1、Designation: E2242 12aStandard Test Method forColumn Percolation Extraction of Mine Rock by theMeteoric Water Mobility Procedure1This standard is issued under the fixed designation E2242; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revis
2、ion, 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 provides a procedure for the columnpercolation extraction of mine rock in order to d
3、etermine 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 i
4、ts 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 and
5、determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1293 Test Methods for pH of WaterD6234 Test Method for Shake Extraction of Mining Wasteby the Synthetic Precipitation Leaching ProcedureD7237 Test Meth
6、od for Free Cyanide with Flow InjectionAnalysis (FIA) Utilizing Gas Diffusion Separation andAmperometric DetectionE50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE135 Terminology Relating to Analytical Chemistry forMetals,
7、Ores, and Related MaterialsE389 Test Method for Particle Size or ScreenAnalysis at No.4 (4.75-mm) Sieve and Coarser for Metal-Bearing Oresand Related MaterialsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE877 Practice for Sampling and Sample Prepara
8、tion of IronOres and Related Materials for Determination of Chemi-cal CompositionE882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical Method2.2 Other References:Meteoric
9、Water Mobility Procedure, Bureau of MiningRegulation and Reclamation, Nevada Division of Envi-ronmental Protection, 9/19/90Standard Methods for the Examination of Water and Waste-water, 18th edition, APHA/AWWA/WEF, 19923. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this test me
10、thod, seeTerminology E135.3.1.2 meteoric waterrainfall that has the potential tocontact materials and mobilize soluble constituents from minerock at a mining or mineral processing site.3.1.3 mine rockore, waste rock or overburden excavatedin order to recover metals or minerals during mining operatio
11、nsor 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 water during a 24 h leachingperiod. The extract is collected and preserved for analysis ofinorganic constituents.5. Significance and U
12、se5.1 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 constituents of thetest sample under the laboratory conditions described in thistest method.1This test method is under the jurisdiction
13、 of 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 Dec. 1, 2012. Published January 2013. Originallyapproved in 2002. Last pre
14、vious edition approved in 2012 as E2242 121. DOI:10.1520/E2242-12A.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 we
15、bsite.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15.2 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.5.3 This test me
16、thod 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 field.5.4 This test method has not been demonstrated to simulateactual site leaching conditions.5.5 This test
17、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 precautions be taken in sample preservation,storage and handling to avoid possible contamination of theextracts.5.6
18、 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 skillfully and safely. It is expected thatwork will be performed in a properly equipped laboratoryunder appr
19、opriate quality control practices such as thosedescribed in Guide E882.6. Interferences6.1 This test method may not be suitable for obtainingextracts from finely divided solids (such as: finely crushed drillcuttings, clays, sludges, mill tailings, etc.), due to difficulty inobtaining a representativ
20、e 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 be required, such as TestMethod D6234.NOTE 1See Appendix X1 for the alternative bottle roll extractionoptio
21、n for fine-grained solids.7. Apparatus7.1 Drying Pans or Dishes, for moisture contentdeterminations, 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.) sieve an
22、dsufficient additional height to contain applied water volumeshould poor percolation occur. For a 5-kg test sample, a 15-cmO.D. 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 solution
23、 discharge outlet situated above the sealed bottom ofthe column and below a perforated support plate.Adrawing 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 filter. An
24、 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 the test samp
25、le 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 length for the
26、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 extraction flui
27、d 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 Chemical S
28、ociety,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 shall be und
29、erstood to mean Type II reagent water at18 C to 27 C conforming to Specification D1193. Type III orIV may be used if they effect no measurable change in theblank or sample.9. Hazards9.1 For precautions to be observed in the use of analyticalmethods associated with this standard, refer to Practices E
30、50.10. Sampling and Sample Preparation10.1 The amount of gross sample to be sent to the laboratoryshould he sufficient to perform the moisture content determi-nation as specified in 10.3, and to provide at least 5 kg of testsample on a dry weight basis for extraction. Gross sampleweights in the rang
31、e of 7 kg to 25 kg are appropriate.NOTE 2Information on obtaining representative samples can also befound in Pierre Gys Sampling Theory and Sampling Practice4and inPractice E877.10.2 In order to prevent sample contamination or constitu-ent loss prior to extraction, keep the samples in closedcontaine
32、rs appropriate to sample type and desired analysis.10.3 Moisture DeterminationRemove 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.3Reagent Chemicals, American Chemical Society Specifications, AmericanC
33、hemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see the United States Pharmacopeia andNational Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.4Pitard, F., Pierre Gys Sampling Theory and Sampling Practice, V
34、ols. I and II,CRC Press, 1989.E2242 12a210.3.1 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 of the test sample asfollows:M 5100B 2 A!B(1)where:A = mass of sample after drying, g,B = wet mass of sample,
35、g, andM = moisture content, %.10.4 Separate the remaining 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 % (Te
36、st Method E389). For highlyfriable material an acceptable end point shall be determinedexperimentally.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 5100CC1D!(2)where:R = weight retained on the 5-cm sieve, %,C = mas
37、s retained on the 5-cm sieve, g, andFIG. 1 Column Percolation Extraction Device (Meteoric Water Mobility Procedure)E2242 12a3D = mass passing the 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 save
38、d fraction passed through the 5-cm sieveand mix the prepared sample.10.7 Thoroughly blend the prepared sample and calculatethe minimum test sample weight containing 5-kg dry weight,based on the feed moisture content from 10.3, as follows:S 55 3105100 2 M!(3)where:S = minimum sample mass for testing,
39、 g andM = moisture content, %.10.8 Divide the prepared sample, 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 ma
40、y be required.10.9 Calculate the dry weight of the test 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 a
41、nd load the laboratory sample incrementally (1-kg/increment) 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
42、 to compact the sample will beemployed. Place filter media 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-kg 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
43、column to pass a weight ofwater equal to the dry weight of 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 wit
44、h Test Methods D1293.Record the time and date that water addition 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 repea
45、t the evaluationusing an alternate testing procedure, such as described in X1.2or Test Method D6234.11.5 Discontinue water addition and effluent collectionwhen the effluent weight is equal to the dry weight of the testsample or 48 h has elapsed, whichever occurs first. If, after 48h, the effluent we
46、ight is not at least 70 % of the dry weight ofthe test sample, abort the test and select an alternate testingmethod for the sample, such as described in X1.3 or TestMethod D6234.11.6 Thoroughly mix the effluent and let the column effluentcontinue to drain into a waste container.11.7 Immediately meas
47、ure and record the final pH of theeffluent in accordance with Test Methods D1293. Record thedate, 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 dissolved
48、constituents. Pre-filtration using a coarse porosity glass filterand centrifuge separation procedures may be necessary prior tofiltration for some difficult to filter effluents. Immediatelymeasure and record the final pH of the extract in accordancewith Test Methods D1293. Record the final effluent
49、and extractweights.11.8.1 Retain a 250-mL portion of the extract for metalsanalysis with its pH 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.11.8.2.1 If the test material is a cyanidation residue orcontains cyanate, perform nutrient analysis on the refrigeratedextract from 11.8.4, since acidification of any cyanate mayresult in conversion to ammonia-nitrogen.11.8.3 Retain a 1-L portion of the extract for cyanideanalysis with its pH adjust
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