1、BS ISO17564:2008ICS 83.060NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDRaw hydrogenatednitrile rubber (HNBR) Determination ofresidual unsaturationby iodine valueThis British Standardwas published under theauthority of the StandardsPolicy and StrategyCommittee
2、 on 31 July 2008 BSI 2008ISBN 978 0 580 58157 1Amendments/corrigenda issued since publicationDate CommentsBS ISO 17564:2008National forewordThis British Standard is the UK implementation of ISO 17564:2008. Itsupersedes BS ISO 17564:2001 which is withdrawn.The UK participation in its preparation was
3、entrusted to TechnicalCommittee PRI/23, Test methods for rubber and non-black compoundingingredients.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are resp
4、onsible for its correct application.Compliance with a British Standard cannot confer immunityfrom legal obligations.BS ISO 17564:2008Reference numberISO 17564:2008(E)ISO 2008INTERNATIONAL STANDARD ISO17564Second edition2008-06-01Raw hydrogenated nitrile rubber (HNBR) Determination of residual unsatu
5、ration by iodine value Caoutchouc nitrile hydrogn (HNBR) brut Dtermination de linsaturation rsiduelle par lindice diode BS ISO 17564:2008ISO 17564:2008(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but s
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10、 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2008 All rights reservedBS ISO 17564:2008ISO 17564:2008(E) ISO 2008 All rights reserved iiiContents Page Foreword iv 1 Scope 1 2 Normative references 1 3 Principle1 4 Reagents.1 5 Apparatus .2 6 Procedure .2 7 Calculation
11、3 8 Precision.3 9 Test report 3 Annex A (normative) Preparation of Wijs solution .4 Annex B (informative) Precision 5 Bibliography 6 BS ISO 17564:2008ISO 17564:2008(E) iv ISO 2008 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of nation
12、al standards bodies (ISO member bodies). 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. Internatio
13、nal organizations, governmental and non-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 rule
14、s given in the ISO/IEC Directives, Part 2. The main task 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 l
15、east 75 % of the member bodies casting a vote. Attention 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 17564 was prepared by Technical Committee ISO/TC 4
16、5, Rubber and rubber products, Subcommittee SC 2, Testing and analysis. This second edition cancels and replaces the first edition (ISO 17564:2001), which has been revised primarily to make the ranges of test portion sizes in Table 1 clearer, to correct the equation in Clause 7 and to include new pr
17、ecision data (now in Annex B). BS ISO 17564:2008INTERNATIONAL STANDARD ISO 17564:2008(E) ISO 2008 All rights reserved 1Raw hydrogenated nitrile rubber (HNBR) Determination of residual unsaturation by iodine value WARNING Persons using this International Standard should be familiar with normal labora
18、tory 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 practices and to ensure compliance with any national regulatory conditions. CAUTION Certain procedures
19、 specified in this International Standard may involve the use or generation of substances, or the generation of waste, that could constitute a local environmental hazard. Reference should be made to appropriate documentation on safe handling and disposal after use. 1 Scope This International Standar
20、d specifies a method using Wijs solution to determine the iodine value (i.e. the residual unsaturation) of raw hydrogenated nitrile rubber (HNBR). 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition
21、cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 1795, Rubber, raw natural and raw synthetic Sampling and further preparative procedures 3 Principle A sample of HNBR is dissolved in chloroform. A known excess of Wijs solutio
22、n is 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 unsat
23、uration) calculated. 4 Reagents During the analysis, unless otherwise stated, use only reagents of recognized analytical grade. 4.1 Water: During the analysis, use only distilled or demineralized water or water of equivalent purity. 4.2 Chloroform. WARNING Chloroform is a harmful solvent if swallowe
24、d or inhaled and irritating to skin. Special safety precautions should therefore be taken, including the use of a fume hood. 4.3 Wijs solution (see Annex A). 4.4 100 g/l aqueous potassium iodide solution. BS ISO 17564:2008ISO 17564:2008(E) 2 ISO 2008 All rights reserved4.5 10 g/l starch solution. 4.
25、6 0,1 mol/l standard volumetric sodium thiosulfate solution. 5 Apparatus 5.1 Mechanical shaker. 5.2 Constant-temperature bath, capable of being maintained at (25 1) C. 5.3 Analytical balance, accurate to 0,1 mg. 5.4 Glass-stoppered conical flask, capacity 300 cm3. 5.5 Pipettes, capacity 10 cm3and 25
26、 cm3. 5.6 Burette, capacity 50 cm3, graduated at 0,1 cm3intervals. 6 Procedure 6.1 From a sample obtained in accordance with ISO 1795, weigh out, to the nearest 0,1 mg, a test portion of size corresponding to the suspected degree of unsaturation (iodine value) as indicated in Table 1 and place it in
27、 a 300 cm3glass-stoppered conical flask. Table 1 Recommended test portion sizes Suspected degree of unsaturation (iodine value) Sample mass g More than 30 0,35 to 0,40 More than 15 and up to 30 0,40 to 0,50 More than 8 and up to 15 0,50 to 0,70 up to 8 0,90 to 1 6.2 Add 50 cm3of chloroform (4.2) to
28、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. 6.3 Remove the flask from the bath and accurately pipette 25 cm3of Wijs solution (4.3) into the flask. Immediately stopp
29、er the flask and swirl gently to mix. Place the flask in the constant-temperature bath for 120 min 5 min to complete the iodine addition reaction. 6.4 Once the iodine addition reaction is complete, remove the flask from the bath and quickly add, by pipette, 10 cm3of potassium iodide solution (4.4).
