ASTM D4239-17 Standard Test Method for Sulfur in the Analysis Sample of Coal and Coke Using High-Temperature Tube Furnace Combustion.pdf
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1、Designation: D4239 17Standard Test Method forSulfur in the Analysis Sample of Coal and Coke Using High-Temperature Tube Furnace Combustion1This standard is issued under the fixed designation D4239; the number immediately following the designation indicates the year oforiginal adoption or, in the cas
2、e 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.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope*1.1 This
3、 test method covers the determination of sulfur insamples of coal or coke by high-temperature tube furnacecombustion.1.1.1 Two analysis methods are described.1.2 When automated equipment is used, either method canbe classified as an instrumental method.1.3 The values stated in SI units are to be reg
4、arded asstandard. No other units of measurement are included in thisstandard.1.4 All percentages are percent mass fractions unless other-wise noted.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this st
5、andard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles f
6、or theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD2013 Practice for
7、 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-Determined to Different BasesD7448 Practice for Establishing the Competence of La
8、bora-tories Using ASTM Procedures in the Sampling andAnalysis of Coal and CokeD7582 Test Methods for Proximate Analysis of Coal andCoke by Macro Thermogravimetric AnalysisE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 ISO Standard:3ISO 11722 Solid
9、 Mineral Fuels-Hard Coal Determinationof Moisture in the general analysis test sample by dryingin nitrogen3. Summary of Test Method3.1 Combustion Method A (1350C)A weighed test por-tion of sample is burned in a tube furnace at a minimumcombustion tube operating temperature of 1350C in a streamof oxy
10、gen. During combustion at temperatures above 1350 C,the sulfur and sulfur compounds contained in the sample aredecomposed and oxidized almost exclusively to gaseous sulfurdioxide, SO2. Moisture and particulates are removed from thegas by filters. The gas stream is passed through a cell in whichsulfu
11、r dioxide is measured by an infrared (IR) absorptiondetector. Sulfur dioxide absorbs IR energy at a precise wave-length within the IR spectrum. Energy is absorbed as the gaspasses through the cell body in which the IR energy is beingtransmitted: thus, at the detector, less energy is received. Alloth
12、er IR energy is eliminated from reaching the detector by aprecise wavelength filter. Thus, the absorption of IR energy canbe attributed only to sulfur dioxide whose concentration isproportional to the change in energy at the detector. One cell isused as both a reference and a measurement chamber. To
13、talsulfur as sulfur dioxide is detected on a continuous basis.3.1.1 One procedure for Method A uses coal or cokereference materials to calibrate the sulfur analyzer. A second1This test method is under the jurisdiction of ASTM Committee D05 on Coaland Coke and is the direct responsibility of Subcommi
14、ttee D05.21 on Methods ofAnalysis.Current edition approved May 15, 2017. Published May 2017. Originallyapproved in 1983. Last previous edition approved in 2013 as D4239 142. DOI:10.1520/D4239-17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at
15、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), 1, ch. dela Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http:/www.iso.ch.*A S
16、ummary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization establis
17、hed in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1procedure for Method A uses a pure substance, BBOT, tocalibrate the sulfur analyzer.3.2 Combustion Method B
18、(1150C)A weighed test por-tion of sample is burned in a quartz combustion tube in astream of oxygen with an equal or excess weight of tungstentrioxide (WO3). Sulfur is oxidized during the reaction of thesample and WO3. The tube furnace is operated at a minimumcombustion tube operating temperature of
19、 1150C and tin (Sn)sample boats are utilized. Moisture and particulates are re-moved from the combustion gas by filters. The gas stream isthen passed through a cell in which sulfur dioxide is measuredby an infrared (IR) absorption detector. Sulfur dioxide absorbsIR energy at a precise wavelength wit
20、hin the IR spectrum.Energy is absorbed as the gas passes through the cell body inwhich the IR energy is being transmitted: thus, at the detector,less energy is received. All other IR energy is eliminated fromreaching the detector by a precise wavelength filter. Thus, theabsorption of IR energy can b
21、e attributed only to sulfur dioxidewhose concentration is proportional to the change in energy atthe detector. One cell is used as both a reference and ameasurement chamber. Total sulfur as sulfur dioxide is de-tected on a continuous basis.4. Significance and Use4.1 Sulfur is part of the ultimate an
22、alysis of coal and coke.4.2 Results of the sulfur analysis are used for evaluation ofcoal preparation and cleaning, evaluation of potential sulfuremissions from coal and coke combustion or conversionprocesses, and evaluation of coal and coke quality in relation tocontract specifications, as well as
23、for scientific purposes.4.3 The competency of laboratories with respect to use ofthis standard can be established through reference to PracticeD7448.5. Sample5.1 Pulverize the sample to pass No. 60 (250-m) sieve andmix thoroughly in accordance with Practice D2013 or PracticeD346.5.2 Analyze a separa
24、te portion of the analysis sample formoisture content in accordance with Test Method D3173,orD7582 or ISO 11722 for calculations to other than theas-determined basis.5.3 Procedures for calculating as-determined sulfur valuesobtained from the analysis sample to other bases are describedin Practices D
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