ASTM D8214-2018 Standard Test Method for Forms of Sulfur in Coal by Inductively Coupled Plasma&x2009 Atomic Emission Spectrometry.pdf
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1、Designation: D8214 18Standard Test Method forForms of Sulfur in Coal by Inductively CoupledPlasma Atomic Emission Spectrometry1This standard is issued under the fixed designation D8214; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisio
2、n, 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 method applies to the determination of sulfatesulfur and pyritic sulfur in coal and calculate
3、s organic sulfur bydifference. This test method is not applicable to coke or othercarbonaceous materials.1.2 The values stated in SI units are to be regarded asstandard. Non-SI units, if provided, are considered informa-tional and are contained within parentheses1.3 This standard does not purport to
4、 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, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.4 This international standard was
5、developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced
6、 Documents2.1 ASTM Standards:2D121 Terminology of Coal and CokeD1193 Specification for Reagent WaterD2013 Practice for Preparing Coal Samples for AnalysisD3173 Test Method for Moisture in the Analysis Sample ofCoal and CokeD3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Di
7、fferent BasesD4239 Test Method for Sulfur in the Analysis Sample ofCoal and Coke Using High-Temperature Tube FurnaceCombustionD7582 Test Methods for Proximate Analysis of Coal andCoke by Macro Thermogravimetric AnalysisE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision o
8、f a Test MethodE832 Specification for Laboratory Filter Papers2.2 ISO Standards:3ISO 5725-6 Accuracy (Trueness and Precision) of Measure-ment Methods and Results Part 6: Use in Practice ofAccuracy Values3. Terminology3.1 For definitions of terms used in this test method, refer toTerminology D121.4.
9、Summary of Test Method4.1 Sulfate Sulfur:4.1.1 Sulfate sulfur is extracted from the analysis samplewith a dilute hydrochloric acid solution. The sulfate sulfur inthe extract is determined by inductively coupled plasma atomicemission spectrometry (ICP-AES). Sulfates are soluble inhydrochloric acid, p
10、yritic sulfur and organic sulfur are notsoluble in hydrochloric acid.4.2 Pyritic Sulfur:4.2.1 Pyritic sulfur is extracted from the pretreated samplewith a dilute nitric acid solution. The pyritic sulfur in theextract is determined by correlating extracted iron content,measured by ICP-AES, as pyritic
11、 sulfur content.4.2.2 Monosulfides (pyrites and FeS2are disulfides) of ironand elements such as cadmium, lead, vanadium, and zinc canbe present in coal. In mass fractions up to 100 gg, thesemonosulfides do not contribute significantly to the total inor-ganic sulfide content.4-61This test method is u
12、nder the jurisdiction of ASTM Committee D05 on Coaland Coke and is the direct responsibility of Subcommittee D05.21 on Methods ofAnalysis.Current edition approved Nov. 1, 2018. Published January 2019. DOI: 10.1520/D8214-18.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orconta
13、ct 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 International Organization for Standardization (ISO), ISOCentral Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 121
14、4 Vernier,Geneva, Switzerland, http:/www.iso.org.4Edwards, A. H., Daybell, G. N., and Pringle, W. J. S., “An Investigation intoMethods for the Determination of Forms of Sulfur in Coal,” Fuel, Vol 37,1958, pp. 47-59.5Burns, M. S., “Determination of Pyritic Sulfur in Australian Coals,” Fuel,Vol49, 197
15、0, pp. 126-133.6Shrimp, N. F., Helfinstine, R. J., and Kuhn, J. K.,“Determination of Forms ofSulfur in Coal,” Symposium on Sulfur and Nitrogen in Coal and Oil Shale, 1975,pp. 99-108.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis
16、international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT
17、) Committee.15. Significance and Use5.1 This test method provides for a separation of coal-associated sulfur into two commonly recognized forms: pyriticand sulfate. Organic sulfur is calculated by difference. Resultsobtained by the test method are used to serve a number ofinterests, including the ev
18、aluation of coal preparation andprocessing operations designed to reduce coal sulfur levels.6. Analysis Sample6.1 The analysis sample is that sample which has beenpulverized to pass a 250 m (No. 60) sieve as prepared inaccordance with Practice D2013.6.2 Determine the moisture in the analysis sample
19、in accor-dance with Test Method D3173 or Test Methods D7582 topermit calculation to other bases.7. Apparatus7.1 Balance, sensitive to 0.1 mg.7.2 Hot Plate, electric or gas-heated with capability fortemperature control.7.3 Inductively Coupled Plasma Atomic Emission Spectrom-eter (ICP-AES)Either a seq
20、uential or simultaneous spectrom-eter is suitable. Because of differences between various makesand models of satisfactory instruments, no detailed operatinginstructions can be provided. Instead, the analyst should followthe instructions provided by the manufacturer of the particularinstrument. Sensi
21、tivity, instrumental detection limits, precision,linear dynamic range, and interference effects shall be inves-tigated and established for each analyte on that particularinstrument. All measurements shall be within the instrumentslinear range in which correction factors are valid. It is theresponsib
22、ility of the analyst to verify that the instrumentconfiguration and operating conditions used satisfy the analyti-cal requirements of this test method. The analyst shall maintainquality control data confirming the instrument performance andanalytical results.8. Reagents and Materials8.1 Purity of Re
23、agentsReagent 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 such specifications are available.7Other grades may beused, provide
24、d that the reagent is of sufficiently high purity topermit its use without lessening the accuracy of the determi-nation.8.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Specification D1193, Type II.8.3 Ethanol, reagent grade, de
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