ASTM D7183-2007e1 781 Standard Test Method for Determination of Total Sulfur in Aromatic Hydrocarbons and Related Chemicals by Ultraviolet Fluorescence《紫外线荧光法测定芳烃和相关化合物中总硫度的标准试验方法》.pdf
《ASTM D7183-2007e1 781 Standard Test Method for Determination of Total Sulfur in Aromatic Hydrocarbons and Related Chemicals by Ultraviolet Fluorescence《紫外线荧光法测定芳烃和相关化合物中总硫度的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM D7183-2007e1 781 Standard Test Method for Determination of Total Sulfur in Aromatic Hydrocarbons and Related Chemicals by Ultraviolet Fluorescence《紫外线荧光法测定芳烃和相关化合物中总硫度的标准试验方法》.pdf(4页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D 7183 07e1Standard Test Method forDetermination of Total Sulfur in Aromatic Hydrocarbons andRelated Chemicals by Ultraviolet Fluorescence1This standard is issued under the fixed designation D 7183; the number immediately following the designation indicates the year oforiginal adoption
2、or, in 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.e1NOTEResearch report was added editorially in September 2007.1. Scope1.1 This test meth
3、od covers the determination of sulfur inaromatic hydrocarbons, their derivatives, and related chemi-cals.1.2 This test method is applicable to samples with sulfurconcentrations from 0.5 to 100 mg/kg.1.3 The following applies for the purposes of determiningthe conformance of the test results using th
4、is test method toapplicable specifications, results shall be rounded off in accor-dance with the rounding-off method of Practice E29.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 This standard does not purport to addre
5、ss 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 9.2. Reference
6、d Documents2.1 ASTM Standards:2D 1555 Test Method for Calculation of Volume and Weightof Industrial Aromatic Hydrocarbons and CyclohexaneD 3437 Practice for Sampling and Handling Liquid CyclicProductsD 6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic Hydrocarbons and Relat
7、ed Ma-terialsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 Other DocumentsOSHA Regulations, 29 CFR, paragraphs 1910.1000 and1910.120033. Terminolog
8、y3.1 oxidative pyrolysis, na process in which a sample iscombusted in an oxygen-rich atmosphere at high temperatureto break down the components of the sample into elementaloxides.3.2 ultraviolet fluorescence, nradiation in the region ofthe electromagnetic spectrum including wavelength from 100to 390
9、0A that excites SO2to (SO2*).4. Summary of Test Method4.1 A specimen is either directly injected or placed in asample boat. The boat is then inserted into a high temperaturecombustion tube where the sulfur is oxidized to sulfur dioxide(SO2) in an oxygen-rich atmosphere. Water produced duringthe samp
10、le combustion is removed and the sample combustiongases are next exposed to ultraviolet (UV) light. The SO2absorbs the energy from the UV light and is converted toexcited sulfur dioxide (SO2*). As it returns to a stable state,light is emitted and detected by a photomultiplier tube and theresulting s
11、ignal is a measure of the sulfur contained in thespecimen.5. Significance and Use5.1 Some process catalysts used in petroleum and chemicalrefining can be poisoned when trace amounts of sulfur-bearingmaterials are contained in the feedstocks. This test method canbe used to determine sulfur in process
12、 feeds, sulfur in finishedproducts, and can also be used for purposes of regulatorycontrol.6. Interferences6.1 Halogens present in the specimen in concentrationsgreater than 10 % and nitrogen concentrations of 1500 mg/kgor greater can interfere.1This test method is under the jurisdiction of ASTM Com
13、mittee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility ofSubcommittee D16.04 on Instrumental Analysis.Current edition approved Jan. 15, 2007. Published April 2007.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service
14、at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.
15、1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Copyright by ASTM Intl (all rights reserved); Mon Apr 14 02:14:21 EDT 2008Downloaded/printed byGuo Dehua (CNIS) pursuant to License Agreement. No further reproductions authorized.6.2 Mo
16、isture produced during the combustion step caninterfere if not removed prior to the gas entering the detectorcell.7. Apparatus7.1 Pyrolysis FurnaceAn electric furnace capable ofmaintaining a temperature sufficient to volatilize and pyrolyzeall the sample and oxidize sulfur to SO2. The actual tempera
17、-ture should be recommended by specific instrument manufac-turer.7.2 Quartz Pyrolysis TubeCapable of withstanding 900 to1200C. The tube should be recommended by the instrumentmanufacturer.7.3 Microlitre SyringeCapable of delivering from 5 to250 L of sample. Check with the instrument manufacturer for
18、recommendations for specific sample requirements.7.4 Constant Rate Injector SystemIf the sample is to beintroduced into the pyrolysis furnace via syringe, use aconstant rate injector or a liquid introduction module.7.5 Liquid Auto-SamplerCapable of injecting 5 to 250 Lof sample.7.6 Automatic Boat Dr
19、ive SystemIf the instrument isequipped with an inlet system, a device for driving the boatinto the furnace at a controlled and repeatable rate is required.7.7 Flow ControlThe instrument must be equipped withflow controllers capable of maintaining a constant supply ofoxygen and carrier gas.7.8 Drier
20、TubeThe instrument must be equipped with amechanism for removal of water vapor.8. Reagents8.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. It is intended that all reagents shall conform tothe specifications of the Committee on Analytical Reagents ofthe American Chemical Socie
21、ty,4where such specifications areavailable, unless otherwise indicated. Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.8.2 Inert GasEither argon (Ar) or helium (He) may beus
22、ed. The purity should be no less than 99.99 mol %.8.3 Oxygen GasThe purity should be no less than 99.99mol %.8.4 SolventThe solvent chosen should be capable ofdissolving the sulfur compound. The solvent of choice shouldhave a boiling point similar to the sample being analyzed.Suggested possibilities
23、 include, but not limited to methanol,iso-octane, and p-xylene (see Note 1 and Note 2).NOTE 1A quick screening can be conducted by injecting the solventand sample once or twice and comparing relative area counts.NOTE 2All solvents should have known sulfur content or known to beless than what will in
24、terfere with results.8.5 DibenzothiopheneFW184.26, 17.399 % (m/m) Sulfur(see Note 3).NOTE 3A correction for chemical impurity is required. Normally98 %.8.6 Quartz WoolIf needed.8.7 Sulfur Stock Solution, approximately 870 to 1044 gS/mlThis standard may be purchased if desired. Prepare astock solutio
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