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!,xb5“9856318www.d
2、in.deDDIN EN ISO 7142Binders for paints and varnishes Epoxy resins General methods of test (ISO 7142:2007)English version of DIN EN ISO 7142:2007-05Bindemittel fr Beschichtungsstoffe Epoxidharze Allgemeine Prfverfahren (ISO 7142:2007)Englische Fassung DIN EN ISO 7142:2007-05SupersedesDIN EN ISO 7142
3、:2004-09www.beuth.deDocument comprises 13 pages 08.07DIN EN ISO 7142:2007-05 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 7142 which was prepared by ISO/TC 3
4、5/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), Technical Committee NA 002-00-02 AA La
5、ckrohstoffe. The DIN Standards corresponding to the International Standards referred to in the EN are as follows: ISO 385 DIN EN ISO 385 ISO 648 DIN 12690 ISO 1523 DIN EN ISO 1523 ISO 2431 DIN EN ISO 2431 ISO 3001 DIN EN ISO 3001 ISO 3146 DIN EN ISO 3146 ISO 3219 DIN EN ISO 3219 ISO 3251 DIN EN ISO
6、3251 ISO 3679 DIN EN ISO 3679 ISO 4615 DIN EN ISO 4615 ISO 4618 DIN EN ISO 4618 ISO 4625-1 DIN EN ISO 4625-1 ISO 4625-2 DIN EN ISO 4625-2 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 15528 DIN EN ISO 15528 ISO 21627-1 DIN EN
7、ISO 21627-1 Amendments This standard differs from DIN EN ISO 7142:2004-09 as follows: a) The normative references have been updated. b) The standard has been editorially revised. Previous editions DIN 53188: 1975-10 DIN EN ISO 7142: 2004-09 DIN EN ISO 7142:2007-05 3 National Annex NA (informative) B
8、ibliography DIN 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 2431, Paints and varnishes Determination of flow time by use of flow cups DIN EN I
9、SO 3001, Plastics Epoxide compounds Determination of epoxide equivalent DIN EN ISO 3146, Plastics Determination of melting behaviour (melting temperature or melting range) of semi-crystalline polymers by capillary tube and polarizing-microscope methods DIN EN ISO 3219, Plastics Polymers/resins in th
10、e liquid state or as emulsions or dispersions Determination of viscosity using a rotational viscometer with defined shear rate DIN ISO 3251, Paints, varnishes and plastics Determination of non-volatile matter content DIN EN ISO 3679, Determination of flash point Rapid equilibrium closed cup method D
11、IN EN ISO 4615, Plastics Unsaturated polyesters and epoxide resins Determination of total chlorine content DIN EN ISO 4618, Paints and varnishes Terms and definitions DIN EN ISO 4625-1, Binders for paints and varnishes Determination of softening point Part 1: Ring-and-ball method DIN EN ISO 4625-2,
12、Binders for paints and varnishes Determination of softening point Part 2: Cup-and-ball method 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: Spectrophoto
13、metric method 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 15528, Paints, varnishes and raw materials for paints
14、 and varnishes Sampling DIN EN ISO 21627-1, Plastics Epoxy resins Determination of chlorine content Part 1: Inorganic chlorine DIN EN ISO 7142:2007-05 4 This page is intentionally blank EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 7142February 2007ICS 87.060.20 Supersedes EN ISO 7142:2004 E
15、nglish VersionBinders for paints and varnishes - Epoxy resins - Generalmethods of test (ISO 7142:2007)Liants pour peintures et vernis - Rsines poxydiques -Mthodes gnrales dessai (ISO 7142:2007)Bindemittel fr Beschichtungsstoffe - Epoxidharze -Allgemeine Prfverfahren (ISO 7142:2007)This European Stan
16、dard 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 lists and bibliographical references concerning s
17、uch 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 responsibility of a CEN member into its own language
18、 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, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembou
19、rg, 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 Stassart, 36 B-1050 Brussels 2007 CEN All rights of
