ASTM D5373-2016 Standard Test Methods for Determination of Carbon Hydrogen and Nitrogen in Analysis Samples of Coal and Carbon in Analysis Samples of Coal and Coke《测定煤和焦碳分析样品中的煤和碳分.pdf

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1、Designation: D5373 16Standard Test Methods forDetermination of Carbon, Hydrogen and Nitrogen inAnalysis Samples of Coal and Carbon in Analysis Samplesof Coal and Coke1This standard is issued under the fixed designation D5373; the number immediately following the designation indicates the year oforig

2、inal adoption or, in 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 Test MethodAcovers the determination of carbon in therange of 5

3、4.9 % to 84.7 %, hydrogen in the range of 3.25 % to5.10 %, and nitrogen in the range of 0.57 % to 1.80 % in theanalysis samples (8.1) of coal and of carbon in analysissamples of coke in the range of 86.6 % to 97.9 %.1.1.1 Test Method B covers the determination of carbon inanalysis samples of coal in

4、 the range of 58.0 % to 84.2 %, andcarbon in analysis samples of coke in the range of 86.3 % to95.2 %.NOTE 1The coals included in the interlaboratory study employed toderive the precision statement for this standard cover ASTM rank ligniteA to low volatile bituminous. Additional information concerni

5、ng thecomposition of these coals appears in Annex A5. The cokes used in theinterlaboratory study employed to derive the precision statement for cokefor Method A included five each metallurgical (met) cokes and seven eachpetroleum (pet) cokes, and Method B included an equal number (fiveeach) of met c

6、okes and pet cokes.1.2 All percentages are percent mass fractions unless other-wise noted.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, assoc

7、iated 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.2. Referenced Documents2.1 ASTM Standards:2D121 Terminology of Coal and CokeD346/D346M Practice for C

8、ollection and Preparation ofCoke Samples for Laboratory AnalysisD2013 Practice for Preparing Coal Samples for AnalysisD3173 Test Method for Moisture in the Analysis Sample ofCoal and CokeD3176 Practice for Ultimate Analysis of Coal and CokeD3180 Practice for Calculating Coal and Coke Analysesfrom As

9、-Determined to Different BasesD5865 Test Method for Gross Calorific Value of Coal andCokeD7582 Test Methods for Proximate Analysis of Coal andCoke by Macro Thermogravimetric Analysis2.2 ISO Standard:ISO 5725-6 Accuracy (Trueness and Precision) of Measure-ment Methods and Results Part 6: Use in Pract

10、ice ofAccuracy Values33. Terminology3.1 For definitions of terms used in this standard, refer toTerminology D121.4. Summary of Test Methods4.1 In Method A, carbon, hydrogen, and nitrogen in coal orcarbon in coke are determined in a single instrumental proce-dure using a furnace operating at temperat

11、ures in the range of900 C to 1050 C for carbon, hydrogen and nitrogen in coal or950 C to 1150 C for carbon in coke. 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 an

12、atmosphere of oxygen. Combustion products which can inter-fere with the subsequent gas analysis are removed. Oxides ofnitrogen (NOx) are reduced to N2before detection. The carbondioxide, water vapor and elemental nitrogen in the gas streamare determined by appropriate instrumental detection proce-du

13、res.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 Sept. 1, 2016. Published September 2016. Originallyapproved in 1993. Last previous edition approved in 2014

14、as D5373 142. DOI:10.1520/D5373-16.2For 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.3Available from American N

15、ational Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States14.2 In Method B, carbon in coal and coke is determined bycombusting the sample in a 1

16、350 C furnace. The H2Ointhecombustion gases is removed and CO2is determined byinfrared absorption.5. Significance and Use5.1 Carbon and hydrogen values can be used to determinethe amount of oxygen (air) required in combustion processesand for calculation of the efficiency of combustion processes.5.2

17、 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.5.3 Carbon and nitrogen values can be used in materialbalance calculations employed for emission ac

18、counting 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 hydrogen content in particular.6. Apparatus6.1 Analytical Instrument for CHN Analysis in Coal orCarb

19、on in Coke (Method A)An instrument capable of ana-lyzing a test portion of 6 mg or greater. For coal, it includes afurnace capable of maintaining a temperature in the range of900 C to 1050 C to ensure quantitative recovery of carbon,hydrogen, and nitrogen as their corresponding gases (CO2,H2O, and N

