ISO 11909 2007

Reference numberISO 11909:2007(E)©ISO 2007INTERNATIONAL STANDARD ISO11909Second edition2007-02-01Binders for paints and varnishes — Polyisocyanate resins — General methods of test Liants pour peintures et vernis — Résines de polyisocyanate — Méthodes générales d essai Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 11909:2007(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobe s licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobe s licensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. 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ISO copyright office Case postale 56 • CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyright@iso.org Web www.iso.org Published in Switzerland ii © ISO 2007 – All rights reservedCopyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 11909:2007(E) © ISO 2007 – All rights reserved iiiForeword 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 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 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. 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 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 casting 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 (ISO 11909:1996), which has been editorially revised and the normative references updated. Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---INTERNATIONAL STANDARD ISO 11909:2007(E)© ISO 2007 – All rights reserved 1Binders 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 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 edition 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 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 — Polymers/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 method 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, Clear 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 resins ISO 15528, Paints, varnishes and raw materials for paints and varnishes — Sampling Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 11909:2007(E) 2 © ISO 2007 – All rights reserved3 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 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, 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 determination 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′-diisocyanate IPDI = Isophorone diisocyanate bFor binders dissolved in highly volatile solvents, a lower temperature may be used. Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 11909:2007(E) © ISO 2007 – All rights reserved 3Annex 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 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. 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 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 portion 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 hydroxide 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 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. Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 11909:2007(E) 4 © ISO 2007 – All rights reservedA.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), 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 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 test 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 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 results 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 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. Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 11909:2007(E) © ISO 2007 – All rights reserved 5A.7 Precision NOTE The precision data were obtained with methanol as solvent. The repeatability r and the reproducibility 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 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 11909:2007); c) the result of the test, as indicated in Clause A.6; d) any deviation from the test method specified; e) the date of the test. Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 11909:2007(E) 6 © ISO 2007 – All rights reservedBibliography [1] ISO 4618:2006, Paints and varnishes — Terms and definitions Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---ISO 11909:2007(E) ICS 87.060.20 Price based on 6 pages © ISO 2007 – All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Not for ResaleNo reproduction or networking permitted without license from IHS--`,,```,,,,````-`-`,,`,,`,`,,`---