ASTM D6234-13(2020)
(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
4.1 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 3: 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 D5744 to determine release rates for constituents of interest. For static testing of metal mining ore and mining or mineral processing waste materials, refer to Test Methods E1915.
4.2 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).
4.3 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.
4.4 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 or Test Method E2242 may be used.
4.5 This test method has not been demonstrated to simulate actual disposal site leaching conditions.
4.6 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.
4.7 This test method has been tested to determine its applicability to certain inorganic components in the waste. This test method has not been...
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 Practice D3987 or Test Method E2242.
Note 2: The method may also be suitable for use in testing of mineral processing waste from metal mining process operations for jurisdictions that do not require the use of Test Method E2242.
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, sample preservation, 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. No other units of measurement are included in this 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...
General Information
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Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D6234 − 13 (Reapproved 2020)
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 priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
1.1 This test method covers a procedure for the shake
1.6 This international standard was developed in accor-
leaching of mining waste containing at least 80 % dry solids
dance with internationally recognized principles on standard-
(≤20 % moisture) in order to generate a solution to be used to
ization established in the Decision on Principles for the
determine the inorganic constituents leached under the speci-
Development of International Standards, Guides and Recom-
fied testing conditions that conform to the synthetic precipita-
mendations issued by the World Trade Organization Technical
tion leaching procedure (SPLP).
Barriers to Trade (TBT) Committee.
1.2 Thistestmethodcallsfortheshakingofaknownweight
2. Referenced Documents
of mining waste with acidic extraction fluid of a specified
composition, as well as the separation of the liquid phase for 2
2.1 ASTM Standards:
analysis. The pH of the extraction fluid is to reflect the pH of
D75/D75M Practice for Sampling Aggregates
acidicprecipitationinthegeographicregioninwhichthewaste
D420 Guide for Site Characterization for Engineering De-
being tested is to be disposed.
sign and Construction Purposes
D653 Terminology Relating to Soil, Rock, and Contained
NOTE 1—Possible sources of information concerning the pH of the
precipitation in the geographic region of interest include state and federal Fluids
environmental agencies, state universities, libraries, etc. pH values given
D1129 Terminology Relating to Water
in USEPAMethod 1312, that are 4.2 east of the Mississippi River and 5.0
D1193 Specification for Reagent Water
westoftheMississippiRiverandarebasedonacidprecipitationmaps,are
D2234/D2234M Practice for Collection of a Gross Sample
examples of values that can be used. If the pH of the laboratory water is
of Coal
less than the desired pH for the site, do not use this test method; use
Practice D3987 or Test Method E2242.
D2777 Practice for Determination of Precision and Bias of
NOTE 2—The method may also be suitable for use in testing of mineral
Applicable Test Methods of Committee D19 on Water
processing waste from metal mining process operations for jurisdictions
D3370 Practices for Sampling Water from Flowing Process
that do not require the use of Test Method E2242.
Streams
1.3 This test method is intended to describe the procedure
D3987 Practice for Shake Extraction of Solid Waste with
for performing single batch extractions only. It does not
Water
describe all types of sampling, sample preservation, and
D5744 Test Method for Laboratory Weathering of Solid
analytical requirements that may be associated with its appli-
Materials Using a Humidity Cell
cation.
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.4 The values stated in SI units are to be regarded as the
E877 Practice for Sampling and Sample Preparation of Iron
standard. No other units of measurement are included in this
Ores and Related Materials for Determination of Chemi-
standard.
cal Composition and Physical Properties
1.5 This standard does not purport to address all of the
E1915 Test Methods forAnalysis of Metal Bearing Ores and
safety concerns, if any, associated with its use. It is the
Related Materials for Carbon, Sulfur, and Acid-Base
responsibility of the user of this standard to establish appro-
Characteristics
E2242 Test Method for Column Percolation Extraction of
Mine Rock by the Meteoric Water Mobility Procedure
This test method is under the jurisdiction of ASTM Committee D34 on Waste
Management and is the direct responsibility of Subcommittee D34.01.04 on Waste
Leaching Techniques. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Sept. 1, 2020. Published September 2020. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1998. Last previous edition approved in 2013 as D6234 – 13. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D6234-13R20. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6234 − 13 (2020)
2.2 EPA Document: samples. This test method has undergone limited testing to
U.S. Environmental Protection Agency, Synthetic Precipita- determine its reproducibility.
tion Leaching Procedure, Method 1312 in SW-846, Test
Methods for Evaluating Solid Waste, Physical/Chemical 5. Apparatus
Methods, Third Edition
5.1 Straightedge, such as a thin-edged yardstick.
3. Terminology 5.2 Impermeable Sheet, of glazed paper, oil cloth, or other
flexible material of a composition suitable to the analytes of
3.1 Definitions—For definitions of terms used in this test
interest.
method, see Terminology D1129.
