ImageVerifierCode 换一换
格式:PDF , 页数:5 ,大小:123.73KB ,
资源ID:518956      下载积分:10000 积分
快捷下载
登录下载
邮箱/手机:
温馨提示:
如需开发票,请勿充值!快捷下载时,用户名和密码都是您填写的邮箱或者手机号,方便查询和重复下载(系统自动生成)。
如填写123,账号就是123,密码也是123。
特别说明:
请自助下载,系统不会自动发送文件的哦; 如果您已付费,想二次下载,请登录后访问:我的下载记录
支付方式: 支付宝扫码支付 微信扫码支付   
注意:如需开发票,请勿充值!
验证码:   换一换

加入VIP,免费下载
 

温馨提示:由于个人手机设置不同,如果发现不能下载,请复制以下地址【http://www.mydoc123.com/d-518956.html】到电脑端继续下载(重复下载不扣费)。

已注册用户请登录:
账号:
密码:
验证码:   换一换
  忘记密码?
三方登录: 微信登录  

下载须知

1: 本站所有资源如无特殊说明,都需要本地电脑安装OFFICE2007和PDF阅读器。
2: 试题试卷类文档,如果标题没有明确说明有答案则都视为没有答案,请知晓。
3: 文件的所有权益归上传用户所有。
4. 未经权益所有人同意不得将文件中的内容挪作商业或盈利用途。
5. 本站仅提供交流平台,并不能对任何下载内容负责。
6. 下载文件中如有侵权或不适当内容,请与我们联系,我们立即纠正。
7. 本站不保证下载资源的准确性、安全性和完整性, 同时也不承担用户因使用这些下载资源对自己和他人造成任何形式的伤害或损失。

版权提示 | 免责声明

本文(ASTM D5135-2016e1 Standard Test Method for Analysis of Styrene by Capillary Gas Chromatography《采用毛细管气相色谱法分析苯乙烯的标准试验方法》.pdf)为本站会员(dealItalian200)主动上传,麦多课文库仅提供信息存储空间,仅对用户上传内容的表现方式做保护处理,对上载内容本身不做任何修改或编辑。 若此文所含内容侵犯了您的版权或隐私,请立即通知麦多课文库(发送邮件至master@mydoc123.com或直接QQ联系客服),我们立即给予删除!

ASTM D5135-2016e1 Standard Test Method for Analysis of Styrene by Capillary Gas Chromatography《采用毛细管气相色谱法分析苯乙烯的标准试验方法》.pdf

1、Designation: D5135 161Standard Test Method forAnalysis of Styrene by Capillary Gas Chromatography1This standard is issued under the fixed designation D5135; 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 () indicates an editorial change since the last revision or reapproval.1NOTETable 3 was editorially corrected in November 2016.1. Scope*1.1 This test method covers the determination of the impu-rities typically foun

3、d in styrene and uses those values todetermine the purity 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 hi

4、gher when using the internal standard procedure.1.3 In 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.

5、 No other units of measurement are included in thisstandard.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

6、of regulatorylimitations prior to use. For a specific hazard statement, seeSection 9.2. Referenced Documents2.1 ASTM Standards:2D3437 Practice for Sampling and Handling Liquid CyclicProductsD4307 Practice for Preparation of Liquid Blends for Use asAnalytical StandardsD4790 Terminology of Aromatic Hy

7、drocarbons and RelatedChemicalsD6809 Guide for Quality Control and Quality AssuranceProcedures for Aromatic Hydrocarbons and Related Ma-terialsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with SpecificationsE355 Practice for Gas Chromatography Terms and Relation-shi

8、psE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE1510 Practice for Installing Fused Silica Open TubularCapillary Columns in Gas Chromatographs2.2 Other DocumentOSHA Regulations, 29 CFR paragraphs 1910.1000 and1910.120033. Terminology3.1 See Terminolo

9、gy D4790 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 compared to the peak area of the internal standard(n-heptane or other suitable known) added to the sample. Fromthe response factors of these impu

10、rities relative to that of theinternal standard and the amount of internal standard added,the concentration of the impurities are calculated. The styrenecontent is obtained by subtracting the total amount of allimpurities from 100.00.5. Significance and Use5.1 This test method is designed to obtain

11、styrene purity onthe basis of impurities normally present in styrene and may beused for final product inspections and process control.5.2 This test method will detect the impurities shown inTable 1, non-aromatic hydrocarbons containing ten carbons orless, and others where specific impurity standards

12、 are available.Absolute purity cannot be determined if unknown impuritiesare present.1This test method is under 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 Aromatic

