ASTM_D_3566_-_03_2014.pdf

Designation:D356603(Reapproved 2014)Standard Practice forRubberDetermination of Bromine in the Presence ofChlorine by Oxygen Combustion1This standard is issued under the fixed designation D3566;the number immediately following the designation indicates the year oforiginal adoption or,in the case 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 procedure 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.1.5 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 safetyprecautions are given in Section 7.2.Referenced Documents2.1 ASTM Standards:2E200 Practice for Preparation,Standardization,and Storageof Standard and Reagent Solutions for Chemical AnalysisE443 Test Method for Sulfur in Organic Compounds byOxygen Flask Combustion(Withdrawn 1996)33.Summary of Practice3.1 Samples of rubber,wrapped in filter paper,are burned inan oxygen combustion flask containing an aqueous solution ofhydrogen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 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 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,withSJ35/25 ball-joint stopper,platinum samplecarrier,and pinch clamp.5.2 Infrared 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.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 electrode11and a calomel electrode,in which the potassium chloride1This practice is under the jurisdiction ofASTM Committee D11 on Rubber andis the direct responsibility of Subcommittee D11.11 on Chemical Analysis.Current edition approved July 1,2014.Published November 2014.Originallyapproved in 1977.Last previous edition approved in 2009 as D3566 03(2009).DOI:10.1520/D3566-03R14.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.4Borosilicate 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 comments 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 satisfactory.8The sole source of supply of the apparatus known to the committee at this timeis A.H.Thomas Co.,Philadelphia,PA,Catalog No.6514-F65.9The sole source of supply of the apparatus known to the committee at this timeis A.H.Thomas Co.,Philadelphia,PA,Catalog No.6513-C75.10A.Beckman pH meter Model SS-2 has been found satisfactory.11Coleman Catalog No.3-571 has been found satisfactory.Any equivalent silverelectrode may be used.The electrode should not be coated by the user,especially forTest Method B.It may,however,be polished with a mild abrasive such as powderedkitchen cleanser,so that it is bright and shiny.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 solution has been replaced by a saturated potassium nitratesolution,or equivalent automatic titrator.6.Reagents6.1 Silver Nitrate Solution(0.001 M)must be freshlyprepared.Pipet 10.0 cm3of stan