1、Designation:E224207 Designation: E2242 12Standard 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, i
2、n 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 provides a procedure for the column percolation extraction of min
3、e rock in order to determine the potentialfor dissolution and mobility of certain constituents by meteoric water.1.2 This test method is intended to describe the procedure for performing column percolation extractions only. It does notdescribe all types of sampling and analytical requirements that m
4、ay be associated with its application.1.3 The values stated in SI units are to be regarded as the standard.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety a
5、nd health practices and determine the applicability of regulatorylimitations 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 Waste by the Synthetic Precipitation Leaching P
6、rocedureD7237 Test Method for Free Cyanide with Flow InjectionAnalysis (FIA) Utilizing Gas Diffusion Separation andAmperometricDetectionE50 Practices forApparatus, Reagents, and Safety Considerations for ChemicalAnalysis of Metals, Ores, and Related MaterialsE135 Terminology Relating toAnalytical Ch
7、emistry for Metals, Ores, and Related Materials E389Test Method for Particle Sizeor Screen Analysis at No. 4(4.75-mm) Sieve and Coarserfor Metal-Bearing Ores andRelated MaterialsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test MethodE877 Practice for Samplin
8、g and Sample Preparation of Iron Ores and Related Materials for Determination of ChemicalCompositionE882 Guide for Accountability and Quality Control in the Chemical Analysis LaboratoryE1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method2.2 Other
9、 References:Meteoric Water Mobility Procedure, Bureau of Mining Regulation and Reclamation, Nevada Division of EnvironmentalProtection, 9/19/90Standard Methods for the Examination of Water and Wastewater, 18th edition, APHA/AWWA/WEF, 19923. Terminology3.1 Definitions:3.1.1 For definitions of terms u
10、sed in this test method, see Terminology E135.3.1.2 meteoric waterrainfall that has the potential to contact materials and mobilize soluble constituents from mine rock ata mining or mineral processing site.1This test method is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for
11、Metals, Ores, and Related Materials and is the direct responsibility ofSubcommittee E01.02 on Ores, Concentrates, and Related Metallurgical Materials.Current edition approved June 1, 2007.2012. Published June 2007.July 2012. Originally approved in 2002. Last previous edition approved in 20022007 as
12、E2242 027.DOI: 10.1520/E2242-07.10.1520/E2242-12.2For 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.1This documen
13、t 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 accurately, ASTM recommends that users consult prior editions as app
14、ropriate. 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 States.3.1.3 mine rockore, waste rock or overburden excavated in or
15、der to recover metals or minerals during mining operations orcoarse processed ore such as heap leach spoils.4. Summary of Test Method4.1 The test material is placed in a plastic column and contacted with an equal weight of water during a 24 h leaching period.The extract is collected and preserved fo
16、r analysis of inorganic constituents.5. Significance and Use5.1 This test method is intended as a means for obtaining an extract from mine rock samples. The extract may be used toestimate the final pH and release of certain constituents of the test sample under the laboratory conditions described in
17、 this testmethod.5.2 The pH of the extraction fluid used in this test method should reflect the pH of precipitation in the geographic region inwhich the mine rock is being evaluated.5.3 This test method is designed to mobilize potential contaminants present in the solids, so that the resulting extra
18、ct can be usedto assess leachate that could potentially be produced from mine rock in the field.5.4 This test method has not been demonstrated to simulate actual site leaching conditions.5.5 This test method produces extracts that are amenable to the determination of both major and minor (trace) con
19、stituents.When minor constituents are being determined, it is especially important that precautions be taken in sample preservation, storageand handling to avoid possible contamination of the extracts.5.6 This test method is a comparative method intended for use as a routine method for monitoring mi
20、ne rock. It is assumed thatall who use this method will be trained analysts capable of performing skillfully and safely. It is expected that work will beperformed in a properly equipped laboratory under appropriate quality control practices such as those described in Guide E882.6. Interferences6.1 T
21、his test method may not be suitable for obtaining extracts from finely divided solids (such as: finely crushed drill cuttings,clays, sludges, mill tailings, etc.), due to difficulty in obtaining a representative extract solution. If it takes more than 48 h for thecolumn to produce an extract which h
22、as a mass equivalent to 70 % of the dry test sample weight, use of an alternate extractionprocedure may be required, such as Test Method D6234.NOTE 1See Appendix X1 for the alternative bottle roll extraction option for fine-grained solids.7. Apparatus7.1 Drying Pans or Dishes, for moisture content d
23、eterminations, 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 and sufficient additional height to contain applied water volume shouldpoor percolation
24、 occur. Fora5kgtest sample, a 15 cm O.D. 3 45 cm high column is recommended. Additional column heightwill be required for test sample quantities greater than 5 kg. The bottom of the column must be sealed and a solution dischargeoutlet situated above the sealed bottom of the column and below a perfor
25、ated support plate. A drawing of a suitable extractioncolumn is shown in Fig. 1.7.3 Filtration Device, of a composition suitable to the nature of the analyses to be performed and equipped with a 0.45 m poresize filter. An assembly for pre-filtration or a centrifuge may be required if 0.45 m filtrati
26、on is difficult.7.4 Filter Media, glass wool (inert) or a plastic fiber pad is placed onto the support plate before loading the laboratory sampleinto the column, to minimize fines migration, and onto the top of the test sample after column loading, to aid in making an evenwater distribution.7.5 Labo
27、ratory Balance, capable of weighing to 1.0 g.7.6 pH Meter, with a readability of 0.01 units and an accuracy of at least 6 0.05 units at 25 C.7.7 Tubing, surgical or synthetic tubing sufficient in diameter and length for the extraction column assembly (pump, columnoutlet).7.8 Water and Extract Contai
