ASTM D6234-98
(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
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.
1.5 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: D 6234 – 98
Standard Test Method for
Shake Extraction of Mining Waste by the Synthetic
Precipitation Leaching Procedure
This standard is issued under the fixed designation D 6234; 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 653 Terminology Relating to Soil, Rock, and Contained
Fluids
1.1 This test method covers a procedure for the shake
D 1129 Terminology Relating to Water
leaching of mining waste containing at least 80 % dry solids
D 1193 Specification for Reagent Water
(# 20 % moisture) in order to generate a solution to be used to
D 2234 Test Methods for Collection of a Gross Sample of
determine the inorganic constituents leached under the speci-
Coal
fied testing conditions, that conform to the synthetic precipi-
D 2777 Practice for Determination of Precision and Bias of
tation leaching procedure (SPLP).
Methods of Committee D-19 on Water
1.2 This test method calls for the shaking of a known weight
D 3370 Practices for Sampling Water
of mining waste with acidic extraction fluid of a specified
D 3987 Test Method for Shake Extraction of Waste with
composition as well as the separation of the liquid phase for
Water
analysis. The pH of the extraction fluid is to reflect the pH of
D 5744 Test Method for Accelerated Weathering of Solid
acidic precipitation in the geographic region in which the waste
Materials Using a Modified Humidity Cell.
being tested is to be disposed.
E 691 Practice for Conduction an Interlaboratory Test Study
NOTE 1—Possible sources of information concerning the pH of the 7
to Determine the Precision of Test Methods
precipitation in the geographic region of interest include state and federal
E 877 Practice for Sampling and Analysis of Iron Ores and
environmental agencies, state universities, libraries, etc. pH values given
Related Materials
in USEPA Method 1312, that are 4.2 east of the Mississippi River and 5.0
2.2 EPA Document:
west of the Mississippi River and are based on acid precipitation maps, are
U.S. Environmental Protection Agency, Synthetic Precipita-
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
tion Leaching Procedure, Method 1312 in SW-846, Test
Method D 3987.
Methods for Evaluating Solid Waste, Physical/Chemical
Methods, Third Edition
1.3 This test method is intended to describe the procedure
for performing single batch extractions only. It does not
3. Terminology
describe all types of sampling and analytical requirements that
3.1 Definitions—For definitions of terms used in this test
may be associated with its application.
method, see Terminology D 1129.
1.4 The values stated in SI units are to be regarded as the
3.2 Definitions of Terms Specific to This Standard:
standard.
3.2.1 mining waste,n—overburden or waste rock excavated
1.5 This standard does not purport to address all of the
and disposed of during mining operations.
safety concerns, if any, associated with its use. It is the
3.3 Symbols:
responsibility of the user of this standard to establish appro-
Variables listed in this test method are defined in the
priate safety and health practices and determine the applica-
individual sections in which they are discussed.
bility of regulatory limitations prior to use.
4. Significance and Use
2. Referenced Documents
4.1 This test method is intended as a means for obtaining an
2.1 ASTM Standards:
extract of mining waste. The extract may be used to estimate
D 75 Practice for Sampling Aggregates
the release of certain inorganic constituents of the waste under
D 420 Guide to Site Characterization for Engineering, De-
sign and Construction Purposes
Annual Book of ASTM Standards, Vol 11.01.
1 5
This test method is under the jurisdiction of ASTM Committee D34 on Waste Annual Book of ASTM Standards, Vol 05.05.
Management and is the direct responsibility of Subcommittee D34.01.04 on Waste Annual Book of ASTM Standards, Vol 11.04.
Leaching Techniques. Annual Book of ASTM Standards, Vol 14.02.
Current edition approved Feb. 10, 1998. Published June 1998. Annual Book of ASTM Standards, Vol 03.06.
2 9
Annual Book of ASTM Standards, Vol 04.03. Available from U.S. Government Printing Office, Washington, DC 20402.
Annual Book of ASTM Standards, Vol 04.08 Request Publication Number 955-001-00000-1.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 6234
the laboratory conditions described in this test method. The 5.14 Carboy-Type Container, with spigot, 20 to 50-L capac-
user is advised to minimize the holding time between sampling ity, of a composition suitable to the nature of the analyses to be
and testing if the waste is suspected to contain reactive sulfide performed (see Practices D 3370).
minerals. 5.15 Large Glass Funnel.
