1、BS EN ISO 15512:2016Plastics Determination ofwater content (ISO 15512:2016)BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS EN ISO 15512:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO 15512:2016. It supersedes BS EN I
2、SO 15512:2014 which iswithdrawn.The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics.A list of organizations represented on this committee can be obtained on request to its secretary.This publication does not purport to include all the necessary pr
3、ovisions of a contract. Users are responsible for its correct application. The British Standards Institution 2016.Published by BSI Standards Limited 2016ISBN 978 0 580 92336 4 ICS 83.080.01 Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was pub
4、lished under the authority of the Standards Policy and Strategy Committee on 30 November 2016.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 15512 November 2016 ICS 83.080.01 Supersedes EN ISO 15512:2014English Versi
5、on Plastics - Determination of water content (ISO 15512:2016) Plastiques - Dosage de leau (ISO 15512:2016) Kunststoffe - Bestimmung des Wassergehaltes (ISO 15512:2016) This European Standard was approved by CEN on 29 September 2016. CEN members are bound to comply with the CEN/CENELEC Internal Regul
6、ations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN membe
7、r. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CE
8、N members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
9、Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in an
10、y form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 15512:2016 EBS EN ISO 15512:2016EN ISO 15512:2016 (E) 3 European foreword This document (EN ISO 15512:2016) has been prepared by Technical Committee ISO/TC 61 “Plastics” in collaboration with Technical Committee CEN
11、/TC 249 “Plastics” the secretariat of which is held by NBN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by May 2017, and conflicting national standards shall be withdrawn at the latest by May 201
12、7. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 15512:2014. According to the CEN-CENELEC Internal R
13、egulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland
14、, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 15512:2016 has been approved by CEN as EN ISO 15512:2016 without any modification. BS EN IS
15、O 15512:2016ISO 15512:2016(E)Foreword vIntroduction vi1 Scope . 12 Normative references 13 Method A Extraction with anhydrous methanol 13.1 Principle 13.2 Reagents 23.3 Apparatus 23.4 Preparation of test sample 23.4.1 Granules or powder . 23.4.2 Finished articles . 23.5 Procedure 33.5.1 Precautions
16、. 33.5.2 Preparation of test portions . 33.5.3 Determination 33.6 Expression of results 33.7 Precision . 44 Method B1 Water vaporization using a heating tube oven . 44.1 Principle 44.2 Reagents 44.3 Apparatus 54.4 Preparation of test sample 74.5 Procedure 74.5.1 Precautions . 74.5.2 Preparation of a
17、pparatus 74.5.3 Equipment check . 74.5.4 Determination 84.6 Expression of results 84.7 Precision . 95 Method B2 Water vaporization using a heated sample vial . 95.1 Principle 95.2 Reagents 95.3 Apparatus . 105.4 Preparation of test sample . 115.5 Procedure . 125.5.1 Preparation of apparatus . 125.5.
18、2 Equipment check 125.5.3 Determination .125.6 Expression of results . 145.7 Precision 146 Method C Manometric method 156.1 Principle . 156.2 Reagents. 156.3 Apparatus . 156.4 Preparation of test sample . 166.5 Procedure . 166.5.1 Equipment 166.5.2 Outgassing 176.5.3 Calibration 176.5.4 Determinatio
19、n .196.6 Expression of results . 206.7 Precision 20 ISO 2016 All rights reserved iiiContents PageBS EN ISO 15512:2016ISO 15512:2016(E)7 Test report 20Annex A (informative) Alternative sample preparation methods and titration methods .21Annex B (informative) Selection of the optimum heating temperatu
20、re for the water content determination 22Annex C (normative) Determination of the water content of a water standard 24Bibliography .25iv ISO 2016 All rights reservedBS EN ISO 15512:2016ISO 15512:2016(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of nati
21、onal 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. Internat
22、ional 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.The procedures used to develop this document and those intende
23、d for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.is
24、o.org/directives).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. Details of any patent rights identified during the development of the document will
25、 be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressio
26、ns related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword Supplementary informationThe committee responsible for this document is ISO/TC 61, Plastics, Subc
27、ommittee SC 5, Physical-chemical properties.This fourth edition cancels and replaces the third edition (ISO 15512:2014), of which it constitutes a minor revision to update information in 6.2.1. ISO 2016 All rights reserved vBS EN ISO 15512:2016ISO 15512:2016(E)IntroductionThe interlaboratory compara
28、bility of the water content determination of plastics is often low. Major causes for this are the sample packaging, sample handling, and differences between equipment and settings. Samples have to, e.g. be packed in special glass containers or water barrier sealed bags. Sample handling is preferably
29、 to be carried out in a dry nitrogen or air environment. For improving the repeatability and reproducibility, the procedure prescribed in this International Standard is intended to be followed strictly.The temperature settings for the vaporization method are not specified in this International Stand
30、ard. For the manometric method, a temperature of 200 C is often used. However, for some condensation materials, this might be too high and could, e.g. cause generation of water due to a condensation reaction.The heating temperature has to be optimized concerning the material to be tested, the equipm
