1、Designation: E1915 11Standard Test Methods forAnalysis of Metal Bearing Ores and Related Materials forCarbon, Sulfur, and Acid-Base Characteristics1This standard is issued under the fixed designation E1915; 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 These test methods cover the determination of totalcarbon and sulfur and acid-base
3、 characteristics in metal bearingores and related materials such as leach residues, tailings, andwaste rock within the following ranges:Analyte Application Range, % Quantitative Range, %TotalCarbon 0to10 0.08to10Total Sulfur 0 to 8.8 0.023 to 8.8NOTE 1The test methods were tested over the following
4、ranges:Total Carbon 0.01 % to 5.87 %Total Sulfur 0.0002 % to 4.70 %Residual Carbon from Pyrolysis 0.002 % to 4.97 %Residual Sulfur from Pyrolysis 0.014 % to 1.54 %Pyrolysis Loss Sulfur 0 % to 4.42 %Hydrochloric Acid Insoluble Carbon 0.025 % to 0.47 %Hydrochloric Acid Loss Carbon 0 % to 5.78 %Hydroch
5、loric Acid Insoluble Sulfur 0.012 % to 4.20 %Acid Neutralization Potential Acidity Titration -1.0 % to 100 %Nitric Acid Insoluble Sulfur 0.006 % to 0.924 %Nitric Acid Loss Sulfur -0.08 % to 4.19 %Sodium Carbonate Insoluble Sulfur 0.007 % to 3.78 %1.2 The quantitative ranges for the partial decomposi
6、tiontest methods are dependent on the mineralogy of the samplesbeing tested. The user of these test methods is advised toconduct an interlaboratory study in accordance with PracticeE1601 on the test methods selected for use at a particularmining site, in order to establish the quantitative ranges fo
7、rthese test methods on a site-specific basis.1.3 The test methods appear in the following order:SectionsCarbon and Sulfur, Total 10.1-10.9Carbon and Sulfur, Residual from Pyrolysis 10.10-10.18Carbon and Sulfur, Hydrochloric Acid Insoluble 10.19-10.27Acid Neutralization Potential Acidity Titration 10
8、.28-10.36Sulfur, Nitric Acid Insoluble 10.37-10.45Sulfur, Sodium Carbonate Insoluble 10.46-10.541.4 The values stated in SI units are to be regarded asstandard.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the use
9、r of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. Specific warningstatements are given in Section 6.2. Referenced Documents2.1 ASTM Standards:2D1067 Test Methods for Acidity or Alkalinity of WaterD1193 Sp
10、ecification for Reagent WaterD1976 Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission SpectroscopyD5673 Test Method for Elements in Water by InductivelyCoupled PlasmaMass SpectrometryD5744 Test Method for Laboratory Weathering of SolidMaterials Using a Humidity Cel
11、lD6234 Test Method for Shake Extraction of Mining Wasteby the Synthetic Precipitation Leaching ProcedureE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals,
12、 Ores, andRelated MaterialsE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE1019 Test Methods for Determination of Carbon, Sulfur,Nitrogen, and Oxygen in Steel, Iron, Nickel, a
13、nd CobaltAlloys by Various Combustion and Fusion TechniquesE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE1950 Practice for Reporting Results from Methods ofChemical AnalysisE2242 Test Method for Column Percolation Extraction ofMine Rock by
14、the Meteoric Water Mobility Procedure3. Terminology3.1 DefinitionsFor definitions of terms used in these testmethods, refer to Terminology E135.1These test methods are under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and are the directrespon
15、sibility of Subcommittee E01.02 on Ores, Concentrates, and Related Metal-lurgical Materials.Current edition approved Nov. 1, 2011. Published December 2011. Originallyapproved in 1997. Last previous edition approved in 2009 as E1915 09. DOI:10.1520/E1915-11.2For referenced ASTM standards, visit the A
16、STM 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 International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, Uni
17、ted States.3.2 Definitions of Terms Specific to This Standard:3.2.1 standardization, vanalysis of samples with knownvalues or known additions, prior to and within groups of testsamples to assure accuracy.3.2.2 standardization sample, ncalibration mixtures orsamples with known values or known additio
18、ns that areanalyzed with test samples to assure accuracy of analysis.4. Significance and Use4.1 These test methods are primarily intended to test mate-rials for compliance with compositional specifications and formonitoring. The determination of carbon and sulfur and acidneutralization potential in
