ASTM D6722-2001(2006) Standard Test Method for Total Mercury in Coal and Coal Combustion Residues by Direct Combustion Analysis《直接燃烧分析法测量煤和煤燃烧残余物中总汞量的标准试验方法》.pdf
《ASTM D6722-2001(2006) Standard Test Method for Total Mercury in Coal and Coal Combustion Residues by Direct Combustion Analysis《直接燃烧分析法测量煤和煤燃烧残余物中总汞量的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM D6722-2001(2006) Standard Test Method for Total Mercury in Coal and Coal Combustion Residues by Direct Combustion Analysis《直接燃烧分析法测量煤和煤燃烧残余物中总汞量的标准试验方法》.pdf(4页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D 6722 01 (Reapproved 2006)Standard Test Method forTotal Mercury in Coal and Coal Combustion Residues byDirect Combustion Analysis1This standard is issued under the fixed designation D 6722; the number immediately following the designation indicates the year oforiginal adoption or, in t
2、he 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.1. Scope1.1 These test methods cover procedures to determine thetotal mercury content in a sampl
3、e of coal or coal combustionresidue.1.2 The values stated in SI units are regarded as thestandard.1.3 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 standard to establish appro-priate safety and health
4、 practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 121 Terminology of Coal and CokeD 2013 Practice for Preparing Coal Samples for AnalysisD 3173 Test Method for Moisture in theAnalysis Sample ofCoal and CokeD 3180 Practice
5、for Calculating Coal and Coke Analysesfrom As-Determined to Different BasesD 4621 Guide for Quality Management in an OrganizationThat Samples or Tests Coal and CokeD 5142 Test Methods for Proximate Analysis of the Analy-sis Sample of Coal and Coke by Instrumental ProceduresIEEE/ASTM SI 10 Standard f
6、or Use of the InternationalSystem of Units (SI): The Modern Metric System3. Terminology3.1 For definitions of terms used in this standard, refer toTerminology D 121.4. Summary of Test Method4.1 Controlled heating of the analysis sample in oxygen isused to liberate mercury. The sample is heated to dr
7、yness in theinstrument and then thermally and chemically decomposed.The decomposition products are carried by flowing oxygen tothe catalytic section of the furnace, where oxidation is com-pleted and halogens as well as nitrogen and sulfur oxides aretrapped. The remaining decomposition products are c
8、arried toa gold amalgamator that selectively traps mercury. After thesystem is flushed with oxygen to remove any remainingdecomposition products, the amalgamator is rapidly heated,releasing mercury vapor. Flowing oxygen carries the mercuryvapor through absorbance cells positioned in the light path o
9、fsingle wavelength atomic absorption spectrophotometer. Ab-sorbance peak height or peak area, as a function of mercuryconcentration, is measured at 253.7 nm.NOTE 1Mercury and mercury salts can be volatized at low tempera-tures. Precautions against inadvertent mercury loss should be taken whenusing t
10、his method.5. Significance and Use5.1 The emission of mercury during coal combustion can bean environmental concern.5.2 When representative test portions are analyzed accord-ing to this procedure, the total mercury is representative ofconcentrations in the sample.6. Apparatus6.1 There are several co
11、nfigurations of the instrumentalcomponents that can be used satisfactorily for this test method.Functionally, the instrument shall have the following compo-nents: drying compartment, decomposition tube, catalyst tube,gold amalgamator, amalgamator furnace, measuring cuvettes,mercury lamp, and detecto
12、r. The following requirements arespecified for all approved instruments. (Note 2).NOTE 2The approval of an instrument with respect to these functionsis paramount to this test method, since such approval tacitly providesapproval of both the materials and the procedures used with the system toprovide
13、these functions.6.1.1 The instrument shall be capable of drying the sampleonce it is weighed and introduced.6.1.2 The instrument shall have a decomposition tube whichshall be operated at a temperature high enough to completelydecompose the sample. The suggested operating temperature is800C.1This tes
14、t 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 and Trace Elements of Coal.Current edition approved April 1, 2006. Published April 2006. Originallyapproved in 2001. Last previous edition approved
15、 in 2001 as D672201.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr H
16、arbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.1.3 The catalyst in the catalytic tube shall be capable ofcompleting the oxidation of the sample and trapping halogensas well as nitrogen and sulfur oxides. The suggested operatingtemperature of the catalytic tube is 550C.6.
17、1.4 The instrument shall contain a gold amalgamator fixedto an inert material and shall be capable of trapping allmercury.6.1.5 The amalgamator shall contain a furnace capable ofrapidly heating the amalgamator to release all trapped mercury.6.1.6 The instrument shall have a absorption cell withmeasu
18、ring cuvettes through which the elemental mercuryreleased from the gold amalgamator flows. The cell shall beheated to avoid any condensation of water or other decompo-sition products.6.1.7 The light source for the atomic absorption processshall be a low pressure mercury lamp.6.1.8 A narrow bandpass
19、interference filter or monochroma-tor, capable of isolating the 253.65 nm mercury line, shall beused.6.1.9 The system may contain a computer for controllingthe various operations of the apparatus, for recording data, andfor reporting results.6.2 Analytical Balance, with a sensitivity of 0.1 mg.6.3 S
20、ample Combustion Boats, made of nickel and conve-nient size suitable for use in the instrument being used.7. Sample7.1 Prepare the analysis sample of coal in accordance withMethod D 2013 by pulverizing the material to pass a 250-mm(No. 60) sieve.7.2 Analyze separate test portions for moisture conten
21、t inaccordance with Test Method D 3173 or Test Methods D 5142.8. Reagents8.1 OxygenHigh purity oxygen, as specified by the instru-ment manufacturer, shall be used.8.2 Certified Reference Materials (CRMs)Use CertifiedReference Material (CRM) coals with dry-basis mercury val-ues for which confidence l
22、imits are issued by a recognizedcertifying agency such as the National Institute of Standardsand Technology (NIST). It is recommended that the user verifythe value with the certifying agency before using the CRM coalfor quality control purposes.8.3 All CRMs, reference coals, or calibrating agents mu
23、sthave precision values of less than or equal to method repeat-ability. Such CRMS, reference coals, or calibrating agents mustbe stable with respect to moisture and be pulverized to pass100 % through a 250 m (No. 60) USAStandard Sieve. CRMs,reference coals, or calibrating agents must be mixed thor-o
24、ughly before each use.9. Instrument Preparation9.1 Assemble the instrumental system in accordance withthe manufacturers instructions. Follow the instrument manu-facturers recommended procedure to optimize the perfor-mance of the instrument.9.2 Adjustment of Response of Measurement SystemWeigh an app
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