1、Designation: D 5373 08Standard Test Methods forInstrumental Determination of Carbon, Hydrogen, andNitrogen in Laboratory Samples of Coal1This standard is issued under the fixed designation D 5373; the number immediately following the designation indicates the year oforiginal adoption or, in the case
2、 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 instrumental the determina-tion of carbon in the range of 54.9
3、% m/m to 84.7 % m/m,hydrogen in the range of 3.25 % m/m to 5.10 % m/m, andnitrogen in the range of 0.57 % m/m to 1.80 % m/m in theanalysis sample (7.1) of coal.NOTE 1The coals included in the interlaboratory study employed toderive the precision statement for this standard cover ASTM rank ligniteA t
4、o low volatile bituminous. Additional information concerning thecomposition of these coals appears in Annex A5.1.2 The values stated in SI units shall be regarded as thestandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is therespons
5、ibility 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.2. Referenced Documents2.1 ASTM Standards:2D 2013 Practice for Preparing Coal Samples for AnalysisD 3173 Test Method for Moisture in theA
6、nalysis Sample ofCoal and CokeD 3176 Practice for Ultimate Analysis of Coal and CokeD 3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different BasesD 5142 Test Methods for Proximate Analysis of the Analy-sis Sample of Coal and Coke by Instrumental ProceduresD 5865 Test Met
7、hod for Gross Calorific Value of Coal andCoke2.2 ISO Standard:ISO 5725-6 Accuracy (Trueness and Precision) of Measure-ment Methods and Results Part 6: Use in Practice ofAccuracy Values33. Summary of Test Methods3.1 Carbon, hydrogen and nitrogen are determined concur-rently in a single instrumental p
8、rocedure. The quantitativeconversion of the carbon, hydrogen and nitrogen into theircorresponding gases (CO2,H2O, and NOx) occurs duringcombustion of the sample at an elevated temperature in anatmosphere of oxygen. Combustion products which can inter-fere with the subsequent gas analysis are removed
9、. Oxides ofnitrogen (NOx) are reduced to N2before detection. The carbondioxide, water vapour and elemental nitrogen in the gas streamare determined by appropriate instrumental detection proce-dures.4. Significance and Use4.1 Carbon and hydrogen values can be used to determinethe amount of oxygen (ai
10、r) required in combustion processesand for calculation of the efficiency of combustion processes.4.2 Carbon and hydrogen determinations can be used incalculations including material balance, reactivity and yields ofproducts relevant to coal conversion processes such as gasifi-cation and liquefaction
11、.4.3 Carbon and nitrogen values can be used in materialbalance calculations employed for emission accounting pur-poses.NOTE 2The bulk composition of coal changes at a rate that variesfrom coal to coal during storage. As a result using coal for calibration canyield incorrect estimates of carbon, and
12、hydrogen content in particular.5. Apparatus5.1 Analytical InstrumentAn instrument capable of ana-lyzing a test portion of 6 mg or greater. It includes a furnacecapable of maintaining a temperature in the range to ensurequantitative recovery of carbon, hydrogen and nitrogen as theircorresponding gase
13、s (CO2,H2O, and NOx). The combustiongases or a representative aliquot shall be treated to remove,1These test methods are under the jurisdiction ofASTM Committee D05 on Coaland Coke and are the direct responsibility of Subcommittee D05.21 on Methods ofAnalysis.Current edition approved Feb. 1, 2008. P
14、ublished February 2008. Originallyapproved in 1993. Last previous edition approved in 2007 as D 5373 02 (2007).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 s
15、tandards Document Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Copyrigh
16、t by ASTM Intl (all rights reserved); Thu Mar 13 03:10:39 EST 2008Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.separate out or convert any components that can interfere withthe measurement of carbon dioxide, water vapour or nitrogen.The det
17、ection system shall include provisions for evaluatingthe response in a manner that correlates accurately with thecarbon dioxide, water vapour and nitrogen present in thetreated combustion gases.5.2 BalanceA stand-alone balance or a balance integratedwith the instrument, with a resolution of at least
18、 0.1 % relativeof the test portion mass.6. Reagents6.1 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 Society,where
