欢迎来到麦多课文档分享! | 帮助中心 海量文档,免费浏览,给你所需,享你所想!
麦多课文档分享
全部分类
  • 标准规范>
  • 教学课件>
  • 考试资料>
  • 办公文档>
  • 学术论文>
  • 行业资料>
  • 易语言源码>
  • ImageVerifierCode 换一换
    首页 麦多课文档分享 > 资源分类 > PDF文档下载
    分享到微信 分享到微博 分享到QQ空间

    UOP 863-2001 TRACE DESORBENT IN C10-C18 MOLEX PRODUCTS BY GC.pdf

    • 资源ID:1074556       资源大小:160.87KB        全文页数:6页
    • 资源格式: PDF        下载积分:10000积分
    快捷下载 游客一键下载
    账号登录下载
    微信登录下载
    二维码
    微信扫一扫登录
    下载资源需要10000积分(如需开发票,请勿充值!)
    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)。
    如需开发票,请勿充值!如填写123,账号就是123,密码也是123。
    支付方式: 支付宝扫码支付    微信扫码支付   
    验证码:   换一换

    加入VIP,交流精品资源
     
    账号:
    密码:
    验证码:   换一换
      忘记密码?
        
    友情提示
    2、PDF文件下载后,可能会被浏览器默认打开,此种情况可以点击浏览器菜单,保存网页到桌面,就可以正常下载了。
    3、本站不支持迅雷下载,请使用电脑自带的IE浏览器,或者360浏览器、谷歌浏览器下载即可。
    4、本站资源下载后的文档和图纸-无水印,预览文档经过压缩,下载后原文更清晰。
    5、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。

    UOP 863-2001 TRACE DESORBENT IN C10-C18 MOLEX PRODUCTS BY GC.pdf

    1、TRACE DESORBENT IN C10-C18MOLEX PRODUCTS BY GCUOP Method 863-01SCOPEMolexis an adsorptive separation process that separates normal paraffins from branched chain andcyclic hydrocarbons.This method is for determining trace amounts of Molex desorbent (n-pentane, isooctane, p-xylene) in C10-C18Molex pro

    2、ducts. The lower limit of detection for n-pentane and isooctane is 5 mass-ppm. Early elutingMolex product may cause interference at the p-xylene site. Therefore, the lower limit of detection for p-xylene can be as high as 50 mass-ppm.OUTLINE OF METHODA repeatable sample volume is injected into a gas

    3、 chromatograph that is equipped with a fused silicacapillary column internally coated with dimethyl polysiloxane, and a flame ionization detector. Theconcentrations of the desorbent components are determined by the external standard method of quantitation,wherein, the peak areas of the desorbent com

    4、ponents in the sample are compared to the peak areas ofdesorbent components in a calibration blend.APPARATUSReferences to catalog numbers and suppliers are included as a convenience to the method user. Othersuppliers may be used.Balance, readability 0.1-mgChromatographic column, 50 m of 0.20-mm ID f

    5、used silica capillary, internally coated to a filmthickness of 0.5-m with cross-linked dimethyl polysiloxane, Agilent Technologies, Cat. No. 19091-SGas chromatograph, capable of temperature ramping, built for capillary column chromatography utilizinga glass injection port insert, and equipped with a

    6、 flame ionization detector that will give a minimumpeak height response of 10 times the background noise for 5 mass-ppm isooctane when operated at therecommended conditions. Agilent Technologies, Model 6890IT IS THE USERS RESPONSIBILITY TO ESTABLISH APPROPRIATE PRECAUTIONARY PRACTICES AND TODETERMIN

    7、E THE APPLICABILITY OF REGULATORY LIMITATIONS PRIOR TO USE. EFFECTIVE HEALTH ANDSAFETY PRACTICES ARE TO BE FOLLOWED WHEN UTILIZING THIS PROCEDURE. FAILURE TO UTILIZE THISPROCEDURE IN THE MANNER PRESCRIBED HEREIN CAN BE HAZARDOUS. MATERIAL SAFETY DATA SHEETS(MSDS) OR EXPERIMENTAL MATERIAL SAFETY DATA

