1、Designation: E 2242 07Standard Test Method forColumn Percolation Extraction of Mine Rock by theMeteoric Water Mobility Procedure1This standard is issued under the fixed designation E 2242; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revi
2、sion, 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 provides a procedure for the columnpercolation extraction of mine rock in order to
3、 determine thepotential for dissolution and mobility of certain constituents bymeteoric water.1.2 This test method is intended to describe the procedurefor performing column percolation extractions only. It does notdescribe all types of sampling and analytical requirements thatmay be associated with
4、 its application.1.3 The values stated in SI units are to be regarded as thestandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices an
5、d determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 1293 Test Methods for pH of WaterD 6234 Test Method for Shake Extraction of Mining Wasteby the Synthetic Precipitation Leaching ProcedureE50 Practi
6、ces for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 389 Test Method for Particle Size or Screen Analysis atNo. 4 (4.75-mm) Sieve and Coarser for M
7、etal-BearingOres and Related MaterialsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE 877 Practice for Sampling and Sample Preparation of IronOres and Related MaterialsE 882 Guide for Accountability and Quality Control in theChemical Analysis Labora
8、toryE 1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical Method2.2 Other References:Meteoric Water Mobility Procedure, Bureau of MiningRegulation and Reclamation, Nevada Division of Envi-ronmental Protection, 9/19/90Standard Methods for the Examination
9、of Water andWastewater, 18th edition, APHA/AWWA/WEF, 19923. Terminology3.1 DefinitionsFor definitions of terms used in this testmethod, see Terminology E 135.3.1.1 meteoric waterrainfall that has the potential tocontact materials and mobilize soluble constituents from minerock at a mining or mineral
10、 processing site.3.1.2 mine rockore, waste rock or overburden excavatedin order to recover metals or minerals during mining operationsor coarse processed ore such as heap leach spoils.4. Summary of Test Method4.1 The test material is placed in a plastic column andcontacted with an equal weight of wa
11、ter during a 24 h leachingperiod. The extract is collected and preserved for analysis ofinorganic constituents.5. Significance and Use5.1 This test method is intended as a means for obtaining anextract from mine rock samples. The extract may be used toestimate the final pH and release of certain con
12、stituents of thetest sample under the laboratory conditions described in thistest method.5.2 The pH of the extraction fluid used in this test methodshould reflect the pH of precipitation in the geographic regionin which the mine rock is being evaluated.1This test method is under the jurisdiction of
13、ASTM Committee E01 onAnalytical Chemistry for Metals, Ores and Related Materials and is the directresponsibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-lurgical Materials.Current edition approved June 1, 2007. Published June 2007. Originallyapproved in 2002. Last previous ed
14、ition approved in 2002 as E 2242 02.2For 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.1Copyright ASTM Internati
15、onal, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.3 This test method is designed to mobilize potentialcontaminants present in the solids, so that the resulting extractcan be used to assess leachate that could potentially beproduced from mine rock in the fiel
16、d.5.4 This test method has not been demonstrated to simulateactual site leaching conditions.5.5 This test method produces extracts that are amenable tothe determination of both major and minor (trace) constituents.When minor constituents are being determined, it is especiallyimportant that precautio
17、ns be taken in sample preservation,storage and handling to avoid possible contamination of theextracts.5.6 This test method is a comparative method intended foruse as a routine method for monitoring mine rock. It isassumed that all who use this method will be trained analystscapable of performing sk
18、illfully and safely. It is expected thatwork will be performed in a properly equipped laboratoryunder appropriate quality control practices such as thosedescribed in Guide E 882.6. Interferences6.1 This test method may not be suitable for obtainingextracts from finely divided solids (such as: finely
19、 crushed drillcuttings, clays, sludges, mill tailings, etc.), due to difficulty inobtaining a representative extract solution. If it takes more than48 h for the column to produce an extract which has a massequivalent to 70 % of the dry test sample weight, use of analternate extraction procedure may
20、be required, such asMethod D 6234.7. Apparatus7.1 Drying Pans or Dishes, for moisture content determina-tions, 1 kg capacity.7.2 Extraction Column, PVC column of 15-cm (6-in.) O.D.of sufficient height to contain a minimum of 5 kg of test samplewith a feed particle size that just passes a 5-cm (2-in.