20、Ox). For coke, it includes a furnace capable ofmaintaining a temperature in the range of 950 C to 1150 C.The use of combustion promoters, including tin foil or capsule,shall be utilized as required by the apparatus manufacturer forquantitative recovery of carbon in coke as its correspondinggas (CO2)

21、. The combustion gases or a representative aliquotshall be treated to remove, separate out or convert anycomponents that can interfere with the measurement of carbondioxide, water vapor or nitrogen. The detection system shallinclude provisions for evaluating the response in a manner thatcorrelates a

22、ccurately with the carbon dioxide, water vapor andnitrogen present in the treated combustion gases.6.2 Analytical Instrumentation for Carbon in Coal andCoke Analysis (Method B)An instrument with a furnacecapable of maintaining a temperature of at least 1350 C at alltimes during the analysis. The hig

23、h temperature helps ensurethe quantitative recovery of carbon from cokes. The infraredabsorption detection system shall include provisions for evalu-ating the response in a manner that correlates accurately withthe carbon dioxide present in the dry combustion gases. Followthe manufacturers recommend

24、ations for sample mass (typi-cally 50 mg to 300 mg).6.3 BalanceA stand-alone balance or a balance integratedwith the instrument, with a resolution of at least 0.1 % relativeof the test portion mass.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise i

25、ndicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to

26、 permit its use without lessening theaccuracy of the determination.7.2 Carrier Gas, as specified for the instrument by themanufacturer.7.3 Oxygen, as specified for the instrument by the manufac-turer.7.4 Additional Reagents, of types and qualities as specifiedfor the instrument by the manufacturer.7

27、.5 Calibration MaterialsCalibration materials shall beaccompanied by a certificate of analysis stating the purity ofthe material. If the certificate of analysis does not provideassigned values for carbon, hydrogen or nitrogen use the purityas stated on the certificate to establish carbon, hydrogen a

28、ndnitrogen from the theoretical values. Store these pure sub-stances in a desiccator under conditions that maintain thecompounds in a dry state.7.6 Reference MaterialsCertified reference material(CRM) coal(s) prepared by a recognized authority to monitorchanges in instrument response that can be aff

29、ected by con-stituents not present in the calibration materials (Note 3) and toverify the acceptability of nitrogen results. Coal(s) and coke(s)traceable to a certified reference material (CRM) coal(s) andcoke(s) can also be used. Follow instructions on the referencematerial certificate with respect

30、 to storage of the referencematerial and use of assigned values. Use only those carbon,hydrogen and nitrogen values that have an assigned uncertaintyor are traceable to a value with an assigned uncertainty.NOTE 3Coal contains mineral constituents as well as acid gas formingconstituents that can affe

31、ct 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 employed forpower production purposes is in the range of 0.5 % to 1.8 %. None of thecalibrants yields percent nitrogen

32、 values within the ranges expected forcoal. For this reason reference material (RM) coal is used to check theacceptability of nitrogen results.7.7 Tungsten Oxide (WO3)as specified for the instrumentby the manufacturer.7.8 Tin (Sn)as specified for the instrument by the manu-facturer.4Reagent Chemical

33、s, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing 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 F

34、ormulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.TABLE 1 Calibration Materials and Their Theoretical Contents ofCarbon, Hydrogen and Nitrogen (Method A)Name Formula C % H % N %EDTA C10H16N2O841.1 5.5 9.6Phenylalanine C9H11NO265.4 6.7 8.5Acetanilide C8H9NO 71.1 6.7 10.4BBOT C26H26N

35、2O2S 72.5 6.1 6.5Graphite C 100.0D5373 1628. Preparation of Analysis Sample8.1 The sample shall be the analysis sample prepared to atop size of less than 250 m (No. 60). Coal samples shall beprepared in accordance with Practice D2013. Coke samplesshall be prepared in accordance with Practice D346/D3

36、46M.9. Instrument Preparation9.1 Instrument Set-UpVerify all instrument operating pa-rameters meet the specifications in the instrument operatingmanual. Verify the condition and quantities of all chemicalscurrently in use are satisfactory for the number of samples to beanalyzed. Prior to any analysi

