1、Designation:D356603(Reapproved 2018)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
2、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 applicab
3、le 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 n
4、ot 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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.Specific safety precautions
5、are given in Section 7.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recom-mendations issued by the World Trade Organizatio
6、n TechnicalBarriers to Trade(TBT)Committee.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and Reagent Solutions for Chemical AnalysisE443 Test Method for Sulfur in Organic Compounds byOxygen Flask Combustion(Withdrawn 1996)33.Summary of
7、 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.Signi
8、ficance 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 n
9、ecessary 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
10、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
11、 a 35-mm extension,black5,8for infrared or white5,9for electrical ignition.1This practice is under the jurisdiction ofASTM Committee D11 on Rubber andRubber-like Materials and is the direct responsibility of Subcommittee D11.11 onChemical Analysis.Current edition approved Nov.1,2018.Published Decemb
12、er 2018.Originallyapproved in 1977.Last previous edition approved in 2014 as D3566 03(2014).DOI:10.1520/D3566-03R18.2For 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 s
13、tandards 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,Catal
14、og 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
15、 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.Copyright ASTM International,100 Barr
16、 Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.1 5.6 pH Meter,10equipped with a billet-type silver electrode11and a calomel electrode,in which the potassium chlor