20、exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 7142:2007: EForeword This document (EN ISO 7142:2007) has been prepared by Technical Committee ISO/TC 35 “Paints and varnishes” in collaboration with Technical Committee CEN/TC 139 “Paints and varnis
21、hes”, 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 national standards shall be withdrawn at the latest by August 2007. This
22、 document supersedes EN ISO 7142:2004. 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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Gre
23、ece, 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 7142:2007 has been approved by CEN as EN ISO 7142:2007 without any modifi
24、cations. 2 EN ISO 7142:2007 (E) 1 Scope This International Standard specifies general methods of test for epoxy resins for use in paints, varnishes and similar products. It is also applicable to those solutions made from epoxy resins that are intended for use as binders for paints and varnishes. The
25、 test methods to be applied to an individual epoxy resin shall be the subject of agreement between the interested parties. The test methods described in this International Standard are not intended for epoxy esters (see Note to 3.1). 2 Normative references The following referenced documents are indi
26、spensable 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 1
27、523, Determination of flash point Closed cup equilibrium method ISO 2431, Paints and varnishes Determination of flow time by use of flow cups ISO 3001, Plastics Epoxy compounds Determination of epoxy equivalent ISO 3146, Plastics Determination of melting behaviour (melting temperature or melting ran
28、ge) of semi-crystalline polymers by capillary tube and polarizing-microscope methods 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 Determi
29、nation of non-volatile-matter content ISO 3679, Determination of flash point Rapid equilibrium closed cup method ISO 4615, Plastics Unsaturated polyesters and epoxide resins Determination of total chlorine content ISO 4625-1, Binders for paints and varnishes Determination of softening point Part 1:
30、Ring-and-ball method ISO 4625-2, Binders for paints and varnishes Determination of softening point Part 2: Cup-and-ball method ISO 4630-1, Clear liquids Estimation of colour by the Gardner colour scale Part 1: Visual method 3 EN ISO 7142:2007 (E) ISO 4630-2, Clear liquids Estimation of colour by the
31、 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 15528, Paints, varnishes and raw
32、 materials for paints and varnishes Sampling ISO 21627-2, Plastics Epoxy resins Determination of chlorine content Part 2: Easily saponifiable chlorine 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 epoxy resin synthetic resin containing epox
33、y groups generally prepared from epichlorhydrin and a bisphenol ISO 4618:2006 NOTE Epoxy esters obtained by reacting materials containing epoxy groups with fatty acids or oils which dry by oxidation are not covered by this International Standard. 4 Sampling Take a representative sample of the produc
34、t to be tested, as described in ISO 15528. 5 Test methods See Table 1. 6 Test report The test report shall contain at least the following information: a) the type and identification of the product tested; b) a reference to this International Standard (ISO 7142:2007); c) the results of the tests, and
35、 the methods used; d) any deviation, by agreement or otherwise, from the procedures specified; e) the dates of the tests. 4 EN ISO 7142:2007 (E) Table 1 Properties and methods of test Property Test method Colour ISO 4630-1 or ISO 4630-2 (Gardner colour scale) or ISO 6271-1 or ISO 6271-2 (Platinum-co
36、balt scale) Viscosity a bISO 3219 or another agreed method Volatile or non-volatile matter ISO 3251 cFlashpoint aISO 1523 ISO 3679 Epoxy equivalent ISO 3001 Hydroxyl value Annex A Total chlorine content ISO 4615 Easily saponifiable chlorine ISO 21627-2 Melting point ISO 3146 Softening point ISO 4625
