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1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS ISO 15671:2000 ICS 83.
2、040.20; 83.060 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Rubber and rubber additives Determination of total sulfur content using an automatic analyser Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI This British
3、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 October 2000 BSI 10-2000 ISBN 0 580 36517 4 BS ISO 15671:2000 Amendments issued since publication Amd. No.D
4、ateComments National foreword This British Standard reproduces verbatim ISO 15671:2000 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: aid enquirers to und
5、erstand 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 in the UK. A list of organizations represented o
6、n 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 usin
7、g 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 immunity fr
8、om legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii and iii, a blank page, pages 1 to 5 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Licensed Copy: shef
9、fieldun sheffieldun, na, Mon Nov 27 07:38:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTERNATIONAL STANDARD ISO 15671 First edition 2000-07-15 Reference number ISO 15671:2000(E) Rubber and rubber additives Determination of total sulfur content using an automatic analyser Caoutchouc et additifs po
10、ur caoutchouc Dosage du soufre total laide dun analyseur automatique Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 15671:2000(E) ii? Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:18 GMT+00:00 2006, Uncontrolled Copy, (c)
11、 BSI ISO 15671:2000(E) ?iii 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 com- mittees. Each member body interes
12、ted 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 liai- son with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical
13、 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. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publicatio
14、n 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 be the subject of patent rights. ISO shall not be held responsible for identifying any or all such
15、 patent rights. International Standard ISO 15671 was prepared by Technical Committee ISO/TC 45,Rubber and rubber products, Subcommittee SC 2,Testing and analyses. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun she
16、ffieldun, na, Mon Nov 27 07:38:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTERNATIONAL STANDARD?ISO 15671:2000(E) ?1 Rubber and rubber additives Determination of total sulfur content using an automatic analyser WARNING Persons using this International Standard should be familiar with normal labo
17、ratory 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. 1Scope This Internationa
18、l Standard specifies an instrumental (automatic analyser) method for the determination of total sul- fur in rubber and rubber additives. 2Terms and definitions For the purposes of this International Standard, the following terms and definitions apply. 2.1 sample unit selected to represent the materi
19、al to be analysed 2.2 test portion actual material used in the analysis 2.3 control sample material with a recognized content of sulfur, analysed with each set of test portions 3Principle 3.1Specified is a reliable, rapid, instrumental (automatic analyser) method for determining total sulfur in rubb
20、er and rubber additives. The sulfur is determined by a single instrumental procedure consisting of weighing a test portion, placing it in the instrument and initiating the (subsequently automatic) analytical process. The analysis may be con- trolled manually to a limited degree, and a capability to
21、perform computations automatically may be provided by the instrument used to perform the analysis. 3.2The actual process can vary substantially from instrument to instrument because a variety of means can be used to meet the primary requirements of the method. The method includes the following: a)co
22、nversion of sulfur-containing materials to sulfur dioxide in an oxygen stream; b)determination of the sulfur dioxide by one of three detection schemes, and hence the total sulfur content. 3.3In the hydrogen peroxide detection configuration, the sulfur dioxide is absorbed in hydrogen peroxide, con- v
23、erting sulfur dioxide to sulfuric acid which is subsequently titrated with standard alkali, enabling the sulfur to be cal- culated. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 15671:2000(E) 2? 3.4In the iodine solution detection conf
24、iguration, the sulfur dioxide is absorbed in standard iodine solution, re- ducing iodine to iodide which is subsequently measured by a polarized dual platinum electrode system, enabling the sulfur to be calculated. 3.5In the sulfur dioxide detection configuration, the sulfur dioxide is passed throug
25、h an infrared absorption de- tector and determined using a sulfur dioxide standard, enabling the sulfur to be calculated. 4Requirements for apparatus 4.1Because a variety of instrumental (automatic analyser) component configurations can be used satisfactorily for this method, no specifications are p
26、resented with regard to overall system design. Functionally, however, the follow- ing requirements are specified for all instruments. 4.2The conditions for combustion of the sample shall be such that (for the full range of applicable samples) sulfur- containing components shall be converted complete
27、ly to sulfur dioxide. General instrumental conditions that affect complete combustion include: a)availability of the oxidant, b)temperature, c)time. 4.3For the configuration described in 3.3, a correction shall be made for acidity when chlorine is present by titration of a portion of the absorption
28、solution for chloride, which is calculated as hydrochloric acid and subtracted from the total acidity. 4.4In the iodine solution and sulfur dioxide detection methods (3.4 and 3.5), the detection system shall determine sulfur without interference and the detector should ideally provide a linear respo
