1、May 2007DEUTSCHE NORM English price group 9No 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!,xbC“9856332www.d
2、in.deDDIN EN ISO 11909Binders for paints and varnishes Polyisocyanate resins General methods of test (ISO 11909:2007)English version of DIN EN ISO 11909:2007-05Bindemittel fr Beschichtungsstoffe Isocyanatharze Allgemeine Prfverfahren (ISO 11909:2007)Englische Fassung DIN EN ISO 11909:2007-05Supersed
3、esDIN EN ISO 11909:1998-12www.beuth.deDocument comprises 12 pages08.07DIN EN ISO 11909:2007-05 2 National foreword This standard falls in the domain of Technical Committee CEN/TC 139 “Paints and varnishes” (Secretariat: DIN, Germany). It is identical with International Standard ISO 11909 which was p
4、repared by Technical Committee ISO/TC 35/SC 10 “Test methods for binders for paints and varnishes” (Secretariat: DIN, Germany). The responsible German body involved in its preparation was the Normenausschuss Beschichtungsstoffe und Beschichtungen (Coatings and Coating Materials Standards Committee),
5、 Technical Committee 2 Lackroh-stoffe. In subclause A.2.1 of ISO 11909:2007 the pressure of the boiling point of water-free distilled dibutylamine is given as being 1,033 kPa, which is incorrect. The correct value of 1 013,25 hPA (normal pressure) is given in the German version of EN ISO 11909:2007
6、and is corrected in a footnote in this English version. The DIN Standards corresponding to the International Standards referred to in this standard are as follows: ISO 385 DIN EN ISO 385 ISO 648 DIN 12690 ISO 1523 DIN EN ISO 1523 ISO 2811-1 DIN EN ISO 2811-1 ISO 2811-2 DIN EN ISO 2811-2 ISO 2811-3 D
7、IN EN ISO 2811-3 ISO 2811-4 DIN EN ISO 2811-4 ISO 3219 DIN EN ISO 3219 ISO 3251 DIN EN ISO 3251 ISO 3679 DIN EN ISO 3679 ISO 3696 DIN ISO 3696 ISO 4618 DIN EN ISO 4618 ISO 4630-1 DIN EN ISO 4630-1 ISO 4630-2 DIN EN ISO 4630-2 ISO 6271-1 DIN EN ISO 6271-1 ISO 6271-2 DIN EN ISO 6271-2 ISO 10283 DIN EN
8、 ISO 10283 ISO 15528 DIN EN ISO 15528 Amendments This standard differs from DIN ISO 11909:1998-12 as follows: a) The normative references has been updated. b) The standard has been editorially revised. Previous editions DIN 53185: 1974-12, 1997-05 DIN EN ISO 11909: 1998-06, 1998-12 DIN EN ISO 11909:
9、2007-05 3 National Annex NA (informative) Detailed precision data for the determination of the isocyanate content The precision data given in A.7 for the determination of the isocyanate content were obtained in an interlaboratory test involving four laboratories. The detailed results were as follows
10、. Table NA.1 Precision data MDI prepolymer Desmodur E 22 HDI biuret Desmodur N 75 TDI adduct or urethane-modified TDI Desmodur L 75 Isocyanate- modified IPDI Vestanat T 1890 L 1 s 1 r (95) 1 7,79 0,01 0,04 16,5 0,04 0,11 13,14 0,03 0,089 11,99 0,05 0,13 2 s 2 r (95) 2 7,67 0,03 0,08 15,99 0,06 0,15
11、13,02 0,03 0,07 11,87 0,02 0,03 3 s 3 r (95) 3 7,4 0,39 1,08 16,34 0,24 0,67 13,17 0,13 0,35 12,18 0,05 0,13 4 s 4 r (95) 4 7,57 0,04 0,12 16,22 0,05 0,13 13,19 0,05 0,14 12,03 0,05 0,13 sr(mean) r (95) for srsRR (95) 7,61 0,2 0,55 0,24 0,67 16,18 0,13 0,36 0,18 0,49 13,13 0,07 0,19 0,1 0,27 12,02 0
12、,04 0,11 0,12 0,34 where 1 is the mean value obtained by laboratory 1 s 1 is the repeatability standard deviation obtained by laboratory 1 r (95) 1 is the repeatability limit obtained by laboratory 1 (confidence level 95 %) 2 is the mean value obtained by laboratory 2 s 2 is the repeatability standa
13、rd deviation obtained by laboratory 2 r (95) 2 is the repeatability limit obtained by laboratory 2 (confidence level 95 %) 3 is the mean value obtained by laboratory 3 s 3 is the repeatability standard deviation obtained by laboratory 3 r (95) 3 is the repeatability limit obtained by laboratory 3 (c
14、onfidence level 95 %) 4 is the mean value obtained by laboratory 4 s 4 is the repeatability standard deviation obtained by laboratory 4 r (95) 4 is the repeatability limit obtained by laboratory 4 (confidence level 95 %) DIN EN ISO 11909:2007-05 4 is the overall mean sr(mean) is the variation of res
15、ults among all laboratories r (95) for sris the mean internal repeatability limit for all laboratories (confidence level 95 %) sRis the reproducibility standard deviation R (95) is the reproducibility limit for all laboratories (confidence level 95 %) National Annex NB (informative) Bibliography DIN
