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1、 Reference number ISO 4650:2005(E) ISO 2005 INTERNATIONAL STANDARD ISO 4650 Second edition 2005-09-15 Rubber Identification Infrared spectrometric method Caoutchouc Identification Mthode spectromtrique dans linfrarouge ISO 4650:2005(E) PDF disclaimer This PDF file may contain embedded typefaces. In
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6、211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2005 All rights reserved -,-,- ISO 4650:2005(E) ISO 2005 All rights reserved iii Contents Page Foreword. v 1 Scope . 1 2 Normative references. 1 3 Principle. 1 4 Types o
7、f rubber. 1 4.1 General. 1 4.2 Exceptions for blends 3 4.3 Reference spectra. 3 5 Reagents 3 6 Apparatus 4 7 Procedure 5 7.1 Procedure for raw rubber films moulded or cast from solution 5 7.2 Procedure for raw rubbers, vulcanizates and films obtained from pyrolysate 5 7.3 Procedure for vulcanized ru
8、bber film obtained after evaporation of the solution solvent. 6 8 Interpretation of spectra 7 8.1 Reference spectra. 7 8.2 Tables of diagnostic absorptions . 8 9 Test report . 8 Annex A (informative) Absorption characteristics and reference spectra. 9 Table A.1 Types of rubber and corresponding refe
9、rence spectra. 10 Table A.2 Acrylic rubber (ACM). 11 Table A.3 Chloropolyethylene (CM). 12 Table A.4 Chlorosulfonylpolyethylene (CSM) 13 Table A.6 Fluorocarbon rubber (FKM) 15 Table A.7 Polychloromethyloxirane (CO) . 16 Table A.8 Copolymer of ethylene oxide and chloromethyloxirane (ECO). 17 Table A.
10、9 Polydimethylsiloxane (MQ). 18 Table A.10 Butadiene rubber (BR). 19 Table A.11 Chloroprene rubber (CR). 21 Table A.12 Isobutene-isoprene rubber (IIR) 22 Table A.13 Bromo-isobutene-isoprene rubber (BIIR) 23 Table A.14 Natural rubber (NR) 24 Table A.15 Isoprene rubber (IR). 25 Table A.16 Acrylonitril
11、e-butadiene rubber (NBR) 27 Table A.17 Hydrogenated acrylonitrile-butadiene rubber (HNBR). 28 Table A.18 Carboxylic-acrylonitrile-butadiene rubber (XNBR). 29 Table A.19 Styrene butadiene rubber (SBR) 30 -,-,- ISO 4650:2005(E) iv ISO 2005 All rights reserved Table A.21 Block copolymer of styrene and
12、butadiene (TPS-SBS)34 Table A.22 Polystyrene-poly(ethylene-butylene)-polystyrene (TPS-SEBS) 35 Table A.23 Block copolymer of styrene and isoprene (TPS-SIS).36 Table A.24 Polystyrene-poly(ethylene-propylene)-polystyrene (TPS-SEPS)37 Table A.25 Syndiotactic poly(1,2-butadiene) (TPZ)38 Table A.26 Copol
13、yester TPE with a soft segment with ester and ether linkages (TPC-EE) 39 Bibliography .40 -,-,- ISO 4650:2005(E) ISO 2005 All rights reserved v Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of pr
14、eparing International Standards is normally carried out through ISO technical committees. 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, i
15、n liaison with ISO, also take part in the work. ISO collaborates closely with the 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 tas
16、k of technical committees is to prepare International Standards. 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. Attentio
17、n is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 4650 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 2, Testin
18、g and analysis. This second edition cancels and replaces the first edition (ISO 4650:1984), which has been technically revised. -,-,- -,-,- INTERNATIONAL STANDARD ISO 4650:2005(E) ISO 2005 All rights reserved 1 Rubber Identification Infrared spectrometric method 1 Scope This International Standard s
19、pecifies a method for the identification of rubbers, including thermoplastic elastomers, either in the raw state or in the form of vulcanized or unvulcanized mixes. The method is based on infrared spectrometric examination using the transmission technique. The method comprises examination of polymer
20、s by their pyrolysis products (pyrolysates), or by films cast from solution or obtained by moulding (for raw rubbers only). Typical spectra are given in Annex A. The principle of the method implies that sample preparation and analysis of the infrared spectra are carried out by experienced personnel
