1、November 2007DEUTSCHE NORM English price group 10No part of this standard may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 87.060.20!$JKH“139403
2、7www.din.deDDIN EN ISO 10283Binders for paints and varnishes Determination of monomeric diisocyanates in isocyanate resins(ISO 10283:2007)English version of DIN EN ISO 10283:2007-11Bindemittel fr Beschichtungsstoffe Bestimmung von monomeren Diisocyanaten in Isocyanatharzen (ISO 10283:2007)Englische
3、Fassung DIN EN ISO 10283:2007-11SupersedesDIN EN ISO 10283:2006-04www.beuth.deDocument comprises 16 pagesDIN EN ISO 10283:2007-11 2 National foreword This standard falls within the responsibility of Technical Committee CEN/TC 139 “Paints and varnishes” (Secretariat: DIN, Germany). It is identical wi
4、th International Standard ISO 10283 which was prepared by Technical Committee ISO/TC 35 “Paints and varnishes”, Subcommittee SC 10 “Test methods for binders for paints and varnishes” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Beschich
5、tungsstoffe und Beschichtungen (Coatings and Coating Materials Standards Committee), Technical Committee NA 002-00-02 AA Lackrohstoffe. In this standard, the unit “ppm” is used. It should, however, be noted that the Gesetz ber Einheiten im Mess-wesen (German Law on units in metrology) prohibits the
6、use of the unit “ppm” for official and commercial purposes in Germany. Note to 8.1.1, 8.1.2, 8.1.3 and 8.1.4: OVis the trade name of the columns supplied by Ohio Valey Specialty Chemical Co. This information is given for the convenience of users of this document and does not constitute an endorsemen
7、t by ISO or CEN of the product named. Equivalent products may be used if they can be shown to lead to the same results. The DIN Standard corresponding to the International Standard referred to in clause 2 of the EN is as follows: ISO 15528 DIN EN ISO 15528 Amendments This standard differs from DIN E
8、N ISO 10283:2006-04 as follows: a) Concerns the German version only. b) The normative references have been updated. c) Concerns the German version only. Previous editions DIN 55956: 1982-11, 1996-10 DIN EN ISO 10283: 2006-04 National Annex NA (informative) Bibliography DIN EN ISO 15528, Paints, varn
9、ishes and raw materials for paints and varnishes Sampling EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 10283 September 2007 ICS 87.060.20 English Version Binders for paints and varnishes - Determination of monomeric diisocyanates in isocyanate resins (ISO 10283:2007) Liants pour peinture
10、s et vernis - Dtermination des diisocyanates monomres dans les rsines isocyanates (ISO 10283:2007) Bindemittel fr Beschichtungsstoffe - Bestimmung von monomeren Diisocyanaten in Isocyanatharzen (ISO 10283:2007) This European Standard was approved by CEN on 21 August 2007. CEN members are bound to co
11、mply with the CEN/CENELEC Internal Regulations 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 Manag
12、ement Centre or to any CEN member. 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 Management Centre has the same status as t
13、he official versions. CEN members are the national standards 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, Slova
14、kia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2007 CEN All rights of exploitation in any form and by any means reserved worldwid
15、e for CEN national Members. Ref. No. EN ISO 10283:2007: EContents Page 2 EN ISO 10283:2007 (E) Foreword 3 Introduction 4 1 Scope . 5 2 Normative references . 5 3 Terms and definitions 5 4 Principle 6 5 Reagents . 6 6 Apparatus 6 7 Sampling . 7 8 Procedure 7 8.1 Operating conditions . 7 8.2 Column co
16、nditioning 12 8.3 Gas-chromatographic determination .12 9 Expression of results .13 9.1 Determination of calibration factor 13 9.2 Calculation of the monomeric diisocyanate content 13 10 Precision .13 10.1 Repeatability (r) 13 10.2 Reproducibility (R) 14 11 Test report 14 Foreword This document (EN
17、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 standard, either by publicati
18、on 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 bound to implement this Eu
19、ropean 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, Switzerland and the Unit
20、ed Kingdom. Endorsement notice The text of ISO 10283:2007 has been approved by CEN as a EN ISO 10283:2007 without any modification. 3 EN ISO 10283:2007 (E) Introduction It is well-known fact that, due to the production methods used, all the commercial isocyanate resins named in this standard contain
21、 a certain amount of 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 d
22、etermination should be 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 i
23、n isocyanate resins, 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 (T
24、DI), hexamethylene diisocyanate (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. 4 EN ISO 10283:2007 (E) 1 Scope This International Standard specifies a gas-chromatograph
25、ic method for determining monomeric diisocyanates such as toluene diisocyanate1), hexamethylene diisocyanate, isophorone diisocyanate2), diphenylmethane diisocyanate3)and other diisocyanates in isocyanate resins as defined in Clause 3 and in solutions prepared from such resins, insofar as these are
26、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 applies. For undated references, the latest edition of the referenced docume
27、nt (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 isocyanate resin synthetic resin, with or without solvent, based on aromat
28、ic, 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 particular toluene diisocyanate (TDI), hexamethylene diisocyanate (HDI), isopho
29、rone 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 “toluene diisocyanate” is used here and in the following text for 4-methyl-1,3
30、-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-trimethylcyclohexylisocyanate. The stereoisomers are identified at the app
31、ropriate 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-diisocyanatodiphenylmethane. 5 EN ISO 10283:2007 (E) 4 Principle The content of monomeric diisoc
32、yanate 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 recognized analytical grade. 5.1 Ethyl acetate, anhydrous (dried with 0,5 n
33、m 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 internal-standard solution (5.7)4). Add about 25 ml of ethyl acetate, close
34、 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 the sample bottle. Dissolve the sample in 40 ml of ethyl acetate. Exam
35、ine 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 internal standard weighed to an accuracy of 0,1 mg can be used instead of t
36、he standard solution. 12 EN ISO 10283:2007 (E) 9 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 mStis the mass of internal standard (tetradecane or anthracene) i
37、n 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 standard. 9.2 Calculation of the monomeric diisocyanate conte
38、nt 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 monomeric diisocyanate in the test solution; A1is the peak ar
39、ea 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 the monomeric diisocyanate under the conditions specified in
40、 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 material by one operator in one laboratory within a short in
41、terval of time using the standardized test method may be expected to lie with a 95 % probability is 0,02 %. 13 EN ISO 10283:2007 (E) 10.2 Reproducibility (R) The value below which the absolute difference between two test results, each the mean of duplicates, obtained on identical material by operato
42、rs 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 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. 14 EN ISO 10283:2007 (E)