30、Immediately stopper the flask and shake vigorously. 6.5 Loosen the stopper slightly and, using a wash bottle, wash the stopper and mouth of the flask with the minimum amount of water (see 4.1), ensuring the washings run directly into the flask. Replace the stopper, swirl gently and allow the flask t
31、o stand for 5 min. 6.6 Within 20 min, titrate with sodium thiosulfate solution (4.6) while swirling the flask gently. When the upper (aqueous) layer becomes slightly yellow, add about 1 cm3of starch solution (4.5). Stopper the flask and shake vigorously. Continue the titration, shaking the flask vig
32、orously 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 solution. BS ISO 17564:2008ISO 17564:2008(E) ISO 2008 All rights reserved 3NOTE It is
33、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. 6.7 Let the flask stand for 30 min. If the colour reappears, add addit
34、ional titrant with vigorous shaking until no additional colour appears on standing for 30 min. 6.8 Conduct a blank titration, performing steps 6.2 to 6.7. 7 Calculation Calculate the iodine value from the following equation: ()0112,69VV cAm= where A is the iodine value (g iodine/100 g of sample); V1
35、is the volume of sodium thiosulfate solution used to titrate the test portion (cm3); V0is the volume of sodium thiosulfate solution used for the blank titration (cm3); m is the mass of the test portion (g); c is the concentration of the sodium thiosulfate solution (mol/l); 12,69 is the atomic mass o
36、f iodine 100/1 000. 8 Precision See Annex B. 9 Test report The test report shall include the following information: a) all details necessary for complete identification of the sample analysed; b) a reference to this International Standard; c) any deviation from this International Standard; d) the io
37、dine value, expressed to the nearest 0,1 iodine value units; e) the date of the analysis. BS ISO 17564:2008ISO 17564:2008(E) 4 ISO 2008 All rights reservedAnnex A (normative) Preparation of Wijs solution A.1 Weigh out, to the nearest 0,1 g, between 4,8 g and 5,2 g of iodine trichloride and place it
38、in a 1 l brown bottle with a PTFE-lined screw cap. A.2 Weigh out, to the nearest 0,1 g, 5,5 g of iodine and place it in a 1 l glass-stoppered conical flask containing 640 cm3 of glacial acetic acid. Stopper the flask and swirl carefully to dissolve the iodine. A.3 Carefully pour the iodine/acetic ac
39、id solution into the brown bottle containing the iodine trichloride. Stopper the bottle and swirl carefully to mix. A.4 Affix a label to the bottle indicating the preparation date. Store the bottle in a dark place. The solution shall not be used more than 30 days after preparation. BS ISO 17564:2008
40、ISO 17564:2008(E) ISO 2008 All rights reserved 5Annex B (informative) Precision B.1 The precision was determined by means of an interlaboratory test programme. Three different materials (grades of HNBR) with different degrees of unsaturation were used in the programme. These were analysed in four la
41、boratories on two different days one week apart. Duplicate analyses were run on each day. B.2 The precision calculations to express repeatability and reproducibility were performed in accordance with ISO/TR 9272:2005. Consult this for precision concepts and nomenclature. B.3 A type 1 interlaboratory
42、 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 and n = 4. The precision analysis followed the general procedure set forth in ISO/TR 9272:2005. The repeatability values
43、contain two undifferentiated sources of variation, replicated within days and between days. The final values of the precision parameters are given in Table B.1. These precision values should not be used for acceptance/rejection of materials without documentation that they are for those materials and
44、 that the test protocols include this test method. B.4 Repeatability: The repeatability r of the iodine value of HNBR has been established as the appropriate value of any parameter tabulated in Table B.1. Two single test results obtained in the same laboratory, under normal test method procedures, t
45、hat differ by more than this tabulated r should be considered suspect and should dictate that some appropriate investigative action be taken. B.5 Reproducibility: The reproducibility R of the iodine value of HNBR has been established as the appropriate value of any parameter tabulated in Table B.1.
46、Two single test results obtained in separate laboratories, under normal test method procedures, that differ by more than this tabulated R should be considered suspect and should dictate that some appropriate investigative action be taken. Table B.1 Precision data Within laboratory Between laboratori
47、es HNBR sample Iodine value (mean) g/100 g srr (r) sRR (R) 1 5,05 0,184 0,520 10,30 0,259 0,732 14,50 2 10,38 0,148 0,420 4,05 0,596 1,686 16,24 3 26,86 0,240 0,679 2,53 0,498 1,409 5,25 sris the within-laboratory standard deviation; r is the repeatability (in measurement units); (r) is the repeatab
48、ility (as percentage of average for material); sRis the between-laboratory standard deviation; R is the reproducibility (in measurement units); (R) is the reproducibility (as percentage of average for material). BS ISO 17564:2008ISO 17564:2008(E) 6 ISO 2008 All rights reservedBibliography 1 ISO/TR 9
49、272:2005, Rubber and rubber products Determination of precision for test method standards 2 ASTM D 5902, Standard Test Method for Rubber Determination of Residual Unsaturation in Hydrogenated Nitrile Rubber (HNBR) by Iodine Value BS ISO 17564:2008BS ISO 17564:2008ISO 17564:2008(E) ICS 83.060 Price based on 6 pages ISO 2008 All rights reserved BS ISO 17564:2008This page has been intentionally left blank
