DIN EN ISO 4629-2-2016 Binders for paints and varnishes - Determination of hydroxyl value - Part 2 Titrimetric method using a catalyst (ISO 4629-2 2016) German version EN ISO 4629-.pdf

1、December 2016 English price group 9No 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!%h=“2596926www.din.deD

2、IN EN ISO 4629-2Binders for paints and varnishes Determination of hydroxyl value Part 2: Titrimetric method using a catalyst (ISO 46292:2016);English version EN ISO 46292:2016,English translation of DIN EN ISO 4629-2:2016-12Bindemittel fr Beschichtungsstoffe Bestimmung der Hydroxylzahl Teil 2: Titri

3、metrisches Verfahren mit Katalysator (ISO 46292:2016);Englische Fassung EN ISO 46292:2016,Englische bersetzung von DIN EN ISO 4629-2:2016-12Liants pour peintures et vernis Dtermination de lindice dhydroxyle Partie 2: Mthode titrimtrique utilisant un catalyseur (ISO 46292:2016);Version anglaise EN IS

4、O 46292:2016,Traduction anglaise de DIN EN ISO 4629-2:2016-12SupersedesDIN 532402:200711www.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 4629-2:2016-12 2 A comma is used as the

5、decimal marker. National foreword This document (EN ISO 4629-2:2016) 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 body involved in its preparat

6、ion 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 varnishes Determination of hyd

7、roxyl 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 2114:2000 DIN EN ISO 2114:2002-06 ISO 3696 DIN ISO 3696 ISO 4618 DIN EN ISO 461

8、8 ISO 4629-1:2016 DIN EN ISO 4629-1:2016-12 ISO 15528 DIN EN ISO 15528 Amendments This standard differs from DIN 53240-2:2007-11 as follows: a) as a result of the adoption of EN ISO 4629-2 at German national level, the standard has been published as the corresponding DIN EN ISO Standard; b) the text

9、 has been editorially revised and normative references have been updated; c) the concentration of the phenolphthalein-indicator solution has been changed. Previous editions DIN 53240-2: 1998-10, 2007-11 DIN EN ISO 4629-2:2016-12 3 National Annex NA (informative) Bibliography DIN EN ISO 2114:2002-06,

10、 Plastics (polyester resins) and paints varnishes (binders) Determination of partial acid value and total acid value (ISO 2114:2000) DIN EN ISO 4618, Paints and varnishes Terms and definitions DIN EN ISO 4629-1:2016-12, Binders for paints and varnishes Determination of hydroxyl value Part 1: Titrime

11、tric method without using a catalyst (ISO 4629-1:2016) 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 4629-2:2016-12 4 This page is intentionally blank EUROPEAN STANDA

12、RD NORME EUROPENNE EUROPISCHE NORM EN ISO 4629-2 June 2016 ICS 87.060.20 English Version Binders for paints and varnishes - Determination of hydroxyl value - Part 2: Titrimetric method using a catalyst (ISO 4629-2:2016) Liants pour peintures et vernis - Dtermination de lindice dhydroxyle - Partie 2:

13、 Mthode titrimtrique utilisant un catalyseur (ISO 4629-2:2016) Bindemittel fr Beschichtungsstoffe - Bestimmung der Hydroxylzahl - Teil 2: Verfahren mit Katalysator (ISO4629-2:2016) This European Standard was approved by CEN on 19 May 2016. CEN members are bound to comply with the CEN/CENELEC Interna

14、l 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 CEN-CENELEC Management Centre or to any CE

15、N 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 has the same status as the official versi

16、ons. 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, Luxembourg, Malta, Netherlands, Norway, P

17、oland, 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 Brussels 2016 CEN All rights of exploitatio

18、n in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 4629-2:2016 EEN ISO 4629-2:2016 (E) 2 Contents Page European foreword . 3 Foreword 4 Introduction 5 1 Scope 6 2 Normative references 6 3 Terms and definitions . 6 4 Principle . 6 5 Reagents . 7 6 Apparatus .

19、7 7 Sampling . 8 8 Procedure. 8 8.1 Number of determinations 8 8.2 Test portion . 8 8.3 Determination 8 8.4 Blank test . 9 8.5 Determination of acid value 9 9 Expression of results 9 10 Precision . 9 10.1 Repeatability . 9 10.2 Reproducibility 9 11 Test report 10 Bibliography . 11 DIN EN ISO 4629-2:

20、2016-12 European foreword This document (EN ISO 4629-2:2016) 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

21、 of a national standard, 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 sub

22、ject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, B

23、ulgaria, 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, Sweden, Switzerland,

24、 Turkey and the United Kingdom. Endorsement notice The text of ISO 4629-2:2016 has been approved by CEN as EN ISO 4629-2:2016 without any modification. DIN EN ISO 4629-2:2016-12 3 EN ISO 4629-2:2016 (E) ForewordISO (the International Organization for Standardization) is a worldwide federation of nat

25、ional 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. Interna

26、tional 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 document and those intend

27、ed 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 Directives, Part 2 (see www.i

28、so.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 development of the document wil

29、l 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 specific terms and expressi

