BS-EN-ISO-11909-1998 BS-6782-9-1996.pdf

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1、BRITISH STANDARD BS EN ISO 11909:1998 BS 6782-9: 1996 Incorporating Amendment No. 1 to BS 6782-9:1996 (renumbers the BS as BS EN ISO 11909:1998), not published separately Binders for paints and varnishes Polyisocyanate resins General methods of test ICS 87.060.20 Licensed Copy: sheffieldun sheffield

2、un, na, Mon Nov 20 02:58:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 11909:1998 This British Standard, having been prepared under the direction of the Sector Board for Materials and Chemicals, was published under the authority of the Standards Board and comes into effect on 15 November 1

3、996 BSI 05-1999 The following BSI references relate to the work on this standard: Committee reference STI/3 Draft for comment 92/56696 DC ISBN 0 580 26478 5 Committees responsible for this British Standard The preparation of this British Standard was entrusted to Technical Committee STI/3, Paints, m

4、edia and related products, upon which the following bodies were represented: British Coatings Federation Ltd. European Resin Manufacturers Association FOSFA International Ministry of Defence Oil and Colour Chemists Association Seed Crushers and Oil Processors Association Amendments issued since publ

5、ication Amd. No.DateComments 10179October 1998 Indicated by a sideline in the margin Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:58:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 11909:1998 BSI 05-1999i Contents Page Committees responsibleInside front cover National forewordii

6、 Foreword2 1Scope3 2Normative references3 3Definition3 4Properties and test methods3 Annex A (normative) Determination of isocyanate content (percentage by mass of isocyanate groups)5 Annex ZA (normative) Normative references to international publications with their relevant European publications7 T

7、able 1 Properties and test methods3 Table 2 Test conditions for the determination of non-volatile matter4 Table A.1 Mass of test portion and permitted difference between results6 List of referencesInside back cover Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:58:43 GMT+00:00 2006, Uncon

8、trolled Copy, (c) BSI BS EN ISO 11909:1998 ii BSI 05-1999 National foreword This Part of BS 6782 has been prepared by Technical Committee STI/3. It is identical with ISO 11909:1996 Binders for paints and varnishes Polyisocyanate resins General methods of test, published by the International Organiza

9、tion for Standardization (ISO). In 1998 the European Committee for Standardization (CEN) accepted ISO 11909:1996 as European Standard EN ISO 11909:1998. The Technical Committee has reviewed the provisions of ISO 385-1:1984, ISO 648:1977, ISO 3679:1983, ISO 6271:1981 and ISO 10283 to which normative

10、reference is made in the text, and has decided that they are acceptable for use in conjunction with this standard. British Standards related to ISO 385-1:1984, ISO 648:1977 and ISO 3679:1983 are BS 846:1985, BS 1583:1986 and BS EN 456:1991 respectively. A British Standard does not purport to include

11、 all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Cross-reference Publication referred to Corresponding British Standard ISO 3696:1987BS

12、EN ISO 3696:1995 Water for analytical laboratory use Specification and test methods (Identical) Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN ISO title page, pages 2 to 8, an inside back cover and a back cover. This standard has been updated (s

13、ee copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:58:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11

14、909 April 1998 ICS 87.060.20 Descriptors: Paints, varnishes, binders (materials), synthetic resins isocyanates, tests, physical tests, chemical tests English version Binders for paints and varnishes Polyisocyanate resins General methods of test (ISO 11909:1996) Liants pour peintures et vernis Rsines

15、 de polyisocyanate Mthodes gnrales dessai (ISO 11909:1996) Bindemittel fr Beschichtungsstoffe Polyisocyanate Allgemeine Prfverfahren (ISO 11909:1996) This European Standard was approved by CEN on 26 March 1998. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate

16、 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 Central Secretariat or to any CEN member. This European Standard exists

17、 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 Central Secretariat has the same status as the official versions. CEN members are the national standards bodie

18、s of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normun

19、g Central Secretariat: rue de Stassart 36, B-1050 Brussels 1998 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11909:1998 E Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:58:43 GMT+00:00 2006, Uncontrolled Copy, (c)

20、 BSI EN ISO 11909:1998 BSI 05-1999 2 Foreword The text of the International Standard from Technical Committee ISO/TC 35, Paints and varnishes, of the International Organization for Standardization (ISO) has been taken over as an European Standard by Technical Committee CEN/TC 139, Paints and varnish

21、es, 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 month of October 1998, and conflicting national standards shall be withdrawn at the latest by October 1

22、998. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway

23、, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard ISO 11909:1996 has been approved by CEN as a European Standard without any modification. NOTENormative references to International Standards are listed in Annex ZA (normative). Li

