1、BS EN ISO 4629-1:2016Binders for paints andvarnishes Determination ofhydroxyl valuePart 1: Titrimetric method without using acatalyst (ISO 4629-1:2016)BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06BS EN ISO 4629-1:2016 BRITISH STANDARDNational forewordThis British
2、Standard is the UK implementation of EN ISO 4629-1:2016. It supersedes BS EN ISO 4629:1998 which iswithdrawn.The UK participation in its preparation was entrusted to Technical Committee STI/3, Paints, media and related products.A list of organizations represented on this committee can be obtained on
3、 request to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2016.Published by BSI Standards Limited 2016ISBN 978 0 580 88334 7 ICS 87.060.20 Compliance with a B
4、ritish Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 July 2016.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE
5、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 lindice dhydroxyle - Part
6、ie 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 bound to comply with the CEN/
7、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 CEN-CENELEC Management Cent
8、re 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 has the same status as the
9、 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, Luxembourg, Malta, Netherl
10、ands, 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 Brussels 2016 CEN All rights
11、 of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 4629-1:2016 EBS EN ISO 4629-1:2016EN ISO 4629-1:2016 (E) 3 European foreword This document (EN ISO 4629-1:2016) has been prepared by Technical Committee ISO/TC 35 “Paints and varnishes” in coll
12、aboration 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 standard, either by publication of an identical text or by endorsement, at the latest by December 2016, and conflicting nationa
13、l 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. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersede
14、s 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 Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Ma
15、cedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 4629-1:2016 has been approved by
16、 CEN as EN ISO 4629-1:2016 without any modification. BS EN ISO 4629-1:2016ISO 4629-1:2016(E)Foreword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 25 Reagents 26 Apparatus . 37 Sampling 38 Procedure. 38.1 Number of determinations . 38.2 Test portion 38.3 Determination .
17、 48.4 Blank test . 58.5 Determination of acid value 59 Expression of results 510 Precision . 511 Test report . 6Bibliography 7 ISO 2016 All rights reserved iiiContents PageBS EN ISO 4629-1:2016ISO 4629-1:2016(E)ForewordISO (the International Organization for Standardization) is a worldwide federatio
18、n 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.
19、 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 document and thos
20、e 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 Directives, Part 2 (s
21、ee 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 development of the docu
22、ment 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 specific terms and
23、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 varnishes, Subcommi
24、ttee 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 and the normat
25、ive 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 catalyst Par
26、t 2: Titrimetric method using a catalystiv ISO 2016 All rights reservedBS EN ISO 4629-1:2016INTERNATIONAL STANDARD ISO 4629-1:2016(E)Binders for paints and varnishes Determination of hydroxyl value Part 1: Titrimetric method without using a catalyst1 ScopeThis part of ISO 4629 specifies a titrimetri
27、c method for determining the free hydroxyl groups in binders and binder solutions for paints and varnishes. The hydroxyl groups may be present as polyhydric alcohols, partial esters, polyester end groups or hydroxylated fatty acids.This method is not applicable to resins containing both hydroxyl gro
28、ups 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 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
29、 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 resins is specified in ISO 71421.2 Normative referencesThe following referenced documents, in whole or in part, are normatively referenced in this docume
30、nt 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 385, Laboratory glassware BurettesISO 648, Laboratory glassware Single-volume pipettesISO 2
31、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 15528, Paints, varnishes and raw materials for paints and varnishes Sampling3 Terms and def
32、initionsFor the purposes of this document, the following terms and definitions apply.3.1hydroxyl valuenumber of milligrams of potassium hydroxide (KOH) corresponding to hydroxyl groups that have been acetylated under specified test conditions in 1 g of the product tested ISO 2016 All rights reserved
33、 1BS EN ISO 4629-1:2016ISO 4629-1:2016(E)4 PrincipleThe hydroxyl groups contained in a test portion are acetylated with acetic anhydride. The excess acetic anhydride is hydrolysed and the resulting acetic acid is titrated with potassium hydroxide solution, either in the presence of a colour indicato
34、r 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 hydroxyl value.5 ReagentsDuring the analysis, use only reagents of recognized analytical grade and only water of at least grade 3 purity as
35、 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 mixture, 3 + 1 by volume.5.5 Acetylating reagent.Dissolve 4,0 g of p-toluenesulfonic acid monohydrate (CH3C6H4SO3HH2O) in 100 ml of e
36、thyl 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 requires on titration a volume of between 40 ml and 50 ml of potassium hydroxide solution (5.6) for neutralization.5.6 Potassium hydroxide,
37、 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 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 ma
38、rk 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 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 dissolve
39、d.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 appears.Calculate the actual concentration, c, in moles of hydroxyl ions (OH-) per litre, of the potassium hydroxide solution, using
40、 Formula (1):cmV=1 000204 22,(1)where2 ISO 2016 All rights reservedBS EN ISO 4629-1:2016ISO 4629-1:2016(E)m 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 g
41、rams 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 volumes of a 1 g/l ethanolic solution of thymol blue with one volume of a 1 g/l ethanolic solution of cresol red.6 Ap
42、paratusOrdinary 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-glass joint to the conical flask (6.1).6.3 Microburette or pipette, complying with the requirements of class A of IS
43、O 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 app
44、aratus, e.g. an oil bath or a sand bath, capable of being maintained at (50 1) C.6.6 Potentiometric titration apparatus, fitted with a glass electrode and a reference electrode. The use of this apparatus is an optional alternative (see 8.3).7 SamplingTake a representative sample of the product to be
45、 tested, as specified in ISO 15528.8 Procedure8.1 Number of determinationsCarry out the determination in duplicate.8.2 Test portionBy reference to Table 1, select the appropriate mass of test portion to be taken. If the hydroxyl value cannot be predicted, take a test portion of 2,0 g and carry out a
46、 preliminary determination. ISO 2016 All rights reserved 3BS EN ISO 4629-1:2016ISO 4629-1:2016(E)Table 1 Mass of test portionExpected hydroxyl value Approximate mass of test portionmg KOH/g g40 7,050 5,660 4,770 4,080 3,590 3,1100 2,8140 2,0180 1,6200 1,4250 1,1280 1,0350 0,8400 0,7500 0,61 000 0,3W
47、eigh to the nearest 1 mg, the test portion into the conical flask (6.1).8.3 DeterminationAdd 5 ml of ethyl acetate (5.2) to the contents of the conical flask and shake, if necessary, with gentle warming, until the test portion (8.2) is dissolved.If the test portion is not soluble in ethyl acetate, a
48、nother solvent may be used.Allow to cool to room temperature, add (5,00 0,02) ml (see Note 1) of the acetylating reagent (5.5) by means of the microburette or pipette (6.3) and fit the reflux condenser (6.2) on the conical flask.Heat the flask in the heating apparatus (6.5), maintained at (50 1) C,
49、for 20 min, shaking every 5 min.Cool the contents of the flask to room temperature, remove the condenser, add 2 ml of water, replace the condenser and vigorously shake the flask. Add 10 ml of the pyridine/water mixture (5.4) from the top of the condenser so as to rinse down the condenser tube. Mix the contents of the flask and allow to stand for 5 min at room temperature. Add 30 ml of the toluene/butanol mixture (5.3) from the top of the condenser and use a further 30 ml of the toluene/butanol mixture to rinse the con