29、nse that correlates directly with sulfur concentration over the full range of possible concentrations from the applicable test samples. 4.5The system shall include provisions for evaluating nonlinear response appropriately, so that nonlinear re- sponses can be correlated accurately with concentratio
30、n. Such provisions can be integral with the instrument or be provided by (auxiliary) computation schemes. 4.6Finally, except for those systems in which the sulfur concentration is expressed as a direct output, the instru- ment shall include an appropriate detector response readout device. 5Reagents
31、Reagent grade chemicals shall be used in all analyses unless otherwise indicated. 5.1Oxygen, as specified by the instrument manufacturer. 5.2Additional reagents as specified by the instrument manufacturer. This specification refers to the reagents used to meet the requirements cited in 3.3 to 3.5. T
32、hese reagents can vary substantially for different instruments; in all cases, however, the reagents specified by the instrument manufacturer shall be used. 6Instrument (automatic analyser) preparation and calibration 6.1Assemble the instrumental (automatic analyser) system in accordance with the man
33、ufacturers instructions. 6.2For the response (drift) adjustment, weigh and analyse (in accordance with the manufacturers instructions) an appropriate test portion of the sulfur calibrating agent. Repeat this procedure, adjusting instrument response, as rec- ommended by the manufacturer, until the ab
34、sence of drift is indicated. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 15671:2000(E) ?3 6.3For the calibration, select calibrating agents and materials specified by the manufacturer that have certified sul- fur contents lying withi
35、n the range of those of the samples to be analysed. At least three such calibrating agents are recommended for each range of sulfur contents to be determined. When possible, two of the calibrating agents shall bracket the range of sulfur contents to be determined, with the third falling within the r
36、ange. 6.4For the calibration procedure, analyse portions of the calibrating agent chosen (see 6.3) to represent the sulfur content in the samples to be tested. Continue analysing until the results from five consecutive determinations fall within the repeatability interval (see 9.3) of this test meth
37、od. Calibrate the instrument in accordance with the manu- facturers instructions using these values. The results obtained shall be within the precision limits stated for the cali- brating agent, otherwise the calibration procedure shall be repeated. 6.5For the periodic calibration verification and r
38、ecalibration, analyse a control sample on a periodic basis. The re- sults obtained for the control sample shall be within established limits. If not, all results obtained since the last successful control check shall be rejected and the calibration procedure repeated. 7Procedure Analyse a test porti
39、on of the sample in accordance with the manufacturers instructions. Carry out the analysis in duplicate. 8Calculation Calculate the percent sulfur?as follows: where is the detector response for sulfur; is the detector response per unit mass established for sulfur during calibration; is the mass of t
40、he test portion, in grams. 9Precision 9.1Although the precision of this test method was calculated from data obtained from the analysis of bituminous coal, it is considered to be directly applicable to the analysis for sulfur in rubber compounds. The precision is ex- pressed in terms as specified in
41、 ISO/TR 9272, on the basis of a?confidence level for the values established for repeatability?and reproducibility?. 9.2The precision data given in this clause give an estimate of the precision of this method with the materials used in the particular interlaboratory test programme. The precision para
42、meters shall not be used for acceptance or rejec- tion testing of any group of materials without documentation that the parameters are applicable to the particular group of materials and the specific test protocols of the method. 9.3The repeatability, in percent sulfur, has been established as the v
43、alue in Table 1. Two results, obtained in one laboratory (same instrument, material, operator) under normal procedures, that differ by more than this tabulated value shall be considered to have come from different or non-identical sample populations. 9.4The reproducibility?, in percent sulfur, has b
44、een established as the value in Table 1. Two results, obtained in different laboratories (same material, but different instrument and different operator) under normal procedures, that differ by more than this tabulated value shall be considered to have come from different or non-identical sample pop
45、- ulations. S S = B C m 100 % B C m 95 % rR r R Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 15671:2000(E) 4? 9.5Bias is eliminated when the apparatus is calibrated properly against certified reference standards. Proper cali- bration
46、includes comparison of test data on calibrating agents that have certified sulfur contents. 10Test report The test report shall include the following information: a)a reference to this International Standard; b)all details necessary for identification of the sample analysed; c)the procedure used (hy
47、drogen peroxide, iodine solution or sulfur dioxide); d)the duplicate percent sulfur results to the nearest?; e)the instrument (automatic analyser) make and model; f)?any deviations from the method; g)the date of the analysis. Table 1 Sulfur analysis precision Within lab?Between labs 0,05?0,09 where?
48、is the repeatability standard deviation. where?is the reproducibility standard deviation. rR r =2,83 sr sr R =2,83 sR sR 0,1 % Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 15671:2000(E) ?5 Bibliography 1 ISO/TR 9272:1986,Rubber and ru
49、bber products Determination of precision for test method standards. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 07:38:18 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 15671:2000 BSI 389 Chiswick High Road London W4 4AL | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BSI British Standards Institution BSI is the independent national bod