ASTM D5284-93(2004)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D 5284 – 93 (Reapproved 2004)
Standard Test Method for
Sequential Batch Extraction of Waste with Acidic Extraction
Fluid
This standard is issued under the fixed designation D 5284; 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 D 1193 Specification for Reagent Water
D 2234 Test Methods for Collection of a Gross Sample of
1.1 This test method provides a procedure for the sequential
Coal
leaching of a waste containing at least 5 % dry solids in order
D 2777 Practice for Determination of Precision and Bias of
to generate solutions to be used to determine the constituents
Methods of Committee D-19 on Water
leached under the specified testing conditions.
D 3370 Practices for Sampling Water
1.2 This test method calls for the shaking of a known weight
D 4793 Test Method for Sequential Batch Extraction of
of waste with acidic extraction fluid of a specified composition
Waste with Water
as well as the separation of the liquid phase for analysis. The
pH of the extraction fluid is to reflect the pH of acidic
3. Terminology
precipitation in the geographic region in which the waste being
3.1 Definitions—For definitions of terms used in this test
tested is to be disposed. The procedure is conducted ten times
method, see Terminology D 1129.
in sequence on the same sample of waste, and it generates ten
3.2 Symbols:Symbols—Variables listed in this test method
solutions.
are defined in the individual sections in which they are
1.3 This test method is intended to describe the procedure
discussed. A list of the defined variables is also provided in
for performing sequential batch extractions only. It does not
Section 11.
describe all types of sampling and analytical requirements that
may be associated with its application.
4. Significance and Use
1.4 The values stated in SI units are to be regarded as the
4.1 This test method is intended as a means for obtaining
standard.
sequential extracts of a waste. The extracts may be used to
1.5 This standard does not purport to address all of the
estimate the release of certain constituents of the waste under
safety problems, if any, associated with its use. It is the
the laboratory conditions described in this test method.
responsibility of the user of this standard to establish appro-
4.2 The pH of the extraction fluid used in this test method is
priate safety and health practices and determine the applica-
to reflect the pH of acidic precipitation in the geographic region
bility of regulatory limitations prior to use.
in which the waste being tested is to be disposed.
2. Referenced Documents
NOTE 1—Possible sources of information concerning the pH of precipi-
2.1 ASTM Standards: tation in the geographic region of interest include state and federal
environmental agencies, state universities, libraries, etc.
D 75 Practice for Sampling Aggregates
NOTE 2—For sequential batch extraction of waste using a nonacidic
D 420 Guide to Site Characterization for Engineering, De-
extraction fluid, see Test Method D 4793.
sign and Construction Purposes
4.3 An intent of this test method is for the final pH of each
D 653 Terminology Relating to Soil, Rock, and Contained
of the extracts to reflect the interaction of the extractant with
Fluids
the buffering capacity of the waste.
D 1129 Terminology Relating to Water
4.4 This test method is not intended to provide extracts that
are representative of the actual leachate produced from a waste
This test method is under the jurisdiction of ASTM Committee D34 on Waste
in the field or to produce extracts to be used as the sole basis
Management and is the direct responsibility of Subcommittee D34.01.04 on
of engineering design.
Ancillary Topics.
4.5 This test method has not been demonstrated to simulate
Current edition approved Sept. 15, 1993. Published November 1993. Originally
published as D 5284–92. Last previous edition D 5284–92.
actual disposal site leaching conditions.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4.6 This test method produces extracts that are amenable to
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
the determination of both major and minor (trace) constituents.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. When minor constituents are being determined, it is especially
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D 5284 – 93 (2004)
important that precautions be taken in sample storage and the impact of the falling sample fragments. The size of the
handling to avoid possible contamination of the samples. container should be selected so that the sample plus extraction
4.7 This test method has been tested to determine its fluid occupy approximately 95 % of the container. The con-
applicability to certain inorganic components in the waste. This tainers must have water-tight closures. Containers for samples
test method has not been tested for applicability to organic in which gases may be released should be provided with
substances, volatile matter (see Note 5), or biologically active venting mechanisms.
samples.
