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1、BRITISH STANDARD BS ISO 7270-2:2005 Rubber Analysis by pyrolytic gas-chromatographic methods Part 2: Determination of styrene/butadiene/isoprene ratio ICS 83.060 ? Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:48:11 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 7270-2:2005 This Briti
2、sh Standard was published under the authority of the Standards Policy and Strategy Committee on 13 April 2005 BSI 13 April 2005 ISBN 0 580 45825 3 National foreword This British Standard reproduces verbatim ISO 7270-2:2005 and implements it as the UK national standard. The UK participation in its pr
3、eparation was entrusted to Technical Committee PRI/23, Test methods for rubber and non-black compounding ingredients, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which imple
4、ment international publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purpor
5、t to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee
6、any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to iv,
7、pages 1 to 9 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:48:11 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Referen
8、ce number ISO 7270-2:2005(E) INTERNATIONAL STANDARD ISO 7270-2 First edition 2005-03-15 Rubber Analysis by pyrolytic gas-chromatographic methods Part 2: Determination of styrene/butadiene/isoprene ratio Caoutchouc Mthodes danalyse par pyrolyse et chromatographie en phase gazeuse Partie 2: Dterminati
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14、+ 9 74 E-mail coirypthgiso.o gr We bwww.is.o gro Pulbisdehi n Switlrez dna ii BS ISO 72702:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:48:11 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iii Contents Page Forewordiv 1 Scope1 2 Normative references .1 3 Principle.1 4 Reagents2 5 Appar
15、atus.2 5.1 Extraction apparatus 2 5.2 Pyrolysis/chromatography system .2 6 Procedure.3 6.1 Preparation of calibration curves3 6.2 Analysis of test samples of unknown composition7 7 Interpretation of results7 8 Precision7 9 Test report9 BS ISO 72702:2005 Licensed Copy: sheffieldun sheffieldun, na, Mo
16、n Nov 27 07:48:11 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical co
17、mmittees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with th
18、e International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft Internati
19、onal 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. Attention is drawn to the possibility that some of the elements of this document may be
20、the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 7270-2 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 2, Testing and analysis. ISO 7270 consists of the following parts, under the general ti
21、tle Rubber Analysis by pyrolytic gas- chromatographic methods: Part 1: Identification of polymers (single polymers and polymer blends) Part 2: Determination of styrene/butadiene/isoprene ratio BS ISO 72702:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:48:11 GMT+00:00 2006, Uncontrol
22、led Copy, (c) BSI 1 Rubber Analysis by pyrolytic gas-chromatographic methods Part 2: Determination of styrene/butadiene/isoprene ratio WARNING Persons using this part of ISO 7270 should be familiar with normal laboratory practice. This part of ISO 7270 does not purport to address all of the safety p
23、roblems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions. 1 Scope This part of ISO 7270 specifies the principles and procedures for determining, by pyrolysis an
24、d subsequent gas chromatography, the styrene (STY)/butadiene (BD)/isoprene (IP) ratio in copolymers, or blends of homopolymers and/or copolymers, in raw rubbers or vulcanized or unvulcanized compounds. It is applicable to copolymers/terpolymers consisting of styrene, butadiene and isoprene, and blen
25、ds of these polymers. NOTE The use of this part of ISO 7270 pre-supposes sufficient working knowledge of the principles and techniques of gas chromatography for the analyst to perform the operations described and interpret the results correctly. 2 Normative references The following referenced docume
26、nts are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 1407, Rubber Determination of solvent extract 3 Principle Calibration curves
27、 are first prepared by pyrolysing samples with known STY/BD/IP ratios and analysing the pyrolysis products by gas chromatography to determine the percentage content of each component (STY, BD and IP), relative to the total of the three components, in the pyrolysis products. Samples of unknown compos
28、ition are then pyrolysed and the pyrolysis products analysed under the same conditions. The STY/BD/IP ratio in the original sample is determined from the calibration curves. BS ISO 72702:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:48:11 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 2
29、 4 Reagents All reagents shall be of analytical grade. 4.1 Solvents for extraction purposes The following solvents are suitable (see 6.1.1): acetone; methanol; methylethylketone. 4.2 Carrier gas nitrogen; helium. 4.3 Gas for flame-ionization detector: hydrogen plus purified compressed air. 5 Apparat
30、us 5.1 Extraction apparatus As specified in ISO 1407. 5.2 Pyrolysis/chromatography system 5.2.1 General The apparatus utilized to obtain pyrograms consists of four parts: the pyrolysis device, the gas chromatograph, the gas-chromatographic column and the data-handling equipment. 5.2.2 Pyrolysis devi
31、ce The following types of pyrolysis device are suitable: micro-furnace pyrolyser; Curie-point pyrolyser; platinum-filament pyrolyser. 5.2.3 Gas chromatograph A wide variety of gas chromatographs using either a flame-ionization detector (FID) or a thermal-conductivity detector (TCD) are suitable for
32、use in this part of ISO 7270. An FID is preferable for use with capillary columns. 5.2.4 Chromatographic columns A variety of column lengths and diameters and stationary and liquid phases are suitable for use in this part of ISO 7270, the main requirement being good resolution of the volatile pyroly
33、sis products styrene, butadiene and isoprene. BS ISO 72702:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:48:11 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 3 NOTE 1 Capillary columns with good separation efficiency are suitable, but not essential. NOTE 2 Capillary columns containing n
34、on-polar polydimethylsiloxanes and partially modified (diphenyl-, cyanopropylphenyl- or other) semi-polar silicones are suitable. 5.2.5 Data-handling equipment A recorder, an integrator or a computer data-analysis system may be used. 6 Procedure 6.1 Preparation of calibration curves 6.1.1 Prepare ca
35、libration samples of known compositions close to that assumed for the unknown (test) sample. 6.1.2 Take a test portion of mass appropriate to the apparatus used. Generally, this will be between 0,1 mg and 5 mg. For good reproducibility, the size of the test portion should be as small as practicable.