24、censed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:58:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 11909:1998 BSI 05-19993 1 Scope This International Standard details general test methods for polyisocyanate resins and solutions of polyisocyanate resins intended for use as binders in

25、paints, varnishes and related products. 2 Normative references The following standards contain provisions which, through reference in this text, constitute provisions of this International Standard. At the time of publication, the editions indicated were valid. All standards are subject to revision,

26、 and parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain registers of currently valid International Standards. ISO 385-1:1984, Laboratory glassw

27、are Burettes Part 1: General requirements. ISO 648:1977, Laboratory glassware One-mark pipettes. ISO 842:1984, Raw materials for paints and varnishes Sampling. ISO 1523:1983, Paints, varnishes, petroleum and related products Determination of flashpoint Closed cup equilibrium method. ISO 2811:1974, P

28、aints and varnishes Determination of density. ISO 3219:1993, Plastics Polymers/resins in the liquid state or as emulsions or dispersions Determination of viscosity using a rotational viscometer with defined shear rate. ISO 3251:1993, Paints and varnishes Determination of non-volatile matter of paint

29、s, varnishes and binders for paints and varnishes. ISO 3679:1983, Paints, varnishes, petroleum and related products Determination of flashpoint Rapid equilibrium method. ISO 3696:1987, Water for analytical laboratory use Specification and test methods. ISO 4630:1981, Binders for paints and varnishes

30、 Estimation of colour of clear liquids by the Gardner colour scale. ISO 6271:1981, Clear liquids Estimation of colour by the platinum-cobalt scale. ISO 10283:, Binders for paints and varnishes Determination of monomeric diisocyanates in polyisocyanate resins1). 3 Definition For the purposes of this

31、International Standard, the following definition applies. 3.1 polyisocyanate resin synthetic resin containing reactive isocyanate groups and based on aromatic, aliphatic or cycloaliphatic isocyanates 4 Properties and test methods Unless otherwise agreed, the properties to be measured and the test me

32、thods to be used shall be as given in Table 1. Table 1 Properties and test methods 1) To be published. PropertyTest method ColourISO 6271 (Platinum-cobalt scale) or ISO 4630 (Gardner colour scale) ViscosityISO 3219 Non-volatile matterISO 3251, together with Table 2 below FlashpointISO 1523 or ISO 36

33、79 DensityISO 2811 Isocyanate contentAnnex A of this International Standard Monomeric diisocyanate contentISO 10283 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:58:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 11909:1998 4 BSI 05-1999 Table 2 Test conditions for the determinat

34、ion of non-volatile matter Resin basisa Period of heating h Test temperatureb C HDI biuret180 HDI cyanurate1105 TDI and MDI polyisocyanates, adducts and prepolymers 1125 IPDI polyisocyanates1150 a HDI = Hexamethylene diisocyanate TDI = Tolylene diisocyanate MDI = Diphenyl-4-methane-4,49-diisocyanate

35、 IPDI = Isophorone diisocyanate b For binders dissolved in highly volatile solvents, a lower temperature may be used. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:58:43 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 11909:1998 BSI 05-19995 Annex A (normative) Determination of isoc

36、yanate 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

37、, 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 dibutyl

38、amine (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 (see A.2.3). Prepare the approximately 0,2 mol/l s

39、olution 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 (see 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 Et

40、hanol, 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, complyi

41、ng with the requirements of ISO 385-1 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 Potentiometric titration apparatus, fitted with a glass electrode and a reference electrode (for use with highly coloured resins see A.5

42、). A.4 Sampling Take a representative sample of the product to be tested, as described in ISO 842. 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 prelimina

43、ry 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 ap

44、propriate 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 change

45、s to yellow. If separation occurs during the titration, add further ethanol. 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 mol/l dibutylamine solution shall be used. In the case of high

46、ly coloured resins, titrate potentiometrically. A.6 Expression of results Calculate the isocyanate content IC, expressed as a percentage by mass, using the following equation: where V1is the volume, in millilitres, of hydrochloric acid required for the standardization of the dibutylamine solution; V

47、2is the volume, in millilitres, of hydrochloric acid required for the determination; cis the actual concentration, in moles per litre, of the hydrochloric acid used; mis the mass, in grams, of the test portion. IC V1V2()c m - -4 ,2= Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:58:43 GMT

48、+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 11909:1998 6 BSI 05-1999 Table A.1 Mass of test portion and permitted difference between results A.7 Precision NOTE 1The precision data were obtained with methanol as solvent. The repeatability r and the reproducibility R depend on the product tested

49、. 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); 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. Isocyanate content % (m/m) Maximum mass of test portion g Permitted difference between individual values and mean value % (abs

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