ASTM E1784-1997(2002) Standard Test Method for Total Peroxides in Acrylonitrile《丙烯腈中过氧化物总含量的标准试验方法》.pdf
《ASTM E1784-1997(2002) Standard Test Method for Total Peroxides in Acrylonitrile《丙烯腈中过氧化物总含量的标准试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM E1784-1997(2002) Standard Test Method for Total Peroxides in Acrylonitrile《丙烯腈中过氧化物总含量的标准试验方法》.pdf(3页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: E 1784 97 (Reapproved 2002)Standard Test Method forTotal Peroxides in Acrylonitrile1This standard is issued under the fixed designation E 1784; 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. Scope1.1 This test method describes a procedure for determiningthe total peroxide content of acrylonitrile in the range of 0.1 to0.6 mg H2O2
3、/kg acrylonitrile (ppm). Peroxides are an undesir-able impurity in acrylonitrile.1.2 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 practices and de
4、termine the applica-bility of regulatory limitations prior to use. Specific hazardstatements are given in Section 7.1.3 Review the current Material Safety Data Sheets (MSDS)for detailed information concerning toxicity, first aid proce-dures, and safety precautions.2. Referenced Documents2.1 ASTM Sta
5、ndards:D 1193 Specification for Reagent Water2E 60 Practice for Analysis of Metals, Ores, and RelatedMaterials by Molecular Absorption Spectrometry3E 180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial Chemicals4E 200 Practice for Preparation, Standardiza
6、tion, and Stor-age of Standard and Reagent Solutions for ChemicalAnalysis43. Summary of Test Method3.1 Peroxides in the sample react with potassium iodide toform the yellow I3ion. The intensity of the color, which isproportional to the concentration of the I3ion, is measured at365 nm. Results are ex
7、pressed as total peroxides as H2O2.4. Significance and Use4.1 This test method provides for the determination of totalperoxide in acrylonitrile in the range of 0.1 to 0.6 ppm. Onlyperoxides or other oxidants that react under the conditions ofthis test method are measured.5. Apparatus5.1 Spectrophoto
8、meter, capable of measuring at 365 nm,5.2 Absorption Cells, 1-cm, borosilicate, matched, and5.3 Buret, 25-mL capacity.NOTE 1Photometers and photometric practice described in this testmethod shall conform to Practice E 60.6. Reagents6.1 Purity of ReagentsUnless otherwise indicated, allreagents shall
9、conform to the specifications of the Committeeon Analytical Reagents of the American Chemical Societywhere such specifications are available.5Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of th
10、e determination.6.2 Purity of WaterUnless otherwise indicated, referencesto water mean Type II or Type III reagent water conforming toSpecification D 1193.6.3 Potassium Iodide.6.4 Acetic Anhydride.6.5 Hydrogen Peroxide, 30 %.6.6 Acrylonitrile, Peroxide FreePrepare by passing acry-lonitrile througha2
11、cm3 40 cm glass column packed with 50mL of activated alumina or acid form ion exchange resin.61This test method is under the jurisdiction of ASTM Committee E15 onIndustrial and Specialty Chemicals and is the direct responsibility of SubcommitteeE15.02 on Product Standards.Current edition approved Oc
12、t. 10, 2002. Published February 2003. Originallyapproved in 1996. Last previous edition approved in 1997 as E 1784 97.2Annual Book of ASTM Standards, Vol 11.01.3Annual Book of ASTM Standards, Vol 03.05.4Annual Book of ASTM Standards, Vol 15.05.5Reagent Chemicals, American Chemical Society Specificat
13、ions, 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 Convention,
14、 Inc. (USPC), Rockville,MD.6Rohm and Haas Amberlyst 15 has been found to be suitable or an equivalentresin may be used.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Flow through the column should be approximately 8 to 10 bedvolumes
15、 per h. The absorbance obtained by following 9.1through 9.3 should be less than 0.01. Alternative means ofpreparation include extraction with 10 % NaOH followed bydistillation. For the extraction technique, extract 100 mL ofacrylonitrile with 50 mL of 10 % NaOH, follow with tripleextraction with wat
16、er. The volume of peroxide free acryloni-trile required for calibration is 500 mL.6.7 Sulfuric Acid Solution, 12 NMeasure 360 mL ofconcentrated sulfuric acid (H2SO4sp gr 1.84) into a 500-mLgraduated cylinder and slowly add it to 400 mL of water in a1000-mL beaker while stirring. Rinse the cylinder w
17、ith waterand add the washings to the beaker with water. Mix theacid-water mixture, allow to cool, and transfer to a 1-Lvolumetric flask. Dilute to volume with water, mix well, andstore in a closed glass container.6.8 Ammonium Molybdate Solution, 3 %Dissolve 1.5 g ofammonium molybdate, (NH4)6Mo7O244H
18、2O in water anddilute to 500 mL. Adjust the pH to 7.0 using 0.01 N NaOH or0.01 N HCl as required.6.9 Sodium Thiosulfate Solution, 0.1 NPrepare and stan-dardize in accordance with Practice E 200.6.10 Starch Indicator Solution, 1 %Prepare in accordancewith Practice E 200.7. Hazards7.1 Acrylonitrile is
19、 potentially hazardous to human health ifnot properly handled. Acrylonitrile is a suspected humancarcinogen. Use acrylonitrile in a well ventilated hood.7.2 Acrylonitrile can contribute to a toxic condition insystems of the human body, from inhalation, swallowing, orcontact with the eyes or skin. Di
20、rect contact with acrylonitrilecan cause skin burns as well.7.3 Acrylonitrile liquid and vapor are readily absorbed intoshoe leather and clothing and will penetrate most rubbers,barrier fabrics, or creams. Contact lenses should not be worn inareas where eye contact with acrylonitrile could occur. Us
21、eimpermeable protective clothing and consult the current MSDSfor recommended materials.8. Standard Solutions and Calibration8.1 Pipet 0.5 mL of 30 % H2O2into a 100-mL volumetricflask, dilute to volume with water, and mix thoroughly. Thisstock peroxide solution contains approximately 0.15 % H2O2.8.2
- 1.请仔细阅读文档,确保文档完整性,对于不预览、不比对内容而直接下载带来的问题本站不予受理。
- 2.下载的文档,不会出现我们的网址水印。
- 3、该文档所得收入(下载+内容+预览)归上传者、原创作者;如果您是本文档原作者,请点此认领!既往收益都归您。
下载文档到电脑,查找使用更方便
5000 积分 0人已下载
下载 | 加入VIP,交流精品资源 |
- 配套讲稿:
如PPT文件的首页显示word图标,表示该PPT已包含配套word讲稿。双击word图标可打开word文档。
- 特殊限制:
部分文档作品中含有的国旗、国徽等图片,仅作为作品整体效果示例展示,禁止商用。设计者仅对作品中独创性部分享有著作权。
- 关 键 词:
- ASTME178419972002STANDARDTESTMETHODFORTOTALPEROXIDESINACRYLONITRILE 丙烯腈 过氧化物 含量 标准 试验 方法 PDF

链接地址:http://www.mydoc123.com/p-529455.html