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1、BRITISH STANDARD BS ISO 16565:2002 Rubber Determination of 5-ethylidenenorbornene (ENB) or dicyclopentadiene (DCPD) in ethylene- propylene-diene (EPDM) terpolymers ICS 83.060 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27
2、 07:43:00 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 16565:2002 This British Standard, having been prepared under the direction of the Materials and Chemicals Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 3 May 2002 B
3、SI 3 May 2002 ISBN 0 580 39605 3 National foreword This British Standard reproduces verbatim ISO 16565:2002 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee PRI/23, Test methods for rubber and non-black compounding ingredient
4、s, 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 implement international or European publications referred to in this document may be found in the BSI Standards Catalogu
5、e under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their corr
6、ect 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 any enquiries on the interpretation, or proposals for change, and keep the UK interests inf
7、ormed; 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, pages 1 to 13 and a back cover. The BSI copyright date displayed in this document indicates
8、 when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:43:00 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 16565:2002(E) INTERNATIONAL STANDARD ISO 16565 First edition 2002-03-15 Rubber
9、 Determination of 5-ethylidenenorbornene (ENB) or dicyclopentadiene (DCPD) in ethylene- propylene-diene (EPDM) terpolymers Caoutchouc Dtermination du 5-thylidnenorbornne (ENB) ou du dicyclopentadine (DCPD) dans les terpolymers dthylne-propylne- dine (EPDM) Licensed Copy: sheffieldun sheffieldun, na,
10、 Mon Nov 27 07:43:00 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 16565:2002(E) ii Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:43:00 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 16565:2002(E) iii Contents Page Foreword.iv 1 Scope1 2 Principle1 3 Apparatus.1 4 Test specimen preparat
11、ion.2 5 Acquisition of spectra.3 6 Calibration of the spectrophotometer.3 7 Diene determination4 8 Precision and bias.8 9 Test report10 Annex A (normative) Procedure for spectral subtraction of water vapour.11 Bibliography13 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:43:00 GMT+00:00 2
12、006, Uncontrolled Copy, (c) BSI ISO 16565:2002(E) 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 committees. E
13、ach 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 the Internati
14、onal 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 3. The main task of technical committees is to prepare International Standards. Draft International Standa
15、rds 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 International Standard may
16、be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 16565 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 2, Testing and analyses. Annex A forms a normative part of this International Standar
17、d. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:43:00 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTERNATIONAL STANDARD ISO 16565:2002(E) 1 Rubber Determination of 5-ethylidenenorbornene (ENB) or dicyclopentadiene (DCPD) in ethylene-propylene-diene (EPDM) terpolymers WARNING Persons usi
18、ng this International Standard should be familiar with normal laboratory practice. This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and to
19、ensure compliance with any national regulatory conditions. 1 Scope This International Standard specifies the methods to be used to determine the content of 5-ethylidenenorbornene (ENB) or dicyclopentadiene (DCPD) in ethylene-propylene-diene (EPDM) terpolymers in the 0,1 % to 15 % range. ENB and DCPD
