ISO INTERNATIONAL STANDARD 12965 First edition 2000-09-15 Butadiene rubber Determination of microstructure by infra-red spectrometry Caoutchouc butadiene-Détermination de la microstructure par spectrometrie a infrarouge Reference number ISO 12965:2000(E) ISO ISO 12965:2000(E) ii ISO 12965:2000(E) BSI Contents Page , Uncontrolled Copy, (c) I Foreword iv 1 Scope 2 Normative references 3 Principle.. 4 Reagent.. 5 Apparatus. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:09 GMT+00:00 2006, 9 Sampling.. 7 Procedure. 8 Precision 9 Test report ii ISO 12965:2000(E) Foreword IsO (the International Organization for Standardization) is a worldwide federation of national standards bodies (isO Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote 20 patent rights. IsO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 12965 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products. Subcommittee SC 2, Testing and analyses. iv ISO 12965:2000(E) INTERNATIONAL STANDARD Butadiene rubber Determination of microstructure by infra-red spectrometry WARNING - Persons using this International Standard should be familiar with normal laboratory practice. the responsibility of the user to establish appropriate safety and health practices and to ensure compliance withany national regulatory conditions. 1 Scope This International Standard specifies a method for the determination of the microstructure of butadiene rubber (BR) by infra-red spectrometry using a cast film. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications donotapply.However,partiestoagreementsbasedonthisInternationalStandardare encouragedto undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. IsO 1407:1992, Rubber — Determination of solvent extract IsO 1795:2000, Rubber, raw natural and raw synthetic - Sampling and further preparative procedures. ISO/TR 9272:1986, Rubber and rubber products Determination of precision for test method standards. 3 Principle 3.1 A small quantity of extracted rubber is dissolved in methylene chloride and cast on a salt plate 3.2 the cis, trans and vinyl contents are calculated. 4 Reagent 4.1 Methylene chloride. 5 Apparatus 5.1 Double-beam infrared spectrophotometer or Fourier-transform infra-red (FTIR) spectrophotometer, axis over the spectral region of 2 000 cm-1 to 600 cm-1. 1 ISO 12965:2000(E) 5.2 Salt plate. 5.3 Balance, weighing to 0,1 mg. BSI 5.4 Vacuum oven, operating at 50 °C to 60 °C. Copy, 6 Sampling Uncontrolled Sample the raw rubber in accordance with ISO 1795. 7 Procedure 7.1 Mill the test sample to as thin a sheet as possible. Extract the rubber in accordance with IsO 1407 using 2006, ethanol/toluene azeotrope (ETA). Dry the extracted rubber under vacuum in the oven at 50 °C to 60 °C. 7.2 Take approximately 100 mg of extracted sample and dissolve it in around 20 ml of methylene chloride. If ge GMT+00:00 is present, filter the solution. 7.3 Ensure that the salt plate is levelled horizontally before the film is cast. Place 3 or 4 drops of the solution on 7.4 Check that the transmittance over the measurement range lies between 50 % and 30 %. If grossly outside 07:38:09 these limits, clean the salt plate and repeat step 7.3 with more or less solution. 7.5 When 7.4 is satisfied, scan over the range 2000 cm-1 to 600 cm-1. 7.6 Nov medium-, low- and high-cis polybutadiene). 7.7 Measure the absorbances at 965 cm-1 (A