1、Designation: D 6234 98 (Reapproved 2007)Standard Test Method forShake Extraction of Mining Waste by the SyntheticPrecipitation Leaching Procedure1This standard is issued under the fixed designation D 6234; the number immediately following the designation indicates the year oforiginal adoption or, in
2、 the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a procedure for the shakeleaching of mining waste containi
3、ng at least 80 % dry solids(#20 % moisture) in order to generate a solution to be used todetermine the inorganic constituents leached under the speci-fied testing conditions, that conform to the synthetic precipi-tation leaching procedure (SPLP).1.2 This test method calls for the shaking of a known
4、weightof mining waste with acidic extraction fluid of a specifiedcomposition as well as the separation of the liquid phase foranalysis. The pH of the extraction fluid is to reflect the pH ofacidic precipitation in the geographic region in which the wastebeing tested is to be disposed.NOTE 1Possible
5、sources of information concerning the pH of theprecipitation in the geographic region of interest include state and federalenvironmental agencies, state universities, libraries, etc. pH values givenin USEPA Method 1312, that are 4.2 east of the Mississippi River and 5.0west of the Mississippi River
6、and are based on acid precipitation maps, areexamples of values that can be used. If the pH of the laboratory water isless than the desired pH for the site, do not use this test method, use TestMethod D 3987.1.3 This test method is intended to describe the procedurefor performing single batch extrac
7、tions only. It does notdescribe all types of sampling and analytical requirements thatmay be associated with its application.1.4 The values stated in SI units are to be regarded as thestandard.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. I
8、t is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D75 Practice for Sampling AggregatesD 420 Guide to Site Characterization for En
9、gineering De-sign and Construction PurposesD 653 Terminology Relating to Soil, Rock, and ContainedFluidsD 1129 Terminology Relating to WaterD 1193 Specification for Reagent WaterD 2234/D 2234M Practice for Collection of a Gross Sampleof CoalD 2777 Practice for Determination of Precision and Bias ofA
10、pplicable Test Methods of Committee D19 on WaterD 3370 Practices for Sampling Water from Closed ConduitsD 3987 Test Method for Shake Extraction of Solid Wastewith WaterD 5744 Test Method for Accelerated Weathering of SolidMaterials Using a Modified Humidity CellE 691 Practice for Conducting an Inter
11、laboratory Study toDetermine the Precision of a Test MethodE 877 Practice for Sampling and Sample Preparation of IronOres and Related Materials2.2 EPA Document:U.S. Environmental Protection Agency, Synthetic Precipita-tion Leaching Procedure, Method 1312 in SW-846, TestMethods for Evaluating Solid W
12、aste, Physical/ChemicalMethods, Third Edition33. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, see Terminology D 1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 mining waste,noverburden or waste rock excavatedand disposed of during mining operations.3.3 Sy
13、mbols:1This test method is under the jurisdiction of ASTM CommitteeD34 on WasteManagement and is the direct responsibility of Subcommittee D34.01.04 on WasteLeaching Techniques.Current edition approved May 1, 2007. Published June 2007. Originallyapproved in 1998. Last previous edition approved in 20
14、02 as D 6234-98(2002).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from U.S. Government Printin
15、g Office, Washington, DC 20402.Request Publication Number 955-001-00000-1.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Variables listed in this test method are defined in theindividual sections in which they are discussed.4. Signi
16、ficance and Use4.1 This test method is intended as a means for obtaining anextract of mining waste. The extract may be used to estimatethe release of certain inorganic constituents of the waste underthe laboratory conditions described in this test method. Theuser is advised to minimize the holding t
17、ime between samplingand testing if the waste is suspected to contain reactive sulfideminerals.NOTE 2This method is not intended to be used as a kinetic test tosimulate weathering of mining wastes. For kinetic testing of miningwastes, refer to Test Method D 5744 to determine release rates forconstitu
18、ents of interest.4.2 The pH of the extraction fluid used in this test method isto reflect the pH of acidic precipitation in the geographic regionin 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 theextract to reflect the interaction
19、of the extractant with thebuffering capacity of the waste.4.4 This test method is not intended to provide an extractthat is representative of the actual leachate produced from awaste in the field or to produce extracts to be used as the solebasis of engineering design. If the conditions of this test
20、method are not suitable for the test material USEPA Method1312 may be used.4.5 This test method has not been demonstrated to simulateactual disposal site leaching conditions.4.6 This test method produces extracts that are amenable tothe determination of both major and minor (trace) inorganicconstitu