19、ores and related materials is neces-sary to classify ores for metallurgical processing and to classifywaste materials from the mining and processing of ores such asleach residues, waste rock, and tailings according to theirpotential to generate acid in the environment. This informationis useful duri
20、ng mine development to assist in mining andmineral processing operations and for proper disposal of wastematerials. These test methods are also used to speciate carbonand sulfur contents of metal-bearing ores and related materialsso that acid-base accounting can be performed (that is, carbon-ate min
21、eral acid neutralization potential (ANP) minus sulfide-sulfur mineral acid generation potential (AGP) = net calciumcarbonate (NCC). Additionally, the test method has utility toidentify the amount of organic carbon contained in gold ores sothat potential for preg robbing can be identified and rectifi
22、edthrough established pretreatment methods prior to cyanidation.(WarningPyrolysis pretreatment at 550 C has a potential tothermally decompose some carbonate minerals: (1) transitionmetal carbonates (for example, siderite, FeCO3, and rhod-ochrosite, MnCO3) decompose, yielding carbon dioxide, CO2,in t
23、he range of 220 C to 520 C; (2) calcite decomposesslightly between 300 C and 500 C, although most decompo-sition occurs above 550 C; (3) dolomite decomposes at800 C to 900 C (Hammack, 1994, p. 440).3)4.2 These test methods also may be used for the classifica-tion of rock to be used in construction,
24、where the potential togenerate acid under environmental conditions exists.4.3 It is assumed that the users of these test methods will betrained analysts capable of performing common laboratoryprocedures skillfully and safely. It is expected that work will beperformed in a properly equipped laborator
25、y and that properwaste disposal procedures will be followed. Appropriate qual-ity control practices such as those described in Guide E882must be followed.5. Reagents and Materials5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thata
26、ll reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.4Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the a
27、ccuracy ofthe determination.5.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedin Type I of Specification D1193.6. Hazards6.1 For hazards to be observed in the use of reagents andapparatus in these test methods, refer to Practices E5
28、0. Usecare when handling hot crucibles or boats and when operatingfurnaces to avoid personal injury by either burn or electricalshock.7. Rounding Calculated Values7.1 Calculated values shall be rounded to the desired num-ber of places as directed in the Rounding Method of PracticeE29.8. Interlaborat
29、ory Studies8.1 These test methods have been evaluated in accordancewith Practice E1601 unless otherwise noted in the precisionand bias section. The lower limit in the scope of these testmethods specifies the lowest analyte content that may beanalyzed with an acceptable error. A warning statement isi
30、ncluded in the scope for test methods not observing thisconvention.8.2 Site-Specific Quantitative RangesAn interlaboratorystudy may be conducted in accordance with Practice E1601 toestablish quantitative ranges for the partial decomposition testmethods selected for a particular site. Test samples sh
31、all beselected for each alteration or lithologic unit, or both, contain-ing high and low concentrations of carbon and sulfur minerals.Each test sample must be analyzed in rapid succession for totalcarbon and sulfur followed by the different partial decompo-sition treatments selected in order to mini
32、mize the between-method variation.9. Sampling and Sample Preparation9.1 Materials SafetySamples must be prepared, stored,and disposed of in accordance with the materials and safetyguidelines in Practices E50.9.2 Prepared SampleDry a representative portion of thegross sample at 80 C to constant weigh
33、t in order to minimizesulfide mineral oxidation. Pulverize or grind the laboratorysample until 100 % passes a No. 100 (150-m) sieve.NOTE 2Results from the interlaboratory study suggest that it may benecessary to grind samples to pass a No. 200 (75-m) sieve in order toimprove precision for samples co
34、ntaining low concentrations of carbon orsulfur.3Hammack, R. W., “Evolved-Gas Analysis: A Method for Determining Pyrite,Marcasite, and Alkaline-Earth Carbonates,” Environmental Geochemistry of Sul-fide Oxidation, Alpers, C., and Blowes, D., eds., Chapter 28, ACS SymposiumSeries 550, American Chemical
35、 Society, Washington, D.C., 1994, pp. 431444.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC, www.chemistry.org. For suggestions on thetesting of reagents not listed by the American Chemical Society, see the UnitedStates Pharmacopeia and Nationa
