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1、BRITISH STANDARD BS ISO 17564:2001 Nitrile rubber Determination of residual unsaturation in hydrogenated nitrile rubber (HNBR) by iodine value ICS 83.060 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:35 GMT+00:00 2
2、006, Uncontrolled Copy, (c) BSI BS ISO 17564:2001 This British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 May 2001 BSI 05-2001 ISBN 0 580 37430 0 Nati
3、onal foreword This British Standard reproduces verbatim ISO 17564:2001 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee PRI/23, Chemical testing of rubber, which has the responsibility to: A list of organizations represented
4、on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by u
5、sing 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 correct application. Compliance with a British Standard does not of itself confer immuni
6、ty 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 informed; monitor related international and European developments and promulgate them i
7、n 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 6, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since pub
8、lication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO/FDIS 17564:2001(E) INTERNATIONAL STANDARD ISO 17564 First edition 2001-02-15 Nitrile rubber Determination of residual unsaturation in hydroge
9、nated nitrile rubber (HNBR) by iodine value Caoutchouc nitrile Dtermination de linsaturation rsiduelle dans le caoutchouc nitrile hydrogn (HNBR) par lindice diode Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 17564:2001(E) ii Licensed
10、Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 17564:2001(E) iii ContentsPage Foreword.iv 1Scope 1 2Normative references1 3Principle1 4Reagents.1 5Apparatus.2 6Procedure.2 7Calculation3 8Precision.3 9Test report4 Annex A (normative) Preparation
11、of Wijs solution.5 Bibliography6 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 17564:2001(E) iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies
12、). The work of preparing 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 no
13、n-governmental, in 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, Par
14、t 3. 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. Attention is drawn to the possibility that some of the elements of t
15、his International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 17564 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee SC 2, Testing and analyses. Annex
16、A forms a normative part of this International Standard. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTERNATIONAL STANDARDISO 17564:2001(E) 1 Nitrile rubber Determination of residual unsaturation in hydrogenated nitrile rubber (HNBR) by
17、 iodine value WARNING Persons using this International Standard should be familiar with normal laboratory practice. This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health p
18、ractices and to ensure compliance with any national regulatory conditions. 1Scope This International Standard specifies a method using Wijs solution to determine the iodine value (i.e. the residual unsaturation) of hydrogenated nitrile rubber (HNBR). 2Normative references The following normative doc
19、uments 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 do not apply. However, parties to agreements based on this International Standard are enco
20、uraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For 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 1
21、795:2000, 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. 3Principle A sample of raw, unvulcanized HNBR is dissolved in chloroform. A known excess of Wijs solution is
22、 added to the solution and a fixed time is allowed for addition of iodine to the residual unsaturation in the HNBR. Unreacted Wijs solution is then neutralized with potassium iodide solution, the iodine thus liberated titrated with standard sodium thiosulfate and the iodine value (residual unsaturat
23、ion) calculated. 4Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and distilled or demineralized water or water of equivalent purity. 4.1Chloroform. 4.2Wijs solution (see Annex A). 4.3100 g/l aqueous potassium iodide solution. 4.410 g/l starch
24、solution. 4.50,1 mol/l standard volumetric sodium thiosulfate solution. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 17564:2001(E) 2 5Apparatus 5.1Mechanical shaker. 5.2Constant-temperature bath, capable of being maintained at (25?1)
25、C. 5.3Analytical balance, accurate to 0,1 mg. 5.4Glass-stoppered conical flask, capacity 300 cm3. 5.5Pipettes, capacity 10 cm3and 25 cm3. 5.6Burette, capacity 50 cm3, graduated at 0,1 cm3intervals. 6Procedure 6.1From a sample obtained in accordance with ISO 1795, weigh out, to the nearest 0,1 mg, a
26、test portion of size corresponding to the suspected degree of unsaturation (iodine value) as indicated in Table 1 and place it in a 300 cm3glass-stoppered conical flask. Table 1 Recommended test portion sizes Suspected degree of unsaturation (iodine value) Mass of test portion g ? 300,35 to 0,40 15
27、to 300,40 to 0,50 8 to 150,50 to 0,70 ?80,90 to 1,0 6.2Add 50 cm3of chloroform (4.1) to the flask, stopper it and place on a mechanical shaker until the test portion has completely dissolved. Then place the flask in a constant-temperature bath at (25?1) C for 30 min. 6.3Remove the flask from the bat
28、h and accurately pipette 25 cm3of Wijs solution (4.2) into the flask. Immediately stopper the flask and swirl gently to mix. Place the flask in the constant-temperature bath for 2 h?5 min to complete the iodine addition reaction. 6.4Once the iodine addition reaction is complete, remove the flask fro
29、m the bath and quickly add, by pipette, 10 cm3of potassium iodide solution (4.3). Immediately stopper the flask and shake vigorously. 6.5Loosen the stopper slightly and, using a wash bottle, wash the stopper and mouth of the flask with the minimum amount of distilled water, ensuring the washings run
