1、Designation:D 3684 01(Reapproved 2006)Standard Test Method forTotal Mercury in Coal by the Oxygen BombCombustion/Atomic Absorption Method1This standard is issued under the fixed designation D 3684;the number immediately following the designation indicates the year oforiginal adoption or,in the case
2、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.1.Scope1.1 This test method describes a procedure for the analysisof total mercury in coal.1.2 This standard
3、does not purport 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.Specific precau-tionary statements a
4、re given in 8.3.1.1.3 The values stated in SI units(IEEE/ASTM SI 10)shallbe regarded as the standard.2.Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 2013 Practice for Preparing Coal Samples for AnalysisD 3173 Test Method for Moisture in theAnalysis Sample ofCoal and
5、 CokeD 3180 Practice for Calculating Coal and Coke Analysesfrom As-Determined to Different BasesD 5142 Test Methods for Proximate Analysis of the Analy-sis Sample of Coal and Coke by Instrumental ProceduresE 144 Practice for Safe Use Of Oxygen Combustion BombsIEEE/ASTM SI 10 Standard for Use of Inte
6、rnational Sys-tem of Units(SI):The Modern Metric System2.2ISO StandardsISO 5725-6:1994Accuracy of measurement methods andresults-Part 633.Summary of Test Method3.1 Total mercury is determined in this test method bycombusting a weighed sample in an oxygen bomb with dilutenitric acid absorbing the mer
7、cury vapors.The bomb is rinsedinto a reduction vessel with dilute nitric acid,and the mercuryis determined by the flameless cold vapor atomic absorptiontechnique.NOTE1Mercury and mercury salts can be volatilized at low tempera-tures.Precautions against inadvertent mercury loss should be taken whenus
8、ing this method.4.Significance and Use4.1 The possible emission of mercury that may be found incoal from coal combustion is an environmental concern.4.2 When test portions are burned according to this proce-dure,the total mercury is quantitatively retained and is repre-sentative of concentrations in
9、 the whole coal.5.Apparatus5.1 Combustion BombThe combustion bomb shall beconstructed of materials that are not affected by the combustionprocess or products.The bomb must be designed so that allliquid combustion products can be completely recovered bywashing the inner surfaces.There must be no gas
10、leakageduring the test.The bomb must be capable of withstanding ahydrostatic pressure test to gage pressure of 20 MPa(approxi-mately 3000 psig)at room temperature without stressing any ofthe parts beyond the elastic limit.5.2 Water BathA container shall be large enough to holdthe combustion bomb,and
11、 enough cooling water shall be usedto dissipate the heat generated during the combustion process.The container should be designed to allow a constant flow ofwater around the combustion bomb.5.3 Combustion CruciblesSamples shall be burned in anopen crucible of platinum,quartz,or acceptable base-metal
12、alloy.5.4 Firing Wire,100 mm of either No.34 B&S(0.160-mm)nickel-chromium alloy,No.34 B&S iron,or No.38 B&S(0.101-mm)gage platinum wire.1This test method is under the jurisdiction of ASTM Committee D05 on Coaland Coke and is the direct responsibility of Subcommittee D05.29 on MajorElements in Ash an
13、d Trace Elements of Coal.Current edition approved April 1,2006.Published April 2006.Originallyapproved in 1978.Last previous edition approved in 2001 as D 3684 01.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of
14、ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.3Available from International Organization for Standardization(ISO),1 rue deVaremb,Case postale 56,CH-1211,Geneva 20,Switzerland.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Consh
15、ohocken,PA 19428-2959,United States.5.5 Firing CircuitA 6-to 16-V alternating or directcurrent is required for ignition purposes with an ammeter orpilot light in the circuit to indicate when current is flowing.Astepdown transformer connected to an alternating currentlighting circuit or batteries may
16、 be used.The ignition circuitswitch shall be of the momentary double-contact type,nor-mally open,except when held closed by the operator.Theswitch should be depressed only long enough to fire the charge.5.6 Analytical Balance,with a sensitivity of 0.1 mg.5.7 Atomic Absorption Spectrophotometer,with a flamelesscold-vapor mercury analysis system comprised of either aclosed recirculating system or an open one-pass system.5.8 Reduction Vessels,biochemical oxygen demand(BOD)bottles,300-mL capacity.6.