21、and that the equipment used for the production of spectra is operated in accordance with the manufacturers instructions for optimum performance. Details of the operation of infrared spectrometers are not included in this International Standard. The method specified is a qualitative method only. 2 No
22、rmative references The following referenced documents 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
23、 of solvent extract ISO 18064, Thermoplastic elastomers Nomenclature and abbreviated terms 3 Principle The extractable material is first extracted from a test sample of the rubber and the rubber then prepared under precise conditions for spectroscopy in the form of raw polymer film, vulcanizate pyro
24、lysate or vulcanizate film. The IR spectrum is recorded and then interpreted by comparison with a set of typical reference spectra. 4 Types of rubber 4.1 General The method is applicable to rubbers in the raw state and, if compounded, in both the vulcanized and unvulcanized states. It is applicable
25、to the following types of rubber occurring either alone or in a binary mixture when the proportion of the minor component is, in general, not less than 10 % to 20 % by mass of the mixture (see, however, exceptions in 4.2). ISO 4650:2005(E) 2 ISO 2005 All rights reserved 4.1.1 M group 4.1.1.1 Acrylic
26、 rubber (ACM): Copolymer of ethyl acrylate (or other acrylates) and a small amount of a monomer which facilitates vulcanization. 4.1.1.2 Chloropolyethylene (CM) and chlorosulfonylpolyethylene (CSM): The method will not differentiate CM from CSM, and it will not differentiate between different types
27、of CSM. 4.1.1.3 Ethylene-propylene copolymer (EPM) and ethylene-propylene-diene terpolymer (EPDM): The method will not differentiate between the two types of polymer. However, examination of the spectrum gives some information about the ethylene-to-propylene ratio. 4.1.1.4 Fluorocarbon rubber (FKM):
28、 Examination of the pyrolysate may give some information about the different grades of fluorocarbon rubber present. 4.1.2 O group 4.1.2.1 Polychloromethyloxirane (CO): Copolymer of ethylene oxide and chloromethyloxirane (ECO) and terpolymers. Examination of the pyrolysate will not differentiate betw
29、een different types of CO. 4.1.3 Q group 4.1.3.1 Polydimethylsiloxane (MQ), polymethylphenylsiloxane (PMQ) and polymethyl- fluorosiloxane (FMQ): Examination of the pyrolysate will differentiate PMQ from MQ. 4.1.4 R group 4.1.4.1 Butadiene rubber (BR): Examination of the pyrolysate will not different
30、iate between butadiene rubbers having different isomer ratios. However, examination of a raw rubber film gives some information about the isomer ratio. 4.1.4.2 Chloroprene rubber (CR): The method will not differentiate between the different types of CR. 4.1.4.3 Isobutene-isoprene rubber (IIR) and ha
31、logenated isobutene-isoprene rubbers (BIIR and CIIR): Under the conditions used for the method, it is not possible to differentiate between IIR, BIIR, CIIR and polyisobutene. 4.1.4.4 Natural rubber (NR) and synthetic isoprene rubber (IR): Natural rubber (1,4-cis-polyisoprene), gutta percha, balata (
32、1,4-trans-polyisoprene) and synthetic isoprene rubber, whatever their microstructure, (1,4-cis, 1,4-trans or 3,4-) are included. 4.1.4.4.1 Examination of a rubber film will differentiate between 1,4-cis, 1,4-trans and 3,4-polyisoprenes; for non-extracted rubbers, it will differentiate natural rubber
33、 from 1,4-cis synthetic isoprene rubber, and 1,4-trans natural polyisoprenes from their synthetic counterparts. Examination of the pyrolysate film obtained from a vulcanizate provides no information on the microstructure of the polyisoprene or its origin, whether natural or synthetic. 4.1.4.5 Acrylo
34、nitrile-butadiene rubber (NBR): The method will differentiate carboxylic acrylonitrile- butadiene rubbers (XNBRs) from hydrogenated acrylonitrile-butadiene rubbers (HNBRs). Associations of butadiene copolymers and PVC are included. Examination of the pyrolysate film gives some information about the
35、acrylonitrile content. 4.1.4.6 Styrene-butadiene rubber (SBR): The method will differentiate -methylstyrene-butadiene rubbers from styrene-butadiene rubbers. Copolymers of styrene and butadiene, as well as of their substituted derivatives (e.g. -methylstyrene), are included. Examination of a pyrolys
