ASTM D5284-93(1999)
(Test Method)Standard Test Method for Sequential Batch Extraction of Waste with Acidic Extraction Fluid
Standard Test Method for Sequential Batch Extraction of Waste with Acidic Extraction Fluid
SCOPE
1.1 This test method provides a procedure for the sequential leaching of a waste containing at least 5% dry solids in order 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 acidic extraction fluid of a specified composition as well as the separation of the liquid phase for analysis. The pH of the extraction fluid is to reflect the pH of acidic precipitation in the geographic region in which the waste being tested is to be disposed. The procedure is conducted ten times in sequence on the same sample of waste, and it generates ten 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 the standard.
1.5 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5284 – 93 (Reapproved 1999)
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 2234 Test Methods for Collection of a Gross Sample of
Coal
1.1 This test method provides a procedure for the sequential
D 2777 Practice for Determination of Precision and Bias of
leaching of a waste containing at least 5 % dry solids in order
Methods of Committee D-19 on Water
to generate solutions to be used to determine the constituents
D 3370 Practices for Sampling Water
leached under the specified testing conditions.
D 4793 Test Method for Sequential Batch Extraction of
1.2 This test method calls for the shaking of a known weight
Waste with Water
of waste with acidic extraction fluid of a specified composition
as well as the separation of the liquid phase for analysis. The
3. Terminology
pH of the extraction fluid is to reflect the pH of acidic
3.1 Definitions—For definitions of terms used in this test
precipitation in the geographic region in which the waste being
method, see Terminology D 1129.
tested is to be disposed. The procedure is conducted ten times
3.2 Symbols:Symbols—Variables listed in this test method
in sequence on the same sample of waste, and it generates ten
are defined in the individual sections in which they are
solutions.
discussed. A list of the defined variables is also provided in
1.3 This test method is intended to describe the procedure
Section 11.
for performing sequential batch extractions only. It does not
describe all types of sampling and analytical requirements that
4. Significance and Use
may be associated with its application.
4.1 This test method is intended as a means for obtaining
1.4 The values stated in SI units are to be regarded as the
sequential extracts of a waste. The extracts may be used to
standard.
estimate the release of certain constituents of the waste under
1.5 This standard does not purport to address all of the
the laboratory conditions described in this test method.
safety problems, if any, associated with its use. It is the
4.2 The pH of the extraction fluid used in this test method is
responsibility of the user of this standard to establish appro-
to reflect the pH of acidic precipitation in the geographic region
priate safety and health practices and determine the applica-
in which the waste being tested is to be disposed.
bility of regulatory limitations prior to use.
NOTE 1—Possible sources of information concerning the pH of precipi-
2. Referenced Documents
tation in the geographic region of interest include state and federal
environmental agencies, state universities, libraries, etc.
2.1 ASTM Standards:
2 NOTE 2—For sequential batch extraction of waste using a nonacidic
D 75 Practice for Sampling Aggregates
extraction fluid, see Test Method D 4793.
D 420 Guide to Site Characterization for Engineering, De-
4.3 An intent of this test method is for the final pH of each
sign and Construction Purposes
of the extracts to reflect the interaction of the extractant with
D 653 Terminology Relating to Soil, Rock, and Contained
the buffering capacity of the waste.
Fluids
4.4 This test method is not intended to provide extracts that
D 1129 Terminology Relating to Water
are representative of the actual leachate produced from a waste
D 1193 Specification for Reagent Water
in the field or to produce extracts to be used as the sole basis
of engineering design.
This test method is under the jurisdiction of ASTM Committee D34 on Waste
4.5 This test method has not been demonstrated to simulate
Management and is the direct responsibility of Subcommittee D34.01.04 on
actual disposal site leaching conditions.
Ancillary Topics.
Current edition approved Sept. 15, 1993. Published November 1993. Originally
published as D 5284–92. Last previous edition D 5284–92.
Annual Book of ASTM Standards, Vol 04.03.
3 5
Annual Book of ASTM Standards, Vol 04.08. Annual Book of ASTM Standards, Vol 05.05.