20、 are dienes introduced into ethylene-propylene rubbers to generate specific cure properties. Since high precision for diene content determination is important, a Fourier transform infrared spectroscopic (FT-IR) method is utilized. NOTE The procedures for mass fraction of ENB and mass fraction of DCP
21、D differ only in the location in the infrared (IR) peak being quantified. 2 Principle A test specimen is moulded between two PTFE-coated aluminium or mylar sheets. The ENB content is determined from its infrared absorbance at 1 681 cm1 to 1 690 cm1, a measure of the exocyclic double bond in ENB. The
22、 DCPD content is determined from its infrared absorbance at 1 605 cm1 to 1 610 cm1, a measure of the monocyclic double bond in DCPD. The second derivative of the absorbance is calculated and ratioed to an internal standard. For ENB, the resulting second-derivative peak near 1 690 cm1 is related to t
23、he ENB mass fraction by calibrating the instrument with known EPDM standards. For DCPD, the resulting second-derivative peak near 1 610 cm1 is related to the DCPD mass fraction in the same way. For oil-extended polymers, the oil must be extracted before the diene content is determined. 3 Apparatus 3
24、.1 Carver-type press, capable of compressing films at 150 C and 10 MPa. 3.2 Mould 3.2.1 The mould primarily used is made of stainless-steel strip 400 m thick with an opening which will give a specimen of the appropriate size for the specimen-film holder described in 3.4 (2 cm by 2 cm). The mould sha
25、ll have approximately the same dimensions as the press platens. 3.2.2 Alternatively, a thinner mould plate may be used. However, precision can be adversely affected at low diene levels. The precision of the method shall be determined when thinner films are utilized. For example, Licensed Copy: sheff
26、ieldun sheffieldun, na, Mon Nov 27 07:43:00 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 16565:2002(E) 2 127-m-thick stainless-steel foil with a 15 mm by 35 mm opening may be used for the simultaneous determination of ethylene and diene. 3.2.3 For liquid EPDMs, a ring washer of 22 mm outer diamete
27、r by 16 mm inner diameter and 400 m thick is used as a spacer between salt plates (NaBr, NaCl) to set a fixed path length. The spacer is sized to cover only the outer edge of the salt plates. 3.3 PTFE-coated aluminium moulding sheets, type A, 36 m thick, or silicone release sheeting. 3.4 Specimen-fi
28、lm holders: Films may be moulded, cut out and transferred to a film holder. Magnetic-film holders are ideal. Alternatively, a mould sized to fit in the spectrophotometer specimen compartment, with an appropriate-size opening, may be used to support the film without removal after compressing. A stand
29、ard salt plate support is used for liquid samples prepared between salt plates. 3.5 Infrared Fourier transform spectrophotometer, capable of measuring absorbances in the range 4 000 cm1 to 600 cm1 with a transmittance specification (accuracy) of 1 % T or better. The instrument shall be capable of sp
30、ectral resolution of 2 cm1. A deuterated triglycerine sulfate (DTGS) or, as an alternative, a mercury cadmium telluride (MCT) detector shall be used. NOTE A specification for the evaluation of the analysis of infrared spectra is given in reference 1. The instrument shall be capable of spectral accum
31、ulation, averaging and subtracting. Water is the primary source of interference in this method. Methods, physical and electronic, that minimize the moisture level and moisture-level variation are required to obtain the highest precision. The preferred method is to use an instrument equipped with a d
32、ry-gas purge and specimen shuttle, which permits alternating and repetitive collection of single-beam specimen and background spectra (see clause 5). Alternatively, should a specimen shuttle be unavailable, careful purging of the specimen compartment with dry nitrogen can yield satisfactory results.