31、ent in use, and the practical circumstances. If the temperature is too low, the total amount of water in the material to be tested will not be evaporated completely, whereas too high temperatures cause water generation due to effects like degradation and condensation reactions.In this International
32、Standard, a procedure is included for optimization of the heating temperature in order to choose the correct temperature for the water content determination and to improve the interlaboratory comparability.vi ISO 2016 All rights reservedBS EN ISO 15512:2016Plastics Determination of water content1 Sc
33、ope1.1 This International Standard specifies methods for the determination of the water content of plastics in the form of powder, granules, and finished articles. These methods do not test for water absorption (kinetics and equilibrium) of plastics as measured by ISO 62.Method A is suitable for the
34、 determination of water content as low as 0,1 % with an accuracy of 0,1 %. Method B and Method C are suitable for the determination of water content as low as 0,01 % with an accuracy of 0,01 %.Water content is an important parameter for processing materials and has to remain below the level specifie
35、d in the appropriate material standard.1.2 Four alternative methods are specified in this International Standard. Method A is an extraction method using anhydrous methanol followed by a Karl Fischer titration of the extracted water. It can be used for all plastics and is applicable to granules small
36、er than 4 mm 4 mm 3 mm. The method can also be used for, e.g. prepolymer materials in the form of a powder that are insoluble in methanol. Method B1 is a vaporization method using a tube oven. The water contained in the test portion is vaporized and carried to the titration cell by a dry air or nitr
37、ogen carrier gas, followed by a Karl Fischer titration of the collected water. It can be used for all plastics and is applicable to granules smaller than 4 mm 4 mm 3 mm. Method B2 is a vaporization method using a heated sample vial. The water contained in the test portion is vaporized and carried to
38、 the titration cell by a dry air or nitrogen carrier gas, followed by a Karl Fischer titration of the collected water. It can be used for all plastics and is applicable to granules smaller than 4 mm 4 mm 3 mm. Method C is a manometric method. The water content is determined from the increase in pres
39、sure, which results when the water is evaporated under a vacuum. This method is not applicable to plastic samples containing volatile compounds, other than water, in amounts contributing significantly to the vapour pressure at room temperature. Checks for the presence of large amounts of volatile co
40、mpounds are to be carried out periodically, for example by gas chromatography. Such checks are particularly required for new types or grades of material.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its appli
41、cation. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 760, Determination of water Karl Fischer method (General method)3 Method A Extraction with anhydrous methanol3.1 PrincipleA test
42、portion is extracted with anhydrous methanol and the extracted water determined by titration using the Karl Fischer method.INTERNATIONAL STANDARD ISO 15512:2016(E) ISO 2016 All rights reserved 1BS EN ISO 15512:2016ISO 15512:2016(E)3.2 ReagentsDuring the analysis, use only reagents of recognized anal
43、ytical grade.3.2.1 Titration medium, methanol anhydrous, having a water content less than 0,1 % by mass. Other solvents can be used if shown to be comparable.3.2.2 Karl Fischer reagent, with an equivalence factor of approximately 3 mg/ml to 5 mg/ml of water. When the reagent is prepared, check its e
44、quivalence factor as specified in ISO 760.3.3 ApparatusOrdinary laboratory apparatus and the following.3.3.1 Glass flasks, approximately 250 ml capacity, provided with a suitable cap preventing moisture uptake or release.3.3.2 Conical titration flasks, approximately 150 ml capacity, with standard gr
45、ound necks and provided with ground-glass stoppers.3.3.3 Reflux condensers, with ground neck capable of being fitted on to the flasks (3.3.2) and on to the tubes (3.3.4).3.3.4 Water-absorption tubes with ground joints, containing calcium chloride or other suitable drying agent.3.3.5 Heaters, suitabl
46、e for the conical titration flasks (3.3.2).3.3.6 Desiccator, containing a suitable desiccant.3.3.7 Analytical balance, accurate to 0,2 mg.3.3.8 Karl Fischer apparatus, for determining water content in accordance with ISO 760.3.4 Preparation of test sample3.4.1 Granules or powderTake a representative
47、 sample of approximately 100 g. Put the sample into a pre-dried glass flask (3.3.1) and immediately close it with a stopper.NOTE It is desirable to pre-dry the container in an oven and then cool it over a suitable desiccant.3.4.2 Finished articlesCut or saw the sample into pieces of appropriate size
48、, i.e. having a maximum size of 4 mm 4 mm 3 mm. Proceed quickly to minimize moisture absorption.2 ISO 2016 All rights reservedBS EN ISO 15512:2016ISO 15512:2016(E)3.5 Procedure3.5.1 PrecautionsDue to the low quantities of water measured, maximum care shall be exercised at all times to avoid contamin
49、ating the sample with water from the sample container, the atmosphere, or transfer equipment. Hygroscopic resin samples shall be protected from the atmosphere.3.5.2 Preparation of test portionsConduct the test on two test portions from the same sample. Use test portions containing 10 mg to 20 mg of water based on the estimated water content of the sample.Using modern coulometric Karl Fischer titration instruments test portions containing less than 10 mg can be applied if the same level of accuracy of results can be ach
