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1、BRITISH STANDARD BS ISO 14899:2001 Plastics Polyols for use in the production of polyurethane Determination of basicity ICS 49.025.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:58 GMT+00:00 2006, Uncontrolled Co
2、py, (c) BSI BS ISO 14899:2001 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 37395 9 National foreword This B
3、ritish Standard reproduces verbatim ISO 14899:2001 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee PRI/42, Fibre reinforced thermosetting plastics and prepregs, which has the responsibility to: A list of organizations repres
4、ented 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”, o
5、r 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 correct application. Compliance with a British Standard does not of itself confer
6、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 informed; monitor related international and European developments and promulgate
7、them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to v, a blank page, pages 1 to 5 and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since public
8、ation Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 14899:2001(E) INTERNATIONAL STANDARD ISO 14899 First edition 2001-02-15 Plastics Polyols for use in the production of polyurethane Determination
9、 of basicity Plastiques Polyols pour la production du polyurthanne Dtermination de la basicit Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 14899:2001(E) f t ii Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:58 GMT+00:00
10、2006, Uncontrolled Copy, (c) BSI ISO 14899:2001(E) iii ContentsPage Foreword.iv Introduction.v 1Scope 1 2Normative references1 3Terms and definitions .1 4Principle2 5Sampling.2 6Interferences 2 7Reagents.2 8Apparatus.2 9Procedure.3 10Expression of results 3 11Precision and bias.4 12Test report4 Bibl
11、iography5 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 14899:2001(E) iv Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparin
12、g 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, in liai
13、son 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 3. Draft Internationa
14、l 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 this International Stand
15、ard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 14899 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. Licensed Copy: sheffieldun sheffieldun, na,
16、 Mon Nov 27 08:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 14899:2001(E) v Introduction This method is for the determination of trace amounts of basicity in polyether polyols, which are used in the preparation of polyurethane prepolymers and polyurethane products. Knowledge of this value is
17、 important to prevent gelation during prepolymer production and to control reaction rates during polyurethane preparation. The method, known as the CPR (controlled polymerization rate) analysis, has become an accepted industry practice, a version of which has been published as part of JIS K 1557. Li
18、censed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI INTERNATIONAL STANDARDISO 14899:2001(E) 1 Plastics Polyols for use in the production of
19、polyurethane Determination of basicity 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 approp
20、riate safety and health practices and to ensure compliance with any national regulatory conditions. 1Scope This International Standard specifies a method for the measurement of trace amounts of basic materials present in polyether polyols used in the production of polyurethanes. It is important to k
21、now the trace amount of basicity in a polyol to prevent gelation of the reaction mass during the production of polyurethane prepolymers. It is also useful to control the basicity in polyols used for polyurethane production to assure consistent and reproducible reaction behaviour. This method is suit
22、able for quality control, as a specification test and for research. The applicable range is 0?g to 50?g/g, expressed as KOH. The method is not applicable to amine-based polyols. The values may be reported as CPR (controlled polymerization rate) units. 2Normative references The following normative do
23、cuments 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 enc
24、ouraged 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
25、3696:1987, Water for analytical laboratory use Specification and test methods. ISO 6353-1:1982, Reagents for chemical analysis Part 1: General test methods. ISO 6353-2:1983, Reagents for chemical analysis Part 2: Specifications First series. ISO 6353-3:1987, Reagents for chemical analysis Part 3: Sp
26、ecifications Second series. 3Terms and definitions For the purposes of this International Standard, the following terms and definitions apply. 3.1 polyurethane a polymer prepared by the reaction of an organic di- or polyisocyanate with compounds containing two or more hydroxyl groups Licensed Copy:
27、sheffieldun sheffieldun, na, Mon Nov 27 08:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 14899:2001(E) 2 3.2 CPR value controlled polymerization rate value the number of microequivalents of base in a 30 g test portion of polyol (i.e. meq of base in 30 kg of polyol) 4Principle A 30 g test port
28、ion of polyol is diluted with methanol and titrated with aqueous 0,01 mol/l HCl. The results are compared with a blank titration of the methanol. 5Sampling Draw samples from a well-mixed vessel into a thoroughly cleaned and dry borosilicate glass container (soft glass containers are not acceptable).