37、s, check for and, if necessarycorrect any leaks in the combustion system, and the carrier gassystem.9.2 Blank AnalysesPerform blank analyses to establishcarbon, hydrogen and nitrogen levels in the combustion andcarrier gases as required by the specific method. The level ofcarbon, hydrogen or nitroge

38、n in these gases shall not exceed1 % relative of the instrument response for the lowest mass ofcalibration material (9.4) for each analyte. Re-determine blankanalyses whenever the carrier gas or oxygen supplies arechanged or any chemicals are renewed.9.3 ConditioningSelect a conditioning sample in t

39、he rangeof 75 % (or more) carbon dry basis. It is recommended that themoisture content be less than 3 %. Carry out four determina-tions on the conditioning sample. Discard the first determina-tion. If the range of the three retained determinations for eithercarbon, hydrogen or nitrogen values exceed

40、 1.2r where r is therepeatability of this standard, instrument stability is suspect. Inthis case take corrective action before proceeding with calibra-tion.9.4 CalibrationIf the instrument has been previously cali-brated in accordance with Annex A1, determinations canproceed provided the calibration

41、 is verified in accordance withAnnex A2. Otherwise calibrate the instrument as described inAnnex A1.9.4.1 Calibration for Carbon in Coal and Coke at 1350C(Method B)Use pure graphite to calibrate instruments oper-ating at 1350C that are used for determining carbon in coaland coke analysis samples.10.

42、 Procedure10.1 Determination:10.1.1 Carry out a determination of the moisture content ofeach analysis sample or each reference material, or both, inaccordance with Test Method D3173 or Test Methods D7582within 48 h of the determination of carbon, hydrogen andnitrogen on each analysis sample.10.1.2 C

43、arry out the determination by weighing out a testportion of each analysis sample within a mass range recom-mended by the manufacturer. Conduct determinations onconsecutive test portions of an analysis sample as needed tomeet quality control requirements.10.1.3 Verify the calibration upon completion

44、of all testdeterminations and as needed to meet quality control require-ments according to Annex A2.10.1.4 Prior to conducting any test determinations, uponcompletion of all test determinations and as needed to meetquality control requirements conduct determinations on con-secutive test portions of

45、a reference material (RM) (7.6). Verifythe acceptability of results for the RM in accordance withAnnex A3.NOTE 5Appendix X2 provides guidance on the selection of the massof a test portion that will yield for a mass of carbon similar to the midrange mass of the calibration material.11. Calculation11.

46、1 Record the total carbon, hydrogen and nitrogen asanalyzed as a percentage by mass. Report the results on drybasis to the nearest 0.1 % for carbon, 0.01 % for hydrogen andto the nearest 0.01 % for nitrogen.11.2 Use the following equations for the calculation to drybasis:11.2.1 For the carbon conten

47、t:Cd5 Cad3100100 2 Mad(1)11.2.2 For the nitrogen content:Nd5 Nad3100100 2 Mad(2)11.2.3 For the hydrogen content:Hd5 Had2 0.1119 3 Mad! 3100100 2 Mad(3)where:d = dry basis,ad = as determined (as analyzed) basis,C = content of carbon, %,N = content of nitrogen, %,H = content of hydrogen, %, andMad= mo

48、isture content of the sample as analyzed, %.12. Precision and Bias512.1 The precision data for Test Method A for the determi-nation of carbon, hydrogen, and nitrogen in coal and carbon in5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Rep

49、ort RR:D05-1034, RR:D05-1046, andRR:D05-1048.TABLE 2 Mass Fractions Range and Limits for Repeatability andReproducibility for Carbon, Hydrogen, and Nitrogen in Coal andCarbon in Coke (Method A)ElementMass FractionRange, %RepeatabilityLimitReproducibility LimitCarbon inCoal54.9 to 84.7 0.45 1.00Hydrogenin Coal3.25 to 5.10 0.10 0.25Nitrogen inCoal0.57 to 1.80 0.05 0.15Carbon inCoke86.6 to 97.9 0.85 2.20D5373 163coke are shown in Table 2. The precision data for Test MethodB for the determination of carbon in coal and coke are shownin Table 3.12.1.1