1、Designation: E 1915 07Standard Test Methods forAnalysis of Metal Bearing Ores and Related Materials byCombustion Infrared-Absorption Spectrometry1This standard is issued under the fixed designation E 1915; the number immediately following the designation indicates the year oforiginal adoption or, in
2、 the case of revision, 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 covers the determination of totalcarbon and sulfur in metal beari
3、ng ores and related materialssuch as tailings and waste 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 ranges:Total Carbon - 0.01 to 5.87 %Total Sulfu
4、r - 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-0to4.42 %Hydrochloric Acid Insoluble Carbon - 0.025 to 0.47 %Hydrochloric Acid Loss Carbon-0to5.78 %Hydrochloric Acid Insoluble Sulfur - 0.012 to 4.20 %.Nitric Ac
5、id 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 decompositiontest methods are dependent on the mineralogy of the samplesbeing tested. The user of these test methods is advise
6、d toconduct an interlaboratory study in accordance with PracticeE 1601 on the test methods selected for use 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 S
7、ulfur, Total 12.1-12.6Carbon and Sulfur, Residual from Pyrolysis 12.7-12.12Carbon and Sulfur, Hydrochloric Acid Insoluble 12.13-12.18Sulfur, Nitric Acid Insoluble 12.19-12.24Sulfur, Sodium Carbonate Insoluble 12.25-12.301.4 The values stated in SI units are to be regarded asstandard.1.5 This standar
8、d 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 warningstatements are
9、 given in Section 7.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 1976 Test Method for Elements in Water by Inductively-Coupled Argon Plasma Atomic Emission SpectroscopyD 5744 Test Method for Accelerated Weathering of SolidMaterials Using a Modified Humidity Cell
10、D 6234 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,
11、 Ores, andRelated MaterialsE 135 Terminology Relating to Analytical Chemistry forMetals, Ores, and Related MaterialsE 882 Guide for Accountability and Quality Control in theChemical Analysis LaboratoryE 1019 Test Methods for Determination of Carbon, Sulfur,Nitrogen, and Oxygen in Steel and in Iron,
12、Nickel, andCobalt AlloysE 1601 Practice for Conducting an Interlaboratory Study toEvaluate the Performance of an Analytical MethodE 1950 Practice for Reporting Results from Methods ofChemical AnalysisE 2242 Test Method for Column Percolation Extraction ofMine Rock by the Meteoric Water Mobility Proc
13、edure3. Terminology3.1 DefinitionsFor definitions of terms used in these testmethods, refer to Terminology E 135.4. Significance and Use4.1 These test methods are primarily intended to test mate-rials for compliance with compositional specifications and for1These test methods are under the jurisdict
14、ion of ASTM Committee E01 onAnalytical Chemistry for Metals, Ores and Related Materials and are 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 1997. Last pre
15、vious edition approved in 2005 as E 1915 05.2For 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 I
16、nternational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.monitoring. The determination of carbon and sulfur in ores andrelated materials is necessary to classify ores for metallurgicalprocessing and to classify waste materials from the mining andprocessing of
17、 ores such as leach spoils, waste rock and tailingsaccording to their potential to generate acid in the environment.This information is useful during mine development to assist inmining and mineral processing operations and proper disposalof waste materials.4.2 These test methods also may be used fo
18、r 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 of performing common laboratoryprocedures skillfully and safely. It is expected t
19、hat 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 E 882must be followed.5. Apparatus5.1 Combustion-Infrared Spectrophotometer, equipped witha combustion chambe
20、r, oxygen carrier stream and infraredabsorption detector, suitable for analysis of sulfur in a mini-mum range instrument from 0.1 to 1.75 % or in a maximumrange instrument from 0.1 to 8.8 % and carbon in the range of0.1 to 10 %, using 0.2-g test portions in ores and relatedmaterials. Instruments, su
