1、Designation:D376196 (Reapproved 2002) Designation: D3761 10Standard Test Method forTotal Fluorine in Coal by the Oxygen Bomb Combustion/IonSelective Electrode Method1This standard is issued under the fixed designation D3761; the number immediately following the designation indicates the year oforigi
2、nal 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.This standard has been approved for use by agencies of the Department of Def
3、ense.1. Scope1.1 This test method covers the analysis of total fluorine in coal.1.2 This test method was successfully tested on coals containing 25 % ash or less.21.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.1.4 This s
4、tandard 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 regulatorylimitations prior to use. For specific hazard statem
5、ents, see Section 7.1.5 All accountability and quality control aspects of Guide D4621 apply to this test method.2. Referenced Documents2.1 ASTM Standards:3D1193 Specification for Reagent WaterD2013 Practice for Preparing Coal Samples for AnalysisD3173 Test Method for Moisture in the Analysis Sample
6、of Coal and CokeD3180 Practice for Calculating Coal and Coke Analyses from As-Determined to Different BasesD4621 Guide for Quality Management in an Organization That Samples or Tests Coal and CokeD5142 Test Methods for Proximate Analysis of the Analysis Sample of Coal and Coke by Instrumental Proced
7、uresE144 Practice for Safe Use of Oxygen Combustion Bombs3. Summary of Test Method3.1 Total fluorine is determined in this test method by combusting a weighed sample in an oxygen bomb with a dilute baseabsorbing the fluorine vapors.The bomb is rinsed into a beaker with water and following the additi
8、on of a citrate buffer, the fluorineis determined by ion-selective electrode.4. Significance and Use4.1 This test method permits measurement of the fluorine content of coal for the evaluation of potential fluorine emission fromcoal combustion or conversion processes. When coal samples are combusted
9、in accordance with this test method, the fluorine isquantitatively retained and is representative of the total fluorine concentration in whole coal.5. Apparatus5.1 Combustion Bomb, constructed of materials that are not affected by the combustion process or products. The bomb mustbe designed so that
10、all liquid combustion products can be quantitatively recovered by washing the inner surfaces. There must beno gas leakage during the test. The bomb must be capable of withstanding a hydrostatic-pressure test to 20 MPa (approximately3000 psig) at room temperature without stressing any part beyond its
11、 elastic limit.5.2 Water BathA container large enough to hold the combustion bomb and enough cooling water to dissipate the heat1This test method is under the jurisdiction of ASTM Committee D05 on Coal and Coke and is the direct responsibility of Subcommittee D05.29 on Major Elements inAsh and Trace
12、 Elements of Coal.Current edition approved April 10, 2002. Published June 1996. Originally published as D376179. Last previous edition D376196. DOI: 10.1520/D3761-96R02.Current edition approved Dec. 1, 2010. Published January 2010. Originally published as D3761 79. Last previous edition D3761 96(200
13、2). DOI: 10.1520/D376110.2This standard is based on a published report by Thomas, J., Jr., and Gluskoter, H. J., “Determination of Fluoride in Coal with the Fluoride Ion-Specific Electrode,”Analytical Chemistry, Vol 46, 1974, pp. 132123.3For referencedASTM standards, visit theASTM website, www.astm.
14、org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standards, Vol 11.01.volume information, refer to the standards Document Summary page on the ASTM website.1This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication
15、 of what changes have been made to the previous version. Becauseit may not be technically 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 conside
16、red the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.generated during the combustion process. The container shall be designed to allow a constant flow of water around the combustionbomb.5.3 Sample HolderSamples sh
17、all be burned in an open crucible of platinum, quartz, or acceptable base metal alloy.Base-metal alloy crucibles are acceptable if after a few preliminary firings the weight does not change significantly between tests.5.4 Ignition Wire, 100-mm, nickel-chromium alloy, No. 34B calorimeter; coal; coal
18、products; fluorine content; ion-selective electrodeASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent righ
19、ts, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for
20、revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing
21、you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.6Midgley, D., and Torrance, K., Potentiometric Water Analysis, John Wiley and Sons, Inc., New York, NY, 1978.6Supporting data have been filed at ASTM International Headquarters and may be obtained by reque
22、sting Research Report RR:D05-1004.D3761 104This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D3761 105