16、 12690, Class A and class B one-mark bulb pipettes for laboratory use DIN EN ISO 385, Laboratory glassware Burettes DIN EN ISO 1523, Determination of flash point Closed cup equilibrium method DIN EN ISO 2811-1, Paints and varnishes Determination of density Part 1: Pyknometer method DIN EN ISO 2811-2
17、, Paints and varnishes Determination of density Part 2: Immersed body (plummet) method DIN EN ISO 2811-3, Paints and varnishes Determination of density Part 3: Oscillation method DIN EN ISO 2811-4, Paints and varnishes Determination of density Part 4: Pressure cup method DIN EN ISO 3219, Plastics Po
18、lymers/resins in the liquid state or as emulsions or dispersions Determination of viscosity using a rotational viscometer with defined shear rate DIN EN ISO 3251, Paints, varnishes and plastics Determination of non-volatile matter content DIN EN ISO 3679, Determination of flash point Rapid equilibri
19、um closed cup method DIN EN ISO 4618, Paints and varnishes Terms and definitions DIN EN ISO 4630-1, Clear liquids Estimation of colour by the Gardner colour scale Part 1: Visual method DIN EN ISO 4630-2, Clear liquids Estimation of colour by the Gardner colour scale Part 2: Spectrophotometric method
20、 DIN EN ISO 6271-1, Clear liquids Estimation of colour by the platinum-cobalt scale Part 1: Visual method DIN EN ISO 6271-2, Clear liquids Estimation of colour by the platinum-cobalt scale Part 2: Spectrophotometric method DIN EN ISO 10283, Binders for paints and varnishes Determination of monomeric
21、 diisocyanates in polyisocyanate resins DIN EN ISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling DIN ISO 3696, Water for analytical laboratory use Specification and test methods EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 11909February 2007ICS 87.060.20 Super
22、sedes EN ISO 11909:1998 English VersionBinders for paints and varnishes - Polyisocyanate resins -General methods of test (ISO 11909:2007)Liants pour peintures et vernis - Rsines de polyisocyanate- Mthodes gnrales dessai (ISO 11909:2007)Bindemittel fr Beschichtungsstoffe - Isocyanatharze -Allgemeine
23、Prfverfahren (ISO 11909:2007)This European Standard was approved by CEN on 6 February 2007.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date li
24、sts and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management 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 translationunder the respo
25、nsibility 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 standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Icela
26、nd, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stass
27、art, 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 11909:2007: EEN ISO 11909:2007 (E) 2Foreword This document (EN ISO 11909:2007) has been prepared by Technical Committee ISO/TC 35 “Paints and varnishes”
28、 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 publication of an identical text or by endorsement, at the latest by August 2007, and conflicting
29、national standards shall be withdrawn at the latest by August 2007. This document supersedes EN ISO 11909:1998. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria
30、, 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 Kingdom. Endorsement notice The text of ISO
31、11909:2007 has been approved by CEN as EN ISO 11909:2007 without any modifications. EN ISO 11909:2007 (E) 31 Scope This International Standard details general test methods for polyisocyanate resins and solutions of polyisocyanate resins intended for use as binders in paints, varnishes and related pr
32、oducts. 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 document (including any amendments) applies. ISO 385, Laborator
33、y glassware Burettes ISO 648, Laboratory glassware One-mark pipettes ISO 1523, Determination of flash point Closed cup equilibrium method ISO 2811-1, Paints and varnishes Determination of density Part 1: Pyknometer method ISO 2811-2, Paints and varnishes Determination of density Part 2: Immersed bod
34、y (plummet) method ISO 2811-3, Paints and varnishes Determination of density Part 3: Oscillation method ISO 2811-4, Paints and varnishes Determination of density Part 4: Pressure cup method ISO 3219, Plastics Polymers/resins in the liquid state or as emulsions or dispersions Determination of viscosi
35、ty using a rotational viscometer with defined shear rate ISO 3251, Paints, varnishes and plastics Determination of non-volatile-matter content ISO 3679, Determination of flash point Rapid equilibrium closed cup method ISO 3696, Water for analytical laboratory use Specification and test methods ISO 4