4 6
Annual Book of ASTM Standards, Vol 11.01. Annual Book of ASTM Standards, Vol 11.04.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 5284
4.6 This test method produces extracts that are amenable to 5.21 Extraction Vessels, cylindrical, wide-mouth, of a com-
the determination of both major and minor (trace) constituents. position suitable to the nature of the waste and analyses to be
When minor constituents are being determined, it is especially performed, constructed of materials that will not allow sorption
important that precautions be taken in sample storage and of the constituents of interest, and sturdy enough to withstand
handling to avoid possible contamination of the samples. the impact of the falling sample fragments. The size of the
4.7 This test method has been tested to determine its container should be selected so that the sample plus extraction
fluid occupy approximately 95 % of the container. The con-
applicability to certain inorganic components in the waste. This
test method has not been tested for applicability to organic tainers must have water-tight closures. Containers for samples
in which gases may be released should be provided with
substances, volatile matter (see Note 5), or biologically active
samples. venting mechanisms.
4.8 The agitation technique, rate, liquid-to-solid ratio, and
NOTE 4—Suitable container sizes range from 4.0 to 4.5 in. in diameter
filtration conditions specified in the procedure may not be
and 8.5 to 13.0 in. in height.
suitable for extracting all types of wastes (see Sections 7 and 8
NOTE 5—The venting of the container has the potential to affect the
and Appendix X1). concentration of volatile compounds in the extracts.
5.21.1 Extraction vessels should be cleaned in a manner
5. Apparatus
consistent with the analyses to be performed (see Section 13 of
Practice D 3370).
5.1 Straight Edge, such as a thin-edged yardstick.
5.2 Impermeable Sheet, of glazed paper, oil cloth, or other
6. Reagents
flexible material of a composition suitable to the analytes of
interest.
6.1 Purity of Reagents—Reagent grade chemicals shall be
5.3 Drying Pans or Dishes (for example, aluminum tins,
used in all tests. Unless otherwise indicated, it is intended that
porcelain dishes, glass weighing pans), two per waste, suitable all reagents shall conform to the specifications of the Commit-
to the waste being tested and the instructions given in 9.2. tee on Analytical Reagents of the American Chemical Society,
5.4 Drying Oven—Any thermostatically controlled drying where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
oven capable of maintaining a steady temperature of 62°C in
a range of 100 to 110°C. sufficiently high purity to permit its use without lessening the
accuracy of the determination.
5.5 Desiccator, having a capacity to hold the drying pans
described in 5.3 and the crucibles described in 5.16. 6.2 Purity of Water—Unless otherwise indicated, references
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).
NOTE 3—Similar devices having a different axial arrangement may be
used if equivalency can be demonstrated.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
5.20 Pressure Filtration Assembly—A pressure filtration
listed by the American Chemical Society, see Analar Standards for Laboratory
device of a composition suitable to the nature of the analyses
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
to be performed and equipped with a 0.45 or 0.8-μm pore size
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
filter (see Note 8). MD.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 5284
FIG. 1 Extractors
would directly affect the leaching characteristics of the sample. 8. Sample Preparation
Waste samples should contain a representative distribution of
8.1 For free-flowing particulate solid wastes, obtain a
particle sizes.
sample of the approximate size required in the test by quarter-
NOTE 6—Information on obtaining representative samples can also be ing the sample (Section 7) received for testing on an imper-
found in Pierre Gy’s Sampling Theory and Sampling Practice.
meable sheet of glazed paper, oil cloth, or other flexible
material having a composition suitable to the analytes of
7.5 In order to prevent sample contamination or constituent
interest, as follows:
loss prior to extraction, keep the samples in closed containers
appropriate to sample type and desired analysis. See Practices 8.1.1 Empty the sample container into the center of the
D 3370 for guidance. Record the storage conditions and sheet.
handling procedures in the report.
8.1.2 Gently flatten the sample out with a suitable straight-
7.6 The time between collection and extraction of the
edge until it is spread uniformly to a depth at least twice the
sample should be determined by the nature of the sample and
maximum particle diameter.
the information desired. See Practices D 3370 for guidance.
8.1.3 Remix the sample by lifting a corner of the sheet and
Report the length of time between sample collection and
drawing it low across to the opposite corner in such a manner
extraction.
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
Pitard, F., Pierre Gy’s Sampling Theory and Sampling Practice, Vols I and II,
CRC Press, 1989. times.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 5284
8.1.4 Lift all four corners of the sheet toward the center and,
where:
holding all four corners together, raise the entire sheet into the
A = mass of sample after drying, g,
air to form a pocket for the sample.
B = original mass of sample, g, and
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
add 2000 mL of water to a 2-L erlenmeyer flask equipped with
NOTE 7—For other acceptable methods of mixing and subsampling
free-flowing solid particulate waste
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.