ASTM D6234-98(2007)
(Test Method)Standard Test Method for Shake Extraction of Mining Waste by the Synthetic Precipitation Leaching Procedure
Standard Test Method for Shake Extraction of Mining Waste by the Synthetic Precipitation Leaching Procedure
SIGNIFICANCE AND USE
This test method is intended as a means for obtaining an extract of mining waste. The extract may be used to estimate the release of certain inorganic constituents of the waste under the laboratory conditions described in this test method. The user is advised to minimize the holding time between sampling and testing if the waste is suspected to contain reactive sulfide minerals.
Note 2—This method is not intended to be used as a kinetic test to simulate weathering of mining wastes. For kinetic testing of mining wastes, refer to Test Method D 5744 to determine release rates for constituents of interest.
The pH of the extraction fluid used in this test method is to reflect the pH of acidic precipitation in the geographic region in which the waste being tested is to be disposed (see 1.2).
An intent of this test method is for the final pH of the extract to reflect the interaction of the extractant with the buffering capacity of the waste.
This test method is not intended to provide an extract that is representative of the actual leachate produced from a waste in the field or to produce extracts to be used as the sole basis of engineering design. If the conditions of this test method are not suitable for the test material USEPA Method 1312 may be used.
This test method has not been demonstrated to simulate actual disposal site leaching conditions.
This test method produces extracts that are amenable to the determination of both major and minor (trace) inorganic constituents. When minor constituents are being determined, it is especially important that precautions be taken in sample storage and handling to avoid possible contamination of the samples.
This test method has been tested to determine its applicability to certain inorganic components in the waste. This test method has not been tested for applicability to organic substances, volatile matter (see Note 4), or biologically active samples. This test method has undergone limited testing to determine it...
SCOPE
1.1 This test method covers a procedure for the shake leaching of mining waste containing at least 80 % dry solids ( 20 % moisture) in order to generate a solution to be used to determine the inorganic constituents leached under the specified testing conditions, that conform to the synthetic precipitation leaching procedure (SPLP).
1.2 This test method calls for the shaking of a known weight of mining 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.Note 1
Possible sources of information concerning the pH of the precipitation in the geographic region of interest include state and federal environmental agencies, state universities, libraries, etc. pH values given in USEPA Method 1312, that are 4.2 east of the Mississippi River and 5.0 west of the Mississippi River and are based on acid precipitation maps, are examples of values that can be used. If the pH of the laboratory water is less than the desired pH for the site, do not use this test method, use Test Method D 3987.
1.3 This test method is intended to describe the procedure for performing single 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.
This standard does not purport to address all of the safety concerns, 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.
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Designation: D6234 − 98(Reapproved 2007)
Standard Test Method for
Shake Extraction of Mining Waste by the Synthetic
Precipitation Leaching Procedure
This standard is issued under the fixed designation D6234; 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 2. Referenced Documents
1.1 This test method covers a procedure for the shake 2.1 ASTM Standards:
leaching of mining waste containing at least 80 % dry solids (≤ D75 Practice for Sampling Aggregates
20 % moisture) in order to generate a solution to be used to D420 Guide to Site Characterization for Engineering Design
determine the inorganic constituents leached under the speci- and Construction Purposes (Withdrawn 2011)
fied testing conditions, that conform to the synthetic precipi- D653 Terminology Relating to Soil, Rock, and Contained
tation leaching procedure (SPLP). Fluids
D1129 Terminology Relating to Water
1.2 Thistestmethodcallsfortheshakingofaknownweight
D1193 Specification for Reagent Water
of mining waste with acidic extraction fluid of a specified
D2234/D2234M Practice for Collection of a Gross Sample
composition as well as the separation of the liquid phase for
of Coal
analysis. The pH of the extraction fluid is to reflect the pH of
D2777 Practice for Determination of Precision and Bias of
acidicprecipitationinthegeographicregioninwhichthewaste
Applicable Test Methods of Committee D19 on Water
being tested is to be disposed.
D3370 Practices for Sampling Water from Closed Conduits
NOTE 1—Possible sources of information concerning the pH of the
D3987 Test Method for Shake Extraction of Solid Waste
precipitation in the geographic region of interest include state and federal
with Water
environmental agencies, state universities, libraries, etc. pH values given
D5744 Test Method for Laboratory Weathering of Solid
in USEPAMethod 1312, that are 4.2 east of the Mississippi River and 5.0
Materials Using a Humidity Cell
westoftheMississippiRiverandarebasedonacidprecipitationmaps,are
examples of values that can be used. If the pH of the laboratory water is E691 Practice for Conducting an Interlaboratory Study to
less than the desired pH for the site, do not use this test method, use Test
Determine the Precision of a Test Method
Method D3987.
E877 Practice for Sampling and Sample Preparation of Iron
1.3 This test method is intended to describe the procedure
Ores and Related Materials for Determination of Chemi-
for performing single batch extractions only. It does not
cal Composition
describe all types of sampling and analytical requirements that
2.2 EPA Document:
may be associated with its application.