36、630-1, Clear liquids Estimation of colour by the Gardner colour scale Part 1: Visual method ISO 4630-2, Clear liquids Estimation of colour by the Gardner colour scale Part 2: Spectrophotometric method ISO 6271-1, Clear liquids Estimation of colour by the platinum-cobalt scale Part 1: Visual method I
37、SO 6271-2, Clear liquids Estimation of colour by the platinum-cobalt scale Part 2: Spectrophotometric method ISO 10283, Binders for paints and varnishes Determination of monomeric diisocyanates in polyisocyanate resins ISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling
38、EN ISO 11909:2007 (E) 4 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 isocyanate resin synthetic resin, containing free or blocked isocyanate groups, based on aromatic, aliphatic or cyclo-aliphatic isocyanates ISO 4618:2006 4 Properties and
39、 test methods Unless otherwise agreed, the properties to be measured and the test methods to be used shall be as given in Table 1. Table 1 Properties and test methods Property Test method Colour ISO 6271-1 or ISO 6271-2 ISO 4630-1 or ISO 4630-2 Viscosity ISO 3219 Non-volatile matter ISO 3251, togeth
40、er with Table 2 below Flashpoint ISO 1523 or ISO 3679 Density ISO 2811-1 to 2811-4 Isocyanate content Annex A of this International Standard Monomeric diisocyanate content ISO 10283 Table 2 Test conditions for the determination of non-volatile matter Resin basis aPeriod of heating Test temperature b
41、h C HDI biuret 1 80 HDI cyanurate 1 105 TDI and MDI polyisocyanates, adducts and prepolymers 1 125 IPDI polyisocyanates 1 150 aHDI = Hexamethylene diisocyanate TDI = Tolylene diisocyanate MDI = Diphenyl-4-methane-4,4-diisocyanate IPDI = Isophorone diisocyanate bFor binders dissolved in highly volati
42、le solvents, a lower temperature may be used. EN ISO 11909:2007 (E) 5Annex A (normative) Determination of isocyanate content (percentage by mass of isocyanate groups) A.1 Principle The polyisocyanate resin is reacted with excess dibutylamine. The excess dibutylamine is then titrated with hydrochlori
43、c acid, either using bromophenol blue as the indicator or potentiometrically. A.2 Reagents During the analysis, use only reagents of recognized analytical grade, and only water of at least grade 3 purity as defined in ISO 3696. A.2.1 Dibutylamine, solutions containing about 2 mol/l and about 0,2 mol
44、/l, respectively. To prepare the approximately 2 mol/l solution, dissolve 65 g of water-free distilled dibutylamine (boiling point 157 C to 162 C at 1,033 kPa)*)in toluene (A.2.2) in a 250 ml one-mark volumetric flask, make up to the mark with the same toluene and mix well. Standardize this solution
45、 by titrating a 20 ml portion with 1 mol/l hydrochloric acid (A.2.3). Prepare the approximately 0,2 mol/l solution in analogous fashion, starting with 6,5 g of dibutylamine. Standardize this solution by titrating a 20 ml portion with 0,1 mol/l hydrochloric acid (A.2.3). A.2.2 Toluene, previously dri
46、ed over calcium chloride and filtered. A.2.3 Hydrochloric acid, c(HCl) = 1 mol/l or 0,1 mol/l. A.2.4 Ethanol, water-free. A.2.5 Bromophenol blue, solution. Triturate 1 g of bromophenol blue in a mortar with 1,5 ml of sodium hydroxide solution, c(NaOH) = 1 mol/l, and dissolve in a mixture of 20 ml of
47、 ethanol (A.2.4) and 10 ml of water. A.3 Apparatus Ordinary laboratory apparatus and glassware, complying with the requirements of ISO 385 and ISO 648, together with the following: A.3.1 Conical flasks, capacity 250 ml and 500 ml, with ground-glass stoppers. A.3.2 Potentionmetric titration apparatus
48、, fitted with a glass electrode and a reference electrode (for use with highly coloured resins see Clause A.5). A.4 Sampling Take a representative sample of the product to be tested, as described in ISO 15528. *)In DIN EN ISO 11909 this is corrected to 1 013,25 hPa. EN ISO 11909:2007 (E) 6 A.5 Proce
49、dure Carry out the determination in duplicate. By reference to Table A.1, select the appropriate mass of test portion. If the approximate isocyanate content is not known, carry out a preliminary determination using a test portion of 3,5 g. Weigh, to the nearest 1 mg (or 0,1 mg see below), the appropriate mass of test portion into a 500 ml conical flask and dissolve it in 25 ml o
