ASTM D3566-2003(2009) Standard Practice for Rubber&8212 Determination of Bromine in the Presence of Chlorine by Oxygen Combustion《用氧燃烧法测定在氯存在时橡胶中的溴含量的标准实施规程》.pdf
《ASTM D3566-2003(2009) Standard Practice for Rubber&8212 Determination of Bromine in the Presence of Chlorine by Oxygen Combustion《用氧燃烧法测定在氯存在时橡胶中的溴含量的标准实施规程》.pdf》由会员分享,可在线阅读,更多相关《ASTM D3566-2003(2009) Standard Practice for Rubber&8212 Determination of Bromine in the Presence of Chlorine by Oxygen Combustion《用氧燃烧法测定在氯存在时橡胶中的溴含量的标准实施规程》.pdf(3页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D 3566 03 (Reapproved 2009)Standard Practice forRubberDetermination of Bromine in the Presence ofChlorine by Oxygen Combustion1This standard is issued under the fixed designation D 3566; the number immediately following the designation indicates the year oforiginal adoption or, in the c
2、ase of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice covers the determination of bromine andchlorine in rubber.1.2 This procedur
3、e is applicable to raw or cured NR, SBR,BR, IR, IIR, CIIR, BIIR, and EPDM rubbers and blends ofthese.1.3 Iodine interferes, but substances such as Zn2+,S,CN,and (CO3)2do not.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.
4、5 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 determine the applica-bility of regulatory limitations prior to use. Specific safetyp
5、recautions are given in Section 7.2. Referenced Documents2.1 ASTM Standards:2E 200 Practice for Preparation, Standardization, and Stor-age of Standard and Reagent Solutions for ChemicalAnalysisE 443 Test Method for Sulphur in Organic Compounds byOxygen Flask Combustion33. Summary of Practice3.1 Samp
6、les of rubber, wrapped in filter paper, are burned inan oxygen combustion flask containing an aqueous solution ofhydrogen peroxide and sodium bisulfite. The carbon andhydrogen of the organic matter are oxidized. The combustedsolution is titrated directly for bromine and chlorine.4. Significance and
7、Use4.1 This practice outlines a method for the determination ofbromine and chlorine, alone or together.4.2 CIIR and BIIR rubbers contain small amounts of chlo-rine and bromine and CR rubbers contain large amounts ofchlorine. For quality control and research and development, itis sometimes necessary
8、to determine the amount of thesehalogens in rubber. This practice can be used for thesepurposes.5. Apparatus5.1 Oxygen Combustion Flask (Schniger Flask)Achemical-resistant,4thick-walled oxygen combustion flask,51000 cm3, with JS35/25 ball-joint stopper, platinum samplecarrier, and pinch clamp.5.2 In
9、frared Safety Igniter,5,6with cabinet and infrared light(an electrical igniter is also satisfactory).5.3 Magnetic Stirring Bar, covered with a chemical-resistant coating,5,7approximately 25 mm (1 in.) long, withouta spinning ring around the center.5.4 Magnetic Stirrer.1This practice is under the jur
10、isdiction ofASTM Committee D11 on Rubber andis the direct responsibility of Subcommittee D11.11 on Chemical Analysis.Current edition approved Jan. 1, 2009. Published March 2009. Originallyapproved in 1977. Last previous edition approved in 2003 as D 3566 03.2For referenced ASTM standards, visit the
11、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.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.4Borosil
12、icate glass has been found satisfactory.5The sole source of supply of the apparatus known to the committee at this timeis A. H. Thomas Co., Philadelphia, PA, Catalog No. 6514-F20. If you are aware ofalternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your commen
13、ts will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.6The sole source of supply of the apparatus known to the committee at this timeis A. H. Thomas Co., Philadelphia, PA, Catalog No. 6516-G10.7Polytetrafluoroethylene has been found satisfacto
14、ry.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.5 Filter Paper, 30 by 30 mm, with a 35-mm extension,black5,8for infrared or white5,9for electrical ignition.5.6 pH Meter,10equipped with a billet-type silver elec-trode11and a calo
15、mel electrode, in which the potassiumchloride solution has been replaced by a saturated potassiumnitrate solution, or equivalent automatic titrator.6. Reagents6.1 Silver Nitrate Solution (0.001 M) must be freshly pre-pared. Pipet 10.0 cm3of standard120.1 M silver nitrate solutioninto a 1-dm3volumetr
16、ic flask. Dilute to volume. Protect fromlight. Determine its molarity by titrating an accurately weighedsample of the reagent grade KCl or NaCl. Calculate themolarity as follows:Molarity 5 A 3 1000/B 3 C! (1)where:A = grams of chloride weighed,B = molecular mass of chloride used, andC = titration vo
17、lume, cm3.6.2 Sodium Bisulfite, 35 % in water,6.3 Hydrogen Peroxide, 3 % solution,6.4 Nitric Acid (6M).6.5 Aluminum Nitrate,6.6 Isopropyl Alcohol,6.7 Methyl Orange Indicator (1 % solution in methyl alco-hol), and6.8 Oxygen in Compressed Gas Cylinder.7. Safety Precautions7.1 The following safety prec
18、autions must be observed inthe combustion of rubber samples:7.1.1 The flask shall not contain residues of organic solventsor vapor, which could cause an explosion. Any such solventsused for cleaning the flask should be rinsed out repeatedly withwater.7.1.2 The pressure generated by the rapid combust
19、ion couldcause the flask to explode. Therefore, combustion shall takeplace in a safety chamber with the door locked or behind asafety shield or hood shield (preferably in a safety chamber thatis behind a shield); the hands and face shall be withdrawnbehind a screen before the flame reaches the sampl
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