ASTM D6234-98(2002)
(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.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D6234–98 (Reapproved 2002)
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 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 D 420 Guide to Site Characterization for Engineering, De-
determine the inorganic constituents leached under the speci- sign and Construction Purposes
fied testing conditions, that conform to the synthetic precipi- D 653 Terminology Relating to Soil, Rock, and Contained
tation leaching procedure (SPLP). Fluids
1.2 Thistestmethodcallsfortheshakingofaknownweight D 1129 Terminology Relating to Water
of mining waste with acidic extraction fluid of a specified D 1193 Specification for Reagent Water
composition as well as the separation of the liquid phase for D 2234 Test Methods for Collection of a Gross Sample of
analysis. The pH of the extraction fluid is to reflect the pH of Coal
acidicprecipitationinthegeographicregioninwhichthewaste D 2777 Practice for Determination of Precision and Bias of
being tested is to be disposed. Methods of Committee D-19 on Water
D 3370 Practices for Sampling Water
NOTE 1—Possible sources of information concerning the pH of the
D 3987 Test Method for Shake Extraction of Waste with
precipitation in the geographic region of interest include state and federal
Water
environmental agencies, state universities, libraries, etc. pH values given
in USEPAMethod 1312, that are 4.2 east of the Mississippi River and 5.0 D 5744 Test Method for Accelerated Weathering of Solid
westoftheMississippiRiverandarebasedonacidprecipitationmaps,are
Materials Using a Modified Humidity Cell.
examples of values that can be used. If the pH of the laboratory water is
E 691 PracticeforConductionanInterlaboratoryTestStudy
less than the desired pH for the site, do not use this test method, use Test
to Determine the Precision of Test Methods
Method D 3987.
E 877 Practice for Sampling and Analysis of Iron Ores and
1.3 This test method is intended to describe the procedure
Related Materials
for performing single batch extractions only. It does not
2.2 EPA Document:
describe all types of sampling and analytical requirements that
U.S. Environmental Protection Agency, Synthetic Precipita-
may be associated with its application.
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
3. Terminology
safety concerns, if any, associated with its use. It is the
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 D 1129.
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 Committee D34 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. Available from U.S. Government Printing Office, Washington, DC 20402.
Current edition approved Feb. 10, 1998. Published June 1998. 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 (2002)
3.2 Definitions of Terms Specific to This Standard: 5.6 Laboratory Balance, capable of weighing to 0.1 g.
3.2.1 mining waste,n—overburden or waste rock excavated 5.7 Erlenmeyer Flask, 2-L capacity, equipped with a mag-
and disposed of during mining operations. netic stir bar.
3.3 Symbols: 5.8 Magnetic Stir Plate.
Variables listed in this test method are defined in the 5.9 Graduated cylinder, 1 or 2-L capacity.
individual sections in which they are discussed. 5.10 Pipet, 1-mL capacity.
5.11 Volumetric Flask, 1-L capacity.
4. Significance and Use
5.12 Pipet, 10-mL capacity. (Various other sized pipets,
4.1 This test method is intended as a means for obtaining an
including micropipets, may be necessary for 9.3.2.)
extract of mining waste. The extract may be used to estimate
5.13 pH Meter—Any pH meter with a readability of 0.01
the release of certain inorganic constituents of the waste under
units and an accuracy of 6 0.05 units at 25°C.
the laboratory conditions described in this test method. The
5.14 Carboy-Type Container, with spigot, 20 to 50-Lcapac-
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
wastes, refer to Test Method D 5744 to determine release rates for 5.17 Wash Bottle, 500-mL capacity.
constituents of interest.
5.18 Agitation Equipment, of any type that rotates the
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
toreflectthepHofacidicprecipitationinthegeographicregion
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
sitionsuitabletothenatureoftheanalysestobeperformedand
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
that is representative of the actual leachate produced from a 5.20 Extraction Vessels, cylindrical, wide-mouth, of a com-
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
basis of engineering design. If the conditions of this test performed,constructedofmaterialsthatwillnotallowsorption
of the constituents of interest, and sturdy enough to withstand
method are not suitable for the test material USEPA Method
1312 may be used. the impact of the falling sample fragments. The size of the
container should he selected so that the sample, plus extraction
4.5 This test method has not been demonstrated to simulate
actual disposal site leaching conditions. fluid occupy approximately 95 % of the container. The con-
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
samples. 6. Reagents
4.7 This test method has been tested to determine its
6.1 Purity of Reagents—Reagent grade chemicals shall be
applicabilitytocertaininorganiccomponentsinthewaste.This
used in all tests. Unless otherwise indicated, it is intended that
test method has not been tested for applicability to organic
all reagents shall conform to the specifications of the Commit-
substances, volatile matter (see Note 4), or biologically active
tee onAnalytical Reagents of theAmerican Chemical Society,
samples. This test method has undergone limited testing to
where such specifications are available. Other grades may be
determine its reproducibility.
used, provided it is first ascertained that the reagent is of
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
5.2 Impermeable Sheet, of glazed paper, oil cloth, or other
to water shall be understood to mean Type IV reagent water at
flexible material of a composition suitable to the analytes of
18 to 27°C conforming to Specification D 1193. The method
interest.
by which the water is prepared, that is, distillation, ion
5.3 Drying Pans or Dishes, (for example, aluminum tins,
porcelain dishes, glass weighing pans), two per waste, suitable
to the waste being tested and the instructions given in 9.2.