5.3 Drying Pans or Dishes, (for example, aluminum tins,
3.2 Definitions of Terms Specific to This Standard:
porcelain dishes, glass weighing pans), two per waste, suitable
3.2.1 mining waste, n—overburden or waste rock excavated
to the waste being tested and the instructions given in 9.2.
and disposed of during mining operations.
5.4 Drying Oven—Any thermostatically controlled drying
3.3 Symbols—Variableslistedinthistestmethodaredefined
oven capable of maintaining a steady temperature of 62°Cin
in the individual sections in which they are discussed.
a range of 100 to 110 °C.
4. Significance and Use
5.5 Desiccator, having a capacity to hold the drying pans
4.1 This test method is intended as a means for obtaining an described in 5.3 and the crucibles described in 5.16.
extract of mining waste. The extract may be used to estimate
5.6 Laboratory Balance, capable of weighing to 0.1 g.
the release of certain inorganic constituents of the waste under
5.7 Erlenmeyer Flask, 2-L capacity, equipped with a mag-
the laboratory conditions described in this test method. The
netic stir bar.
user is advised to minimize the holding time between sampling
and testing if the waste is suspected to contain reactive sulfide
5.8 Magnetic Stir Plate.
minerals.
5.9 Graduated Cylinder, 1 or 2-L capacity.
NOTE 3—This method is not intended to be used as a kinetic test to
5.10 Pipet, 1-mL capacity.
simulate weathering of mining wastes. For kinetic testing of mining
wastes, refer to Test Method D5744 to determine release rates for
5.11 Volumetric Flask, 1-L capacity.
constituents of interest. For static testing of metal mining ore and mining
or mineral processing waste materials, refer to Test Methods E1915.
5.12 Pipet, 10-mL capacity. (Various other sized pipets,
4.2 The pH of the extraction fluid used in this test method is
including micropipets, may be necessary for 9.3.2.)
toreflectthepHofacidicprecipitationinthegeographicregion
5.13 pH Meter—Any pH meter with a readability of 0.01
in which the waste being tested is to be disposed (see 1.2).
units and an accuracy of 60.05 units at 25 °C.
4.3 An intent of this test method is for the final pH of the
5.14 Carboy-Type Container, with spigot, 20 to 50-L
extract to reflect the interaction of the extractant with the
capacity, of a composition suitable to the nature of the analyses
buffering capacity of the waste.
to be performed (see Practices D3370).
4.4 This test method is not intended to provide an extract
5.15 Large Glass Funnel.
that is representative of the actual leachate produced from a
waste in the field or to produce extracts to be used as the sole
5.16 Crucibles, porcelain, 20-mL capacity each, two per
basis of engineering design. If the conditions of this test
waste.
method are not suitable for the test material, USEPA Method
5.17 Wash Bottle, 500-mL capacity.
1312 or Test Method E2242 may be used.
5.18 Agitation Equipment, of any type that rotates the
4.5 This test method has not been demonstrated to simulate
extraction vessel in an end-over-end fashion at a rate of 30 6
actual disposal site leaching conditions.
2 r/min such that the axis of rotation is horizontal and it passes
4.6 This test method produces extracts that are amenable to
through the center of the bottle (see Fig. 1).
the determination of both major and minor (trace) inorganic
5.19 Pressure Filtration Assembly—A pressure filtration
constituents. When minor constituents are being determined, it
device using pressure regulated compressed gas of a compo-
is especially important that precautions be taken in sample
sitionsuitabletothenatureoftheanalysestobeperformedand
storage and handling to avoid possible contamination of the
equipped with a 0.45 or 0.8-µm pore size filter (see Note 7).
samples.
