BS-EN-ISO-2114-2000 BS-2782-4-METHOD-432B-2000.pdf

BRITISH STANDARD BS EN ISO 2114:2000 BS 2782-4: Method 432B:2000 Incorporating Corrigendum No.1 Plastics (polyester resins) and paints and varnishes (binders) Determination of partial acid value and total acid value The European Standard EN ISO 2114:2000 has the status of a British Standard ICS 83.080.10 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:38:15 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN ISO 2114:2000 This British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 November 2000 © BSI 3 April 2002 ISBN 0 580 36545 X National foreword This British Standard is the official English language version of EN ISO 2114:2000. It is identical with ISO 2114:2000. It supersedes BS EN ISO 2114:1997 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee PRI/42, Fibre reinforced thermosetting plastics and prepegs, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding European publications. The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include 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. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to iv, pages 1 to 10, the Annex ZA page and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. DateComments 13829 Corrigendum No. 1 3 April 2002Incorporating Annex ZA Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:38:15 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM EN ISO 2114 August 2000 ICS 83.080.10Supersedes EN ISO 2114:1996 English version Plastics (polyester resins) and paints and varnishes (binders) - Determination of partial acid value and total acid value (ISO 2114:2000) Plastiques (résines de polyesters) et peintures et vernis (liants) - Détermination de l'indice d'acide partiel et de l'indice d'acide total (ISO 2114:2000) Kunststoffe (Polyester) und Beschichtungsstoffe (Bindemittel) - Bestimmung der partiellen Säurezahl und der Gesamtsäurezahl (ISO 2114:2000) This European Standard was approved by CEN on 1 August 2000. CEN members are bound 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 Central Secretariat 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 Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG Central Secretariat: rue de Stassart, 36 B-1050 Brussels © 2000 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 2114:2000 E Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:38:15 GMT+00:00 2006, Uncontrolled Copy, (c) BSI CORRECTED 2002-03-13 Foreword This document (ISO 2114:2000) has been prepared by Technical Committee ISO/TC 61 “Plastics“ in collaboration with Technical Committee CEN/TC 249 “Plastics“, the secretariat of which is held by IBN. 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 February 2001, and conflicting national standards shall be withdrawn at the latest by February 2001. This document supersedes EN ISO 2114:1996. 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, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard ISO 2114:2000 has been approved by CEN as a European Standard without any modifications. NOTE Normative references to International Standards are listed in annex ZA (normative). EN ISO 2114:2000 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:38:15 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Reference number ISO 2114:2000(E) INTERNATIONAL STANDARD ISO 2114 Third edition 2000-08-01 Plastics (polyester resins) and paints and varnishes (binders) Determination of partial acid value and total acid value Plastiques (résines de polyesters) et peintures et vernis (liants) Détermination de l'indice d'acide partiel et de l'indice d'acide total EN ISO 2114:2000 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:38:15 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ii EN ISO 2114:2000 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:38:15 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iii Contents Page Foreword.iv 1 Scope 1 2 Normative references1 3 Terms and definitions .1 4 Principle2 5 Reagents.2 6 Apparatus.3 7 Procedure.4 8 Calculation and expression of results.6 9 Precision.7 10 Test report8 Annex A (informative) Checking the concentration of the standard potassium hydroxide solution.9 EN ISO 2114:2000 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:38:15 GMT+00:00 2006, Uncontrolled Copy, (c) BSI iv Foreword ISO (the International Organization for Standardization) is a worldwide 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 that 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. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 2114 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. This third edition cancels and replaces the second edition (ISO 2114:1996) as well as ISO 3682:1996, which have been technically revised. EN ISO 2114:2000 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:38:15 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 1 Plastics (polyester resins) and paints and varnishes (binders) Determination of partial acid value and total acid value 1 Scope This International Standard specifies methods of determining the partial acid value (method A) and the total acid value (method B) of polyester resins and binders for paints and varnishes. It is not applicable to phenolic resins. It is intended to provide quality-control data for the acceptance or rejection of such products in accordance with the terms of a specification, as well as to be used in research and development to monitor the completion of the polycondensation reaction. 