21、ents. When minor constituents are being determined, itis especially important that precautions be taken in samplestorage and handling to avoid possible contamination of thesamples.4.7 This test method has been tested to determine itsapplicability to certain inorganic components in the waste. Thistes
22、t method has not been tested for applicability to organicsubstances, volatile matter (see Note 4), or biologically activesamples. This test method has undergone limited testing todetermine its reproducibility.5. Apparatus5.1 Straight Edge, such as a thin-edged yardstick.5.2 Impermeable Sheet, of gla
23、zed paper, oil cloth, or otherflexible material of a composition suitable to the analytes ofinterest.5.3 Drying Pans or Dishes, (for example, aluminum tins,porcelain dishes, glass weighing pans), two per waste, suitableto the waste being tested and the instructions given in 9.2.5.4 Drying OvenAny th
24、ermostatically controlled dryingoven capable of maintaining a steady temperature of 6 2C ina range of 100 to 110C.5.5 Desiccator, having a capacity to hold the drying pansdescribed in 5.3 and the crucibles described in 5.16.5.6 Laboratory Balance, capable of weighing to 0.1 g.5.7 Erlenmeyer Flask, 2
25、-L capacity, equipped with a mag-netic stir bar.5.8 Magnetic Stir Plate.5.9 Graduated cylinder, 1 or 2-L capacity.5.10 Pipet, 1-mL capacity.5.11 Volumetric Flask, 1-L capacity.5.12 Pipet, 10-mL capacity. (Various other sized pipets,including micropipets, may be necessary for 9.3.2.)5.13 pH MeterAny
26、pH meter with a readability of 0.01units and an accuracy of 6 0.05 units at 25C.5.14 Carboy-Type Container, with spigot, 20 to 50-L capac-ity, of a composition suitable to the nature of the analyses to beperformed (see Practices D 3370).5.15 Large Glass Funnel.5.16 Crucibles, porcelain, 20-mL capaci
27、ty each, two perwaste.5.17 Wash Bottle, 500-mL capacity.5.18 Agitation Equipment, of any type that rotates theextraction vessel in an end-over-end fashion at a rate of 30 62 r/min such that the axis of rotation is horizontal and it passesthrough the center of the bottle (see Fig. 1).5.19 Pressure Fi
28、ltration AssemblyA pressure filtrationdevice using pressure regulated compressed gas of a compo-sition suitable to the nature of the analyses to be performed andequipped with a 0.45 or 0.8-m pore size filter (see Note 6).5.20 Extraction Vessels, cylindrical, wide-mouth, of a com-position suitable to
29、 the nature of the waste and analyses to beperformed, constructed of materials that will not allow sorptionof the constituents of interest, and sturdy enough to withstandthe impact of the falling sample fragments. The size of thecontainer should he selected so that the sample, plus extractionfluid o
30、ccupy approximately 95 % of the container. The con-tainers must have water-tight closures.5.20.1 Extraction vessels should be cleaned in a mannerconsistent with the analyses to he performed (see Section 13 ofPractice D 3370).6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in al
31、l tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is of
32、sufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean Type IV reagent water at18 to 27C conforming to Specification D 1193. The methodby which the water is prepared,
33、that is, distillation, ionexchange, reverse osmosis, electrodialysis, or a combinationthereof, should remain constant throughout testing.6.3 Sulfuric Acid/Nitric Acid SolutionA 60/40 weightpercent (weight %) mixture prepared using 95 to 98 weight %4Reagent Chemicals, American Chemical Society Specif
34、ications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Conven
35、tion, Inc. (USPC) , Rockville,MD.D 6234 98 (2007)2sulfuric acid and 69 to 71 weight % nitric acid. (See 9.3 forinstructions on the preparation of this solution.)7. Sampling7.1 Obtain a representative sample of the mining waste to betested by using, where available, ASTM sampling methodsdeveloped for
36、 the specific industry (see Practice D75, GuideD 420, Terminology D 653, Test Method D 2234, and PracticeE 877).7.2 Sampling methodology for materials of similar physicalform shall be used where no specific methods are available.7.3 The amount of sample to be sent to the laboratoryshould he sufficie
37、nt to perform the solids content determinationas specified in 9.2, and to provide 100 g of sample on a dryweight basis for extraction.7.4 It is important that the sample of the mining waste berepresentative with respect to the inorganic constituents to bedetermined.NOTE 3Information on obtaining rep
38、resentative samples can also befound in Pierre Gys Sampling Theory and Sampling Practice.57.5 In order to prevent sample contamination or constituentloss prior to extraction, keep the samples in closed containersappropriate to sample type and desired analysis. See PracticesD 3370 for guidance. Recor
39、d the storage conditions andhandling procedures in the report.7.6 The time between collection and extraction of thesample should be determined by the nature of the sample andthe information desired. See Practices D 3370 for guidance.Report the length of time between sample collection andextraction.