33、 High precision of calibration-standard data is indicative of adequate purging. When moisture interference is not removed by purging, spectral subtraction of water vapour can be used. A procedure for further development of the method is described in annex A. 4 Test specimen preparation 4.1 Primary m
34、ethod Place 0,20 g 0,05 g of the material to be analysed between two sheets (see 3.3) in the mould (see 3.2.1). Place the mould between the press platens heated to 125 C 5 C and apply 4 MPa pressure for 60 s 10 s. Should the material be highly viscous, the mould may be heated to 175 C 5 C. Cool the
35、material to ambient temperature. Cut out a piece of film approximately 15 mm by 50 mm. Detach the specimen film from the sheets (see 3.3) and position it on the spectrophotometer specimen compartment window. 4.2 Alternative method When using the thinner mould described in 3.2.2, place a small piece
36、(0,04 g to 0,06 g) of the material to be analysed in the mould opening between two sheets (see 3.3) and compress as in 4.1. Remove the mould from the press, turn it over and compress it again. Then remove the mould from the press and allow it to cool to ambient temperature. When cool, carefully remo
37、ve the sheets (see 3.3), allowing the specimen film to remain attached to the mould. 4.3 Alternative method for liquid polymer film preparation Place a washer (see 3.2.3) on top of a salt plate. Place a small amount (about 0,3 g) of the liquid EPDM polymer to be analysed in the centre of the washer,
38、 filling the hole completely. Place a second salt plate on top of the filled washer. Gently place a 1 kg weight on top of the salt plate/washer assembly and allow the weighted assembly to sit for 2 min to 3 min. (For viscous samples, it may be necessary to warm the sample prior to compressing.) Remo
39、ve the 1 kg weight and, if necessary, allow to cool. Wipe off any excess material that may have been pressed out of Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:43:00 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 16565:2002(E) 3 the assembly. Hold the assembly up to the light and inspe
40、ct for bubbles and/or voids. Should there be imperfections, repeat the preparation with a larger amount of material. 5 Acquisition of spectra 5.1 With a specimen shuttle 5.1.1 The data-acquisition parameters shall be: resolution: 2 cm1; scans/scan time: total scan time, split between specimen scans
41、and background scans, about 90 s. 5.1.2 Place the test specimen in the specimen compartment, allow purge to re-establish and, in alternating fashion, collect single-beam specimen and empty specimen compartment spectra. Eight passes of the shuttle shall be made (eight specimen and eight empty-compart
42、ment collections), collecting four scans at each position. 5.1.3 Calculate the specimen absorbance spectrum as minus log10 of the ratio of the accumulated single-beam specimen to the empty-compartment spectrum: A = log10(P/P0) where A is the absorbance of the specimen at a given wavelength; P0 is th
43、e empty specimen compartment light-beam intensity at that wavelength; P is the single-beam specimen light-beam intensity at that wavelength. 5.2 Without a specimen shuttle 5.2.1 The data-acquisition parameters shall be: resolution: 2 cm1; scans/scan time: background scans: 32 scans, 120 s total; spe
44、cimen scans: 32 scans, 120 s total. 5.2.2 Establish a dry atmosphere inside the empty specimen compartment and collect the empty specimen compartment spectra. 5.2.3 Place the test specimen in the specimen compartment and re-establish a dry atmosphere inside the compartment. Collect the single-beam s
45、pecimen spectra and calculate the specimen absorption spectrum as described in 5.1.3. 6 Calibration of the spectrophotometer 6.1 Obtain a series of known standards covering the diene content range 0 % to 10 %. Calibration may be based on secondary standards qualified by other laboratories using this
46、 method or, more generally, by primary standards whose diene content is well known. Primary standards may be established via use of hydrogen nuclear magnetic resonance (H-NMR), in conjunction with other techniques. The ENB calibration standards1) employed in the 1) The sole source of supply of the E
47、NB standards is Exxon Chemical Polymer Laboratories, PO Box 5200, Baytown, TX 77522, USA. For DCPD standards, the sole source is Uniroyal Chemical Company, World Headquarters, Chemical Characterization Laboratory, Benson Road, Middlebury, CT 06749, USA. Licensed Copy: sheffieldun sheffieldun, na, Mo
48、n Nov 27 07:43:00 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 16565:2002(E) 4 development of this method were determined by a combination of refractive index and H-NMR (utilizing samples dissolved in deuterated o-dichlorobenzene at 120 C; the ENB assignment was based exclusively on the exocyclic
49、olefinic protons of ENB). The DCPD standards1) were determined by a similar H-NMR technique involving the cyclic olefinic protons of DCPD. The use of four standards at the (copolymer) 2 %, 5 % and 10 % levels is the minimum recommended. 6.2 Using the procedure in clause 5, acquire a minimum of five absorbance spectra for each of the calibration standards described in 6.1. Several repetitions on separate specimens of each standard may be averaged to improve the accuracy of the calibration. 6.3 Using the procedure in clause 7