ASTM D5373-2013 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

1、Designation: D5373 08D5373 13Standard Test Methods forInstrumental Determination of Carbon, Hydrogen,Hydrogenand Nitrogen in LaboratoryAnalysis Samples of Coal andCarbon in Analysis Samples of Coal and Coke1This standard is issued under the fixed designation D5373; the number immediately following t

2、he designation indicates the year oforiginal 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 This test methodTest Me

3、thod A covers the instrumental the determination of carbon in the range of 54.9 % m/m to 84.7 %m/m, 84.7 %, hydrogen in the range of 3.25 % m/m to 5.10 % m/m, 5.10 %, and nitrogen in the range of 0.57 % m/m to 1.80 %m/m in the analysis samplesamples (7.1) of coal.1.1.1 Test Method B covers the deter

4、mination of carbon in analysis samples of coal in the range of 58.0 % to 84.2 %, and carbonin analysis samples of coke in the range of 86.3 % to 95.2 %.NOTE 1The coals included in the interlaboratory study employed to derive the precision statement for this standard cover ASTM rank lignite A tolow v

5、olatile bituminous. Additional information concerning the composition of these coals appears in Annex A5. The cokes used in the interlaboratorystudy employed to derive the precision statement for coke included an equal number of met cokes and pet cokes.1.2 The values stated in SI units shall are to

6、be regarded as the standard. No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices

7、 and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D346/D346M Practice for Collection and Preparation of Coke Samples for Laboratory AnalysisD2013 Practice for Preparing Coal Samples for AnalysisD3173 Test Method for Moisture in the Anal

8、ysis Sample of Coal and CokeD3176 Practice for Ultimate Analysis of Coal and CokeD3180 Practice for Calculating Coal and Coke Analyses from As-Determined to Different BasesD5142D5865 Test Methods for Proximate Analysis of the Analysis Sample of Method for Gross Calorific Value of Coal andCoke by Ins

9、trumental Procedures (Withdrawn 2010)D5865D7582 Test Method for Gross Calorific Value Methods for Proximate Analysis of Coal and Coke by MacroThermogravimetric Analysis2.2 ISO Standard:ISO 5725-6 Accuracy (Trueness and Precision) of Measurement Methods and Results Part 6: Use in Practice of Accuracy

10、Values33. Summary of Test Methods3.1 Carbon, In MethodA, carbon, hydrogen and nitrogen in coal are determined concurrently in a single instrumental procedure.procedure using a furnace operating at temperatures in the range of 900 C to 1050C. The quantitative conversion of the carbon,hydrogen and nit

11、rogen into their corresponding gases (CO2, H2O, and NOx) occurs during combustion of the sample at an elevatedtemperature in an atmosphere of oxygen. Combustion products which can interfere with the subsequent gas analysis are removed.1 These test methods are under the jurisdiction of ASTM Committee

12、 D05 on Coal and Coke and are the direct responsibility of Subcommittee D05.21 on Methods ofAnalysis.Current edition approved Feb. 1, 2008Oct. 15, 2013. Published February 2008 November 2013. Originally approved in 1993. Last previous edition approved in 20072008as D5373 02 (2007).D5373 08. DOI: 10.

13、1520/D5373-08.10.1520/D5373-13.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from American Nati

14、onal Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically

15、 possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C70

16、0, West Conshohocken, PA 19428-2959. United States1Oxides of nitrogen (NOx) are reduced to N2 before detection. The carbon dioxide, water vapourvapor and elemental nitrogen inthe gas stream are determined by appropriate instrumental detection procedures.3.2 In Method B, carbon in coal and coke is de

17、termined by combusting the sample in a 1350C furnace. The H2O in thecombustion gases is removed and CO2 is determined by infrared absorption.4. Significance and Use4.1 Carbon and hydrogen values can be used to determine the amount of oxygen (air) required in combustion processes and forcalculation o

18、f the efficiency of combustion processes.4.2 Carbon and hydrogen determinations can be used in calculations including material balance, reactivity and yields ofproducts relevant to coal conversion processes such as gasification and liquefaction.4.3 Carbon and nitrogen values can be used in material

19、balance calculations employed for emission accounting purposes.NOTE 2The bulk composition of coal changes at a rate that varies from coal to coal during storage. As a result using coal for calibration can yieldincorrect estimates of carbon, and hydrogen content in particular.5. Apparatus5.1 Analytic

