1、BRITISH STANDARDBS EN ISO 10283:2007Binders for paints and varnishes Determination of monomeric diisocyanates in isocyanate resinsThe European Standard EN ISO 10283:2007 has the status of a British StandardICS 87.060.20g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g
2、54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN ISO 10283:2007This British Standard was published under the authority of the Standards Policy and Strategy Committe on 28 September 2007 BSI 2007ISBN 978 0 580 59009 2National
3、 forewordThis British Standard is the UK implementation of EN ISO 10283:2007. It supersedes BS EN ISO 10283:2006 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee STI/3, Paints, media and related products.A list of organizations represented on this commi
4、ttee can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations.Amendments issued since publica
5、tionAmd. No. Date CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 10283September 2007ICS 87.060.20English VersionBinders for paints and varnishes - Determination of monomericdiisocyanates in isocyanate resins (ISO 10283:2007)Liants pour peintures et vernis - Dtermination desdiisocyanat
6、es monomres dans les rsines isocyanates(ISO 10283:2007)Bindemittel fr Beschichtungsstoffe - Bestimmung vonmonomeren Diisocyanaten in Isocyanatharzen (ISO10283:2007)This European Standard was approved by CEN on 21 August 2007.CEN members are bound to comply with the CEN/CENELEC Internal Regulations w
7、hich stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European St
8、andard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national sta
9、ndards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kin
10、gdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 10283:2007: E3 For
11、eword This document (EN ISO 10283:2007) has been prepared by Technical Committee ISO/TC 35 “Paints and varnishes“ in collaboration with Technical Committee CEN/TC 139 “Paints and varnishes“, the secretariat of which is held by DIN. This European Standard shall be given the status of a national stand
12、ard, either by publication of an identical text or by endorsement, at the latest by March 2008, and conflicting national standards shall be withdrawn at the latest by March 2008. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bo
13、und to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden,
14、Switzerland and the United Kingdom. Endorsement notice The text of ISO 10283:2007 has been approved by CEN as a EN ISO 10283:2007 without any modification. EN ISO 10283:2007Reference numberISO 10283:2007(E)INTERNATIONAL STANDARD ISO10283Second edition2007-09-01Binders for paints and varnishes Determ
15、ination of monomeric diisocyanates in isocyanate resins Liants pour peintures et vernis Dtermination des diisocyanates monomres dans les rsines isocyanates EN ISO 10283:2007ii iiiContents Page Foreword iv Introduction v 1 Scope . 1 2 Normative references . 1 3 Terms and definitions. 1 4 Principle. 2
16、 5 Reagents 2 6 Apparatus 2 7 Sampling 3 8 Procedure 3 8.1 Operating conditions 3 8.2 Column conditioning 8 8.3 Gas-chromatographic determination 8 9 Expression of results . 9 9.1 Determination of calibration factor. 9 9.2 Calculation of the monomeric diisocyanate content 9 10 Precision 9 10.1 Repea
17、tability (r). 9 10.2 Reproducibility (R) 10 11 Test report . 10 EN ISO 10283:2007iv 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 thro
18、ugh 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 liaison with ISO, also take part in the work. ISO collabor
19、ates 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 2. The main task of technical committees is to prepare International Standa
20、rds. 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
21、his document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 10283 was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Subcommittee SC 10, Test methods for binders for paints and varnishes. This second edition
22、 cancels and replaces the first edition (ISO 10283:1997), in which the normative references clause has been updated. EN ISO 10283:2007vIntroduction It is well-known fact that, due to the production methods used, all the commercial isocyanate resins named in this standard contain a certain amount of
23、volatile monomeric isocyanates. This amount is generally less than 0,5 % relative to the resin as supplied. In view of the regulations relating to the handling of hazardous substances, it has become a matter of special concern that a generally accepted and applicable method of determination should b
24、e available. This standard is not intended to present a method suitable for the analytical determination of volatile isocyanates in any form and in any quantity. The standard specifies a method confined to determining the amounts of volatile isocyanates which occur in practice in isocyanate resins,
25、namely about 0,1 % to 0,4 %. A further objective of the standard was to develop a method for determining with adequate accuracy as many as possible of the monomeric isocyanates which occur in isocyanate resins. It detects the principle isocyanates, namely toluene diisocyanate (TDI), hexamethylene di
26、isocyanate (HDI), diphenylmethane diisocyanate (MDI) and isophorone diisocyanate (IPDI), and is a method considered by industry, authorities and institutes alike to be the state of the art. EN ISO 10283:2007blank1Binders for paints and varnishes Determination of monomeric diisocyanates in isocyanate