29、 If sampling from a line or valve, flush the line thoroughly with the product before starting to draw the sample. Seal the sample until analysis. 6Interferences Any acidic or basic materials inadvertently introduced into the sample will cause errors in the analysis. Any material capable of serving a
30、s a buffer may interfere with the analysis by obscuring the titration end point. Some samples may contain traces of several different compounds which may have the effect of causing multiple breaks in the titration curve, making interpretation difficult. This analysis is not applicable to amine-based
31、 polyols. 7Reagents Reagent-grade chemicals shall be used in all determinations. Unless otherwise indicated, it is intended that all reagents conform to the specifications of ISO 6353-1, ISO 6353-2 and ISO 6353-3, although other grades may be used provided that it is first determined that the reagen
32、t is of sufficiently high purity to permit its use without lessening the accuracy of the determination. Unless otherwise indicated, references to water shall be understood to mean grade 2 reagent water as defined by ISO 3696:1987. 7.1Hydrochloric acid, standard solution, 0,01 mol/l. Prepare and stan
33、dardize in accordance with good practice, using potassium acid phthalate (7.2) as a primary standard. Standardize to detect changes of 0,000 1 mol/l. 7.2Potassium acid phthalate. Use a certified primary standard. 7.3Methanol, reagent grade, conforming to ISO 6353-2. 8Apparatus 8.1Autotitrator, capab
34、le of determining multiple end points, equipped with a pair of electrodes or a combination glass calomel electrode, a 5 ml burette and a recorder. 8.2Burette, or other automatic dispensing device, capable of dispensing 50 ml?0,1 ml. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:58 GMT
35、+00:00 2006, Uncontrolled Copy, (c) BSI ISO 14899:2001(E) 3 8.3Balance, capable of weighing 30 g test portions to?1 mg. 8.4Titration flask, 100 ml, or other suitable titration vessel. 8.5Magnetic stirrer, equipped with an inert stirrer bar, or equivalent. 9Procedure 9.1Set up the titrator (8.1) for
36、titrations having a maximum titrant volume of 5 ml. 9.2Add 50 ml of methanol (7.3) to a 100 ml titration flask (8.4) for use as a solvent blank. NOTESome popular automatic titrimeters are equipped with 100 ml titration vessels. With other titrimeters, an acceptable variation of the method is to use
37、100 ml of methanol in a 150 ml titration vessel, as is done in JIS K 1557. 9.3Titrate the solvent blank with 0,01 mol/l HCl (7.1) and record the volume of titrant used. The end point is taken as the point of inflection of the last end point on the titration curve. The blank should consume less than
38、0,2 ml of 0,01 mol/l HCl. 9.4Into a 100 ml titration flask, weigh about 30 g of sample to the nearest 1 mg. Add 50 ml of methanol and stir until well mixed. (See the note to 9.2.) 9.5Titrate with 0,01 mol/l HCl and record the volume of titrant up to the last end point. NOTEDepending on the sample be
39、ing analysed, as many as three inflection points may be seen. Use the last end point. 10 Expression of results 10.1Calculate the CPR value using the following equation: CPR value = SB 30 ()1000VVM m ? where VSis the volume of HCl needed to titrate the test portion, in ml; VBis the volume of HCl need
40、ed to titrate the blank, in ml; Mis the molarity of the HCl, in mol/l; mis the mass of the test portion, in g. 10.2The basicity may also be calculated as?g KOH/g of sample using the following equation: ?g KOH/g of sample = SB 56,1 ()1000VVM m ? Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27
41、08:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 14899:2001(E) 4 11 Precision and bias 11.1 Precision 11.1.1Use the criteria for repeatability and reproducibility shown in 11.1.2 and 11.1.3 to judge the acceptability of results. NOTEPrecision data were determined by a round-robin test conduct
42、ed by eight laboratories using five different commercially available polyol samples covering a range of 0,3 CPR units to 1,2 CPR units. Data may be obtained from ASTM Committee D-20 or from the PURMAC committee of the American Plastics Council. 11.1.2Repeatability (single analyst): Duplicate results
43、 obtained by the same analyst using the same equipment on the same day should only be considered suspect if they differ by more than 0,2 CPR units. This repeatability was calculated from pooled experimental data following ASTM E 180. 11.1.3Reproducibility (multilaboratory): Results, each the mean of
44、 duplicates, obtained on identical test materials in separate laboratories should only be considered different if they differ from that of another laboratory by more than 0,6 CPR units. This reproducibility was calculated from pooled experimental data following ASTM E 180. 11.2 Bias Bias is the diff
45、erence between the expectation of the test results and an accepted reference value. The bias of this test has not been determined. 12 Test report The test report shall include the following: a)a reference to this International Standard; b)all details necessary to identify the product analysed; c)the
46、 results obtained, expressed as CPR units to the nearest 0,1 CPR unit, or as?g KOH/g; d)any incident or detail not stipulated in this International Standard which may have influenced the result; e)the date of the analysis. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:58 GMT+00:00 200
47、6, Uncontrolled Copy, (c) BSI ISO 14899:2001(E) 5 Bibliography 1Japanese Industrial Standard K 1557:1970, Testing Method of Polyether for Polyurethane (English translation). 2ASTM E 180, Standard Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial Chemicals.
48、 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:58 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 14899:2001 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 U
49、K view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions British Standards are updated by amendment or revision. Users of British Standards should make sure that they possess the latest amendments or editions. It is the constant aim of BSI to improve the quality of our products and services. We would be grateful if anyone finding an inaccuracy or ambiguity while using this British Standard would inform the Secretary of the technical committee responsible, the identity of which can be found on th
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