5.20 Extraction Vessels, cylindrical, wide-mouth, of a com-
4.7 This test method has been tested to determine its
position suitable to the nature of the waste and analyses to be
applicabilitytocertaininorganiccomponentsinthewaste.This
performed,constructedofmaterialsthatwillnotallowsorption
test method has not been tested for applicability to organic
of the constituents of interest, and sturdy enough to withstand
substances, volatile matter (see Note 5), or biologically active
the impact of the falling sample fragments. The size of the
container should he selected so that the sample plus extraction
fluid occupy approximately 95 % of the container. The con-
Available from U.S. Government Printing Office, Washington, DC 20402.
Request Publication Number 955-001-00000-1. tainers must have watertight closures.
D6234 − 13 (2020)
FIG. 1 Extractors
5.20.1 Extraction vessels should be cleaned in a manner used, provided it is first ascertained that the reagent is of
consistent with the analyses to he performed (see Section 13 of sufficiently high purity to permit its use without lessening the
Practices D3370).
accuracy of the determination.
6.2 Purity of Water—Unless otherwise indicated, references
6. Reagents
to water shall be understood to mean Type IV reagent water at
6.1 Purity of Reagents—Reagent grade chemicals shall be
18 to 27 °C conforming to Specification D1193. The method
used in all tests. Unless otherwise indicated, it is intended that
by which the water is prepared, that is, distillation, ion
all reagents shall conform to the specifications of the Commit-
exchange, reverse osmosis, electrodialysis, or a combination
tee onAnalytical Reagents of theAmerican Chemical Society,
thereof, should remain constant throughout testing.
where such specifications are available. Other grades may be
6.3 Sulfuric Acid/Nitric Acid Solution—A 60/40 weight
Reagent Chemicals, American Chemical Society Specifications, American
percent (weight %) mixture prepared using 95 to 98 weight %
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
sulfuric acid and 69 to 71 weight % nitric acid. (See 9.3 for
listed by the American Chemical Society, see Analar Standards for Laboratory
instructions on the preparation of this solution.)
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD.
D6234 − 13 (2020)
7. Sampling merely slide along. Continue the operation with each corner,
proceeding in a clockwise direction. Repeat this operation ten
7.1 Obtainarepresentativesampleoftheminingwastetobe
times.
tested by using, where available, ASTM sampling methods
8.1.4 Liftallfourcornersofthesheettowardthecenterand,
developed for the specific industry (see Practice D75/D75M,
holding all four corners together, raise the entire sheet into the
Guide D420, Terminology D653, Practice D2234/D2234M,
air to form a pocket for the sample.
and Practice E877).
8.1.5 Repeat the procedure described in 8.1.2 to flatten the
7.2 Sampling methodology for materials of similar physical
sample out.
form shall be used where no specific methods are available.
8.1.6 With a straightedge (such as a thin-edged yardstick) at
least as long as the flattened mound of sample, gently divide
7.3 The amount of sample to be sent to the laboratory
thesampleintoquarters.Makeanefforttoavoidusingpressure
shouldbesufficienttoperformthesolidscontentdetermination
on the straightedge sufficient to cause damage to the particles.
as specified in 9.2, and to provide 100 g of sample on a
8.1.7 Discard the alternate quarters.
dry-weight basis for extraction.
8.1.8 If further reduction of the sample size is necessary,
7.4 It is important that the sample of the mining waste be
repeat the steps given in 8.1.3 – 8.1.7. Use a sample size to
representative with respect to the inorganic constituents to be
provide at least 100 g of solid on a dry-weight basis. Provide
determined.
additional samples for the determination of solids content (see
9.2). Use of a sample size less than 100 g of solid on a
NOTE 4—Information on obtaining representative samples can also be
found in Pierre Gy’s Sampling Theory and Sampling Practice.
dry-weight basis for extraction is not recommended; however,
if a different sample size is used, report this fact.
7.5 In order to prevent sample contamination or constituent
loss prior to extraction, keep the samples in closed containers
NOTE 5—For other acceptable methods of mixing and subsampling
appropriate to sample type and desired analysis. See Practices
free-flowing solid particulate wastes, see Pierre Gy’s Sampling Theory
and Sampling Practice. The method of subsampling should be deter-
D3370 for guidance. Record the storage conditions and han-
mined by the physical properties of the waste, analytes of interest, and
dling procedures in the report.
equipment available.
7.6 The time between collection and extraction of the
sample should be determined by the nature of the sample and
9. Procedure
the information desired. See Practices D3370 for guidance.
9.1 Record a physical description of the sample to be tested,
Report the length of time between sample collection and
including particle size so far as it is known.
extraction. The user is advised to minimize the holding time
...
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