ASTM D4239-2017 Standard Test Method for Sulfur in the Analysis Sample of Coal and Coke Using High-Temperature Tube Furnace Combustion《采用高温管式炉燃烧法测定煤和焦炭分析样品中硫含量的标准试验方法》.pdf
《ASTM D4239-2017 Standard Test Method for Sulfur in the Analysis Sample of Coal and Coke Using High-Temperature Tube Furnace Combustion《采用高温管式炉燃烧法测定煤和焦炭分析样品中硫含量的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM D4239-2017 Standard Test Method for Sulfur in the Analysis Sample of Coal and Coke Using High-Temperature Tube Furnace Combustion《采用高温管式炉燃烧法测定煤和焦炭分析样品中硫含量的标准试验方法》.pdf(8页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D4239 142D4239 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, i
2、n 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.This standard has been approved for use by agencies of the U.S. Department of Defense.1 NOTESu
3、mmary of Changes added and Tables 3 and A1.4 corrected editorially in November 2014.2 NOTEAdded research report footnotes to Tables A1.2, A1.3, and A1.4 editorially in March 2015.1. Scope*1.1 This test method covers the determination of sulfur in samples of coal or coke by high-temperature tube furn
4、ace combustion.1.1.1 Two analysis methods are described.1.2 When automated equipment is used, either method can be classified as an instrumental method.1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.4 All percentages ar
5、e percent mass fractions unless otherwise noted.1.5 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 and determine the applicability of regu
6、latorylimitations prior to use.1.6 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organi
7、zation Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D346 Practice for Collection and Preparation of Coke Samples for Laboratory AnalysisD2013 Practice for Preparing Coal Samples for AnalysisD3173 Test Method for Moisture in the Analysis Sample of Coal and Co
8、keD3176 Practice for Ultimate Analysis of Coal and CokeD3180 Practice for Calculating Coal and Coke Analyses from As-Determined to Different BasesD7448 Practice for Establishing the Competence of Laboratories UsingASTM Procedures in the Sampling andAnalysis of Coaland CokeD7582 Test Methods for Prox
9、imate Analysis of Coal and Coke by Macro Thermogravimetric AnalysisE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method2.2 ISO Standard:3ISO 11722 Solid Mineral Fuels-Hard Coal Determination of Moisture in the general analysis test sample by drying in nit
10、rogen3. Summary of Test Method3.1 Combustion Method A (1350C)A weighed test portion of sample is burned in a tube furnace at a minimum combustiontube operating temperature of 1350C in a stream of oxygen. During combustion at temperatures above 1350 C, the sulfur andsulfur compounds contained in the
11、sample are decomposed and oxidized almost exclusively to gaseous sulfur dioxide, SO2.Moisture and particulates are removed from the gas by filters. The gas stream is passed through a cell in which sulfur dioxide is1 This test method is under the jurisdiction of ASTM Committee D05 on Coal and Coke an
12、d is the direct responsibility of Subcommittee D05.21 on Methods of Analysis.Current edition approved March 1, 2014May 15, 2017. Published March 2014May 2017. Originally approved in 1983. Last previous edition approved in 2013 asD4239 13D4239 1412. DOI: 10.1520/D4239-14.10.1520/D4239-17.2 For refere
13、ncedASTM 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 International Organization for Standardization (ISO), 1,
14、 ch. de la Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http:/www.iso.ch.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 possibl
15、e 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.*A Summary of Changes section appears at the end of this standardCopyri
16、ght ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1measured by an infrared (IR) absorption detector. Sulfur dioxide absorbs IR energy at a precise wavelength within the IR spectrum.Energy is absorbed as the gas passes through the cell body in
17、which the IR energy is being transmitted: thus, at the detector, lessenergy is received.All other IR energy is eliminated from reaching the detector by a precise wavelength filter. Thus, the absorptionof IR energy can be attributed only to sulfur dioxide whose concentration is proportional to the ch
18、ange in energy at the detector.One cell is used as both a reference and a measurement chamber. Total sulfur as sulfur dioxide is detected on a continuous basis.3.1.1 One procedure for Method A uses coal or coke reference materials to calibrate the sulfur analyzer. A second procedurefor Method A uses
19、 a pure substance, BBOT, to calibrate the sulfur analyzer.3.2 Combustion Method B (1150C)A weighed test portion of sample is burned in a quartz combustion tube in a stream ofoxygen with an equal or excess weight of tungsten trioxide (WO3). Sulfur is oxidized during the reaction of the sample and WO3
20、.The tube furnace is operated at a minimum combustion tube operating temperature of 1150C and tin (Sn) sample boats areutilized. Moisture and particulates are removed from the combustion gas by filters. The gas stream is then passed through a cellin which sulfur dioxide is measured by an infrared (I
21、R) absorption detector. Sulfur dioxide absorbs IR energy at a precisewavelength within the IR spectrum. Energy is absorbed as the gas passes through the cell body in which the IR energy is beingtransmitted: thus, at the detector, less energy is received. All other IR energy is eliminated from reachi
22、ng the detector by a precisewavelength filter. Thus, the absorption of IR energy can be attributed only to sulfur dioxide whose concentration is proportionalto the change in energy at the detector. One cell is used as both a reference and a measurement chamber. Total sulfur as sulfurdioxide is detec
23、ted on a continuous basis.4. Significance and Use4.1 Sulfur is part of the ultimate analysis of coal and coke.4.2 Results of the sulfur analysis are used for evaluation of coal preparation and cleaning, evaluation of potential sulfuremissions from coal and coke combustion or conversion processes, an
24、d evaluation of coal and coke quality in relation to contractspecifications, as well as for scientific purposes.4.3 The competency of laboratories with respect to use of this standard can be established through reference to Practice D7448.5. Sample5.1 Pulverize the sample to pass No. 60 (250-m) siev
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