5.4 Drying Oven—Any thermostatically controlled drying
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
oven capable of maintaining a steady temperature of 6 2°C in
listed by the American Chemical Society, see Analar Standards for Laboratory
a range of 100 to 110°C.
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
5.5 Desiccator, having a capacity to hold the drying pans
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC) , Rockville,
described in 5.3 and the crucibles described in 5.16. MD.
D6234–98 (2002)
FIG. 1 Extractors
exchange, reverse osmosis, electrodialysis, or a combination 7.4 It is important that the sample of the mining waste be
thereof, should remain constant throughout testing. representative with respect to the inorganic constituents to be
6.3 Sulfuric Acid/Nitric Acid Solution—A 60/40 weight determined.
percent (weight %) mixture prepared using 95 to 98 weight %
NOTE 3—Information on obtaining representative samples can also be
sulfuric acid and 69 to 71 weight % nitric acid. (See 9.3 for 5
found in Pierre Gy’s Sampling Theory and Sampling Practice.
instructions on the preparation of this solution.)
7.5 In order to prevent sample contamination or constituent
7. Sampling
loss prior to extraction, keep the samples in closed containers
appropriate to sample type and desired analysis. See Practices
7.1 Obtainarepresentativesampleoftheminingwastetobe
D 3370 for guidance. Record the storage conditions and
tested by using, where available, ASTM sampling methods
handling procedures in the report.
developed for the specific industry (see PracticeD75, Guide
7.6 The time between collection and extraction of the
D 420, Terminology D 653, Test Method D 2234, and Practice
sample should be determined by the nature of the sample and
E 877).
the information desired. See Practices D 3370 for guidance.
7.2 Sampling methodology for materials of similar physical
Report the length of time between sample collection and
form shall be used where no specific methods are available.
7.3 The amount of sample to be sent to the laboratory
shouldhesufficienttoperformthesolidscontentdetermination
as specified in 9.2, and to provide 100 g of sample on a dry
Pitard, F., Pierre Gy’s Sampling Theory and Sampling Practice, 2nd Edition,
weight basis for extraction. CRC Press, Boca Raton, FL, 1993.
D6234–98 (2002)
extraction. The user is advised to minimize the holding time 9.2.2 Place at least 50 g of the waste to be tested into each
between sampling and testing if the waste is suspected to pan. Record the mass of sample in each pan to 6 0.1 g.
contain reactive sulfide minerals. Sample containing sulfide
9.2.3 Dry for 16 to 20 h at 104 6 2°C. Record the
minerals may be preserved by filling the container with
temperature and time of the drying period.
nitrogen gas and storing at 10°C.
9.2.4 Cool to room temperature in a desiccator and reweigh.
Record the mass to 6 0.1 g.
8. Sample Preparation
9.2.5 Repeat the steps given in 9.2.3 and 9.2.4, if necessary,
8.1 Pass the gross sample through a 9.5-mm (3/8 in.) sieve
until constant container-sample masses are obtained. Record
and stage crush any oversize material no more than necessary
the final weights and discard the dried samples following
to pass it through the sieve. Divide the gross sample in a riffle
completion of this step.
splitter with 25-mm (1 in.) chutes, repeatedly if necessary, to
9.2.6 Calculate the solids weight fraction of the sample
obtain a representative laboratory sample with a weight in the
from the data obtained in 9.2.1, 9.2.2, and 9.2.4 as follows:
range of 250 to 500 g. Obtain a sample of the approximate size
S5A/B (1)
required in the test by quartering the sample received for
testing on an impermeable sheet of glazed paper, oil cloth, or
where:
other flexible material having a composition suitable to the
A = mass of sample after drying, g,
analytes of interest, as follows:
B = original mass of sample, g, and
8.1.1 Empty the sample container into the center of the S = solids weight fraction, g/g.
sheet.
Average the two values obtained. Record the solids weight
8.1.2 Gently flatten the sample out with a suitable straight-
fraction.
edge until it is spread uniformly to a depth at least twice the
9.3 Preparation of Extraction Fluid:
maximum particle diameter.
9.3.1 Acid Solution A—Prepare 60/40 weight % mixture of
8.1.3 Remix the sample by lifting a corner of the sheet and
sulfuric acid/nitric acid. Cautiously mix 60 g of concentrated
drawing it low across to the opposite corner in such a manner
sulfuric acid with 40 g of concentrated nitric acid. The
that the material is made to roll over and over and does not
preparationofthismixtureshouldbeperformedinalaboratory
merely slide along. Continue the operation with each corner,
fume hood.
proceeding in a clockwise direction. Repeat this operation ten
9.3.2 Acid Working Solution—Add1mLofAcidSolutionA
times.
(See 9.3.1) to 900 mLof water in a 1-Lvolumetric flask, dilute
8.1.4 Liftallfourcornersofthesheettowardthecenterand,
to the mark and mix (1/1000 solution).
holding all four corners together, raise the entire sheet into the
9.3.3 Extraction Fluid—Using the acid working
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.