1、Designation: E1915 13Standard 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 %Acid Neutralization Potential Acidity Titration Low Range -1.0 % to 2 % CaCO3Nitric Acid Insoluble Sulfur 0.006 % to 0.924 %Nitric Acid Loss Sulfur -0.08 % to 4.19 %Sodium Carbonate Insoluble
6、Sulfur 0.007 % to 3.78 %1.2 The quantitative ranges for the partial decompositiontest 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
7、 at a particularmining site, in order to establish the quantitative ranges forthese 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
8、 Acid Insoluble 10.19-10.27Acid Neutralization Potential Acidity Titration 10.28-10.36Acid Neutralization Potential Acidity Titration Low Range 10.37-10.46Sulfur, Nitric Acid Insoluble 10.47-10.55Sulfur, Sodium Carbonate Insoluble 10.56-10.641.4 The values stated in SI units are to be regarded assta
9、ndard.1.5 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 determine the applica-bility of regulatory limitations prior to use. Specific
10、 warningstatements are given in Section 6.2. Referenced Documents2.1 ASTM Standards:2D1067 Test Methods for Acidity or Alkalinity of WaterD1193 Specification for Reagent WaterD1976 Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission SpectroscopyD5673 Test Method for
11、 Elements in Water by InductivelyCoupled PlasmaMass SpectrometryD5744 Test Method for Laboratory Weathering of SolidMaterials Using a Humidity CellD6234 Test Method for Shake Extraction of Mining Wasteby the Synthetic Precipitation Leaching ProcedureE29 Practice for Using Significant Digits in Test
12、Data toDetermine Conformance with SpecificationsE50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated MaterialsE135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE882 Guide for Accountability and Quali
13、ty Control in theChemical Analysis LaboratoryE1019 Test Methods for Determination of Carbon, Sulfur,Nitrogen, and Oxygen in Steel, Iron, Nickel, and CobaltAlloys by Various Combustion and Fusion TechniquesE1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analyti
14、cal MethodE1950 Practice for Reporting Results from Methods ofChemical Analysis1These test methods are under the jurisdiction of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores, and Related Materials and are the directresponsibility of Subcommittee E01.02 on Ores, Concentrates, and Relate
15、d Metal-lurgical Materials.Current edition approved April 1, 2013. Published September 2013. Originallyapproved in 1997. Last previous edition approved in 2011 as E1915 11. DOI:10.1520/E1915-13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at s
16、erviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E2242 Test Method for Column Percolation Extraction o
17、fMine Rock by the Meteoric Water Mobility Procedure3. Terminology3.1 DefinitionsFor definitions of terms used in these testmethods, refer to Terminology E135.3.2 Definitions of Terms Specific to This Standard:3.2.1 standardization, vanalysis of samples with knownvalues or known additions, prior to a
18、nd within groups of testsamples to assure accuracy.3.2.2 standardization sample, ncalibration mixtures orsamples with known values or known additions that areanalyzed with test samples to assure accuracy of analysis.4. Significance and Use4.1 These test methods are primarily intended to test mate-ri
19、als for compliance with compositional specifications and formonitoring.4.1.1 The determination of carbon and sulfur and acidneutralization potential in ores and related materials is neces-sary to classify ores for metallurgical processing and to classifywaste materials from the mining and processing
20、 of ores such asleach residues, waste rock, and tailings according to theirpotential to generate acid in the environment. This informationis useful during mine development to assist in mining andmineral processing operations and for proper disposal of wastematerials.4.1.1.1 The use of the acid neutr
21、alization potential titrationlow range method is most useful where acidity is present in thesamples and when acid potential by titration is desired in theuncertain content range below 2 % CaCO3.4.1.2 These test methods are also used to isolate mineralsbased on carbon and sulfur contents of metal-bea
22、ring ores andrelated materials so that acid-base accounting can be performed(that is, carbonate mineral acid neutralization potential (ANP)minus sulfide-sulfur mineral acid generation potential (AGP) =net calcium carbonate (NCC).4.1.3 Additionally, the carbon hydrochloric acid insolubletest method h
23、as utility to identify the amount of organic carboncontained in gold ores so that potential for preg robbing can beidentified and rectified through established pretreatment meth-ods prior to cyanidation. WarningPyrolysis pretreatment at550 C has a potential to thermally decompose some carbonateminer
24、als: (1) transition metal carbonates (for example, siderite,FeCO3, and rhodochrosite, MnCO3) decompose, yielding car-bon dioxide, CO2, in the range of 220 C to 520 C; (2) calcitedecomposes slightly between 300 C and 500 C, althoughmost decomposition occurs above 550 C; (3) dolomite decom-poses at 80
25、0 C to 900 C (Hammack, 1994, p. 440).34.2 These test methods also may be used for the classifica-tion of rock to be used in construction, 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 o
