1、BRITISH STANDARDBS EN ISO 11909:2007Binders for paints and varnishes Polyisocyanate resins General methods of testThe European Standard EN ISO 11909:2007 has the status of a British StandardICS 87.060.20g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3
2、g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN ISO 11909:2007This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 March 2007 BSI 2007ISBN 978 0 580 50380 1National forewordThis Briti
3、sh Standard was published by BSI. It is the UK implementation of EN ISO 11909:2007. It supersedes BS EN ISO 11909:1998 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee STI/3, Paints, media and related products.A list of organizations represented on STI/
4、3 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 publicatio
5、nAmd. No. Date CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 11909February 2007ICS 87.060.20 Supersedes 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 polyi
6、socyanate- Mthodes gnrales dessai (ISO 11909:2007)Bindemittel fr Beschichtungsstoffe - Isocyanatharze -Allgemeine 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 c
7、onditions 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 Standard exists in thr
8、ee 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 standards bodies of Aus
9、tria, 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 Kingdom.EUROPEAN COMMIT
10、TEE 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 11909:2007: EForeword This document (E
11、N ISO 11909:2007) 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 publica
12、tion of an identical text or by endorsement, at the latest by August 2007, and conflicting 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 fo
13、llowing countries are bound 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, S
14、lovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 11909:2007 has been approved by CEN as EN ISO 11909:2007 without any modifications. EN ISO 11909:2007Reference numberISO 11909:2007(E)INTERNATIONAL STANDARD ISO11909Second edition2007-02-01Binders for paints a
15、nd varnishes Polyisocyanate resins General methods of test Liants pour peintures et vernis Rsines de polyisocyanate Mthodes gnrales dessai EN ISO 11909:2007ii iiiForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodie
16、s). 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. International organizations, governmental and n
17、on-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. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Pa
18、rt 2. The main task of technical committees is to prepare International Standards. 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 castin
19、g a vote. ISO 11909 was prepared by Technical Committee ISO/TC 35, Paints and varnishes, Subcommittee SC 10, Test methods for binders for paints and varnishes, in collaboration with CEN Technical Committee CEN/TC 139, Paints and varnishes. This second edition cancels and replaces the first edition (
20、ISO 11909:1996), which has been editorially revised and the normative references updated. EN ISO 11909:2007blank1Binders for paints and varnishes Polyisocyanate resins General methods of test 1 Scope This International Standard details general test methods for polyisocyanate resins and solutions of
21、polyisocyanate resins intended for use as binders in paints, varnishes and related products. 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 edit
22、ion of the referenced document (including any amendments) applies. ISO 385, Laboratory 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
23、method ISO 2811-2, Paints and varnishes Determination of density Part 2: Immersed body (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 Polyme
24、rs/resins in the liquid state or as emulsions or dispersions Determination of viscosity 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 meth
25、od ISO 3696, Water for analytical laboratory use Specification and test methods ISO 4630-1, 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, Cl
26、ear liquids Estimation of colour by the platinum-cobalt scale Part 1: Visual method ISO 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 res
27、ins ISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling EN ISO 11909:20072 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 a
28、romatic, aliphatic or cyclo-aliphatic isocyanates ISO 4618:2006 4 Properties and 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
29、ISO 4630-1 or ISO 4630-2 Viscosity ISO 3219 Non-volatile matter ISO 3251, together 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 determ
30、ination of non-volatile matter Resin basis aPeriod of heating Test temperature bh CHDI 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-diis
31、ocyanate IPDI = Isophorone diisocyanate bFor binders dissolved in highly volatile solvents, a lower temperature may be used. EN ISO 11909:20073Annex A (normative) Determination of isocyanate content (percentage by mass of isocyanate groups) A.1 Principle The polyisocyanate resin is reacted with exce
32、ss dibutylamine. The excess dibutylamine is then titrated with hydrochloric 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
33、. A.2.1 Dibutylamine, solutions containing about 2 mol/l and about 0,2 mol/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
34、to the mark with the same toluene and mix well. Standardize this solution 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 portio
35、n with 0,1 mol/l hydrochloric acid (A.2.3). A.2.2 Toluene, previously dried 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 hyd
36、roxide solution, c(NaOH) = 1 mol/l, and dissolve in a mixture of 20 ml of 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
37、ml, with ground-glass stoppers. A.3.2 Potentionmetric titration apparatus, 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. EN ISO 11909:2007
38、4 A.5 Procedure 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),
39、 the appropriate mass of test portion into a 500 ml conical flask and dissolve it in 25 ml of toluene (A.2.2), if necessary with slight heating. After cooling to room temperature, pipette 20 ml of the appropriate dibutylamine solution (A.2.1) into the flask. Close the flask and allow to stand for 15
40、 min, swirling occasionally. Dilute with 150 ml of ethanol (A.2.4), add a few drops of bromophenol blue solution (A.2.5) and titrate with the appropriate hydrochloric acid (A.2.3) until the colour changes to yellow. If separation occurs during the titration, add further ethanol. Table A.1 Mass of te
41、st portion and permitted difference between results Isocyanate content Maximum mass of test portion Permitted difference between individual values and mean value % (by mass) g % (absolute) below 1 25 1 to 10 12 above 10 to 20 6 above 20 to 25 5 0,15 above 25 to 30 4 above 30 to 40 3,5 above 40 to 50
42、 3 0,2 If 0,1 mol/l hydrochloric acid is used, the test portion shall be weighed to the nearest 0,1 mg, its mass shall be about one-tenth that in Table A.1 and the 0,2 ml/l dibutylamine solution shall be used. In the case of highly coloured resins, titrate potentiometrically. A.6 Expression of resul
43、ts Calculate the isocyanate content, IC, expressed as a percentage by mass, using the following equation: (),12IC 4 2VV cm= where V1is the volume, in millilitres, of hydrochloric acid required for the standardization of the dibutylamine solution; V2is the volume, in millilitres, of hydrochloric acid
44、 required for the determination; c is the actual concentration, in moles per litre, of the hydrochloric acid used; m is the mass, in grams, of the test portion. EN ISO 11909:20075A.7 Precision NOTE The precision data were obtained with methanol as solvent. The repeatability r and the reproducibility
45、 R depend on the product tested. Repeatability Reproducibility r R IPDI trimer NCO content about 12 % (by mass) 0,11 0,34 HDI biuret NCO content about 16 % (by mass) 0,36 0,50 TDI adduct NCO content about 13 % (by mass) 0,19 0,27 MDI prepolymer NCO content about 7 % (by mass) 0,55 0,67 A.8 Test repo
46、rt 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 11909:2007); c) the result of the test, as indicated in Clause A.6; d) any deviation from the test method specified; e) the
47、 date of the test. EN ISO 11909:20076 Bibliography 1 ISO 4618:2006, Paints and varnishes Terms and definitions EN ISO 11909:2007blankBS EN ISO 11909:2007BSI389 Chiswick High RoadLondonW4 4ALBSI British Standards InstitutionBSI is the independent national body responsible for preparing British Standa
48、rds. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter.RevisionsBritish 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
49、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 the inside front cover. Tel: +44 (0)20 8996 9000. Fax: +44 (0)20 8996 7400.BSI offers members an individual updating service called PLUS which ensures that subscribers automatically receive the latest editions of s