5.16 Crucibles, porcelain, 20-mL capacity each, two per
NOTE 2—This method is not intended to be used as a kinetic test to
waste.
simulate weathering of mining wastes. For kinetic testing of mining
5.17 Wash Bottle, 500-mL capacity.
wastes, refer to Test Method D 5744 to determine release rates for
5.18 Agitation Equipment, of any type that rotates the
constituents of interest.
extraction vessel in an end-over-end fashion at a rate of 30 6
4.2 The pH of the extraction fluid used in this test method is
2 r/min such that the axis of rotation is horizontal and it passes
to reflect the pH of acidic precipitation in the geographic region
through the center of the bottle (see Fig. 1).
in which the waste being tested is to be disposed (see 1.2).
5.19 Pressure Filtration Assembly—A pressure filtration
4.3 An intent of this test method is for the final pH of the
device using pressure regulated compressed gas of a compo-
extract to reflect the interaction of the extractant with the
sition suitable to the nature of the analyses to be performed and
buffering capacity of the waste.
equipped with a 0.45 or 0.8-μm pore size filter (see Note 6).
4.4 This test method is not intended to provide an extract
5.20 Extraction Vessels, cylindrical, wide-mouth, of a com-
that is representative of the actual leachate produced from a
position suitable to the nature of the waste and analyses to be
waste in the field or to produce extracts to be used as the sole
performed, constructed of materials that will not allow sorption
basis of engineering design. If the conditions of this test
of the constituents of interest, and sturdy enough to withstand
method are not suitable for the test material USEPA Method
the impact of the falling sample fragments. The size of the
1312 may be used.
container should he selected so that the sample, plus extraction
4.5 This test method has not been demonstrated to simulate
fluid occupy approximately 95 % of the container. The con-
actual disposal site leaching conditions.
tainers must have water-tight closures.
4.6 This test method produces extracts that are amenable to
5.20.1 Extraction vessels should be cleaned in a manner
the determination of both major and minor (trace) inorganic
consistent with the analyses to he performed (see Section 13 of
constituents. When minor constituents are being determined, it
Practice D 3370).
is especially important that precautions be taken in sample
storage and handling to avoid possible contamination of the
6. Reagents
samples.
6.1 Purity of Reagents—Reagent grade chemicals shall be
4.7 This test method has been tested to determine its
used in all tests. Unless otherwise indicated, it is intended that
applicability to certain inorganic components in the waste. This
all reagents shall conform to the specifications of the Commit-
test method has not been tested for applicability to organic
tee on Analytical Reagents of the American Chemical Society,
substances, volatile matter (see Note 4), or biologically active
where such specifications are available . Other grades may be
samples. This test method has undergone limited testing to
used, provided it is first ascertained that the reagent is of
determine its reproducibility.
sufficiently high purity to permit its use without lessening the
5. Apparatus
accuracy of the determination.
5.1 Straight Edge, such as a thin-edged yardstick. 6.2 Purity of Water—Unless otherwise indicated, references
to water shall be understood to mean Type IV reagent water at
5.2 Impermeable Sheet, of glazed paper, oil cloth, or other
flexible material of a composition suitable to the analytes of 18 to 27°C conforming to Specification D 1193. The method
by which the water is prepared, that is, distillation, ion
interest.
5.3 Drying Pans or Dishes, (for example, aluminum tins, exchange, reverse osmosis, electrodialysis, or a combination
thereof, should remain constant throughout testing.
porcelain dishes, glass weighing pans), two per waste, suitable
to the waste being tested and the instructions given in 9.2. 6.3 Sulfuric Acid/Nitric Acid Solution—A 60/40 weight
percent (weight %) mixture prepared using 95 to 98 weight %
5.4 Drying Oven—Any thermostatically controlled drying
sulfuric acid and 69 to 71 weight % nitric acid. (See 9.3 for
oven capable of maintaining a steady temperature of 6 2°C in
instructions on the preparation of this solution.)
a range of 100 to 110°C.
5.5 Desiccator, having a capacity to hold the drying pans
7. Sampling
described in 5.3 and the crucibles described in 5.16.
7.1 Obtain a representative sample of the mining waste to be
5.6 Laboratory Balance, capable of weighing to 0.1 g.
tested by using, where available, ASTM sampling methods
5.7 Erlenmeyer Flask, 2-L capacity, equipped with a mag-
developed for the specific industry (see Practice D 75, Guide
netic stir bar.
