1、Designation: D6234 98 (Reapproved 2007)D6234 13Standard Test Method forShake Extraction of Mining Waste by the SyntheticPrecipitation Leaching Procedure1This standard is issued under the fixed designation D6234; the number immediately following the designation indicates the year oforiginal adoption
2、or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers a procedure for the shake leaching of mining waste co
3、ntaining at least 80 % dry solids ( 20 %(20 % moisture) in order to generate a solution to be used to determine the inorganic constituents leached under the specifiedtesting conditions,conditions that conform to the synthetic precipitation leaching procedure (SPLP).1.2 This test method calls for the
4、 shaking of a known weight of mining waste with acidic extraction fluid of a specifiedcomposition as well as the separation of the liquid phase for analysis. The pH of the extraction fluid is to reflect the pH of acidicprecipitation in the geographic region in which the waste being tested is to be d
5、isposed.NOTE 1Possible sources of information concerning the pH of the precipitation in the geographic region of interest include state and federalenvironmental 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
6、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 thanthe desired pH for the site, do not use this test method,method; use Test Method D3987 or Test Method E2242.NOTE 2The method may also be suitable
7、for use in testing of mineral processing waste from meal mining process operations for jurisdictions thatdo 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 alltypes of sampling samp
8、ling, 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 concern
9、s, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D75 Practice for Sampling AggregatesD420 Guid
10、e to Site Characterization for Engineering Design and Construction Purposes (Withdrawn 2011)3D653 Terminology Relating to Soil, Rock, and Contained FluidsD1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2234/D2234M Practice for Collection of a Gross Sample of CoalD2777 Practi
11、ce for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on WaterD3370 Practices for Sampling Water from Closed ConduitsD3987 Practice for Shake Extraction of Solid Waste with WaterD5744 Test Method for Laboratory Weathering of Solid Materials Using a Humidity CellE691
12、Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test MethodE877 Practice for Sampling and Sample Preparation of Iron Ores and Related Materials for Determination of ChemicalComposition1 This test method is under the jurisdiction ofASTM Committee D34 on Waste Manageme
13、nt and is the direct responsibility of Subcommittee D34.01.04 on Waste LeachingTechniques.Current edition approved May 1, 2007Sept. 1, 2013. Published June 2007September 2013. Originally approved in 1998. Last previous edition approved in 20022007 asD6234-98(2002).D6234-98(2007). DOI: 10.1520/D6234-
14、98R07.10.1520/D6234-13.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 The last approved version of this hi
15、storical standard is referenced on www.astm.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurate
16、ly, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1
17、E1915 Test Methods forAnalysis of Metal Bearing Ores and Related Materials for Carbon, Sulfur, andAcid-Base CharacteristicsE2242 Test Method for Column Percolation Extraction of Mine Rock by the Meteoric Water Mobility Procedure2.2 EPA Document:U.S. Environmental ProtectionAgency, Synthetic Precipit
18、ation Leaching Procedure, Method 1312 in SW-846, Test Methods forEvaluating Solid Waste, Physical/Chemical Methods, Third Edition43. Terminology3.1 DefinitionsFor definitions of terms used in this test method, see Terminology D1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 mining wast
19、e,nwaste, noverburden or waste rock excavated and disposed of during mining operations.3.3 Symbols: Variables listed in this test method are defined in the individual sections in which they are discussed.4. Significance and Use4.1 This test method is intended as a means for obtaining an extract of m
20、ining waste. The extract may be used to estimate therelease of certain inorganic constituents of the waste under the laboratory conditions described in this test method. The user isadvised to minimize the holding time between sampling and testing if the waste is suspected to contain reactive sulfide
21、 minerals.NOTE 3This method is not intended to be used as a kinetic test to simulate weathering of mining wastes. For kinetic testing of mining wastes, referto Test Method D5744 to determine release rates for constituents of interest. For static testing of metal mining ore and mining or mineral proc
22、essing wastematerials, refer to Test Method 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 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 the
23、extract to reflect the interaction of the extractant with the bufferingcapacity 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 wastein the field or to produce extracts to be used as the sole basis of engineering d
24、esign. If the conditions of this test method are notsuitable 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 d
25、etermination of both major and minor (trace) inorganicconstituents. When minor constituents are being determined, it is especially important that precautions be taken in sample storageand handling to avoid possible contamination of the samples.4.7 This test method has been tested to determine its ap
26、plicability to certain inorganic components in the waste.This test methodhas not been tested for applicability to organic substances, volatile matter (see Note 45), or biologically active samples. This testmethod has undergone limited testing to determine its reproducibility.5. Apparatus5.1 Straight
27、 Edge, such as a thin-edged yardstick.5.2 Impermeable Sheet, of glazed paper, oil cloth, or other flexible material of a composition suitable to the analytes of interest.5.3 Drying Pans or Dishes, (for example, aluminum tins, porcelain dishes, glass weighing pans), two per waste, suitable to thewast
28、e being tested and the instructions given in 9.2.5.4 Drying OvenAny thermostatically controlled drying oven capable of maintaining a steady temperature of 6 2C 62Cin a range of 100 to 110C.5.5 Desiccator, having a capacity to hold the drying pans described in 5.3 and the crucibles described in 5.16.