    8、 SHEETS (EMSDS) FOR ALL OF THE MATERIALS USED INTHIS PROCEDURE SHOULD BE REVIEWED FOR SELECTION OF THE APPROPRIATE PERSONAL PROTECTIONEQUIPMENT (PPE). COPYRIGHT 1985, 2001 UOP LLCALL RIGHTS RESERVEDUOP Methods are available through ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshoh

    9、ocken PA 19428-2959,United States. The Methods may be obtained through the ASTM website, www.astm.org, or by contacting Customer Service atserviceastm.org, 610.832.9555 FAX, or 610.832.9585 PHONE2 of 6863-01Gas purifier, hydrogen, used to remove oxygen from the carrier gas, Mat/Sen, Fisher Scientifi

    10、c, Cat. No.P200-1Integrator, electronic, for obtaining peak areas, ChemStation, Agilent TechnologiesLeak detector, gas, Alltech Associates, Cat. No. 21-250Recorder (optional), used to supplement integrator plotRegulator, air, two-stage, high purity, Matheson Gas Products, Model 3122-590Regulator, he

    11、lium, two-stage, high purity, Matheson Gas Products, Model 3122-580Regulator, hydrogen, two-stage, high purity, Matheson Gas Products, Model 3122-350Sample injector, syringe or injector capable of injecting a reproducible 2-L volume of sample. Use of anautomatic injection system (autosampler) is str

    12、ongly recommended, Agilent Technologies, Model 7683REAGENTS AND MATERIALSReferences to catalog numbers and suppliers are included as a convenience to the method user. Othersuppliers may be used.Air, zero-gas, total hydrocarbons less than 2 ppm as methaneHelium, zero-gas, total hydrocarbons less than

    13、 0.5 ppm as methaneHydrogen, zero-gas, 99.95% minimum purity, total hydrocarbons less than 0.5 ppm as methaneIsooctane (2,2,4-trimethylpentane), 99% minimum purity, Acros Organics, Cat. No. 42456-5000n-Undecane, 99% minimum purity, Acros Organics, Cat. No. 14066-5000p-Xylene, 99% minimum purity, Acr

    14、os Organics, Cat. No.15877-5000PROCEDUREChromatographic Technique1. Install the gas purifier in the supply line between the carrier gas source and the carrier gas inlet on thegas chromatograph Column life is significantly reduced if a gas purifier is not used.2. Install the column in the gas chromat

    15、ograph. CAUTION: Hydrogen gas leakage into the confined volume of the column oven can cause a violentexplosion. It is, therefore, mandatory to check for leaks each time a connection is made and periodicallythereafter.3. Establish the recommended operating conditions as given in Table 1. Other condit

    16、ions may be used provided they produce the required sensitivity and chromatographicseparations equivalent to those shown in the Typical Chromatogram (Figure).3 of 6863-014. Program the column oven to 250C and maintain this temperature until a stable baseline has beenobtained at the required sensitiv

    17、ity.5 Cool the column oven to a stabilized 50C.Table 1Recommended Operating ConditionsCarrier gas hydrogenColumn head pressure 100 C,Constant pressure 105 kPa gauge (15 psig)Equivalent flow 0.7 mL/minEquivalent linear velocity 25 cm/secInjection port temperature 250 CColumn temperature programInitia

    18、l temperature 50 CInitial time 0 minProgramming rate A 4 C/minIntermediate temperature 120 CIntermediate time 0 minProgramming rate B 20 C/minFinal temperature 230 CFinal time 38 minDetectorTemperature 275 CHydrogen flow rate* 30 mL/minAir flow rate* 400 mL/minMakeup helium flow rate* 30 mL/minSampl

    19、e size2.0 L_* Consult the manufacturers instrument manual for suggested flow rates.6. Inject 2.0 L of sample into the gas chromatograph and start the integrator and the column ovenprogramming sequence.7. Identify the desorbent components using the Typical Chromatogram as a guide (Figure).Calibration

    20、Quantitative results are based on the injection of a repeatable volume of a sample and of a referenceblend. Absolute response factors are used to relate the peak area of the desorbent components to mass-ppm.Since n-pentane is quite volatile, and it has about the same detector response as isooctane,