NOTE 4—Suitable container sizes range from 4.0 to 4.5 in. in diameter
4.8 The agitation technique, rate, liquid-to-solid ratio, and
and 8.5 to 13.0 in. in height.
filtration conditions specified in the procedure may not be
NOTE 5—The venting of the container has the potential to affect the
suitable for extracting all types of wastes (see Sections 7 and 8 concentration of volatile compounds in the extracts.
and Appendix X1).
5.21.1 Extraction vessels should be cleaned in a manner
consistent with the analyses to be performed (see Section 13 of
5. Apparatus
Practice D 3370).
5.1 Straight Edge, such as a thin-edged yardstick.
6. Reagents
5.2 Impermeable Sheet, of glazed paper, oil cloth, or other
flexible material of a composition suitable to the analytes of
6.1 Purity of Reagents—Reagent grade chemicals shall be
interest.
used in all tests. Unless otherwise indicated, it is intended that
5.3 Drying Pans or Dishes (for example, aluminum tins,
all reagents shall conform to the specifications of the Commit-
porcelain dishes, glass weighing pans), two per waste, suitable
tee on Analytical Reagents of the American Chemical Society,
to the waste being tested and the instructions given in 9.2.
where such specifications are available. Other grades may be
5.4 Drying Oven—Any thermostatically controlled drying
used, provided it is first ascertained that the reagent is of
oven capable of maintaining a steady temperature of 62°C in
sufficiently high purity to permit its use without lessening the
a range of 100 to 110°C.
accuracy of the determination.
5.5 Desiccator, having a capacity to hold the drying pans
6.2 Purity of Water—Unless otherwise indicated, references
described in 5.3 and the crucibles described in 5.16.
to water shall be understood to mean Type IV reagent water at
5.6 Laboratory Balance, capable of weighing to 0.1 g.
18 to 27°C conforming to Specification D 1193. The method
5.7 Erlenmeyer Flask, 2-L capacity, equipped with a mag-
by which the water is prepared, that is, distillation, ion
netic stir bar.
exchange, reverse osmosis, electrodialysis, or a combination
5.8 Magnetic Stir Plate.
thereof, should remain constant throughout testing.
5.9 Graduated Cylinder, 1 or 2-L capacity.
6.3 Sulfuric Acid/Nitric Acid Solution—A 60/40 weight
5.10 Pipet, 1-mL capacity.
percent (wt %) mixture prepared using 95 to 98 wt % sulfuric
5.11 Volumetric Flask, 1-L capacity.
acid and 69 to 71 wt % nitric acid. (See 9.3 for instructions on
5.12 Pipet, 10-mL capacity. (Various other sized pipets,
the preparation of this solution.)
including micropipets, may be necessary for 9.3.2.)
5.13 pH Meter—Any pH meter with a readability of 0.01 7. Sampling
units and an accuracy of 60.05 units at 25°C.
7.1 Obtain a representative sample of the waste to be tested
5.14 Carboy-type Container, with spigot, 20 to 50-L capac-
by using, where available, ASTM sampling methods developed
ity, of a composition suitable to the nature of the analyses to be
for the specific industry (see Practice D 75, Guide D 420,
performed (see Practices D 3370).
Terminology D 653, and Test Method D 2234).
5.15 Large Glass Funnel.
7.2 Sampling methodology for materials of similar physical
5.16 Crucibles, porcelain, 20-mL capacity each, two per
form shall be used where no specific methods are available.
waste.
7.3 The amount of sample to be sent to the laboratory
5.17 Analytical Balance, capable of weighing to 0.1 mg.
should be sufficient to perform the solids content determination
5.18 Wash Bottle, 500-mL capacity.
as specified in 9.2, and to provide 100 g of sample on a dry
5.19 Agitation Equipment, of any type that rotates the
weight basis for each extraction.
extraction vessel in an end-over-end fashion at a rate of 30 6
7.4 It is important that the sample of the waste be represen-
2 r/min such that the axis of rotation is horizontal and it passes
tative with respect to surface area, as variations in surface area
through the center of the bottle (see Fig. 1 and Appendix X1).
would directly affect the leaching characteristics of the sample.
Waste samples should contain a representative distribution of
NOTE 3—Similar devices having a different axial arrangement may be
particle sizes.
used if equivalency can be demonstrated.
5.20 Pressure Filtration Assembly—A pressure filtration NOTE 6—Information on obtaining representative samples can also be
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
filter (see Note 8).