27、 resins 1 Scope This International Standard specifies a gas-chromatographic method for determining monomeric diisocyanates such as toluene diisocyanate1), hexamethylene diisocyanate, isophorone diisocyanate2), diphenylmethane diisocyanate3)and other diisocyanates in isocyanate resins as defined in C
28、lause 3 and in solutions prepared from such resins, insofar as these are used in the formulation of paints and similar coating materials. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited app
29、lies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 i
30、socyanate resin synthetic resin, with or without solvent, based on aromatic, aliphatic or cycloaliphatic isocyanates containing isocyanate (NCO) groups NOTE For the purposes of this International Standard, such isocyanate resins comprise: those which are manufactured from any diisocyanate, in partic
31、ular toluene diisocyanate (TDI), hexamethylene diisocyanate (HDI), isophorone diisocyanate (IPDI) or diphenylmethane diisocyanate (MDI), and which contain urethane and/or biuret and/or isocyanurate groups; those which are prepared from mixtures of the isocyanate resins given above. 1) The term “tolu
32、ene diisocyanate” is used here and in the following text for 4-methyl-1,3-phenylene diisocyanate (2,4-toluene diisocyanate) and 2-methyl-1,3-phenylene diisocyanate (2,6-toluene diisocyanate). 2) The term “isophorone diisocyanate” is used here and in the following text for 2-isocyanatomethyl)-3,5,5-t
33、rimethylcyclohexylisocyanate. The stereoisomers are identified at the appropriate points in the text by (I) and (II). 3) The term “diphenylmethane diisocyanate” is used here and in the following text for 4,4-diisocyanatodiphenylmethane, 2,4-diisocyanatodiphenylmethane and 2,2-diisocyanatodiphenylmet
34、hane. EN ISO 10283:20072 4 Principle The content of monomeric diisocyanate in isocyanate resins is determined by gas chromatography, using tetradecane or, in the case of diisocyanates of low volatility, anthracene as the internal standard. 5 Reagents During the analysis, use only reagents of recogni
35、zed analytical grade. 5.1 Ethyl acetate, anhydrous (dried with 0,5 nm molecular sieve) and ethanol-free (ethanol content 0,5 but u 1 1 1 but u 2 0,5 2 but u 4 0,2 4 0,1 Weigh the test sample to the nearest 0,1 mg (mass m0) into a conical flask (6.2). Using the pipette (6.3), add 10 ml of the interna
36、l-standard solution (5.7)4). Add about 25 ml of ethyl acetate, close the conical flask and shake well to dissolve the test sample. NOTE The test sample can also be weighed to the nearest 0,1 mg into a 50 ml sample bottle fitted with a septum seal. Add about (15 0,1) mg of the internal standard to th
37、e sample bottle. Dissolve the sample in 40 ml of ethyl acetate. Examine 1 l of this solution (test solution) by gas chromatography. The following sequence shall be observed for each determination: inject calibration solution at least twice; inject test solution twice. 4) Approx. 15 mg of the interna
38、l standard weighed to an accuracy of 0,1 mg can be used instead of the standard solution. EN ISO 10283:200799 Expression of results 9.1 Determination of calibration factor From each calibration chromatogram, calculate the calibration factor f, using the following equation: DI StSt DImAfmA=where mSti
39、s the mass of internal standard (tetradecane or anthracene) in the internal-standard solution (5.7); mDIis the mass of monomeric diisocyanate in the reference solution (5.8); ADIis the peak area for the monomeric diisocyanate contained in the reference solution; AStis the peak area for the internal
40、standard. 9.2 Calculation of the monomeric diisocyanate content Calculate the content of monomeric diisocyanate wDIfrom the peak areas, using the following equation: 12DI21mA fwmA=where m1is the mass of internal standard in the test solution; m2is the mass of test sample; A2is the peak area for the
41、monomeric diisocyanate in the test solution; A1is the peak area for the internal standard in the test solution. Calculate the mean of two determinations, this mean being corrected by the average value of the calibration factor f calculated for each determination. Detection limit: 0,01 % (by mass) of
42、 the monomeric diisocyanate under the conditions specified in 8.1. 10 Precision for a content of monomeric diisocyanate of (0,50 0,05) % (by mass). 10.1 Repeatability (r) The value below which the absolute difference between two single test results, each the mean of duplicates, obtained on identical
43、 material by one operator in one laboratory within a short interval of time using the standardized test method may be expected to lie with a 95 % probability is 0,02 %. EN ISO 10283:200710 10.2 Reproducibility (R) The value below which the absolute difference between two test results, each the mean
44、of duplicates, obtained on identical material by operators in different laboratories using the standardized test method may be expected to lie with a 95 % probability is 0,05 %. 11 Test report The test report shall contain at least the following information: a) all details necessary to identify the
45、product tested; b) a reference to this International Standard (ISO 10283); c) the individual values and means of the content of monomeric diisocyanates (as indicated in 9.2); d) any deviation from the method specified; e) the date of the test. EN ISO 10283:2007blankBS EN ISO 10283:2007BSI389 Chiswic
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