U.S. Environmental Protection Agency, Synthetic Precipita-
tion Leaching Procedure, Method 1312 in SW-846, Test
1.4 The values stated in SI units are to be regarded as the
Methods for Evaluating Solid Waste, Physical/Chemical
standard.
Methods, Third Edition
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
3.1 Definitions—For definitions of terms used in this test
priate safety and health practices and determine the applica-
method, see Terminology D1129.
bility of regulatory limitations prior to use.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
This test method is under the jurisdiction of ASTM CommitteeD34 on Waste Standards volume information, refer to the standard’s Document Summary page on
Management and is the direct responsibility of Subcommittee D34.01.04 on Waste the ASTM website.
Leaching Techniques. The last approved version of this historical standard is referenced on
Current edition approved May 1, 2007. Published June 2007. Originally www.astm.org.
approvedin1998.Lastpreviouseditionapprovedin2002asD6234-98(2002).DOI: Available from U.S. Government Printing Office, Washington, DC 20402.
10.1520/D6234-98R07. Request Publication Number 955-001-00000-1.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6234 − 98 (2007)
3.2 Definitions of Terms Specific to This Standard: 5.4 Drying Oven—Any thermostatically controlled drying
oven capable of maintaining a steady temperature of 6 2°C in
3.2.1 mining waste,n—overburden or waste rock excavated
a range of 100 to 110°C.
and disposed of during mining operations.
3.3 Symbols: Variables listed in this test method are defined 5.5 Desiccator, having a capacity to hold the drying pans
in the individual sections in which they are discussed. described in 5.3 and the crucibles described in 5.16.
5.6 Laboratory Balance, capable of weighing to 0.1 g.
4. Significance and Use
5.7 Erlenmeyer Flask, 2-L capacity, equipped with a mag-
4.1 This test method is intended as a means for obtaining an
netic stir bar.
extract of mining waste. The extract may be used to estimate
the release of certain inorganic constituents of the waste under
5.8 Magnetic Stir Plate.
the laboratory conditions described in this test method. The
5.9 Graduated cylinder, 1 or 2-L capacity.
user is advised to minimize the holding time between sampling
and testing if the waste is suspected to contain reactive sulfide
5.10 Pipet, 1-mL capacity.
minerals.
5.11 Volumetric Flask, 1-L capacity.
NOTE 2—This method is not intended to be used as a kinetic test to
simulate weathering of mining wastes. For kinetic testing of mining
5.12 Pipet, 10-mL capacity. (Various other sized pipets,
wastes, refer to Test Method D5744 to determine release rates for
including micropipets, may be necessary for 9.3.2.)
constituents of interest.
5.13 pH Meter—Any pH meter with a readability of 0.01
4.2 The pH of the extraction fluid used in this test method is
units and an accuracy of 6 0.05 units at 25°C.
toreflectthepHofacidicprecipitationinthegeographicregion
in which the waste being tested is to be disposed (see 1.2).
5.14 Carboy-Type Container, with spigot, 20 to 50-L
capacity, of a composition suitable to the nature of the analyses
4.3 An intent of this test method is for the final pH of the
to be performed (see Practices D3370).
extract to reflect the interaction of the extractant with the
buffering capacity of the waste.
5.15 Large Glass Funnel.
4.4 This test method is not intended to provide an extract
5.16 Crucibles, porcelain, 20-mL capacity each, two per
that is representative of the actual leachate produced from a
waste.
waste in the field or to produce extracts to be used as the sole
basis of engineering design. If the conditions of this test 5.17 Wash Bottle, 500-mL capacity.
method are not suitable for the test material USEPA Method
5.18 Agitation Equipment, of any type that rotates the
1312 may be used.
extraction vessel in an end-over-end fashion at a rate of 30 6
4.5 This test method has not been demonstrated to simulate
2 r/min such that the axis of rotation is horizontal and it passes
actual disposal site leaching conditions.
through the center of the bottle (see Fig. 1).
4.6 This test method produces extracts that are amenable to
5.19 Pressure Filtration Assembly—A pressure filtration
the determination of both major and minor (trace) inorganic
device using pressure regulated compressed gas of a compo-
constituents. When minor constituents are being determined, it
sitionsuitabletothenatureoftheanalysestobeperformedand
is especially important that precautions be taken in sample
equipped with a 0.45 or 0.8-µm pore size filter (see Note 6).
storage and handling to avoid possible contamination of the
5.20 Extraction Vessels, cylindrical, wide-mouth, of a com-
samples.
position suitable to the nature of the waste and analyses to be
4.7 This test method has been tested to determine its
performed,constructedofmaterialsthatwillnotallowsorption
applicabilitytocertaininorganiccomponentsinthewaste.This
of the constituents of interest, and sturdy enough to withstand
test method has not been tested for applicability to organic
the impact of the falling sample fragments. The size of the
substances, volatile matter (see Note 4), or biologically active
container should he selected so that the sample, plus extraction
samples. This test method has undergone limited testing to
fluid occupy approximately 95 % of the container. The con-
determine its reproducibility.
tainers must have water-tight closures.