30、ons 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 varnishes, Subcommittee SC

31、10, Test methods for binders for paints and varnishes.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 catalyst Part 2: Titrimetric method using a catalystDIN EN ISO 4629-2:2

32、016-12 4EN ISO 4629-2:2016 (E) IntroductionThere are several different methods standardized for determining the hydroxyl value of resins. The classic method using pyridine without a catalyst is specified in ISO 4629-1. The advantages of the method using a catalyst are the following: the solvents use

33、d are less hazardous to health; the solvent consumption is lower; the method is faster due to shorter reaction times; the end point of the titration is easier to see; polyols are more readily soluble.DIN EN ISO 4629-2:2016-12 5 EN ISO 4629-2:2016 (E) 1 ScopeThis part of ISO 4629 specifies a titrimet

34、ric method for determining the hydroxyl value of resins, binders for paints and varnishes, primary alcohols, glycols and fats. Whether it can be applied for hydro carboxylic acids, phenolic hydroxyl groups, polyols such as trimethyl propane and substances containing aromatic groups have been activat

35、ed for Friedel-Crafts acylation shall be decided on case-to-case basis.Under the right conditions, the method is also applicable for determining the hydroxyl value of castor oil and its derivatives.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this

36、 document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 660, Animal and vegetable fats and oils Determination of acid value and acidityISO 2

37、114:2000, Plastics (polyester resins) and paints and varnishes (binders) Determination of partial acid value and total acid valueISO 3696, Water for analytical laboratory use Specification and test methodsISO 4618, Paints and varnishes Terms and definitionsISO 15528, Paints, varnishes and raw materi

38、als for paints and varnishes Sampling3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 4618 and the following apply.3.1hydroxyl valuenumber of milligrams of potassium hydroxide (KOH) corresponding to hydroxyl groups that have been acetylated under speci

39、fied test conditions in 1 g of the product testedSOURCE: ISO 4629-1:2016, 3.14 PrincipleThe hydroxyl groups in polyols are acetylated with acetic anhydride. The excess acetic anhydride is titrated with alcoholic potassium hydroxide solution.DIN EN ISO 4629-2:2016-12 6EN ISO 4629-2:2016 (E) 5 Reagent

40、sDuring 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 N-Methylpyrrolidone (NMP).NOTE Commission chemists workgroup validate methodologies using less dangerous substances such as dioxolane and other hetero cycles.

41、5.2 Potassium hydroxide solution, c = 0,5 mol/l in methanol.Ethanol may also be used if the product to be tested is soluble in ethanol.5.2.1 PreparationWeigh, to the 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 mar

42、k with methanol and mix well.5.2.2 StandardizationWeigh, to the nearest 0,01 g, 2,5 g of potassium hydrogen phthalate, previously dried at about 120 C to constant 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.Titra

43、te the potassium hydroxide solution prepared in 5.2.1, using phenolphthalein solution as indication, until a red coloration that remains for at least 10 s appears.Calculate the actual concentration, c, in moles of hydroxyl ions (OH-) per litre, of the potassium hydroxide solution using Formula (1):c

44、mV=1 000204 22,(1)wherem is the mass, in grams, of potassium hydrogen phthalate taken;V is the volume, in millilitres, of potassium hydroxide solution used for the titration;204,22 is the relative molecular mass, in grams per mole, of potassium hydrogen phthalate.5.3 Methyl ethyl ketone (MEK).5.4 De

45、mineralized water.5.5 Acetylating reagent, make up a 10 % solution of acetic anhydride in NMP (5.1).5.6 Catalyst solution, make up a 1 % (by mass) solution of 4-N-dimethylaminopyridine in NMP (5.1).5.7 Indicator solution, make up a 1 % (by mass) solution of either thymolphthalein or 0,05 % (by mass)

46、 solution of phenolphthalein in NMP (5.1).6 ApparatusOrdinary laboratory equipment and glassware, together with the following.DIN EN ISO 4629-2:2016-12 7 EN ISO 4629-2:2016 (E) 6.1 Automatic titrator.6.2 Analytical balance.6.3 250 ml conical flask with grounded joint.6.4 50 ml motorized piston buret

47、te.6.5 Hot plate.6.6 Magnetic stirrer.7 SamplingTake a representative sample of the product to be tested, as specified in ISO 15528.8 Procedure8.1 Number of determinationsCarry out the determination in triplicate by titrating the sample potentiometrically or using a colour indicator.8.2 Test portion

48、The initial sample mass required for the determination depends on the expected hydroxyl value and shall be calculated using Formula (2):m =300HVe(2)wherem is the initial sample mass, in grams;HVeis the expected hydroxyl value, in milligrams of KOH per gram, of the product.Weigh, to the nearest 1 mg,

49、 the test portion into the 250 ml conical flask (6.3).8.3 DeterminationAdd 30 ml of catalyst solution (5.6) and 10 ml of acetylating reagent (5.5). Close the flask with the stopper and dissolve the sample by stirring and, if necessary, by heating the mixture. Then, while stirring continuously on the magnetic stirrer (6.6), allow the reaction to take place for at least 15 min at ambient temperature (23 2) C.All products contain