40、The user is advised to minimize the holding timebetween sampling and testing if the waste is suspected tocontain reactive sulfide minerals. Sample containing sulfide5Pitard, F., Pierre Gys Sampling Theory and Sampling Practice, 2nd Edition,CRC Press, Boca Raton, FL, 1993.FIG. 1 ExtractorsD 6234 98 (
41、2007)3minerals may be preserved by filling the container withnitrogen gas and storing at 10C.8. Sample Preparation8.1 Pass the gross sample through a 9.5-mm (3/8 in.) sieveand stage crush any oversize material no more than necessaryto pass it through the sieve. Divide the gross sample in a rifflespl
42、itter with 25-mm (1 in.) chutes, repeatedly if necessary, toobtain a representative laboratory sample with a weight in therange of 250 to 500 g. Obtain a sample of the approximate sizerequired in the test by quartering the sample received fortesting on an impermeable sheet of glazed paper, oil cloth
43、, orother flexible material having a composition suitable to theanalytes of interest, as follows:8.1.1 Empty the sample container into the center of thesheet.8.1.2 Gently flatten the sample out with a suitable straight-edge until it is spread uniformly to a depth at least twice themaximum particle d
44、iameter.8.1.3 Remix the sample by lifting a corner of the sheet anddrawing it low across to the opposite corner in such a mannerthat the material is made to roll over and over and does notmerely slide along. Continue the operation with each corner,proceeding in a clockwise direction. Repeat this ope
45、ration tentimes.8.1.4 Lift all four corners of the sheet toward the center and,holding all four corners together, raise the entire sheet into theair to form a pocket for the sample.8.1.5 Repeat the procedure described in 8.1.2 to flatten thesample out.8.1.6 With a straightedge (such as a thin-edged
46、yardstick) atleast as long as the flattened mound of sample, gently dividethe sample into quarters. Make an effort to avoid using pressureon the straightedge sufficient to cause damage to the particles.8.1.7 Discard the alternate quarters.8.1.8 If further reduction of the sample size is necessary,re
47、peat the steps given in 8.1.3 through 8.1.7. Use a sample sizeto provide at least 100 g of solid on a dry weight basis. Provideadditional samples for the determination of solids content (see9.2). Use of a sample size less than 100 g of solid on a dryweight basis for extraction is not recommended; ho
48、wever, if adifferent sample size is used, report this fact.NOTE 4For other acceptable methods of mixing and subsamplingfree-flowing solid particulate wastes, see Pierre Gys Sampling Theoryand Sampling Practice.5The method of subsampling should be deter-mined by the physical properties of the waste,
49、analytes of interest, andequipment available.9. Procedure9.1 Record a physical description of the sample to be tested,including particle size so far as it is known.9.2 Solids ContentDetermine the solids weight fraction oftwo separate portions of the sample as follows:9.2.1 Dry to a constant weight, at 104 6 2C, two dishes orpans of size suitable to the solid waste being tested. Cool in adesiccator and weigh. Record the values to 6 0.1 g.9.2.2 Place at least 50 g of the waste to be tested into eachpan. Record the mass of sample in each pan to 6 0.1 g.9.2.3 Dry f
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