19、such specifications are available.4Other 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.6.2 Carrier Gas, as specified for the instrument by themanufacturer.6.3 Oxygen, as specifie
20、d for the instrument by the manufac-turer.6.4 Additional Reagents, of types and qualities as specifiedfor the instrument by the manufacturer.6.5 Calibration MaterialsCalibration materials shall beaccompanied by a certificate of analysis stating the purity ofthe material. If the certificate of analys
21、is does not provideassigned values for carbon, hydrogen or nitrogen use the purityas stated on the certificate to establish carbon, hydrogen andnitrogen from the theoretical values. Store these pure sub-stances in a desiccator under conditions that maintain thecompounds in a dry state.6.6 Reference
22、MaterialsCertified reference material(CRM) coal(s) prepared by a recognized authority to monitorchanges in instrument response that can be affected by con-stituents not present in the calibration materials (Note 3) and toverify the acceptability of nitrogen results. Coal(s) traceable toa certified r
23、eference material (CRM) coal(s) can also be used.Follow instructions on the reference material certificate withrespect to storage of the reference material and use of assignedvalues. Use only those carbon, hydrogen and nitrogen valuesthat have an assigned uncertainty or are traceable to a valuewith
24、an assigned uncertainty.NOTE 3Coal contains mineral constituents as well as acid gas formingconstituents that can affect the performance of chemicals used to ensurethe consistent and uniform conversion and recovery of carbon, hydrogenand nitrogen.NOTE 4The amount of nitrogen in the majority of coal
25、employed forpower production purposes is in the range of 0.5 % m/m to 1.8 % m/m.None of the calibrants yields percent nitrogen values within the rangesexpected for coal. For this reason reference material (RM) coal is used tocheck the acceptability of nitrogen results.7. Preparation of Analysis Samp
26、le7.1 The sample shall be the analysis sample prepared to atop size of less than 250 m (60 mesh). The samples shall beprepared in accordance with Practice D 2013.8. Instrument Preparation8.1 Instrument Set-UpVerify all instrument operating pa-rameters meet the specifications in the instrument operat
27、ingmanual. Verify the condition and quantities of all chemicalscurrently in use are satisfactory for the number of samples to beanalyzed. Prior to any analysis, check for and, if necessarycorrect any leaks in the combustion system, and the carrier gassystem.8.2 Blank AnalysesPerform blank analyses t
28、o establishcarbon, hydrogen and nitrogen levels in the combustion andcarrier gases. The level of carbon, hydrogen or nitrogen inthese gases shall not exceed 1 % relative of the instrumentresponse for the lowest mass of calibration material (8.4) foreach analyte. Re-determine blank analyses whenever
29、the car-rier gas or oxygen supplies are changed or any chemicals arerenewed.8.3 ConditioningSelect a coal conditioning sample in therange of 75 % m/m carbon dry basis. The moisture contentshould be less than 3 % m/m. Carry out four determinations onthe conditioning sample. Discard the first determin
30、ation. If therange of the three retained determinations for either carbon,hydrogen or nitrogen values exceed 1.2r where r is therepeatability of this standard, instrument stability is suspect. Inthis case take corrective action before proceeding with calibra-tion.8.4 CalibrationIf the instrument has
31、 been previouslycalibrated in accordance with Annex A1, determinations canproceed provided the calibration is verified in accordance withAnnex A2. Otherwise calibrate the instrument as described inAnnex A1.9. Procedure9.1 Determination:9.1.1 Carry out a determination of the moisture content ofeach a
32、nalysis sample or each reference material coal, or both,in accordance with Test Method D 3173 or Test MethodsD 5142 within 48 h of the determination of carbon, hydrogenand nitrogen on each analysis sample.9.1.2 Carry out the determination by weighing out a testportion of each analysis sample within
33、a mass range recom-mended by the manufacturer. Conduct determinations onconsecutive test portions of an analysis sample as needed tomeet quality control requirements.4Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testin
34、g of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.TABLE 1 Calibration Materials and Their Theoretic
