Phenolic, amino and condensation resins - Determination of free-formaldehyde content (ISO 11402:2004)

Will replace EN ISO 9397:1997 and EN ISO 11402:1998 (CC/010807) ++ Withdrawn from VA because FDIS at ISO level --> UAP on ISO published (NT/030901)

Phenol-, Amin- und Kondensationsharze - Bestimmung des Gehalts an freiem Formaldehyd (ISO 11402:2004)

Diese Internationale Norm legt drei Verfahren zum Bestimmen des Gehaltes an freiem Formaldehyd in den folgenden Harzen fest:

Résines phénoliques, aminiques et de condensation - Dosage du formaldéhyde libre (ISO 11402:2004)

L'ISO 11402:2004 prescrit trois méthodes de dosage du formaldéhyde libre dans les produits suivants.
Les résines phénoliques, par titrage potentiométrique en solution aqueuse ou organique (méthode au chlorhydrate d'hydroxylamine). Cette méthode est applicable aux résines dont la teneur en formaldéhyde libre est inférieure ou égale à 15 % en masse. Si la teneur en formaldéhyde libre est comprise entre 15 % en masse et 30 % en masse, il peut être nécessaire d'ajuster en conséquence les concentrations des solutions titrées utilisées.
Les aminorésines et les résines furanniques (méthode au sulfite de sodium). Cette méthode est applicable aux résines résultant de la polycondensation de l'urée et de la mélamine avec du formaldéhyde, et aux résines furanniques résultant de la polycondensation d'alcool furfurylique avec du formaldéhyde sans autre modification.
Les résines de condensation (méthode au cyanure de potassium), comprenant les résines d'urée, les résines furanniques, les résines de mélamine et les résines phénoliques, ainsi que les combinaisons et modifications de ces résines.
La présente Norme internationale a pour objet d'établir des modes opératoires de dosage reconnus et utiles (par exemple dans le but de vérifier si les règlements officiels concernant la manipulation des produits dangereux sur les lieux de travail sont observés). Dans la mesure du possible, toutes les résines contenant du formaldéhyde sont à inclure dans ce propos.
La quantité de formaldéhyde libre déterminée dans les résines de condensation du formaldéhyde en utilisant la présente Norme internationale représente la teneur réelle au moment de l'essai. La valeur n'a pas de relation quantitative avec le formaldéhyde libre qui pourrait apparaître pendant ou après la transformation.

Fenolne, amino in kondenzacijske smole - Določevanje prostega formaldehida (ISO 11402:2004)

General Information

Status
Published
Publication Date
30-Apr-2005
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-May-2005
Due Date
01-May-2005
Completion Date
01-May-2005

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.PDOGHKLGDPhenol-, Amin- und Kondensationsharze - Bestimmung des Gehalts an freiem Formaldehyd (ISO 11402:2004)Résines phénoliques, aminiques et de condensation - Dosage du formaldéhyde libre (ISO 11402:2004)Phenolic, amino and condensation resins - Determination of free-formaldehyde content (ISO 11402:2004)83.080.10DuromeriThermosetting materialsICS:Ta slovenski standard je istoveten z:EN ISO 11402:2005SIST EN ISO 11402:2005en,fr,de01-maj-2005SIST EN ISO 11402:2005SLOVENSKI

STANDARDSIST EN ISO 9397:1999SIST EN ISO 9020:1998SIST EN ISO 11402:20001DGRPHãþD

SIST EN ISO 11402:2005
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN ISO 11402

February 2005 ICS 83.080.10 Supersedes EN ISO 11402:1998, EN ISO 9397:1997 English version

Phenolic, amino and condensation resins - Determination of free-formaldehyde content (ISO 11402:2004)

Résines phénoliques, aminiques et de condensation - Dosage du formaldéhyde libre (ISO 11402:2004)

Phenol-, Amin- und Kondensationsharze -Bestimmung des Gehalts an freiem Formaldehyd (ISO 11402:2004) This European Standard was approved by CEN on 3 February 2005.

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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: rue de Stassart, 36

B-1050 Brussels © 2005 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11402:2005: ESIST EN ISO 11402:2005

EN ISO 11402:2005 (E)
Foreword

The text of ISO 11402:2004 has been prepared by Technical Committee ISO/TC 61 "Plastics” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 11402:2005 by 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 August 2005, and conflicting national standards shall be withdrawn at the latest by August 2005.