5.20.1 Extraction vessels should be cleaned in a manner
5. Apparatus
consistent with the analyses to he performed (see Section 13 of
5.1 Straight Edge, such as a thin-edged yardstick.
Practice D3370).
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
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
to the waste being tested and the instructions given in 9.2. tee onAnalytical Reagents of theAmerican Chemical Society,
D6234 − 98 (2007)
FIG. 1 Extractors
where such specifications are available. Other grades may be reverse osmosis, electrodialysis, or a combination thereof,
used, provided it is first ascertained that the reagent is of
should remain constant throughout testing.
sufficiently high purity to permit its use without lessening the
6.3 Sulfuric Acid/Nitric Acid Solution—A 60/40 weight
accuracy of the determination.
percent (weight %) mixture prepared using 95 to 98 weight %
6.2 Purity of Water—Unless otherwise indicated, references
sulfuric acid and 69 to 71 weight % nitric acid. (See 9.3 for
to water shall be understood to mean Type IV reagent water at
instructions on the preparation of this solution.)
18 to 27°C conforming to Specification D1193.The method by
which the water is prepared, that is, distillation, ion exchange,
7. Sampling
5 7.1 Obtainarepresentativesampleoftheminingwastetobe
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not tested by using, where available, ASTM sampling methods
listed by the American Chemical Society, see Analar Standards for Laboratory
developed for the specific industry (see Practice D75, Guide
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
D420, Terminology D653, Test Method D2234/D2234M, and
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC) , Rockville,
MD. Practice E877).
D6234 − 98 (2007)
7.2 Sampling methodology for materials of similar physical 8.1.6 With a straightedge (such as a thin-edged yardstick) at
form shall be used where no specific methods are available. least as long as the flattened mound of sample, gently divide
thesampleintoquarters.Makeanefforttoavoidusingpressure
7.3 The amount of sample to be sent to the laboratory
on the straightedge sufficient to cause damage to the particles.
shouldhesufficienttoperformthesolidscontentdetermination
8.1.7 Discard the alternate quarters.
as specified in 9.2, and to provide 100 g of sample on a dry
8.1.8 If further reduction of the sample size is necessary,
weight basis for extraction.
repeat the steps given in 8.1.3 through 8.1.7. Use a sample size
7.4 It is important that the sample of the mining waste be
to provide at least 100 g of solid on a dry weight basis. Provide
representative with respect to the inorganic constituents to be
additional samples for the determination of solids content (see
determined.
9.2). Use of a sample size less than 100 g of solid on a dry
weight basis for extraction is not recommended; however, if a
NOTE 3—Information on obtaining representative samples can also be
found in Pierre Gy’s Sampling Theory and Sampling Practice.
different sample size is used, report this fact.
7.5 In order to prevent sample contamination or constituent
NOTE 4—For other acceptable methods of mixing and subsampling
loss prior to extraction, keep the samples in closed containers
free-flowing solid particulate wastes, see Pierre Gy’s Sampling Theory
and Sampling Practice. The method of subsampling should be deter-
appropriate to sample type and desired analysis. See Practices
mined by the physical properties of the waste, analytes of interest, and
D3370 for guidance. Record the storage conditions and han-
equipment available.
dling procedures in the report.
7.6 The time between collection and extraction of the
9. Procedure
sample should be determined by the nature of the sample and
9.1 Record a physical description of the sample to be tested,
the information desired. See Practices D3370 for guidance.
including particle size so far as it is known.
Report the length of time between sample collection and
9.2 Solids Content—Determine the solids weight fraction of
extraction. The user is advised to minimize the holding time
two separate portions of the sample as follows:
between sampling and testing if the waste is suspected to
9.2.1 Dry to a constant weight, at 104 6 2°C, two dishes or
contain reactive sulfide minerals. Sample containing sulfide
pans of size suitable to the solid waste being tested. Cool in a
minerals may be preserved by filling the container with
desiccator and weigh. Record the values to 6 0.1 g.
nitrogen gas and storing at 10°C.
9.2.2 Place at least 50 g of the waste to be tested into each
pan. Record the mass of sample in each pan to 6 0.1 g.
8. Sample Preparation
9.2.3 Dry for 16 to 20 h at 104 6 2°C. Record the
8.1 Pass the gross sample through a 9.5-mm (3/8 in.) sieve
temperature and time of the drying period.
and stage crush any oversize material no more than necessary
9.2.4 Cool to room temperature in a desiccator and reweigh.
to pass it through the sieve. Divide the gross sample in a riffle
Record the mass to 6 0.1 g.
splitter with 25-mm (1 in.) chutes, repeatedly if necessary, to
9.2.5 Repeat the steps given in 9.2.3 and 9.2.4, if necessary,
obtain a representative laboratory sample with a weight in the
until constant container-sample masses are obtained. Record
range of 250 to 500 g. Obtain a sample of the approximate size
the final weights and discard the dried samples following
required in the test by quartering the sample received for
completion of this step.
testing on
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