26、f performing common laboratoryprocedures skillfully and safely. It is expected that work will beperformed in a properly equipped laboratory and that properwaste disposal procedures will be followed. Appropriate qual-ity control practices such as those described in Guide E882must be followed.5. Reage
27、nts and Materials5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.4Other gr
28、ades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.5.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedin Type I of Spe
29、cification D1193.6. Hazards6.1 For hazards to be observed in the use of reagents andapparatus in these test methods, refer to Practices E50. Usecare when handling hot crucibles or boats and when operatingfurnaces to avoid personal injury by either burn or electricalshock.7. Rounding Calculated Value
30、s7.1 Calculated values shall be rounded to the desired num-ber of places as directed in the Rounding Method of PracticeE29.8. Interlaboratory Studies8.1 These test methods have been evaluated in accordancewith Practice E1601 unless otherwise noted in the precisionand bias section. The lower limit in
31、 the scope of these testmethods specifies the lowest analyte content that may beanalyzed with an acceptable error. A warning statement isincluded in the scope for test methods not observing thisconvention.8.2 Site-Specific Quantitative RangesAn interlaboratorystudy may be conducted in accordance wit
32、h Practice E1601 toestablish quantitative ranges for the partial decomposition testmethods selected for a particular site. Test samples shall beselected for each alteration or lithologic unit, or both, contain-ing high and low contents of carbon and sulfur minerals. Eachtest sample must be analyzed
33、in rapid succession for totalcarbon and sulfur followed by the different partial decompo-sition treatments selected in order to minimize the between-method variation.3Hammack, R. W., “Evolved-Gas Analysis: A Method for Determining Pyrite,Marcasite, and Alkaline-Earth Carbonates,” Environmental Geoch
34、emistry of SulfideOxidation, Alpers, C., and Blowes, D., eds., Chapter 28, ACS Symposium Series550, American Chemical Society, Washington, D.C., 1994, pp. 431444.4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC, www.chemistry.org. For suggestions
35、 on thetesting of reagents not listed by the American Chemical Society, see the UnitedStates Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention,Inc. (USPC), Rockville, MD, http:/www.usp.org.E1915 1329. Sampling and Sample Preparation9.1 Materials SafetySamples must be prepared, store
36、d,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 mass in order to minimizesulfide mineral oxidation. Pulverize or grind the laboratorysample until 100 % passes a No. 100 (15
37、0-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 containing low contents of carbon or sulfur.9.3 Diluted SampleIf the content of sulfur in the testmaterial exceeds 1.75 % f
38、or the minimum range instrument,prepare a diluted sample as in 9.3.1.9.3.1 Weigh 10.0 g 6 0.1 g prepared sample and 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
39、glassbottle.10. ProceduresTOTAL CARBON AND SULFUR10.1 ScopeThis test method covers the determination oftotal carbon in the content range between 0.1 % and 10 % andtotal sulfur contents in the range between 0.1 % and 8.8 %.10.2 Summary of Test Method:10.2.1 The carbon in the test sample is converted
40、to carbondioxide and the sulfur to sulfur dioxide by combustion in astream of oxygen.10.2.2 The amount of carbon dioxide and sulfur dioxide aremeasured by infrared absorption.10.3 Apparatus:10.3.1 Combustion-Infrared Spectrophotometer, equippedwith a combustion chamber, oxygen carrier stream, and in
41、fra-red absorption detector, suitable for analysis of sulfur in aminimum range instrument from 0.1 % to 1.75 % or in amaximum range 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 Test
42、Methods E1019 that can be shown to give equivalent resultsmay also be used 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 h and store in a 250-mL glass bottle.10.4.
43、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 Calcium Carbonate (CaCO3), Anhydrous, contai
44、ns12.00 % carbon (purity 99.9 % minimum). Dry 100 g for 2 h at120 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 equivalentdevice. Grind until 100 % passes through a
45、 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 to final mixing.10.4.1.5 Calibration Mixture
46、sTransfer 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 mass to 40.0 g in each mill, grindto 100 % passing a No. 100 (150-m) sieve, pass the mixturethrough the screen, mix, and
47、store in 250-mL glass bottles.These mixtures contain: 0.2 %, 0.5 %, 1.0 %, and 1.5 % forboth carbon and sulfur.(1) Alternatively, grind the reagents separately, mix, andpass through the screen prior to final mixing.(2) Commercially-produced calibration mixtures, whichmeet these specifications, may a
48、lso 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).10.4.1.8 Vanadium Pentoxide (V2O5) (purity 99 %
49、 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 instruments require the use of V2O5or H2WO4for thedetermination of sulfur in this test method. Use a 0.200 g 60.01 g mass 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 d
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