This document will supersede EN ISO 9397:1997 and EN ISO 11402:1998.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

Endorsement notice

The text of ISO 11402:2004 has been approved by CEN as EN ISO 11402:2005 without any modifications.

SIST EN ISO 11402:2005
Reference numberISO 11402:2004(E)© ISO 2004

INTERNATIONAL STANDARD ISO11402Second edition2004-03-15Phenolic, amino and condensation resins — Determination of free-formaldehyde content Résines phénoliques, aminiques et de condensation — Dosage du formaldéhyde libre

SIST EN ISO 11402:2005

ISO 11402:2004(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a trademark of Adobe Systems Incorporated. Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.

ISO 2004 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISO's member body in the country of the requester. ISO copyright office Case postale 56 • CH-1211 Geneva 20 Tel.

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© ISO 2004 – All rights reserved
SIST EN ISO 11402:2005
ISO 11402:2004(E) © ISO 2004 – All rights reserved

iii Contents Page Foreword............................................................................................................................................................iv 1 Scope......................................................................................................................................................1 2 Normative references............................................................................................................................1 3 Terms and definitions...........................................................................................................................2 4 Test procedures....................................................................................................................................2 4.1 General...................................................................................................................................................2 4.2 Hydroxylamine hydrochloride procedure...........................................................................................2 4.3 Sulfite procedure...................................................................................................................................4 4.4 KCN procedure......................................................................................................................................7 5 Test report............................................................................................................................................10 Annex A (informative)

Suitability of the procedures for different types of resin.......................................11 Annex B (informative)

Removal of Hg2+ and CN– from mercury and cyanide residues............................12

SIST EN ISO 11402:2005
ISO 11402:2004(E) iv

© ISO 2004 – All rights reserved 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 2. The main task of technical committees is to prepare International Standards. 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 document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 11402 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. This second edition cancels and replaces the first edition (ISO 11402:1993), as well as ISO 9020:1994 and ISO 9397:1995. The three standards have been combined into one, the sulfite procedure being taken from ISO 9020 and the hydroxylamine hydrochloride procedure from ISO 9397. SIST EN ISO 11402:2005

INTERNATIONAL STANDARD ISO 11402:2004(E) © ISO 2004 – All rights reserved

1 Phenolic, amino and condensation resins — Determination of free-formaldehyde content 1 Scope This International Standard specifies three methods for determining the free-formaldehyde content in the following: a) Phenolic resins, by potentiometric titration in aqueous or organic solution (hydroxylamine hydrochloride procedure). The method is applicable to resins with free-formaldehyde contents up to and including 15 % by mass. For free-formaldehyde contents between 15 % by mass and 30 % by mass, it may be necessary to adjust the concentrations of the standard volumetric solutions used accordingly. b) Amino resins and furan resins (sulfite procedure). The method is applicable to resins resulting from the polycondensation of urea and melamine with formaldehyde and to furan resins resulting from the polycondensation of furfuryl alcohol with formaldehyde without further modification. c) Condensation resins (KCN procedure), including urea resins, furan resins, melamine resins and phenolic resins, as well as combinations and modifications of these resins. The purpose of this International Standard is to establish recognized and useful determination procedures (for instance in order to check whether official regulations on the handling of hazardous workplace materials are observed). As far as possible, all formaldehyde-containing resins are to be included in this connection. The free-formaldehyde content determined in formaldehyde condensation resins using this International Standard represents the actual content at the time of the determination. The value bears no quantitative relationship to the free-formaldehyde content during or after processing. 2 Normative references The following referenced documents are indispensable 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 385-1, Laboratory glassware — Burettes — Part 1: General requirements ISO 648, Laboratory glassware — One-mark pipettes ISO 3696, Water for analytical laboratory use — Specification and test methods ISO 15528, Paints, varnishes and raw materials for paints and varnishes — Sampling SIST EN ISO 11402:2005

ISO 11402:2004(E) 2

© ISO 2004 – All rights reserved 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 free formaldehyde formaldehyde that is present in unbound form as formaldehyde, formaldehyde dihydrate (dihydroxymethylene) or polyoxymethylene in a condensation resin 4 Test procedures 4.1 General The choice of test procedure for the determination of free formaldehyde in condensation resins is made in accordance with Table 1. Table 1 — Selection of procedure Procedure Suitable for testing of Hydroxylamine hydrochloride procedure Phenolic resins, furan resinsa (unmodified with urea or melamine resin) Sulfite procedure Urea resins, melamine resins, furan resinsa, urea-melamine resins, furan-urea resins KCN procedureb Melamine-phenolic resins, urea-phenolic resins, urea-melamine-phenolic resins a See Annex A, Clause A.2. b See Annex A, Clause A.3.