21、ch as those shown in Test MethodsE 1019 and in the section entitled Apparatus for Determinationof Total Carbon by Direct Combustion and the section entitledApparatus for the Determination of Sulfur by Direct Combus-tion of Practices E 50, that can be shown to give equivalentresults may also be used
22、for these test methods.6. Reagents and Materials6.1 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 specifi
23、cations are available.3Other grades 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.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent w
24、ater as definedin Type I of Specification D 1193.6.3 Reagents:6.3.1 Barium Sulfate (BaSO4), Anhydrous, contains 13.74 %sulfur (purity: 99.9 % minimum). Dry 100 g at 120 C for 2 hand store in a 250-mL glass bottle.6.3.2 Blank Reference SamplePrepare a blank referencesample by pulverizing or grinding
25、100 g silica (see 6.3.6), passthrough a No. 100 (150-m) sieve, and mixing and storing ina 250-mL glass bottle. This blank contains 0.00 % carbon andsulfur.6.3.3 Calcium Carbonate (CaCO3), Anhydrous, contains12.00 % carbon (purity: 99.9 % minimum). Dry 100 g for 2 hat 120C and store in a 250-mL glass
26、 bottle.6.3.4 Calibration Mixture A(1g=20mgCand20mgS)Combine 16.67 g CaCO3, 14.56 g BaSO4and 68.77 gSiO2in a ring and puck grinding mill or equivalent device.Grind until 100 % passes through a No. 100 (150-m) sieve,pass the mixture through the screen to break up any lumps, mixand store in a glass bo
27、ttle. This mixture contains 2.00 % carbonand sulfur.6.3.4.1 Alternatively, grind the reagents separately, mix, andpass through the screen prior to final mixing.6.3.5 Calibration MixturesTransfer 4.00, 10.00, 20.00and 30.00 g of Calibration MixtureAto ring and puck grindingmills or equivalent devices
28、. Add the amount of dried SiO2needed to bring the total weight to 40.0 g in each mill, grind to100 % passing a No. 100 (150-m) sieve, pass the mixturethrough the screen, mix and store in 250-mL glass bottles.These mixtures contain: 0.2, 0.5, 1.0, and 1.5 % for bothcarbon and sulfur.6.3.5.1 Alternati
29、vely, grind the reagents separately, mix, andpass through the screen prior to final mixing.6.3.5.2 Commerciallyproduced calibration mixtures,which meet these specifications, may also be used.6.3.6 Silica (SiO2), (purity: 99.9 % minimum), Ottawa sand,washed and ignited, containing less than 0.01 % ca
30、rbon andsulfur. Dry at 120C for 2 h and store in a 250-mL glass bottle.6.3.7 Sodium Carbonate Solution (10 %)Transfer 100 gof sodium carbonate (purity: 99.0 % minimum) to 500-mL ofwater in a 1-L volumetric flask. Dilute to the mark and mix.6.4 Materials:6.4.1 Glass FiltersFine-porosity glass micro f
31、ilters, car-bon content must be less than 0.15 %, sulfur content must beless than 0.05 % and the filter weight must be less than 0.2 g.6.4.1.1 Filtering crucibles may also be used if they areshown to provide equivalent results.7. Hazards7.1 For hazards to be observed in the use of reagents andappara
32、tus in these test methods, refer to Practices E 50. Usecare when handling hot crucibles or boats and when operatingfurnaces to avoid personal injury by either burn or electricalshock.8. Rounding Calculated Values8.1 Calculated values shall be rounded to the desired num-ber of places as directed in t
33、he Rounding Method of PracticeE 29.9. Interlaboratory Studies9.1 These test methods have been evaluated in accordancewith Practice E 1601 unless otherwise noted in the precisionand bias section. The lower limit in the scope of these testmethods specifies the lowest analyte content that may beanalyze
34、d with an acceptable error. A warning statement isincluded in the scope for test methods not observing thisconvention.9.2 Site-Specific Quantitative RangesAn interlaboratorystudy may be conducted in accordance with Practice E 1601 to3Reagent Chemicals, American Chemical Society Specifications , Amer
35、icanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society and the United States Pharmacopeia andNational Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.E1915072establish quantitative ranges for the partial decomp