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
5.21 Extraction Vessels, cylindrical, wide-mouth, of a com-
listed by the American Chemical Society, see Analar Standards for Laboratory
position suitable to the nature of the waste and analyses to be
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
performed, constructed of materials that will not allow sorption
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
of the constituents of interest, and sturdy enough to withstand MD.
D 5284 – 93 (2004)
FIG. 1 Extractors
found in Pierre Gy’s Sampling Theory and Sampling Practice.
ing the sample (Section 7) received for testing on an imper-
meable sheet of glazed paper, oil cloth, or other flexible
7.5 In order to prevent sample contamination or constituent
material having a composition suitable to the analytes of
loss prior to extraction, keep the samples in closed containers
interest, as follows:
appropriate to sample type and desired analysis. See Practices
D 3370 for guidance. Record the storage conditions and 8.1.1 Empty the sample container into the center of the
handling procedures in the report. sheet.
7.6 The time between collection and extraction of the
8.1.2 Gently flatten the sample out with a suitable straight-
sample should be determined by the nature of the sample and
edge until it is spread uniformly to a depth at least twice the
the information desired. See Practices D 3370 for guidance.
maximum particle diameter.
Report the length of time between sample collection and
8.1.3 Remix the sample by lifting a corner of the sheet and
extraction.
drawing it low across to the opposite corner in such a manner
that the material is made to roll over and over and does not
8. Sample Preparation
merely slide along. Continue the operation with each corner,
8.1 For free-flowing particulate solid wastes, obtain a
proceeding in a clockwise direction. Repeat this operation ten
sample of the approximate size required in the test by quarter-
times.
8.1.4 Lift all four corners of the sheet toward the center and,
holding all four corners together, raise the entire sheet into the
Pitard, F., Pierre Gy’s Sampling Theory and Sampling Practice, Vols I and II,
CRC Press, 1989. air to form a pocket for the sample.
D 5284 – 93 (2004)
8.1.5 Repeat the procedure described in 8.1.2 to flatten the
S = solids content, g/g.
sample out.
Average the two values obtained. Record the solids content.
8.1.6 With a straightedge (such as a thin-edged yardstick) at
9.3 Preparation of Extraction Fluid—Prepare a 60/40 wt %
least as long as the flattened mound of sample, gently divide
mixture of sulfuric acid/nitric acid. Cautiously mix 60 g of
the sample into quarters. Make an effort to avoid using pressure
concentrated sulfuric acid with 40 g of concentrated nitric acid.
on the straightedge sufficient to cause damage to the particles.
The preparation of this mixture should be performed in a
8.1.7 Discard the alternate quarters.
laboratory fume hood.
8.1.8 If further reduction of the sample size is necessary,
9.3.1 Using the 60/40 sulfuric acid/nitric acid mixture,
repeat the steps given in 8.1.3 through 8.1.7. Use a sample size
prepare a second solution by diluting 1.0 mL of the 60/40
to provide 100 g of solid on a dry weight basis for each
mixture to 1000 mL using water and a 1-L volumetric flask.
extraction. Provide additional samples for the determination of
9.3.2 Using the 1/1000 solution prepared in 9.3.1, prepare
solids content (see 9.2). Use of a sample size other than 100 g
the extraction fluid having the desired pH 6 0.05 (see 4.2) by
of solid on a dry weight basis for extraction is not recom-
pipeting a volume of the 1/1000 solution into 2000 mL of water
mended; however, if a different sample size is used, report this
with mixing until the desired pH 6 0.05 is achieved. A
fact.
recommended method for preparing the extraction fluid is to
NOTE 7—For other acceptable methods of mixing and subsampling
add 2000 mL of water to a 2-L erlenmeyer flask equipped with
free-flowing solid particulate wastes, see Pierre Gy’s Sampling Theory
a magnetic stir bar. Place the erlenmeyer flask on a magnetic
and Sampling Practice. The method of subsampling should be deter-
stir plate, and add the 1/1000 solution to the flask with stirring.
mined by the physical properties of the waste, analytes of interest, and
Shake the mixture vigorously, and measure its pH once the
equipment available.
solution is static. Continue this process until the desired
8.2 For field-cored solid wastes or castings produced in the
solution pH 6 0.05 is reached. Record the
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