20、al InstrumentInstrument for CHN Analysis (Method A)An instrument capable of analyzing a test portion of 6mg or greater. It includes a furnace capable of maintaining a temperature (900C to 1050C) in the range to ensure quantitativerecovery of carbon, hydrogen and nitrogen in coal as their correspondi

21、ng gases (CO2, H2O, and NOx). The combustion gases ora representative aliquot shall be treated to remove, separate out or convert any components that can interfere with the measurementof carbon dioxide, water vapour or nitrogen. The detection system shall include provisions for evaluating the respon

22、se in a mannerthat correlates accurately with the carbon dioxide, water vapour and nitrogen present in the treated combustion gases.5.2 Analytical Instrumentation for Carbon in Coal and Coke Analysis (Method B)An instrument with a furnace capable ofmaintaining a temperature of at least 1350C at all

23、times during the analysis. The high temperature helps ensure the quantitativerecovery of carbon from cokes. The infrared absorption detection system shall include provisions for evaluating the response ina manner that correlates accurately with the carbon dioxide present in the dry combustion gases.

24、 Follow the manufacturersrecommendations for sample mass (typically 50 mg to 300 mg).5.3 BalanceA stand-alone balance or a balance integrated with the instrument, with a resolution of at least 0.1 % relative ofthe test portion mass.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall be us

25、ed in all tests. Unless otherwise indicated, it is intended that allreagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, wheresuch specifications are available.4 Other grades may be used, provided it is first ascertained that the reag

26、ent is of sufficiently highpurity to permit its use without lessening the accuracy of the determination.6.2 Carrier Gas, as specified for the instrument by the manufacturer.6.3 Oxygen, as specified for the instrument by the manufacturer.6.4 Additional Reagents, of types and qualities as specified fo

27、r the instrument by the manufacturer.6.5 Calibration MaterialsCalibration materials shall be accompanied by a certificate of analysis stating the purity of thematerial. If the certificate of analysis does not provide assigned values for carbon, hydrogen or nitrogen use the purity as statedon the cer

28、tificate to establish carbon, hydrogen and nitrogen from the theoretical values. Store these pure substances in a desiccatorunder conditions that maintain the compounds in a dry state.4 Reagent Chemicals, American Chemical Society Specifications , American Chemical Society, Washington, DC. For sugge

29、stions on the testing of reagents not listed bythe American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and NationalFormulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville, MD.TABLE 1 Calibration Materia

30、ls and Their Theoretical Contents ofC, H and N Carbon, Hydrogen and Nitrogen (Method A)Name Formula C %m/m H %m/m N %m/mEDTA C10H16N2O8 41.1 5.5 9.6Phenylalanine C9H11NO2 65.4 6.7 8.5Acetanilide C8H9NO 71.1 6.7 10.4BBOT C26H26N2O2S 72.5 6.1 6.5Graphite C 100.0D5373 1326.6 Reference MaterialsCertifie

31、d reference material (CRM) coal(s) prepared by a recognized authority to monitor changes ininstrument response that can be affected by constituents not present in the calibration materials (Note 3) and to verify theacceptability of nitrogen results. Coal(s) traceable to a certified reference materia

32、l (CRM) coal(s) can also be used. Followinstructions on the reference material certificate with respect to storage of the reference material and use of assigned values. Useonly those carbon, hydrogen and nitrogen values that have an assigned uncertainty or are traceable to a value with an assignedun

33、certainty.NOTE 3Coal contains mineral constituents as well as acid gas forming constituents that can affect the performance of chemicals used to ensure theconsistent and uniform conversion and recovery of carbon, hydrogen and nitrogen.NOTE 4The amount of nitrogen in the majority of coal employed for

34、 power production purposes is in the range of 0.5 % m/m to 1.8 % m/m Noneof the calibrants yields percent nitrogen values within the ranges expected for coal. For this reason reference material (RM) coal is used to check theacceptability of nitrogen results.7. Preparation of Analysis Sample7.1 The s

35、ample shall be the analysis sample prepared to a top size of less than 250 m (60 mesh). TheCoal samples shall beprepared in accordance with Practice D2013. Coke samples shall be prepared in accordance with Practice D346/D346M.8. Instrument Preparation8.1 Instrument Set-UpVerify all instrument operat