    21、the isooctane inthe blend is used to calibrate for both n-pentane and isooctane in the sample; p-xylene in the blendcalibrates for p-xylene in the sample.4 of 6863-011. Prepare, following ASTM Method D 4307, one or more calibration blends containing isooctane andp-xylene in n-undecane at the concent

    22、rations expected in the samples.2. Analyze the blend in triplicate as described under Steps 6 and 7, Chromatographic Technique.Average the peak areas for each desorbent component from the three runs. The peak areas from each of the three runs should not deviate from the average by more than 2%. Ifgr

    23、eater deviation is found, check equipment and technique, and make further runs until the requiredrepeatability is obtained.3. Calculate the response factor for each desorbent component as follows:MFP= (1)where:F = absolute response factor for desorbent componentM = concentration of desorbent compone

    24、nt in the blend, mass-ppmP = average peak area for the desorbent component in the blendCALCULATIONSCalculate the concentration of the total amount of each desorbent component in the sample as follows:Molex desorbent component, mass-ppm = FS (2)where:F = absolute response factor for the component (us

    25、e the isooctane factor for n-pentane)S = peak area for the component in the sampleReport results to the nearest 1 mass-ppm.PRECISIONThe GC used to perform the precision study was equipped with an autoinjector. Precision statements weredetermined using UOP Method 999.ASTM and UOP RepeatabilityA neste

    26、d design was carried out for determining Molex desorbent components in Molex product with twoanalysts in one laboratory. Each analyst carried out tests on two separate days, performing two tests eachday for each sample. The total number of tests for each constituent was 16. The precision data aresum

    27、marized in Table 2. Two tests performed by the same analyst on the same day should not differ by morethan the ASTM allowable difference with 95% confidence. Two tests performed in one laboratory bydifferent analysts on different days should not differ by more than the UOP allowable difference with 9

    28、5%confidence.The data in Table 2 are a short-term estimate of repeatability. When the test is run routinely, a controlstandard and chart should be used to develop a better estimate of the long-term repeatability.5 of 6863-01ReproducibilityThere is insufficient data to calculate the reproducibility o

    29、f the test at this time.Table 2ASTM and UOP Repeatability, mass-ppmASTM Repeatability UOP RepeatabilityCompoundMeanConc.Within-Day esdAllowableDifferenceWithin-Lab esdAllowableDifferenceSample 1n-Pentane 8 0.32 1.3 0.29 1.1Isooctane 8 0.25 1.0 0.26 1.0p-Xylene 9 0.50 2.0 0.50 2.0Sample 2n-Pentane 73

    30、 0.38 1.5 1.0 5.Isooctane 73 0.56 2.2 0.56 2.2p-Xylene 77 0.52 2.1 0.52 2.0TIME FOR ANALYSISThe elapsed time for one analysis is 1.3 hour. The labor requirement is 0.3 hour.REFERENCESASTM Method D 4307, www.astm.orgUOP Method 999, “Precision Statements in UOP Methods”SUGGESTED SUPPLIERSAcros Organic

    31、s, Fisher Scientific, 711 Forbes Ave., Pittsburgh, PA 15219 (412-562-8300)Agilent Technologies, 2850 Centerville Rd., Wilmington, DE 19808-1610 (302-633-8000)Alltech Associates, Inc., 2051 Waukegan Rd., Deerfield, IL 60015 (847-948-8600) Fisher Scientific, 711 Forbes Ave., Pittsburgh, PA 15219 (412-562-8300) Matheson Gas Products, P.O. Box 85, East Rutherford, NJ 07073 (201-933-2400)6 of 6863-01FigureTypical ChromatogramMolex Product


    注意事项

    本文(UOP 863-2001 TRACE DESORBENT IN C10-C18 MOLEX PRODUCTS BY GC.pdf)为本站会员(tireattitude366)主动上传,麦多课文档分享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档分享(点击联系客服),我们立即给予删除!




    关于我们 - 网站声明 - 网站地图 - 资源地图 - 友情链接 - 网站客服 - 联系我们

    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 

    收起
    展开