29、5.6 Laboratory Balance, capable of weighing to 0.1 g.5.7 Erlenmeyer Flask, 2-L capacity, equipped with a magnetic 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
30、pipets, including micropipets, may be necessary for 9.3.2.)4 Available from U.S. Government Printing Office, Washington, DC 20402. Request Publication Number 955-001-00000-1.D6234 1325.13 pH MeterAny pH meter with a readability of 0.01 units and an accuracy of 6 0.05 60.05 units at 25C.5.14 Carboy-T
31、ype Container, with spigot, 20 to 50-L capacity, of a composition suitable to the nature of the analyses to beperformed (see Practices D3370).5.15 Large Glass Funnel.5.16 Crucibles, porcelain, 20-mL capacity each, two per waste.5.17 Wash Bottle, 500-mL capacity.5.18 Agitation Equipment, of any type
32、that rotates the extraction vessel in an end-over-end fashion at a rate of 30 6 2 r/minsuch that the axis of rotation is horizontal and it passes through the center of the bottle (see Fig. 1).5.19 Pressure Filtration AssemblyA pressure filtration device using pressure regulated compressed gas of a c
33、ompositionsuitable to the nature of the analyses to be performed and equipped with a 0.45 or 0.8-m pore size filter (see Note 67).5.20 Extraction Vessels, cylindrical, wide-mouth, of a composition suitable to the nature of the waste and analyses to beperformed, constructed of materials that will not
34、 allow sorption of the constituents of interest, and sturdy enough to withstand theimpact of the falling sample fragments. The size of the container should he selected so that the sample, plus extraction fluid occupyapproximately 95 % of the container. The containers must have water-tight closures.5
35、.20.1 Extraction vessels should be cleaned in a manner consistent with the analyses to he performed (see Section 13 of PracticeD3370).FIG. 1 ExtractorsD6234 1336. Reagents6.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreag
36、ents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.5 Other grades may be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening th
37、e accuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean Type IV reagent water at 18to 27C conforming to Specification D1193. The method by which the water is prepared, that is, distillation, ion exchange, reverseosmosis, electrod
38、ialysis, or a combination thereof, should remain constant throughout testing.6.3 Sulfuric Acid/Nitric Acid SolutionA 60/40 weight percent (weight %) mixture prepared using 95 to 98 weight % sulfuricacid and 69 to 71 weight % nitric acid. (See 9.3 for instructions on the preparation of this solution.
39、)7. Sampling7.1 Obtain a representative sample of the mining waste to be tested by using, where available, ASTM sampling methodsdeveloped for the specific industry (see Practice D75, Guide D420, Terminology D653, Test Method D2234/D2234M, and PracticeE877).7.2 Sampling methodology for materials of s
40、imilar physical form shall be used where no specific methods are available.7.3 The amount of sample to be sent to the laboratory should hebe sufficient to perform the solids content determination asspecified in 9.2, and to provide 100 g of sample on a dry weight basis for extraction.7.4 It is import
41、ant that the sample of the mining waste be representative with respect to the inorganic constituents to bedetermined.NOTE 4Information on obtaining representative samples can also be found in Pierre Gys Sampling Theory and Sampling Practice.67.5 In order to prevent sample contamination or constituen
42、t loss prior to extraction, keep the samples in closed containersappropriate to sample type and desired analysis. See Practices D3370 for guidance. Record the storage conditions and handlingprocedures in the report.7.6 The time between collection and extraction of the sample should be determined by
43、the nature of the sample and theinformation desired. See Practices D3370 for guidance. Report the length of time between sample collection and extraction. Theuser is advised to minimize the holding time between sampling and testing if the waste is suspected to contain reactive sulfideminerals. miner
44、als (seeTest Methods E1915). Sample containing reactive sulfide minerals may be preserved by filling the containerwith nitrogen gas and storing at 10C.8. Sample Preparation8.1 Pass the gross sample through a 9.5-mm (3/8 in.) sieve and stage crush any oversize material no more than necessary to passi
45、t through the sieve. Divide the gross sample in a riffle splitter with 25-mm (1 in.) chutes, repeatedly if necessary, to obtain arepresentative laboratory sample with a weight in the range of 250 to 500 g. Obtain a sample of the approximate size required inthe test by quartering the sample received
46、for testing on an impermeable sheet of glazed paper, oil cloth, or other flexible materialhaving a composition suitable to the analytes of interest, as follows:8.1.1 Empty the sample container into the center of the sheet.8.1.2 Gently flatten the sample out with a suitable straightedge until it is s
47、pread uniformly to a depth at least twice the maximumparticle diameter.8.1.3 Remix the sample by lifting a corner of the sheet and drawing it low across to the opposite corner in such a manner thatthe material is made to roll over and over and does not merely slide along. Continue the operation with
48、 each corner, proceedingin a clockwise direction. Repeat this operation ten times.8.1.4 Lift all four corners of the sheet toward the center and, holding all four corners together, raise the entire sheet into the airto form a pocket for the sample.8.1.5 Repeat the procedure described in 8.1.2 to fla
49、tten the sample out.8.1.6 With a straightedge (such as a thin-edged yardstick) at least as long as the flattened mound of sample, gently divide thesample into quarters. Make an effort to avoid using pressure on the straightedge sufficient to cause damage to the particles.8.1.7 Discard the alternate quarters.5 Reagent Chemicals, American Chemical Society Specifications, , American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poo