37、-1 or ISO 4625-2 aFor epoxy resin solutions, liquid resins and resins in test solutions only. Solid epoxy resins shall be tested in a standard test solution of 40 % (by mass) in diethylene glycol mono-n-butyl ether. The solvent used and the concentration of the test solution shall be indicated in th
38、e test report. bIf the flow-time is used for the characterization of the flow behaviour, it shall be determined by the method specified in ISO 2431. cTake a test portion of 5 g and heat it at 140 C for 3 h without addition of solvent, as described in ISO 3251. 5 EN ISO 7142:2007 (E) Annex A (normati
39、ve) Hydroxyl value A.1 Reagents During the analysis, use only reagents of recognized analytical grade and only distilled water or water of equivalent purity. WARNING Take all necessary safety precautions when using the reagents A.1.1 to A.1.3. A.1.1 Pyridine. The pyridine shall be clear and shall no
40、t cause any significant colour during the blank test. A.1.2 Pyridinium perchlorate. Slowly add 144 g of 70 % (by mass) perchloric acid to 120 ml of pyridine, keeping the mixture cool. Recrystallize the precipitate twice in hot water and allow it to dry in air. A.1.3 Acetic anhydride/pyridine mixture
41、. Mix 12 g of 95 % (by mass) acetic anhydride with 88 g of pyridine. Store the mixture in an airtight bottle and in the dark. A.1.4 Potassium hydroxide, methanolic standard volumetric solution, c(KOH) = 1 mol/l. A.1.5 Phenolphthalein, 10 g/l solution in 95 % (by volume) ethanol, methanol or 2-propan
42、ol. A.2 Apparatus Ordinary laboratory apparatus and A.2.1 Conical flask, of capacity about 250 ml, fitted with a ground-glass joint. A.2.2 Reflux condenser, with ground-glass joint, fitting on the conical flask (A.2.1). A.2.3 Burette, of capacity 50 ml, complying with the requirements of ISO 385, fo
43、r the potassium hydroxide solution (A.1.4). A.2.4 Pipette, of capacity 25 ml, complying with the requirements of ISO 648. A.2.5 Suitable heating device. A.3 Procedure A.3.1 General Carry out the determination in duplicate. 6 EN ISO 7142:2007 (E) A.3.2 Test portion Select the mass of the test portion
44、 according to the expected epoxy equivalent (see Table A.1). Weigh, to the nearest 1 mg, the test portion into the conical flask (A.2.1). Table A.1 Mass of test portion Mass of test portion Mass of pyridinium perchlorate Epoxy equivalent g g up to 180 4,00 above 180 to 195 3,50 above 195 to 215 3,25
45、 above 215 to 240 2,5 3,00 above 240 to 290 3,00 above 290 to 350 2,50 above 350 to 425 2,00 above 425 to 515 1,75 above 515 to 650 1,35 above 650 to 760 1,10 above 760 3,0 1,00 A.3.3 Determination Weigh the corresponding mass of pyridinium perchlorate (A.1.2) given in Table A.1 into the conical fla
46、sk (A.2.1). Add by the pipette (A.2.4) 25 ml of acetic anhydride/pyridine mixture (A.1.3). Warm the mixture until the test portion is completely dissolved. Fit the reflux condenser (A.2.2) onto the conical flask, heat to boiling and maintain at the boiling point under reflux for 30 min. Add 2 ml of
47、water and 10 ml to 15 ml of pyridine (A.1.1) to the top of the condenser so as to rinse the condenser tube. Mix the contents of the flask and cool to ambient temperature. Add 3 drops of phenolphthalein solution (A.1.5) and titrate with potassium hydroxide solution (A.1.4). A.3.4 Blank test Carry out
48、 a blank test, following the same procedure but omitting the test portion and the pyridinium perchlorate (A.1.2). A.4 Expression of results A.4.1 Calculation Calculate the hydroxyl equivalent by the equation (),20111000HE5 5692 000EEmVVm=+7 EN ISO 7142:2007 (E) Calculate the hydroxyl value by the eq
49、uation ,56 109 1000 56 109HVHE HE= where EE is the epoxy equivalent, in grams per mole, determined by the method specified in ISO 3001; HE is the hydroxyl equivalent, in grams of resin per equivalent of hydroxyl group (OH); HV is the hydroxyl value, in grams of potassium hydroxide per kilogram; m1is the mass, in grams, of the test portion (A.3.2); m2is the mass, in grams, of pyridinium perchlorate (A.1.2) used; V0is the volume, in mil