36、ate will not differentiate emulsion- polymerized rubbers from solution-polymerized rubbers. However, examination of a spectrum gives some information about the monomer ratio. ISO 4650:2005(E) ISO 2005 All rights reserved 3 4.1.4.7 Polynorbornene. 4.1.5 T group 4.1.5.1 Polysulfide rubbers. 4.1.6 U gr
37、oup 4.1.6.1 Polyester urethane (AU) and polyether urethane (EU): The method covers only millable polyurethanes. 4.1.7 TPE group 4.1.7.1 As defined in ISO 18064. 4.2 Exceptions for blends 4.2.1 Analysis of a blend of ethylene-propylene rubber with other rubbers presents difficulties when its ethylene
38、-propylene content is below 40 %. 4.2.2 The method will not differentiate between blends of ethylene-propylene rubber with chlorinated polyethylene and/or chloro-sulfonated polyethylene. 4.2.3 Analysis of a blend of natural and/or synthetic polyisoprene and chloroprene rubber may present difficultie
39、s, and identification of the minor component may only be possible when the content is equal to or greater than 30 % in the blend. 4.2.4 The method will not differentiate NBR from NBR/BR blends or NBR blends, nor will it differentiate SBR from SBR/BR blends or SBR blends. 4.2.5 The presence of high q
40、uantities of sulfur in a vulcanizate may affect some characteristic bands. 4.2.6 The method will not differentiate NBR/PVC blends from blends of NBR with other halogenated polymers or additives. 4.3 Reference spectra Tables of absorption characteristics and reference spectra from 4 000 cm1 to 600 cm
41、1 for typical rubbers are given in Annex A. 5 Reagents 5.1 Nitrogen, in pressurized cylinders. 5.2 Extraction solvents, chosen to achieve maximum extraction (alternative solvents may be used on condition that it can be shown that they do not interfere with the interpretation of the infrared spectrum
42、): 5.2.1 Methanol. 5.2.2 Acetone. 5.3 Solvents for rubber dissolution and film preparation, water-free and free from residues (see ISO 1407): 5.3.1 Chloroform. -,-,- ISO 4650:2005(E) 4 ISO 2005 All rights reserved 5.3.2 1,2-dichlorobenzene. 5.4 Sodium sulfate, anhydrous. 5.5 Universal pH-indicator p
43、aper. 6 Apparatus 6.1 Extraction apparatus. The apparatus specified in ISO 1407 is satisfactory. 6.2 Pyrolysis apparatus (see Figure 1), comprising a glass tube A having inward projections to prevent the sample from falling to the bottom of the tube, and a lateral condenser tube. The tube A has a st
44、andard ground-glass joint B that carries a small glass adductor tube. A collecting tube C is placed under the condenser tube. A thermoregulated electric furnace D accommodates an aluminium block E with holes for one or more tubes A. Key A glass tube for sample B ground-glass joint C collecting tube
45、D thermoregulated electric furnace E aluminium block, bored to hold tubes F thermocouple Figure 1 Temperature-controlled pyrolysis apparatus -,-,- ISO 4650:2005(E) ISO 2005 All rights reserved 5 6.3 Capillary pipettes. 6.4 Oven, capable of being maintained at 200 C 5 C. 6.5 Water bath. 6.6 Polished
46、potassium bromide salt plates. 6.7 Filter aid, e.g. diatomaceous earth or similar. 6.8 Infrared spectrometer, of either the Fourier transform or dispersive type, with a wavenumber range of 4 000 cm1 to 600 cm1 and a spectral resolution of 4 cm1 or higher. 7 Procedure 7.1 Procedure for raw rubber fil
47、ms moulded or cast from solution 7.1.1 Using a suitable solvent (see 5.2), extract the extractable material from a test sample of 2 g to 5 g in accordance with the procedure given in ISO 1407. 7.1.2 Dissolve a sufficient amount of the extracted rubber in a suitable solvent (see 5.3), at room tempera
48、ture or under reflux, to give a concentrated solution. 7.1.3 Place a few drops of the concentrated solution on a potassium bromide salt plate (6.6) and allow the solvent to evaporate. 7.1.4 Films of raw rubber of a suitable thickness may also be obtained by moulding. 7.1.5 Record the spectrum from 4 000 cm1 to 600 cm1 using the infrared spectrometer (6.8). 7.1.6 After recording the spectrum, verify that no solvent absorption bands are present and check that