13、Hydrocarbons.Current edition approved June 1, 2016. Published October 2016. Originallyapproved in 1990. Last previous edition approved in 2014 as D5135 14. DOI:10.1520/D5135-16E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org

14、. 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.*A Summary of Chan

15、ges section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States16. Interferences6.1 The internal standard chosen must be satisfactorilyresolved from any impurity as well as the product peak.Apeakwill be

16、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 flameionization detector that can be operated at the

17、 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-linked polyethylene glycol has been found to bes

18、atisfactory. Any column can be used that is capable ofresolving all significant impurities from styrene and from theinternal standard. The choice of column is based on resolutionrequirements. Any column may be used that is capable ofresolving all significant impurities from the major component.The c

19、olumn and conditions described in Table 2 have beenused successfully and shall be used as a referee in cases ofdispute.7.2.1 “Total non-aromatics” are defined as all componentseluting before o-xylene, excluding benzene, toluene,ethylbenzene, p-xylene, m-xylene, and cumene. The internalstandard used

20、for calibration is also excluded. Generally,non-aromatics are summed and reported as a group. In certaincases, one or more individual non-aromatic components, suchas 1,4-dioxane, may be reported separately. In those cases, thegrouping would not include the separately reportedcomponent(s), and the re

21、maining non-aromatics would bereported as “Nonaromatics other than (component(s).”7.2.2 “Total C9plus aromatics” are defined as cumene, plusall components eluting after o-xylene. Generally, C9plusaromatics are summed and reported as a group. In certaincases, one or more individual C9plus aromatic co

22、mponents,such as cumene or p-diethylbenzene, may be reported sepa-rately. In those cases, the grouping would not include theseparately reported component(s) and the remaining C9plusaromatics would be reported as “C9plus aromatics other than(component(s).” Very heavy non-aromatics may also elute inth

23、is region, but they are not common in materials within thescope of Committee D16, and are not considered in thedefinition.7.3 RecorderElectronic integration, with tangent capabili-ties is recommended.7.4 100-mL Volumetric Flask.7.5 Microsyringes, assorted volumes.8. Reagents and Materials8.1 Purity

24、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 specifications are available.8.2 Carrier Gas, makeup and de

25、tector 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 contain less than 0.1 ppm THC.8.4 n-Heptane, 99.0 % minimu

26、m 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, shall be those com-pounds that are typically present in co

27、mmercial styrene. Theseshould be at least 99 % pure as they are to be used fordetermining response factors.9. Hazards9.1 Consult current OSHA regulations, suppliers SafetyData Sheets, and local regulations for all materials used in thisprocedure.4Reagent Chemicals, American Chemical Society Specific

28、ations, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Conventio

29、n, Inc. (USPC), Rockville,MD.TABLE 1 Impurities Known or Suggested to be Present inCommercial StyreneEthylbenzeneo-xylenem-xylenep-xyleneIsopropylbenzenen-propylbenzenem-ethyltoluenep-ethyltoluene-methylstyrenem-vinyltoluenep-vinyltoluenePhenylacetyleneTABLE 2 Recommended Operating ConditionsCarrier

30、 gas heliumCarrier gas flow rate at 110C, mL/min 1.2Detector flame ionizationDetector temperature, C 240Injection port temperature, C 230Hydrogen flow rate, mL/min 30Air flow rate, mL/min 275Make up gas nitrogenMake up gas flow rate, mL/min 23Split flow, mL/min 150Column 60 m 0.32 mm ID 0.5 mbonded

31、polyethylene glycol-fused silica capillaryColumn temperature, C 110Chart speed, cm/min 1Sample size, L 0.6D5135 161210. Sampling10.1 Sample the material in accordance with PracticeD3437.11. Preparation of Apparatus11.1 Follow manufacturers instructions for mounting andconditioning the column into th

32、e chromatograph and adjustingthe instrument conditions described in Table 2, allowingsufficient time for the equipment to reach equilibrium. SeePractices E355 and E1510 for additional information on gaschromatographic practices and terminology.12. Calibration12.1 Prepare a calibration mixture contai

33、ning approximately99.5 weight % styrene and the expected significant impuritiesat their expected concentration (see Practice D4307). Weigh allcomponents to the accuracy required to calculate the concen-tration of each to the nearest 0.001 %.12.2 With a microsyringe, add 50 L of internal standard toa

34、 100mL volumetric flask about three-fourths full of calibra-tion mixture. Mix well. Add calibration mixture to mark andagain mix well. If n-heptane is used as the internal standard,using a density of 0.684 for n-heptane and 0.906 for styrene,this solution will contain 0.0377 weight % n-heptane.12.3