36、l Formulary, U.S. Pharmacopeial Convention,Inc. (USPC), Rockville, MD, http:/www.usp.org.E1915 1129.3 Diluted SampleIf the concentration of sulfur in thetest material exceeds 1.75 % for the minimum range instru-ment, prepare a diluted sample as in 9.3.1.9.3.1 Weigh 10.0 g 6 0.1 g prepared sample and
37、 combinewith 40.0 g 6 0.1 g dry silica (SiO2). Grind the mixture in aring and puck mill, or equivalent, until 100 % will pass througha No. 100 (150-m) sieve; mix, and store in a 250-mL glassbottle.10. ProceduresTOTAL CARBON AND SULFUR10.1 ScopeThis test method covers the determination oftotal carbon
38、 in the concentration range between 0.1 % and10 % and total sulfur concentrations in the range between0.1 % and 8.8 %.10.2 Summary of Test Method:10.2.1 The carbon in the test sample is converted to CO2and the sulfur to sulfur dioxide by combustion in a stream ofoxygen.10.2.2 The amount of CO2and su
39、lfur dioxide are measuredby infrared absorption.10.3 Apparatus:10.3.1 Combustion-Infrared Spectrophotometer, equippedwith a combustion chamber, oxygen carrier stream, and infra-red absorption detector, suitable for analysis of sulfur in aminimum range instrument from 0.1 % to 1.75 % or in amaximum r
40、ange instrument from 0.1 % to 8.8 % and carbon inthe range of 0.1 % to 10 %, using 0.2-g test portions of oresand related materials. Instruments, such as those shown in TestMethods E1019 and in the sections Apparatus for Determina-tion of Total Carbon by Direct Combustion and Apparatus forthe Determ
41、ination of Sulfur by Direct Combustion of PracticesE50, that can be shown to give equivalent results may also beused for these test methods.10.4 Reagents and Materials:10.4.1 Reagents:10.4.1.1 Barium Sulfate (BaSO4), Anhydrous, contains13.74 % sulfur (purity 99.9 % minimum). Dry 100 g at 120 Cfor 2
42、h and store in a 250-mL glass bottle.10.4.1.2 Blank Reference SamplePrepare a blank refer-ence sample by pulverizing or grinding 100 g of SiO2(see10.4.1.6), to pass through a No. 100 (150-m) sieve, mix, andstore in a 250-mL glass bottle. This blank contains 0.00 %carbon and 0.00 % sulfur.10.4.1.3 Ca
43、lcium Carbonate (CaCO3), Anhydrous, con-tains 12.00 % carbon (purity 99.9 % minimum). Dry 100 g for2 h at 120 C and store in a 250-mL glass bottle.10.4.1.4 Calibration Mixture A(1 g = 20 mg C and20 mg S)Combine 16.67 g CaCO3, 14.56 g BaSO4, and68.77 g SiO2in a ring and puck grinding mill or equivale
44、ntdevice. Grind until 100 % passes through a No. 100 (150-m)sieve, pass the mixture through the screen to break up anylumps, mix, and store in a glass bottle. This mixture contains2.00 % carbon and 2.00 % sulfur.(1) Alternatively, grind the reagents separately, mix, andpass through the screen prior
45、to final mixing.10.4.1.5 Calibration MixturesTransfer 4.00 g, 10.00 g,20.00 g, and 30.00 g of Calibration Mixture A to ring and puckgrinding mills or equivalent devices. Add the amount of driedSiO2needed to bring the total weight to 40.0 g in each mill,grind to 100 % passing a No. 100 (150-m) sieve,
46、 pass themixture through the screen, mix, and store in 250-mL glassbottles. These mixtures contain: 0.2 %, 0.5 %, 1.0 %, and1.5 % for both carbon and sulfur.(1) Alternatively, grind the reagents separately, mix, andpass through the screen prior to final mixing.(2) Commercially-produced calibration m
47、ixtures, whichmeet these specifications, may also be used.10.4.1.6 Silica (SiO2) (purity 99.9 % minimum), Ottawasand, washed and ignited, containing less than 0.01 % carbonand 0.01 % sulfur. Dry at 120 C for 2 h and store in a 250-mLglass bottle.10.4.1.7 Tungstic Acid (H2WO4) (purity 99 % minimum).1
48、0.4.1.8 Vanadium Pentoxide (V2O5) (purity 99 % mini-mum).10.4.2 Materials:10.4.2.1 Crucibles or boats, suitable for combustion analy-ses.10.5 Calibration and Standardization:10.5.1 ApparatusOperate and calibrate the instrument inaccordance with the manufacturers instructions. Resistancefurnace instr
49、uments require the use of V2O5or H2WO4for thedetermination of sulfur in this test method. Use a 0.200 g 60.1 g weight for all calibration mixtures, reference materials,blank reference materials, test samples, and diluted testsamples in this test method.10.5.1.1 Certain instruments may require different sampleweights for certain concentration ranges, which is permissibleas long as the precision and bias requirements of these testmethods are fulfilled.10.5.2 Ignite the crucibles or boats for test samples andstandard samples in a muffle furnace
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