30、 directly into the flask. Replace the stopper, swirl gently and allow the flask to stand for 5 min. 6.6Within 20 min, titrate with sodium thiosulfate solution (4.5) while swirling the flask gently. When the upper (aqueous) layer becomes slightly yellow, add about 1 cm3of starch solution (4.4). Stopp
31、er the flask and shake vigorously. Continue the titration, shaking the flask vigorously at intervals, until the purple colour of the iodine/starch complex vanishes. It is important that the titration with sodium thiosulfate be completed within 30 min after the addition of the potassium iodide soluti
32、on. NOTEIt is important to shake the flask vigorously after addition of the starch solution in order to ensure complete removal of the iodine from the chloroform into the water layer where it becomes available for the reaction with the starch. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 0
33、7:38:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 17564:2001(E) 3 6.7Let the flask stand for 30 min. Should the colour reappear, add additional titrant with vigorous shaking until no additional colour appears on standing for 30 min. 6.8Conduct a blank titration, performing steps 6.2 to 6.7. 7Ca
34、lculation Calculate the iodine value from the following equation: 10 ()12,69VVc A m ? ? where Ais the iodine value (g iodine/100 g of sample); V1is the volume of sodium thiosulfate solution used to titrate the test portion (cm3); V0is the volume of sodium thiosulfate solution used for the blank titr
35、ation (cm3); mis the mass of the test portion (g); cis the concentration of the sodium thiosulfate solution (mol/l); 12,69is the atomic mass of iodine?100/1000. 8Precision 8.1The precision was determined by means of an interlaboratory trials programme. Three different materials (grades of HNBR) with
36、 different degrees of unsaturation were used in the programme. These were analysed in four laboratories on two different days one week apart. Duplicate analyses were run on each day. 8.2The precision calculations to express repeatability and reproducibility were performed in accordance with ISO/TR 9
37、272. Consult this for precision concepts and nomenclature. 8.3Type 1/Class II interlaboratory precision was determined. Both the repeatability and the reproducibility determined are short-term, since a period of one week separates test results. For all data,p= 4,q= 3 andn= 4. The precision analysis
38、followed the general procedure set forth in ISO/TR 9272:1986. Each cell in Figure 1 of ISO/TR 9272:1986 contains four values (two test days, two results each day). The repeatability values contain two undifferentiated sources of variation, replicated within days and between days. The final values of
39、 the precision parameters are given in Table 2. These precision values shall not be used for acceptance/rejection of materials without documentation that they are for those materials and that the test protocols include this test method. 8.4Repeatability:The repeatabilityrof the iodine value of HNBR
40、has been established as the appropriate value of any parameter tabulated in Table 2. Two single test results obtained in the same laboratory, under normal test method procedures, that differ by more than this tabulatedrshall be considered suspect and shall dictate that some appropriate investigative
41、 action be taken. 8.5Reproducibility:The reproducibilityRof the iodine value of HNBR has been established as the appropriate value of any parameter tabulated in Table 2. Two single test results obtained in separate laboratories, under normal test method procedures, that differ by more than this tabu
42、latedrshall be considered suspect and shall dictate that some appropriate investigative action be taken. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 17564:2001(E) 4 Table 2 Precision data Within laboratoryBetween laboratories HNBR sa
43、mple Iodine value (mean) g/100 g srr(r)sRR(R) 16,390,0460,2153,360,2480,4987,79 212,570,0270,1641,300,5680,4543,61 328,750,0510,2260,7861,4331,1974,16 where sris the within-laboratory standard deviation; ris the repeatability (in measurement units); (r)is the repeatability (as percentage of average
44、for material); sRis the between-laboratory standard deviation; Ris the reproducibility (in measurement units); (R)is the reproducibility (as percentage of average for material). 9Test report The test report shall include the following information: a)a reference to this International Standard; b)all
45、details necessary for complete identification of the sample analysed; c)the iodine value, expressed to the nearest 0,1 iodine value units. d)the date of the analysis. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 17564:2001(E) 5 Annex
46、A (normative) Preparation of Wijs solution A.1Weigh out, to the nearest 0,1 g, between 4,8 g and 5,2 g of iodine trichloride and place it in a 1 l brown bottle with a PTFE-lined screw cap. A.2Weigh out, to the nearest 0,1 g, 5,5 g of iodine and place it in a 1 l glass-stoppered conical flask contain
47、ing 640 cm3of glacial acetic acid. Stopper the flask and swirl carefully to dissolve the iodine. A.3Carefully pour the iodine/acetic acid solution into the brown bottle containing the iodine trichloride. Stopper the bottle and swirl carefully to mix. A.4Affix a label to the bottle indicating the pre
48、paration date. Store the bottle in a dark place. The solution shall not be used more than 30 days after preparation. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 17564:2001(E) 6 Bibliography 1ASTM D 5902-96, Standard Test Method for R
49、ubber Determination of Residual Unsaturation in Hydrogenated Nitrile Rubber (HNBR) by Iodine Value. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:35 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 17564:2001 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the intern