4.2 Hydroxylamine hydrochloride procedure 4.2.1 Principle The formaldehyde is converted to the oxime with hydroxylamine hydrochloride. The hydrochloric acid formed during this reaction is determined by potentiometric back-titration, using sodium hydroxide solution. Oximation reaction: CH2O + NH2OH⋅HCl → CH2NOH + HCl + H2O 4.2.2 Reagents During the analysis, use only reagents of recognized analytical grade and only water of at least grade 3 purity as defined in ISO 3696. 4.2.2.1 Hydroxylamine hydrochloride, 10 % by mass solution, the pH of which has been adjusted to 3,5 by the addition of sodium hydroxide solution. 4.2.2.2 Sodium hydroxide, standard volumetric solutions, c(NaOH) = 1 mol/l and c(NaOH) = 0,1 mol/l. 4.2.2.3 Hydrochloric acid, standard volumetric solutions, c(HCl) = 1 mol/l and c(HCl) = 0,1 mol/l. 4.2.2.4 Methanol, free of aldehydes and ketones. SIST EN ISO 11402:2005

ISO 11402:2004(E) © ISO 2004 – All rights reserved

3 4.2.2.5 Propan-2-ol, free of aldehydes and ketones. 4.2.3 Apparatus Ordinary laboratory apparatus and glassware, together with the following: 4.2.3.1 Balance, accurate to 0,1 mg. 4.2.3.2 pH-meter, sensitive to 0,1 pH-units, equipped with a glass indicating electrode and a standard calomel reference electrode. 4.2.3.3 Magnetic stirrer. 4.2.3.4 Graduated burettes, of capacity 10 ml and 25 ml, the latter being for use if the formaldehyde content is likely to be greater than 5 % by mass. 4.2.4 Sampling Take a representative sample of the product to be tested, as described in ISO 15528. 4.2.5 Procedure 4.2.5.1 Test temperature Carry out the test at (23 ± 1) °C. 4.2.5.2 Test portion Weigh, to the nearest 0,1 mg, into a 250 ml beaker, a test portion of mass from 1 g to 5 g, depending on the assumed formaldehyde content (see Table 2). Table 2 — Mass of test portion Assumed formaldehyde content% by mass Mass of test portion g < 2 5,0 ± 0,2 2 to 4 3,0 ± 0,2 > 4 1 to 2

4.2.5.3 Determination Add 50 ml of methanol (4.2.2.4), or 50 ml of a mixture of 3 volumes of propan-2-ol (4.2.2.5) and 1 volume of water, to the contents of the beaker, switch on the magnetic stirrer (4.2.3.3) and stir until the resin has dissolved and the temperature has stabilized at (23 ± 1) °C. Introduce the electrodes of the pH-meter (4.2.3.2) into the solution and, using the 0,1 mol/l solution of hydrochloric acid (for neutralized resins) or the 1 mol/l solution (for highly alkaline resins) (see 4.2.2.3), adjust the pH to 3,5. Pipette into the solution approximately 25 ml of hydroxylamine hydrochloride solution (4.2.2.1) at (23 ± 1) °C. Stir for (10 ± 1) min. SIST EN ISO 11402:2005

ISO 11402:2004(E) 4

© ISO 2004 – All rights reserved Titrate rapidly, using the 1 mol/l solution of sodium hydroxide (or the 0,1 mol/l solution for low formaldehyde contents) (see 4.2.2.2) contained in a suitable-capacity burette (4.2.3.4), until the pH is 3,5. 4.2.5.4 Blank test Conduct a blank test in parallel with the determination, by the same procedure, using the same reagents as in the determination, but omitting the test portion. 4.2.6 Expression of results Calculate the free-formaldehyde content w(CH2O, free), expressed as a percentage by mass, using the equation: w(CH2O, free) = 103()cVVm− where c is the actual concentration, in moles per litre, of the solution of sodium hydroxide (4.

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