraction liquid-to-solid ratio and the duration of the
density polyethylene (HDPE), polypropylene (PP), or polyvi-
extraction, which may or may not agree with the concentration
nylchloride (PVC) may be used when only inorganics are of
of an equilibrium.
concern.
6. Apparatus and Materials 6.4 Filters, made of borosilicate glass fiber, containing no
binder materials, and having an effective pore size of 0.6 to
6.1 Agitation Apparatus, capable of rotating the extraction
0.8μ m. Pre-filters must not be used. When inorganic analytes
vessel in an end-over-end fashion (see Fig. 2), at 30 6 2 r/min,
are of concern, the filter shall be acid washed prior to use by
such that the axis of rotation is horizontal and passes through
rinsing with 1 N nitric acid followed by three consecutive
the center of the bottle.
rinses with Type II reagent water as defined in Specification
NOTE 1—Similar devices may be used having a different axle arrange-
D 1193. (A minimum of 1 L per rinse is recommended.) Glass
ment if equivalency can be demonstrated.
fiber filters are fragile and should be handled with care.
6.5 pH Meter, with a readability of 0.01 unit and an
11 accuracy of 60.05 unit at 25°C.
Federal Register, Vol 53, No. 100, May 24, 1988. Proposed Cage Modification
6.6 Laboratory Balance, accurate to within 60.01 g. (All
of TCLP.
weight measurements are to be within6 0.1 g.)
6.7 Beakers or Erlenmeyer Flasks, glass 500-mL, and 2-L.
6.8 Watch-Glass, with an appropriate diameter to cover the
beaker or Erlenmeyer flask.
6.9 Magnetic Stirrer.
6.10 Mold, cylindrical, made of inert, non-adsorbing and
non-contaminating material for casting of laboratory samples.
6.11 Straightedge, made of stainless steel.
6.12 Impermeable Sheet or Glazed Paper.
6.13 Volumetric Flask, 1-L size.
6.14 Drying Oven—Any thermostatically controlled drying
oven capable of maintaining a temperature between 85 and
FIG. 2 Rotary Agitation Apparatus 115°C within 65°C.
D 5233
6.15 Graduated Pipet, readable to 0.1 mL. 8.3 Where no specific methods are available, sampling
6.16 Hot Plate, equipped for agitation and temperature methodology for materials of similar physical form shall be
control capable of maintaining a 50 6 3°C temperature. used.
6.17 Graduated Measuring Cylinder, with a precision of 8.4 It is important that the sample of the waste be represen-
63%. tative with respect to surface area, as variations in surface area
would directly affect the extraction characteristics of the
7. Reagents
sample. Waste samples should contain a representative distri-
bution of particle sizes.
7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
NOTE 3—Information on obtaining representative samples can also be
all reagents shall conform to the specifications of the Commit-
found in Pierre Gy’s Sampling Theory and Practice.
tee on Analytical Reagents of the American Chemical Society,
8.5 Approximately 100 g of solid phase samples are re-
where such specifications are available. Other grades may be
quired for each extraction. Preliminary evaluation also requires
used, provided it is first ascertained that the reagent is of
100 g of solid phase sample. A larger sample size may be
sufficiently high purity to permit its use without lessening the
required, depending on the solids content of the waste sample
accuracy of the determination.
(percent solids; see 10.2.9).
7.2 Purity of Water—Reagent water is defined as water in
8.6 Enough extract should be generated such that the
which an interfering analyte is not observed at or above the
volume will be sufficient to support all of the analyses required.
method detection limit of the analyte(s) of interest. Type II of
If the volume of extract generated by the performance of a
Specification D 1193 or equivalent meets the definition of
single extraction will not be sufficient to perform all of the
reagent water.
analyses to be conducted, it is recommended that more than
7.3 Hydrochloric Acid (HCl), 1 N, made from ACS reagent
one extraction be performed and that the extracts from each
grade.
extraction be combined and then aliquoted for analysis.
7.4 Nitric Acid (HNO ), 1 N, made from ACS reagent
8.7 For the evaluation of solidified or stabilized wastes, or
grade.
both, samples may be cast in the form of a cylinder that will fit
7.5 Sodium
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