35、al Contents ofC, H and NName FormulaC%m/mH%m/mN%m/mEDTA C10H16N2O841.1 5.5 9.6Phenylalanine C9H11NO265.4 6.7 8.5Acetanilide C8H9NO 71.1 6.7 10.4BBOT C26H26N2O2S 72.5 6.1 6.5D5373082Copyright by ASTM Intl (all rights reserved); Thu Mar 13 03:10:39 EST 2008Downloaded/printed byGuo Dehua (CNIS) pursuan
36、t to License Agreement. No further reproductions authorized.9.1.3 Verify the calibration upon completion of all testdeterminations and as needed to meet quality control require-ments according to Annex A2.9.1.4 Prior to conducting any test determinations, uponcompletion of all test determinations an
37、d as needed to meetquality control requirements conduct determinations on con-secutive test portions of a reference material (RM) coal (6.6).Verify the acceptability of results for the RM coal in accor-dance with Annex A3.NOTE 5Appendix X2 provides guidance on the selection of the massof a test port
38、ion that will yield for a mass of carbon similar to the midrange mass of the calibration material.10. Calculation10.1 Record the total carbon, hydrogen and nitrogen asanalyzed as a percentage by mass. Report the results on drybasis to the nearest 0.1 % m/m for carbon, 0.01 % m/m forhydrogen and to t
39、he nearest 0.01 % m/m for nitrogen.10.2 Use the following equations for the calculation to drybasis:10.2.1 For the carbon content:Cd5 Cad3100100 Mad(1)10.2.2 For the nitrogen content:Nd5 Nad3100100 Mad(2)10.2.3 For the hydrogen content:Hd5 Had 0.1119 3 Mad! 3100100 Mad(3)where:d = dry basis,ad = as
40、determined (as analyzed) basis,C = content of carbon, % m/m,N = content of nitrogen, % m/m,H = content of hydrogen, % m/m, andMad= moisture content of the sample as analyzed, % m/m.11. Precision and Bias511.1 The precision of this test method for the determinationof carbon, hydrogen, and nitrogen in
41、 coal are shown in Table 2.11.1.1 Repeatability Limit (r)The value below which theabsolute difference between two test results calculated to a drybasis (Practices D 3180 and D 3176) of separate and consecu-tive test determinations, carried out on the same sample, in thesame laboratory, by the same o
42、perator, using the same appa-ratus on samples taken at random from a single quantity ofhomogeneous material, may be expected to occur with aprobability of approximately 95 %.11.1.2 Reproducibility Limit (R)The value below whichthe absolute difference between two test results calculated to adry basis
43、 (Practices D 3180 and D 3176), carried out indifferent laboratories, using samples taken at random from asingle quantity of material that is as homogeneous as possible,may be expected to occur with a probability of approximately95 %.NOTE 6Additional information concerning precision statistics ap-pe
44、ars inAnnexA4 as well as the composition of the coals employed in theinterlaboratory study (RR:D051034) appears in Annex A5.11.2 BiasTwo materials EDTA and phenylalanine distrib-uted from a common source were included in the interlabora-tory study as reference pure substances. Each participatinglabo
45、ratory calibrated their instrument using one or more of thepure substances (6.5) obtained from a different source. Thereference pure substances were analyzed in two phases of thestudy conducted one year apart. Acomparison of the certificateof analysis values and those obtained in the interlaboratory
46、study for the reference pure substances are shown in Table 3.NOTE 7Guidelines for reporting test sample results that do not meetthe repeatability requirements of this standard when all calibrationverification and reference material check sample acceptance requirementsare met are provided in Appendix
47、 X3.12. Calculation to Other Bases12.1 Report results from the carbon, hydrogen, and nitrogendeterminations on any of the several common bases that differsolely with respect to moisture. Procedures for converting theas-determined concentrations to the other bases are specified inPractices D 3176 and
48、 D 3180.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D05-1034.TABLE 2 Concentrations Range and Limits for Repeatability andReproducibility for Carbon, Hydrogen, and Nitrogen in CoalElementConcentration Range,%m/mRepeatability
49、Limit,r %m/mReproducibilityLimit,R %m/mCarbon 54.9 to 84.7 0.45 1.00Hydrogen 3.25 to 5.10 0.10 0.25Nitrogen 0.57 to 1.80 0.05 0.15D5373083Copyright by ASTM Intl (all rights reserved); Thu Mar 13 03:10:39 EST 2008Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.ANNEXES(Mandatory Information)A1. NUMBER OF CALIBRATION POINTSA1.1 To meet the precision requirements of this method 6calibration points are required for a linear fit and 8 calibrationpoints are required for a non linear fit. These requirem