2 Normative references The following normative documents contain provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 385-1:1984, Laboratory glassware Burettes Part 1: General requirements. ISO 3251:1993, Paints and varnishes Determination of non-volatile matter of paints, varnishes and binders for paints and varnishes. ISO 3696:1987, Water for analytical laboratory use Specification and test methods. ISO 6353-2:1983, Reagents for chemical analysis Part 2: Specifications First series. 3 Terms and definitions For the purposes of this International Standard, the following terms and definitions apply. 3.1 acid value the number of milligrams of potassium hydroxide (KOH) required to neutralize 1 g of resin under the test conditions 3.2 partial acid value acid value corresponding to the neutralization of all the carboxyl-terminated groups and free acids plus half the free anhydrides in a resin 3.3 total acid value acid value corresponding to the neutralization of all the carboxyl-terminated groups and free acids plus all the free anhydrides in a resin EN ISO 2114:2000 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:38:15 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 2 4Principle 4.1 General The free acids/anhydrides contained in a test portion are titrated with potassium hydroxide solution, either potentiometrically or in the presence of a colour indicator. 4.2 Method A A weighed quantity of resin is dissolved in a solvent mixture. The solution is titrated potentiometrically (see note 1) with a standard volumetric solution of potassium hydroxide in ethanol, giving the following reaction: The amount, in milligrams, of potassium hydroxide used to neutralize 1 g of resin is then calculated. Method A is recommended for binders for paints and varnishes (as generally only small amounts of free anhydrides are present) but is also suitable for unsaturated-polyester resins. 4.3 Method B A weighed quantity of resin is dissolved in a solvent mixture including water. The free anhydrides are allowed to hydrolyse for 20 min before titrating potentiometrically (see note 1) with a standard volumetric solution of potassium hydroxide in ethanol, giving the following reaction: The amount, in milligrams, of potassium hydroxide used to neutralize 1 g of resin is then calculated. Method B is useful for unsaturated-polyester resins in which there are significant amounts of free anhydrides. NOTE 1 The use of a colour indicator for the titration is an optional alternative in both methods. NOTE 2 When titrating pure maleic polyester resins, it is better to use a methanolic solution of potassium hydroxide. 5 Reagents During the analysis, use only reagents of recognized analytical grade in accordance with ISO 6353-2 and water of at least grade 3 as defined in ISO 3696. 5.1 Solvent for method A: solvent mixture containing 2 parts of toluene (5.7) and 1 part of ethanol (5.5) by volume. Neutralize the solvent mixture with potassium hydroxide solution (5.3) prior to use, using phenolphthalein as indicator if the determination is to be carried out by potentiometric titration (see 7.2.2) or, if the determination is to be carried out using an indicator (see 7.2.3), using the same indicator as will be used for the determination. EN ISO 2114:2000 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 20 02:38:15 GMT+00:00 2006, Uncontrolled Copy, (c) BSI 3 5.2 Solvent for method B: solvent mixture containing 400 ml of pyridine (5.8), 750 ml of methyl ethyl ketone (5.9) and 50 ml of water. 5.3 Potassium hydroxide, 0,1 mol/l standard volumetric solution in ethanol (5.5) or in methanol (5.6), free from carbonates. Check the concentration of this solution on the day of use (see annex A). If more than 25 ml of titrant will be required with a 0,1 mol/l solution, use a 0,5 mol/l solution to avoid the additional errors involved in refilling the burette (6.3). 5.4 Acetone, containing less than 0,3 % by mass of water. 5.5 Ethanol, anhydrous, containing less than 0,2 % by mass of water. 5.6 Methanol, anhydrous, containing 99,8 % by mass. 5.7 Toluene, anhydrous, containing less than 0,005 % by mass of water. 5.8 Pyridine, containing less than 0,05 % by mass of water. WARNING Pyridine is toxic and flammable. Take proper precautions when handling this reagent. Avoid contact with the skin or eyes. Use only in a well ventilated area in order to avoid breathing in the vapour. 5.9 Methyl ethyl ketone, containing less than 0,01 % by mass of water. 5.10Indicators (for optional alternative): 5.10.1Bromothymol blue, 0,1 % solution in ethanol (5.5). 5.10.2Phenolphthalein, 1 % solution in ethanol (5.5). 6 Apparatus Ordinary laboratory apparatus and glassware, plus the following: 6.1 Conical flasks, of capacities 100 ml and 250 ml, with a wide neck. 6.2 Conical flask, of capacity 250 ml, with a narrow neck and fitted with a ground-glass stopper. 6.3 Burette, of capacity 25 ml (graduated in 0,05 ml divisions), complying with the requirements of ISO 385-1. 6.4 Magnetic stirrer. 6.5 Pipettes, of capacity 25 ml and 50 ml. 6.6 Automatic pipettes, of capacity 25 ml, 50 ml and 60 ml. 6.7 Analytical balance, accurate to 1 mg. 6.8 Potentiometric-titration apparatus, comprising a suitable potentiometer