36、 6.1.3 Place the test portion in the pyrolysis device and pyrolyse it. An appropriate pyrolysis temperature is 500 C to 600 C for a micro-furnace or Curie-point pyrolyser, and 600 C to 750 C for a platinum-filament pyrolyser. Use the same pyrolysis temperature for all of a series of related measurem
37、ents. The gas-chromatographic conditions will depend on the column used. Typical operating conditions are given in Tables 1 to 3 and examples of chromatograms obtained using each set of conditions are given in Figures 1 to 3. NOTE The type of pyrolysis device used and the pyrolysis temperature will
38、affect the results. 6.1.4 Record the peak areas X, Y and Z for STY, BD and IP, respectively, in the pyrolysis products and calculate, for each of these components, the percentage peak area relative to their total, as follows: percentage peak area for styrene X/(X + Y + Z) 100 percentage peak area fo
39、r butadiene Y/(X + Y + Z) 100 percentage peak area for isoprene Z/(X + Y + Z) 100 6.1.5 For each of the three components STY, BD and IP, prepare a calibration curve by plotting the known percentage of the component (relative to the total of the three) in the unpyrolysed sample against the percentage
40、 peak area for the component in the pyrolysis products. An example of one such calibration curve (for butadiene) is shown in Figure 4. NOTE 1 When using an ordinary (30 m) length of capillary column, it is difficult to completely separate isobutene from butadiene. In pyrolytic gas-chromatographic me
41、thods, isobutene, which is a decomposition product of rubber containing the isoprene unit, is detected in the near retention range of butadiene. It is possible, however, to discriminate between isoprene and butadiene even without complete separation by means of the calibration curves. NOTE 2 A longe
42、r (60 m) capillary column with a thicker film affords better separation of these components. BS ISO 72702:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:48:11 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 4 Table 1 Recommended operating conditions for micro-furnace pyrolysis followed by
43、 chromatography with a 30 m capillary column Pyrolysis Device Micro-furnace Pyrolysis temperature 550 C Gas-chromatographic column Liquid phase 5 % diphenyldimethylpolysiloxane Film thickness 1,0 m Column diameter 0,25 mm ID Column length 30 m Chromatographic conditions Carrier gas and flow rate Hel
44、ium, 0,8 ml/min Injector temperature 250 C Type of detector FID Detector temperature 300 C Temperature programme Isothermal for 2 min at 50 C then 20 C/min from 50 C to 280 C then isothermal for 10 min at 280 C Table 2 Recommended operating conditions for micro-furnace pyrolysis followed by chromato
45、graphy with a 60 m capillary column Pyrolysis Device Micro-furnace Pyrolysis temperature 550 C Gas-chromatographic column Liquid phase 5 % diphenyldimethylpolysiloxane Film thickness 1,0 m Column diameter 0,25 mm ID Column length 60 m Chromatographic conditions Carrier gas and flow rate Helium, 0,8
46、ml/min Injector temperature 250 C Type of detector FID Detector temperature 300 C Temperature programme Isothermal for 7 min at 50 C then 10 C/min from 50 C to 280 C then isothermal for 10 min at 280 C BS ISO 72702:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:48:11 GMT+00:00 2006,
47、Uncontrolled Copy, (c) BSI 5 Table 3 Recommended operating conditions for Curie-point pyrolysis followed by chromatography with a packed column Pyrolysis Device Curie-point pyrolyser Pyrolysis temperature 590 C (3 s) Gas-chromatographic column Liquid phase 20 % silicone 710/Chromosorb W60 to W80 mes
48、h Column diameter/material 3 mm ID/stainless steel Column length 3 m Chromatographic conditions Carrier gas Helium Type of detector FID Temperature programme Isothermal for 2 min at 50 C then 10 C/min from 50 C to 220 C then isothermal for 10 min at 220 C Key X time (minutes) 1 butadiene 2 isoprene
49、3 styrene Figure 1 Example of chromatogram obtained with 30 m capillary column BS ISO 72702:2005 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:48:11 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 6 Key 1 butadiene 2 isoprene 3 styrene Figure 2 Example of chromatogram obtained with 60 m capillary column Key X time (minutes) 1 butadiene 2 isoprene 3 styrene Figure 3 Example of chromatogram obtained