21、) sieve andsufficient additional height to contain applied water volumeshould poor percolation occur. Fora5kgtest sample, a 15 cmO.D. 3 45 cm high column is recommended. Additionalcolumn height will be required for test sample quantitiesgreater than 5 kg. The bottom of the column must be sealed anda
22、 solution discharge outlet situated above the sealed bottom ofthe column and below a perforated support plate. A drawing ofa suitable extraction column is shown in Fig. 1.7.3 Filtration Device, of a composition suitable to thenature of the analyses to be performed and equipped with a0.45 m pore size
23、 filter. An assembly for pre-filtration or acentrifuge may be required if 0.45 m filtration is difficult.7.4 Filter Media, glass wool (inert) or a plastic fiber pad isplaced onto the support plate before loading the laboratorysample into the column, to minimize fines migration, and ontothe top of th
24、e test sample after column loading, to aid inmaking an even water distribution.7.5 Laboratory Balance, capable of weighing to 1.0 g.7.6 pH Meter, with a readability of 0.01 units and anaccuracy of at least 6 0.05 units at 25 C.7.7 Tubing, surgical or synthetic tubing sufficient in diam-eter and leng
25、th for the extraction column assembly (pump,column outlet).7.8 Water and Extract Containers, sufficient in size tocontain the water added during extraction. Containers must becovered to avoid contamination.7.9 Water Metering Device, a metering pump or constanthead device to insure constant rate extr
26、action fluid applicationduring column percolation.8. Reagents and Materials8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American
27、 Chemical Society,where such specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, referencesto water s
28、hall be understood to mean Type II reagent water at18 C to 27 C conforming to Specification D 1193.9. Hazards9.1 For precautions to be observed in the use of analyticalmethods associated with this standard, refer to Practices E50.10. Sampling and Sample Preparation10.1 The amount of gross sample to
29、be sent to the laboratoryshould he sufficient to perform the solids content determinationas specified in 10.3, and to provide at least 5 kg of test sampleon a dry weight basis for extraction. Gross sample weights inthe range of 7 to 25 kg are appropriate.NOTE 1Information on obtaining representative
30、 samples can also befound in Pierre Gys Sampling Theory and Sampling Practice4and inPractice E 877.10.2 In order to prevent sample contamination or constitu-ent loss prior to extraction, keep the samples in closedcontainers appropriate to sample type and desired analysis.10.3 Moisture DeterminationR
31、emove the gross samplefrom the container and blend by coning or rolling to obtain asample for feed moisture content with a minimum of 500 g dryweight.10.3.1 Weigh the moisture test sample and dry to constantweight (6 0.05 %) at 105 C 6 2 C and record the weight.10.3.2 Calculate the moisture content
32、of the test sample asfollows:M 5100B 2 A!B(1)3Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington. DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Poole, Dorset, U.K., and the UnitedStates Pharmacopeia and
33、National Formulary, U.S. Pharmaceutical Convention,Inc. (USPC), Rockville, MD.4Pitard, F., Pierre Gys Sampling Theory and Sampling Practice, Vols. I and II,CRC Press, 1989.E2242072where:A = mass of sample after drying, g,B = wet mass of sample, g, andM = moisture content, %.10.4 Separate the remaini
34、ng laboratory sample on a 5-cm(2-in.) sieve. Save the minus 5-cm fraction for recombinationwith the crushed plus 5-cm fraction. The screening time or endpoint is when additional periods of shaking fail to change theresults by more than 0.3 % (Method E 389). For highly friablematerial an acceptable e
35、nd point shall be determined experi-mentally.10.5 Weigh the plus and minus 5-cm sieve fractions, calcu-late and record the weight percent retained on the 5-cm sieveas follows:R 5100CC 1 D!(2)where:R = weight retained on the 5-cm sieve, %,C = mass retained on the 5-cm sieve, g, andD = mass passing th
36、e 5-cm sieve, g.10.6 Crush or hand break the materials retained on the 5-cmsieve so that they just pass through the 5-cm (2-in.) sieve,combine with the saved fraction passed through the 5-cm sieveand mix the prepared sample.10.7 Thoroughly blend the prepared sample and calculatethe minimum test samp