36、osition testmethods selected for a particular site. Test samples shall 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 di
37、fferent partial decompo-sition treatments selected in order to minimize the between-method variation.10. Sampling and Sample Preparation10.1 Materials SafetySamples must be prepared, storedand disposed of in accordance with the materials and safetyguidelines in Practices E 50.10.2 Prepared SampleDry
38、 a representative portion of thegross sample at 80 C to constant weight. Pulverize or grind thelaboratory sample 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 p
39、recision for samples containing low concentrations of carbon orsulfur.10.3 Diluted SampleIf the concentration of sulfur in thetest material exceeds 1.75 % for the minimum range instru-ment, prepare a diluted sample as in 10.3.1.10.3.1 Weigh 10.0 6 0.1 g prepared sample and combinewith 40.0 6 0.1 g d
40、ry SiO2. Grind the mixture in a ring andpuck mill, or equivalent, until 100 % will pass through a No.100 (150-m) sieve; mix, and store in a 250-mL glass bottle.11. Calibration and Standardization11.1 ApparatusOperate and calibrate the instrument inaccordance with the manufacturers instructions. Resi
41、stancefurnace instruments require the use of vanadium pentoxide ortungstenic acid for the determination of sulfur in these testmethods. Use a 0.200 6 0.1 g weight for all calibrationmixtures, reference materials, blank reference materials, testsamples and diluted test samples in these test methods.1
42、1.1.1 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.11.2 Ignite the crucibles or boats for test samples andstandard samples in a muffle furnace for1hat550
43、6 10 C.11.3 Laboratory Test Method PerformanceDemonstrationA demonstration of laboratory test methodperformance must be performed before this test method may beused in a laboratory for the first time. This demonstration isparticularly important if the laboratory needs to modify the testmethod in any
44、 way. The demonstration must be repeatedwhenever the test method is significantly modified.11.3.1 Linearity VerificationMeasure total carbon andsulfur for the blank reference sample, calibration mixtures,barium sulfate and calcium carbonate in increasing order usingthe same weight of calibration mix
45、tures selected for testsamples, in accordance with the manufacturers instructions.Record the calibration mixture weights used and the carbonand sulfur results measured by the instrument. Check forlinearity by linear regression or by a graphical method to meeta deviation less than 10 % relative for e
46、ach of the calibrationmaterial results at or above a concentration of 0.2 % carbonand sulfur and a correlation coefficient of at least 0.99. Correctany problems with the instrument before proceeding with theanalysis of test samples.11.3.1.1 Linearity may also be verified by the use of bariumsulfate
47、and calcium carbonate weights equivalent to the contentof the calibration mixtures.11.3.2 Blank Sample Precision VerificationAnalyze tenreplicates of the blank reference sample. If the standarddeviation of the replicate analyses exceeds 0.02 % for carbonor 0.01 % for sulfur, correct any instrumental
48、 problems andrepeat the blank sample precision verification before proceed-ing with test method implementation.11.3.3 Low Calibration Mixture Precision VerificationAnalyze four replicates of the 0.2 % calibration mixture. If anyresult for the 0.2 % calibration mixture exceeds the limitsshown in Tabl
49、e 1, correct any instrumental problems and repeatthe low calibration mixture precision verification before pro-ceeding with test method implementation.11.4 Method Quality Control:11.4.1 Calibration VerificationAnalyze a calibration mix-ture with a concentration greater than or equal to 0.5 % carbonand sulfur prior to and within each group of fifty test samples.If the calibration mixture result exceeds the limits in Table 1,correct any instrumental problems and repeat the linearityverification before proceeding with analysis of test samples,and discar
