ASTM D5135-2007 Standard Test Method for Analysis of Styrene by Capillary Gas Chromatography《用毛细管气相色谱法分析苯乙烯的标准试验方法》.pdf
《ASTM D5135-2007 Standard Test Method for Analysis of Styrene by Capillary Gas Chromatography《用毛细管气相色谱法分析苯乙烯的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM D5135-2007 Standard Test Method for Analysis of Styrene by Capillary Gas Chromatography《用毛细管气相色谱法分析苯乙烯的标准试验方法》.pdf(4页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D 5135 07Standard Test Method forAnalysis of Styrene by Capillary Gas Chromatography1This standard is issued under the fixed designation D 5135; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision
2、. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method covers the determination of the impu-rities typically found in styrene and uses those values todetermine the pur
3、ity of styrene by difference by gas chroma-tography. Typical impurities in commercial styrene are foundin Table 1.1.2 This test method is applicable to impurity concentra-tions in the range of 0.001 to 1.00 % and for styrene purities of99 % or higher when using the internal standard procedure.1.3 In
4、 determining the conformance of the test results usingthis method to applicable specifications, results shall berounded off in accordance with the rounding-off method ofPractice E29.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thissta
5、ndard.1.5 This standard does not purport to address all the safetyconcerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety andhealth practices and determine the applicability of regulatorylimitations prior to use. For a specific
6、hazard statement, seeSection 9.2. Referenced Documents2.1 ASTM Standards:2D 3437 Practice for Sampling and Handling Liquid CyclicProductsD 4307 Practice for Preparation of Liquid Blends for Use asAnalytical StandardsD 4790 Terminology of Aromatic Hydrocarbons and Re-lated ChemicalsE29 Practice for U
7、sing Significant Digits in Test Data toDetermine Conformance with SpecificationsE 355 Practice for Gas Chromatography Terms and Rela-tionshipsE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE 1510 Practice for Installing Fused Silica Open TubularCapil
8、lary Columns in Gas Chromatographs2.2 Other DocumentOSHA Regulations, 29 CFR paragraphs 1910.1000 and1910.120033. Terminology3.1 See Terminology D 4790 for definitions of terms used inthis test method.4. Summary of Test Method4.1 In this test method, the chromatogram peak area for eachimpurity is co
9、mpared to the peak area of the internal standard(n-heptane or other suitable known) added to the sample. Fromthe response factors of these impurities relative to that of theinternal standard and the amount of internal standard added,the concentration of the impurities are calculated. The styrenecont
10、ent is obtained by subtracting the total amount of allimpurities from 100.00.5. Significance and Use5.1 This test method is designed to obtain styrene purity onthe basis of impurities normally present in styrene and may beused for final product inspections and process control.1This test method is un
11、der the jurisdiction of ASTM Committee D16 onAromatic Hydrocarbons and Related Chemicals and is the direct responsibility ofSubcommittee D16.07 on Styrene, Ethylbenzene and C9 and C10 AtomaticHydrocarbons.Current edition approved June 1, 2007. Published June 2007. Originallyapproved in 1990. Last pr
12、evious edition approved in 2002 as D 5135 02e1.2For 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.3Available fro
13、m U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.TABLE 1 Impurities Known or Suggested to be Present inCommercial StyreneEthylbenzeneo-xylenem-xylenep-xyleneIsopropylbenzenen-propylbenzenem-ethyltolue
14、nep-ethyltoluenea-methylstyrenem-vinyltoluenep-vinyltoluenePhenylacetylene1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.2 This test method will detect the impuriti
15、es shown inTable 1, non-aromatic hydrocarbons containing ten carbons orless, and others where specific impurity standards are available.Absolute purity cannot be determined if unknown impuritiesare present.6. Interferences6.1 The internal standard chosen must be satisfactorilyresolved from any impur
16、ity as well as the product peak.Apeakwill be satisfactorily resolved from a neighboring peak if thedistance from the valley to the baseline between the two peaksis not greater than 50 % of the peak height of the smaller of thetwo peaks.7. Apparatus7.1 Gas ChromatographAny instrument having a flameio
17、nization detector that can be operated at the conditions givenin Table 2. The system shall have sufficient sensitivity to obtaina minimum peak height response for 0.001 weight % impurityof twice the height of the background noise.7.2 ColumnA capillary column containing a stationaryphase of cross-lin
18、ked polyethylene glycol has been found to besatisfactory. Any column can be used that is capable ofresolving all significant impurities from styrene and from theinternal standard.7.3 RecorderElectronic integration, with tangent capabili-ties is recommended.7.4 100-mL Volumetric Flask.7.5 Microsyring
19、es, assorted volumes.8. Reagents and Materials8.1 Purity of ReagentReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee onAnalytical Reagents of theAmerican Chemical Society,4where such sp
20、ecifications are available.8.2 Carrier Gas, makeup and detector gases 99.999 %purity. Oxygen in carrier gas less than 1 ppm, less than 0.5 ppmis preferred. Purify carrier, makeup and detector gases toremove oxygen, water, and hydrocarbons.8.3 Air, purify to remove hydrocarbons and water. Airshould c
21、ontain less than 0.1 ppm THC.8.4 n-Heptane, 99.0 % minimum purity, or other internalstandard, such as n-octane, previously analyzed to be free ofcompounds coeluting with impurities in the sample.8.5 Styrene, the highest purity available, but not less than99.7 %.8.6 Pure Compounds, for calibration, s
22、hall be those com-pounds that are typically present in commercial styrene. Theseshould be at least 99 % pure as they are to be used fordetermining response factors.9. Hazards9.1 Consult current OSHA regulations, suppliers MaterialSafety Data Sheets, and local regulations for all materials usedin thi
23、s procedure.10. Sampling10.1 Sample the material in accordance with PracticeD 3437.11. Preparation of Apparatus11.1 Follow manufacturers instructions for mounting andconditioning the column into the chromatograph and adjustingthe instrument conditions described in Table 2, allowingsufficient time fo
24、r the equipment to reach equilibrium. SeePractices E 355 and E 1510 for additional information on gaschromatographic practices and terminology.12. Calibration12.1 Prepare a calibration mixture containing approximately99.5 weight % styrene and the expected significant impuritiesat their expected conc
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