1、December 2016 English price group 10No part of this translation 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!%b3“2596316www.din.de
2、DIN EN ISO 4629-1Binders for paints and varnishes Determination of hydroxyl value Part 1: Titrimetric method without using a catalyst (ISO 46291:2016);English version EN ISO 46291:2016,English translation of DIN EN ISO 4629-1:2016-12Bindemittel fr Beschichtungsstoffe Bestimmung der Hydroxylzahl Teil
3、 1: Titrimetrisches Verfahren ohne Katalysator (ISO 46291:2016);Englische Fassung EN ISO 46291:2016,Englische bersetzung von DIN EN ISO 4629-1:2016-12Liants pour peintures et vernis Dtermination de lindice dhydroxyle Partie 1: Mthode titrimtrique sans catalyseur (ISO 46291:2016);Version anglaise EN
4、ISO 46291:2016,Traduction anglaise de DIN EN ISO 4629-1:2016-12SupersedesDIN 532401:201306 andDIN EN ISO 4629:199807www.beuth.deDocument comprises 15 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.12.16 DIN EN ISO 4629-1:2016-
5、12 2 A comma is used as the decimal marker. National foreword This document (EN ISO 4629-1:2016) has been prepared by Technical Committee ISO/TC 35 “Paints and varnishes” in collaboration with Technical Committee CEN/TC 139 “Paints and varnishes” (Secretariat: DIN, Germany). The responsible German b
6、ody involved in its preparation was DIN-Normenausschuss Beschichtungsstoffe und Beschichtungen (DIN Standards Committee Coatings and Coating Materials), Working Committee NA 002-00-02 AA Lackrohstoffe. DIN EN ISO 4629 consists of the following parts, under the general title Binders for paints and va
7、rnishes Determination of hydroxyl value: Part 1: Titrimetric method without using a catalyst Part 2: Titrimetric method using a catalyst The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 385 DIN EN ISO 385 ISO 648 DIN EN ISO 648 ISO 2114:
8、2000 DIN EN ISO 2114:2002-06 ISO 3696 DIN ISO 3696 ISO 7142 DIN EN ISO 7142 ISO 15528 DIN EN ISO 15528 Amendments This standard differs from DIN 53240-1:2013-06 and DIN EN ISO 4629:1998-07 as follows: a) the two standards have been combined and renumbered; b) the text has been editorially revised an
9、d normative references have been updated; c) the concentration of the phenolphthalein-indicator solution has been changed. Previous editions DIN 53240: 1971-12 DIN ISO 4629: 1979-11 DIN 53240-1: 2013-06 DIN EN ISO 4629: 1998-07 DIN EN ISO 4629-1:2016-12 3 National Annex NA (informative) Bibliography
10、 DIN EN ISO 385, Laboratory glassware Burettes DIN EN ISO 648, Laboratory glassware Single-volume pipettes DIN EN ISO 2114:2002-06, Plastics (polyester resins) and paints varnishes (binders) Determination of partial acid value and total acid value (ISO 2114:2000) DIN EN ISO 7142, Binders for paints
11、and varnishes Epoxy resins General methods of test 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 DIN EN ISO 4629-1:2016-12 4 This page is intentionally blank EUROPEAN STANDARD N
12、ORME EUROPENNE EUROPISCHE NORM EN ISO 4629-1 June 2016 ICS 87.060.20 Supersedes EN ISO 4629:1998English Version Binders for paints and varnishes - Determination of hydroxyl value - Part 1: Titrimetric method without using a catalyst (ISO 4629-1:2016) Liants pour peintures et vernis - Dtermination de
13、 lindice dhydroxyle - Partie 1: Mthode titrimtrique sans catalyseur (ISO 4629-1:2016) Bindemittel fr Beschichtungsstoffe - Bestimmung der Hydroxylzahl - Teil 1: Titrimetrisches Verfahren ohne Katalysator (ISO 4629-1:2016) This European Standard was approved by CEN on 19 May 2016. CEN members are bou
14、nd to comply with the CEN/CENELEC Internal Regulations which stipulate 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 C
15、EN-CENELEC 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 translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre
16、has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
17、Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Br
18、ussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 4629-1:2016 EEN ISO 4629-1:2016 (E) 2 Contents Page European foreword . 3 Foreword 4 1 Scope 5 2 Normative references 5 3 Terms and definitions . 5 4 Principle . 6 5 R
19、eagents . 6 6 Apparatus . 7 7 Sampling . 7 8 Procedure. 7 8.1 Number of determinations 7 8.2 Test portion . 7 8.3 Determination 8 8.4 Blank test . 9 8.5 Determination of acid value 9 9 Expression of results 9 10 Precision . 9 11 Test report 10 Bibliography . 11 DIN EN ISO 4629-1:2016-12European fore
20、word This document (EN ISO 4629-1:2016) 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 standa
21、rd, either by publication of an identical text or by endorsement, at the latest by December 2016, and conflicting national standards shall be withdrawn at the latest by December 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights
22、. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 4629:1998. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standar
23、d: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain
24、, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 4629-1:2016 has been approved by CEN as EN ISO 4629-1:2016 without any modification. 3 EN ISO 4629-1:2016 (E) DIN EN ISO 4629-1:2016-12ForewordISO (the International Organization for Standardization) is a worldw
25、ide 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 th
26、at 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.The procedures used to develop this docu
27、ment and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directiv
28、es, Part 2 (see www.iso.org/directives).Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the developmen
29、t of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specif