D 420, Terminology D 653, Test Method D 2234, and Practice
5.8 Magnetic Stir Plate.
E 877).
5.9 Graduated cylinder, 1 or 2-L capacity.
5.10 Pipet, 1-mL capacity.
5.11 Volumetric Flask, 1-L capacity.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
5.12 Pipet, 10-mL capacity. (Various other sized pipets,
listed by the American Chemical Society, see Analar Standards for Laboratory
including micropipets, may be necessary for 9.3.2.)
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
5.13 pH Meter—Any pH meter with a readability of 0.01
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC) , Rockville,
units and an accuracy of 6 0.05 units at 25°C. MD.
D 6234
FIG. 1 Extractors
7.2 Sampling methodology for materials of similar physical D 3370 for guidance. Record the storage conditions and
form shall be used where no specific methods are available. handling procedures in the report.
7.3 The amount of sample to be sent to the laboratory
7.6 The time between collection and extraction of the
should he sufficient to perform the solids content determination sample should be determined by the nature of the sample and
as specified in 9.2, and to provide 100 g of sample on a dry
the information desired. See Practices D 3370 for guidance.
weight basis for extraction. Report the length of time between sample collection and
7.4 It is important that the sample of the mining waste be
extraction. The user is advised to minimize the holding time
representative with respect to the inorganic constituents to be between sampling and testing if the waste is suspected to
determined.
contain reactive sulfide minerals. Sample containing sulfide
minerals may be preserved by filling the container with
NOTE 3—Information on obtaining representative samples can also be
11 nitrogen gas and storing at 10°C.
found in Pierre Gy’s Sampling Theory and Sampling Practice.
7.5 In order to prevent sample contamination or constituent
8. Sample Preparation
loss prior to extraction, keep the samples in closed containers
8.1 Pass the gross sample through a 9.5-mm (3/8 in.) sieve
appropriate to sample type and desired analysis. See Practices
and stage crush any oversize material no more than necessary
to pass it through the sieve. Divide the gross sample in a riffle
11 splitter with 25-mm (1 in.) chutes, repeatedly if necessary, to
Pitard, F., Pierre Gy’s Sampling Theory and Sampling Practice, 2nd Edition,
CRC Press, Boca Raton, FL, 1993. obtain a representative laboratory sample with a weight in the
D 6234
S5A/B (1)
range of 250 to 500 g. Obtain a sample of the approximate size
required in the test by quartering the sample received for
where:
testing on an impermeable sheet of glazed paper, oil cloth, or
A = mass of sample after drying, g,
other flexible material having a composition suitable to the
B = original mass of sample, g, and
analytes of interest, as follows:
S = solids weight fraction, g/g.
8.1.1 Empty the sample container into the center of the
Average the two values obtained. Record the solids weight
sheet.
fraction.
8.1.2 Gently flatten the sample out with a suitable straight-
9.3 Preparation of Extraction Fluid:
edge until it is spread uniformly to a depth at least twice the
9.3.1 Acid Solution A—Prepare 60/40 weight % mixture of
maximum particle diameter.
sulfuric acid/nitric acid. Cautiously mix 60 g of concentrated
8.1.3 Remix the sample by lifting a corner of the sheet and
sulfuric acid with 40 g of concentrated nitric acid. The
drawing it low across to the opposite corner in such a manner
preparation of this mixture should be performed in a laboratory
that the material is made to roll over and over and does not
fume hood.
merely slide along. Continue the operation with each corner,
9.3.2 Acid Working Solution—Add 1 mL of Acid Solution A
proceeding in a clockwise direction. Repeat this operation ten
(See 9.3.1) to 900 mL of water in a 1-L volumetric flask, dilute
times.
to the mark and mix (1/1000 solution).
8.1.4 Lift all four corners of the sheet toward the center and,
9.3.3 Extraction Fluid—Using the acid working solution
holding all four corners together, raise the entire sheet into the
prepared in 9.3.2, prepare the extraction fluid having the
air to form a pocket for the sample.
desired pH 6 0.05 (see 4.2) by adding a volume of the Acid
8.1.5 Repeat the procedure described in 8.1.2 to flatten the
Working Solution into 2000 mL of water with mixing until the
sample out.
desired pH 6 0.05 is achieved. A recommended method for
8.1.6 With a straightedge (such as a thin-edged yardstick) at
preparing the extraction fluid is to add 2000 mL of water
...
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