37、le weight containing 5 kg dry weight,based on the feed moisture content from 10.3, as follows:S 55 3 105100 2 M!(3)where:FIG. 1 Column Percolation Extraction Device (Meteoric Water Mobility Procedure)E2242073S = minimum sample mass for testing, g andM = moisture content, %.10.8 Divide the prepared s
38、ample, if necessary, to obtain atest sample suitable for processing in the column apparatus butnot less than the minimum sample weight from 10.7. and weighto 6 1 g. Label and reserve any excess prepared sample for anyadditional testing which may be required.10.9 Calculate the dry weight of the test
39、sample as follows:L 5E100 2 M!100(4)where:L = dry mass of the test sample, g,E = gross mass of the test sample, g, andM = moisture content of the gross sample, %.11. Procedure11.1 Place filter media (7.4) in the bottom of the extractioncolumn and load the laboratory sample incrementally (1-kg/increm
40、ent) into the column. To minimize particle segregationand compaction during column loading, the sample portionsshall be dropped from no more than 0.6 m (24 in.) whenintroduced from the top of the column, and no tamping,shaking, or other methods to compact the sample will beemployed. Place filter med
41、ia over the test sample in thecolumn.11.2 Use a water addition rate of 3.5 mL/min for minimumweight samples in the range of 5 to 5.5 kg dry weight.11.2.1 For samples greater than 5.5 kg dry weight, calculatethe rate of water addition to the column to pass a weight ofwater equal to the dry weight of
42、the test sample during the 24h test period as follows:F 5L1440(5)where:F = water addition rate, mL/min, andL = dry mass of the laboratory sample, g.11.3 Measure and record the initial temperature and pH ofthe leaching water in accordance with Test Methods D 1293.Record the time and date that water a
43、ddition is started.11.4 Add water to the column at the rate specified in 11.2until the weight of the effluent is equal to the dry mass of thelaboratory sample. If the water will not freely percolatethrough the column, abort the test and repeat the evaluationusing an alternate testing procedure, such
44、 as Test MethodD 6234.11.5 Discontinue water addition and effluent collectionwhen the effluent weight is equal to the dry weight of the testsample or 48 h has elapsed, which ever occurs first. If, after 48h, the effluent weight is not at least 70 % of the dry weight ofthe test sample, abort the test
45、 and select an alternate testingmethod for the sample, such as Test Method D 6234.11.6 Thoroughly mix the effluent and let the column effluentcontinue to drain into a waste container.11.7 Immediately measure and record the final pH of theeffluent in accordance with Test Methods D 1293. Record thedat
46、e, time and final effluent weight.11.8 ExtractQuantitatively transfer a 2-L portion of theeffluent through a large glass funnel to a filtration deviceequipped with a 0.45 m filter for analyses of dissolvedconstituents. Pre-filtration using a coarse porosity glass filterand centrifuge separation proc
47、edures may be necessary prior tofiltration for some difficult to filter effluents. Immediatelymeasure and record the final pH of the extract in accordancewith Test Methods D 1293. Record the final effluent and extractweights.11.8.1 Retain a 250-mL portion of the extract for metalsanalysis with its p
48、H adjusted to less than 2 with nitric acid.11.8.2 Retain a 250-mL portion of the extract for nutrientsanalysis with its pH adjusted to less than 2 with sulfuric acid.11.8.3 Retain a 1-L portion of the extract for cyanideanalysis with its pH adjusted to between 12 and 12.5 withsodium hydroxide. Store
49、 in a dark bottle at 4 C 6 2 C, if thecyanide analysis is not performed immediately.11.8.4 Refrigerate the remaining extract at 4 C 6 2Cformineral analyses.11.9 Analyze the unfiltered effluent for specific constituentsor properties, or use for biological testing procedures asnecessary.11.10 Analyses should be performed using appropriateASTM test methods. Where no appropriate ASTM test meth-ods exist, other test methods may be used, such as StandardMethods for the Examination of Water and Wastewater, andrecord the methods used in the report. Whether visible
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