30、ic terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 35, Paints and varnis
31、hes, Subcommittee SC 10, Test methods for binders for paints and varnishes.This first edition of ISO 4629-1 cancels and replaces ISO 4629:1996, which has been technically revised with the following changes:a) the standard has been numbered as ISO 4629-1;b) the standard has been editorially revised a
32、nd the normative references have been updated;c) the concentration of the phenolphthalein-indicator solution has been changed.ISO 4629 consists of the following parts, under the general title Binders for paints and varnishes Determination of hydroxyl value: Part 1: Titrimetric method without using a
33、 catalyst Part 2: Titrimetric method using a catalyst4EN ISO 4629-1:2016 (E) DIN EN ISO 4629-1:2016-121 ScopeThis part of ISO 4629 specifies a titrimetric method for determining the free hydroxyl groups in binders and binder solutions for paints and varnishes. The hydroxyl groups may be present as p
34、olyhydric alcohols, partial esters, polyester end groups or hydroxylated fatty acids.This method is not applicable to resins containing both hydroxyl groups and epoxy groups, because the latter will also be included in the result. Also the method is not applicable to cellulose nitrate or to phenolic
35、 resins.NOTE 1 If, in the case of binder solutions, the hydroxyl value of the binder only is to be determined, the possibility that other constituents of the binder solution may contain hydroxyl groups has to be taken into account.NOTE 2 A method for the determination of the hydroxyl value of epoxy
36、resins is specified in ISO 71421.2 Normative referencesThe following referenced documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of t
37、he referenced document (including any amendments) applies.ISO 385, Laboratory glassware BurettesISO 648, Laboratory glassware Single-volume pipettesISO 2114:2000, Plastics (polyester resins) and paints and varnishes (binders) Determination of partial acid value and total acid valueISO 3696, Water fo
38、r analytical laboratory use Specification and test methodsISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1hydroxyl valuenumber of milligrams of potassium hydroxide (
39、KOH) corresponding to hydroxyl groups that have been acetylated under specified test conditions in 1 g of the product tested5 EN ISO 4629-1:2016 (E) DIN EN ISO 4629-1:2016-124 PrincipleThe hydroxyl groups contained in a test portion are acetylated with acetic anhydride. The excess acetic anhydride i
40、s hydrolysed and the resulting acetic acid is titrated with potassium hydroxide solution, either in the presence of a colour indicator or potentiometrically.NOTE Primary and secondary amines, if present, will also be acetylated. In such cases, this will have to be allowed when calculating the hydrox
41、yl value.5 ReagentsDuring the analysis, use only reagents of recognized analytical grade and only water of at least grade 3 purity as specified in ISO 3696.5.1 Potassium hydrogen phthalate C6H4(COOH) (COOK).5.2 Ethyl acetate, anhydrous.5.3 Toluene/butanol mixture, 1 + 2 by volume.5.4 Pyridine/water
42、mixture, 3 + 1 by volume.5.5 Acetylating reagent.Dissolve 4,0 g of p-toluenesulfonic acid monohydrate (CH3C6H4SO3HH2O) in 100 ml of ethyl acetate (5.2), preferably using a magnetic stirrer.To this solution, add slowly, while stirring, 33 ml of acetic anhydride. Check that 5 ml of this reagent requir
43、es on titration a volume of between 40 ml and 50 ml of potassium hydroxide solution (5.6) for neutralization.5.6 Potassium hydroxide, standard volumetric solution, c(KOH) 0,5 mol/l, in methanol.Ethanol may also be used if the product to be tested is soluble in ethanol.5.6.1 PreparationWeigh, to the
44、nearest 0,05 g, 28 g of potassium hydroxide, dissolve in the minimum quantity of water in a 1 000 ml one-mark flask, dilute to the mark with methanol and mix well.5.6.2 StandardizationWeigh, to the nearest 0,01 g, 2,5 g of potassium hydrogen phthalate (5.1), previously dried at about 120 C to consta
45、nt mass and allowed to cool in a desiccator, into a 250 ml flask. Add 150 ml freshly boiled and cooled water and swirl until dissolved.Titrate the potassium hydroxide solution prepared in 5.6.1, using phenolphthalein solution (5.7) as indication, until a red coloration that remains for at least 10 s
46、 appears.Calculate the actual concentration, c, in moles of hydroxyl ions (OH-) per litre, of the potassium hydroxide solution, using Formula (1):cmV=1 000204 22,(1)where6EN ISO 4629-1:2016 (E) DIN EN ISO 4629-1:2016-12m is the mass, in grams, of potassium hydrogen phthalate taken;V is the volume, i
47、n millilitres, of potassium hydroxide solution used for the titration;204,22 is the relative molecular mass, in grams per mole, of potassium hydrogen phthalate.5.7 Phenolphthalein, 0,5 g/l solution in 95 % (by volume) ethanol, in methanol or in isopropanol.5.8 Mixed-indicator solution.Mix three volu
48、mes of a 1 g/l ethanolic solution of thymol blue with one volume of a 1 g/l ethanolic solution of cresol red.6 ApparatusOrdinary laboratory equipment and glassware, together with the following.6.1 Conical flask, capacity about 250 ml, with a ground-glass joint.6.2 Reflux condenser, with a ground-gla
49、ss joint to the conical flask (6.1).6.3 Microburette or pipette, complying with the requirements of class A of ISO 648, of capacity 5 ml, for acetylating reagent (5.5).WARNING If a pipette is used, this shall not be a mouth pipette in view of the corrosive nature of the reagent.6.4 Burette, of capacity 50 ml, complying with the requirements of ISO 385, for the potassium hydroxide solution (5.6).6.5 Heating apparatus, e.g. an
