1、Designation: D 3761 96 (Reapproved 2002)Standard Test Method forTotal Fluorine in Coal by the Oxygen Bomb Combustion/IonSelective Electrode Method1This standard is issued under the fixed designation D 3761; 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 (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1
3、This test method covers the analysis of total fluorine incoal.1.2 This test method was successfully tested on coalscontaining 25 % ash or less.21.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does not purp
4、ort to 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 and health practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardstatements, see Section 7.
5、1.5 All accountability and quality control aspects of GuideD 4621 apply to this test method.2. Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water3D 2013 Practice for Preparing Coal Samples for Analysis4D 3173 Test Method for Moisture in theAnalysis Sample ofCoal and Coke4D
6、 3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different Bases4D 4621 Guide for Quality Management in an Organizationthat Samples or Tests Coal and Coke4D 5142 Test Methods for Proximate Analysis of the Analy-sis Sample of Coal and Coke by Instrumental Procedures4E 144 Pr
7、actice for Safe Use of Oxygen CombustionBombs53. Summary of Test Method3.1 Total fluorine is determined in this test method bycombusting a weighed sample in an oxygen bomb with a dilutebase absorbing the fluorine vapors. The bomb is rinsed into abeaker with water and following the addition of a citr
8、ate buffer,the fluorine is determined by ion-selective electrode.4. Significance and Use4.1 This test method permits measurement of the fluorinecontent of coal for the evaluation of potential fluorine emissionfrom coal combustion or conversion processes. When coalsamples are combusted in accordance
9、with this test method, thefluorine is quantitatively retained and is representative of thetotal fluorine concentration in whole coal.5. Apparatus5.1 Combustion Bomb, constructed of materials that are notaffected by the combustion process or products. The bombmust be designed so that all liquid combu
10、stion products can bequantitatively recovered by washing the inner surfaces. Theremust be no gas leakage during the test. The bomb must becapable of withstanding a hydrostatic-pressure test to 20 MPa(approximately 3000 psig) at room temperature without stress-ing any part beyond its elastic limit.5.
11、2 Water BathA container large enough to hold thecombustion bomb and enough cooling water to dissipate theheat generated during the combustion process. The containershall be designed to allow a constant flow of water around thecombustion bomb.5.3 Sample HolderSamples shall be burned in an opencrucibl
12、e of platinum, quartz, or acceptable base metal alloy.Base-metal alloy crucibles are acceptable if after a fewpreliminary firings the weight does not change significantlybetween tests.5.4 Ignition Wire, 100-mm, nickel-chromium alloy, No. 34B calorimeter; coal; coalproducts; fluorine content; ion-sel
13、ective 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 rights, and the riskof infringement of
14、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 revision of this standard or for ad
15、ditional 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 you shouldmake your views known to
16、the ASTM Committee on Standards, at the address shown below.This 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).8Supporting data are available from ASTM Headquarters. Request RR:D05-1004.D 3761 96 (2002)4