28、ners , sufficient in size to contain the water added during extraction. Containers must be coveredto avoid contamination.7.9 Water Metering Device, a metering pump or constant head device to insure constant rate extraction fluid application duringcolumn percolation.8. Reagents and Materials8.1 Purit
29、y of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, whereE2242 122such specifications are available.3Other grades may
30、 be used, provided it is first ascertained that the reagent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.8.2 Purity of WaterUnless otherwise indicated, references to water shall be understood to mean Type II reagent water at 18C to 27 C conformi
31、ng to Specification D1193. . Type III or V may be used if they effect no measurable change in the blank orsample.9. Hazards9.1 For precautions to be observed in the use of analytical methods associated with this standard, refer to Practices E50.10. Sampling and Sample Preparation10.1 The amount of g
32、ross sample to be sent to the laboratory should he sufficient to perform the solidsmoisture contentdetermination as specified in 10.3, and to provide at least 5 kg of test sample on a dry weight basis for extraction. Gross sample3Reagent Chemicals, American Chemical Society Specifications, American
33、Chemical Society, Washington., DC. For suggestions on the testing of reagents not listed bythe American Chemical Society, see Poole, Dorset, U.K., and the United States Pharmacopeia and National Formulary, U.S. PharmaceuticalPharmacopeial Convention, Inc.(USPC), Rockville, MD.FIG. 1 Column Percolati
34、on Extraction Device (Meteoric Water Mobility Procedure)E2242 123weights in the range of 7 kg to 25 kg are appropriate.NOTE 12Information on obtaining representative samples can also be found in Pierre Gys Sampling Theory and Sampling Practice4and in PracticeE877.10.2 In order to prevent sample cont
35、amination or constituent loss prior to extraction, keep the samples in closed containersappropriate to sample type and desired analysis.10.3 Moisture DeterminationRemove the gross sample from the container and blend by coning or rolling to obtain a samplefor feed moisture content with a minimum of 5
36、00 g dry weight.10.3.1 Weigh the moisture test sample and dry to constant weight (6 0.05 %) at 105 C 6 2 C and record the weight.10.3.2 Calculate the moisture content of the test sample as follows:M 5100B 2 A!B(1)E2242-12_1where:A = mass of sample after drying, g,B = wet mass of sample, g, andM = mo
37、isture content, %.10.4 Separate the remaining laboratory sample on a 5-cm (2-in.) sieve. Save the minus 5-cm fraction for recombination withthe crushed plus 5-cm fraction. The screening time or end point is when additional periods of shaking fail to change the resultsby more than 0.3% (Method E389).
38、0.3 %. For highly friable material an acceptable end point shall be determined experimentally.10.5 Weigh the plus and minus 5-cm sieve fractions, calculate and record the weight percent retained on the 5-cm sieve asfollows:E2242-12_2where:R = weight retained on the 5-cm sieve, %,C = mass retained on
39、 the 5-cm sieve, g, andD = mass passing the 5-cm sieve, g.10.6 Crush or hand break the materials retained on the 5-cm sieve so that they just pass through the 5-cm (2-in.) sieve, combinewith the saved fraction passed through the 5-cm sieve and mix the prepared sample.10.7 Thoroughly blend the prepar
40、ed sample and calculate the minimum test sample weight containing 5 kg dry weight, basedon the feed moisture content from 10.3, as follows:E2242-12_3where:S = minimum sample mass for testing, g andM = moisture content, %.10.8 Divide the prepared sample, if necessary, to obtain a test sample suitable
41、 for processing in the column apparatus but notless than the minimum sample weight from 10.7. and weigh to 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 sample as follows:E2242-12_4where:L = dry mass of t
42、he 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 extraction column and load the laboratory sample incrementally(1-kg/increment) into the column. To minimize particle segregation and
43、compaction during column loading, the sample portionsshall be dropped from no more than 0.6 m (24 in.) when introduced from the top of the column, and no tamping, shaking, or othermethods to compact the sample will be employed. Place filter media over the test sample in the column.11.2 Use a water a
44、ddition rate of 3.5 mL/min for minimum weight 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, calculate the rate of water addition to the column to pass a weight of waterequal to the dry weight of the test sample during the 24 h test period as fol
45、lows:4Pitard, F., Pierre Gys Sampling Theory and Sampling Practice, Vols. I and II, CRC Press, 1989.E2242 124E2242-12_5where:F = water addition rate, mL/min, andL = dry mass of the laboratory sample, g.11.3 Measure and record the initial temperature and pH of the leaching water in accordance with Te
46、st Methods D1293. Recordthe time and date that water addition is started.11.4 Add water to the column at the rate specified in 11.2 until the weight of the effluent is equal to the dry mass of thelaboratory sample. If the water will not freely percolate through the column, abort the test and repeat
47、the evaluation using analternate testing procedure, such as described in X1.2 or Test Method D6234.11.5 Discontinue water addition and effluent collection when the effluent weight is equal to the dry weight of the test sampleor 48 h has elapsed, whichever occurs first. If, after 48 h, the effluent w
48、eight is not at least 70 % of the dry weight of the test sample,abort the test and select an alternate testing method for the sample, such as described in X1.3 or Test Method D6234.11.6 Thoroughly mix the effluent and let the column effluent continue to drain into a waste container.11.7 Immediately
49、measure and record the final pH of the effluent in accordance with Test Methods D1293. Record the date, timeand final effluent weight.11.8 ExtractQuantitatively transfer a 2-L portion of the effluent through a large glass funnel to a filtration device equippedwith a 0.45 m filter for analyses of dissolved constituents. Pre-filtration using a coarse porosity glass filter and centrifugeseparation procedures may be necessary prior to filtration for some difficult to filter effluents. Immediately measure and record thefinal pH of the extract in accordance with T
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