35、Also prepare a sample of the styrene used for thecalibration blend with and without n-heptane to determine theconcentration of existing impurities and interfering compoundswith internal standard. If impurities in the styrene emerge withthe chosen internal standard, an alternate internal standardmust

36、 be used.12.4 Inject an appropriate amount of sample into the chro-matograph and obtain a chromatogram.12.5 Measure the areas of all peaks, including the internalstandard, except the styrene peak.12.6 Calculate the response factors for each impurity rela-tive to the internal standard as follows:RFi5

37、CiCs!SAiAsi2AbAsbD(1)where:RFi= response factor relative to the internal standard,Asi= area of internal standard in calibration mixture,Ai= area of impurity peak in calibration mixture,Asb= area of internal standard in styrene used in makingcalibration mixture,Ab= area of impurity in styrene used to

38、 make calibrationmixture,Cs= weight percent internal standard in calibrationmixture, andCi= weight percent impurity in calibration mixture.13. Procedure13.1 Establish stable instrument operation at the prescribedor selected operating conditions. Reference should be made toinstructions provided by th

39、e manufacturer of the chromato-graph.13.2 Prepare sample as described in 12.2.13.3 Inject appropriate amount of sample into the chromato-graph and obtain the chromatogram.Atypical chromatogram isshown in Fig. 1.14. Calculation14.1 Measure the areas of all peaks, including the internalstandard, excep

40、t the styrene peak.14.2 Calculate the weight percent of the individualimpurities, Ci, as follows:Ci5Ai!RFi!Cs!As(2)where:Ai= area of impurity,As= area of internal standard,RFi= response factor for impurity, relative to the internalstandard, andCs= concentration of internal standard, in weight percen

41、t.14.3 Calculate the styrene content by subtracting the sum ofthe impurities from 100.00. Styrene weight per-cent = 100.00 (sum of impurities).15. Report15.1 Report the concentration of impurities to the nearest0.001 % and the styrene content to the nearest 0.01 %.16. Precision and Bias516.1 Precisi

42、onThe following criteria should be used tojudge the acceptability (95 % probability level) of resultsobtained by this test method (see Practice E691).16.1.1 The criteria presented in Table 3 and Table 4 werederived from a Interlaboratory Study (ILS) among six labora-tories. The data were run on two

43、days using different operators.16.1.2 The criteria and precision data presented in Table 5were derived from a commercial Proficiency Testing schemeperformed during the years 1997 through 2014 (no formal PTreport available, however data are available to ASTM).16.2 Intermediate Precision (formerly cal

44、ledRepeatability)Results in the same laboratory should not beconsidered suspect unless they differ by more than the normalamount shown in Table 3 and Table 4.16.3 ReproducibilityThe results by each of two laborato-ries should not be considered suspect unless they differ bymore than the amount shown

45、in Table 3, Table 4 and Table 5.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D16-1031. ContactASTM CustomerService at serviceastm.org.D5135 161316.4 BiasBias of this test method for the analysis ofstyrene has not been determi

46、ned because no acceptable refer-ence material is available.17. Quality Guidelines17.1 Laboratories shall have a quality control system inplace.17.1.1 Confirm the performance of the test instrument ortest method by analyzing a quality control sample followingthe guidelines of standard statistical qua

47、lity control practices.17.1.2 A quality control sample is a stable material isolatedfrom the production process and representative of the samplebeing analyzed.17.1.3 When QA/QC protocols are already established inthe testing facility, these protocols are acceptable when theyconfirm the validity of t

48、est results.17.1.4 When there are no QA/QC protocols established inthe testing facility, use the guidelines described in GuideD6809 or similar statistical quality control practices.18. Keywords18.1 analysis by gas chromatography; impurities in styrene;purity of styrene; styrene; styrene monomerFIG.

49、1 Typical Chromatogram (see Table 2)TABLE 3 ILS Precision for Styrene and Impurities at StatedLevelsComponentConcentration,weight %IntermediatePrecision,weight %Reproducibility,weight %Styrene 99.74 0.017 0.054-methylstyrene 0.028 0.001 0.004Isopropylbenzene 0.008 0.001 0.001n-propylbenzene 0.004 0.0003 0.001m- and p-ethyltoluene 0.014 0.001 0.005p, m-xylene 0.125 0.005 0.007o-xylene 0.030 0.001 0.042 Editorially corrected.TABLE 4 ILS Precision for High Purity Styrene and Impurities atStated LevelsComponentConcentration,weight %Interme

copyright@ 2008-2019 麦多课文库(www.mydoc123.com)网站版权所有
备案/许可证编号:苏ICP备17064731号-1