36、ing parameters meet the specifications in the instrument operating manual.Verify the condition and quantities of all chemicals currently in use are satisfactory for the number of samples to be analyzed. Priorto any analysis, check for and, if necessary correct any leaks in the combustion system, and

37、 the carrier gas system.8.2 Blank AnalysesPerform blank analyses to establish carbon, hydrogen and nitrogen levels in the combustion and carriergases. gases as required by the specific method. The level of carbon, hydrogen or nitrogen in these gases shall not exceed 1 %relative of the instrument res

38、ponse for the lowest mass of calibration material (8.4) for each analyte. Re-determine blank analyseswhenever the carrier gas or oxygen supplies are changed or any chemicals are renewed.8.3 ConditioningSelect a coal conditioning sample in the range of 75 % m/m (or more) carbon dry basis. The It isre

39、commended that the moisture content should be less than 3 % m/m. 3 %. Carry out four determinations on the conditioningsample. Discard the first determination. If the range of the three retained determinations for either carbon, hydrogen or nitrogenvalues exceed 1.2r where r is the repeatability of

40、this standard, instrument stability is suspect. In this case take corrective actionbefore proceeding with calibration.8.4 CalibrationIf the instrument has been previously calibrated in accordance with Annex A1, determinations can proceedprovided the calibration is verified in accordance with Annex A

41、2. Otherwise calibrate the instrument as described in Annex A1.8.4.1 Calibration for Carbon in Coal and Coke at 1350C (Method B)Use pure graphite to calibrate instruments operatingat 1350C that are used for determining carbon in coal and coke analysis samples.9. Procedure9.1 Determination:9.1.1 Carr

42、y out a determination of the moisture content of each analysis sample or each reference material coal, or both, inaccordance with Test Method D3173 or Test Methods D5142D7582 within 48 h of the determination of carbon, hydrogen andnitrogen on each analysis sample.9.1.2 Carry out the determination by

43、 weighing out a test portion of each analysis sample within a mass range recommended bythe manufacturer. Conduct determinations on consecutive test portions of an analysis sample as needed to meet quality controlrequirements.9.1.3 Verify the calibration upon completion of all test determinations and

44、 as needed to meet quality control requirementsaccording to Annex A2.9.1.4 Prior to conducting any test determinations, upon completion of all test determinations and as needed to meet qualitycontrol requirements conduct determinations on consecutive test portions of a reference material (RM) coal (

45、6.6). Verify theacceptability of results for the RM coal in accordance with Annex A3.NOTE 5Appendix X2 provides guidance on the selection of the mass of a test portion that will yield for a mass of carbon similar to the mid rangemass of the calibration material.10. Calculation10.1 Record the total c

46、arbon, hydrogen and nitrogen as analyzed as a percentage by mass. Report the results on dry basis to thenearest 0.1 % m/m for carbon, 0.01 % m/m for hydrogen and to the nearest 0.01 % m/m for nitrogen.10.2 Use the following equations for the calculation to dry basis:10.2.1 For the carbon content:Cd

47、5Cad3 1001002Mad(1)D5373 13310.2.2 For the nitrogen content:Nd 5Nad3 1001002Mad(2)10.2.3 For the hydrogen content:Hd 5Had20.11193Mad!3 1001002Mad(3)where:d = dry basis,ad = as determined (as analyzed) basis,C = content of carbon, % m/m,C = content of carbon, % ,N = content of nitrogen, % m/m,N = con

48、tent of nitrogen, % ,H = content of hydrogen, % m/m, andH = content of hydrogen, % , andMad = moisture content of the sample as analyzed, % m/m.Mad = moisture content of the sample as analyzed, % .11. Precision and Bias511.1 The precision of this test method for data for Test Method A for the determ

49、ination of carbon, hydrogen, and nitrogen incoal are shown in Table 2. The precision data for Test Method B for the determination of carbon in coal and coke are shown inTable 3.11.1.1 Repeatability Limit (r)The value below which the absolute difference between two test results calculated to a dry basis(Practices D3180 and D3176) of separate and consecutive test determinations, carried out on the same sample, in the samelaboratory, by the same operator, using the same apparatus on samples taken at random from a single quantity of homogeneousmateria