Surface active agents - Alkoxylated derivatives - Determination of hydroxyl value - N-methyl imidazole method

This draft European Standard specifies a method for the determination of hydroxyl value of aliphatic and alicyclic hydroxyl compounds such as polyols, sorbitan esters, plasticisers and surface active agent alcohols and ethoxylates with hydroxyl values greater than 20 mg/g KOH.

Grenzflächenaktive Stoffe - Alkoxylierte Derivate - Bestimmung der Hydroxylzahl - N-Methylimidazol-Verfahren

Diese Europäische Norm legt ein Verfahren zur Bestimmung der Hydroxylzahl von aliphatischen und alizyklischen Hydroxylbestandteilen wie Polyalkoholen, Sorbitanestern, grenzflächenaktiven Alkoholen und Ethoxylaten mit Hydroxylzahlen größer als 20 mg/g KOH fest.

Agents de surface - Dérivés alkyloxylés - Détermination de l'indice d'hydroxyle - Méthode a la N-méthylimidazole

La présente Norme européenne spécifie une méthode de détermination de l'indice d'hydroxyle de composés hydroxy aliphatiques et alicycliques tels que les polyols, les esters de sorbitan, les plastifiants et les agents de surface sur base alcool et alkyloxylés avec des indices d'hydroxyle supérieurs a 20 mg KOH/g.

Površinsko aktivne snovi - Alkoksilatni derivati - Določevanje hidroksilne vrednosti - Metoda z N-metil imidazolom

General Information

Status
Published
Publication Date
30-Apr-2003
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-May-2003
Due Date
01-May-2003
Completion Date
01-May-2003

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EN 13926:2003
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.GURNVLOQHGrenzflächenaktive Stoffe - Alkoxylierte Derivate - Bestimmung der Hydroxylzahl - N-Methylimidazol-VerfahrenAgents de surface - Dérivés alkyloxylés - Détermination de l'indice d'hydroxyle - Méthode a la N-méthylimidazoleSurface active agents - Alkoxylated derivatives - Determination of hydroxyl value - N-methyl imidazole method71.100.40Površinsko aktivna sredstvaSurface active agentsICS:Ta slovenski standard je istoveten z:EN 13926:2003SIST EN 13926:2003en01-maj-2003SIST EN 13926:2003SLOVENSKI
STANDARD



SIST EN 13926:2003



EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13926March 2003ICS 71.100.40English versionSurface active agents - Alkoxylated derivatives - Determinationof hydroxyl value - N-methyl imidazole methodAgents de surface - Dérivés alkyloxylés - Détermination del'indice d'hydroxyle - Méthode à la N-méthylimidazoleGrenzflächenaktive Stoffe - Alkoxylierte Derivate -Bestimmung der Hydroxylzahl - N-Methylimidazol-VerfahrenThis European Standard was approved by CEN on 29 November 2002.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the 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 translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Slovakia, Spain, Sweden, Switzerland and UnitedKingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2003 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13926:2003 ESIST EN 13926:2003



EN 13926:2003 (E)2ContentspageForeword.31Scope.42Normative references.43Term and definition.44Principle.45Reagents.46Apparatus.57Sampling.58Procedure.59Expression of results.610Precision.811Test report.8Annex A (informative)
Results of interlaboratory test.9Annex B (informative)
Example for potentiometric operating parameters.11Annex C (informative)
Example for a typical titration curve and its derivative.12Bibliography.13SIST EN 13926:2003



EN 13926:2003 (E)3ForewordThis document (EN 13926:2003) has been prepared by Technical Committee CEN/TC 276 "Surface active agents",the secretariat of which is held by AFNOR.This European Standard shall be given the status of a national standard, either by publication of an identical text orby endorsement, at the latest by September 2003, and conflicting national standards shall be withdrawn at thelatest by September 2003.Annexes A, B, and C are informative.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal,Slovakia, Spain, Sweden, Switzerland and the United Kingdom.SIST EN 13926:2003



EN 13926:2003 (E)41 ScopeThis European Standard specifies a method for the determination of hydroxyl value of aliphatic and alicyclichydroxyl compounds such as polyols, sorbitan esters, plasticisers and surface active agent alcohols andalkoxylates with hydroxyl values greater than 20 mg KOH/g.2 Normative referencesThis European Standard incorporates by dated or undated reference, provisions from other publications. Thesenormative references are cited at the appropriate places in the text, and the publications are listed hereafter. Fordated references, subsequent amendments to or revisions of any of these publications apply to this EuropeanStandard only when incorporated in it by amendment or revision. For undated references the latest edition of thepublication referred to applies (including amendments).ISO 607, Surface active agents and detergents – Methods of sample division.ISO 4314, Surface active agents – Determination of free alkalinity or free acidity – Titrimetric method.3 Term and definitionFor the purposes of this European Standard, the following term and definition apply.3.1hydroxyl value I(OH)number of milligrams of potassium hydroxide needed to neutralize the acetic acid required to esterify the hydroxylgroups in 1 g of the material, or the number of milligrams of potassium hydroxide corresponding to the hydroxylgroups in 1 g of the material4 PrincipleA known mass of test sample is esterified with an excess of acetic anhydride/tetrahydrofuran solution usingN-methyl imidazole as a catalyst. The excess of acetic anhydride is hydrolysed and then the formed acetic acidistitrated potentiometrically with ethanolic potassium hydroxide standard volumetric solution. The hydroxyl value iscalculated from the difference in titration volumes of a blank test and the test sample.5 Reagents5.1GeneralDuring the analysis, unless otherwise specified, use only reagents of recognized analytical grade and have beenchecked in advance as to not interfere with the analytical results.WARNING — Tetrahydrofuran and N-methylimidazole being hazardous chemicals, all the operations shallbe conducted under a well ventilated fume hood.5.2Tetrahydrofuran, C4H8O.5.3Acetic anhydride, C4H6O3.5.4N-methyl imidazole, C4H6N2.5.5 Potassium hydrogen phthalate, C8H5O4K, w(C8H5O4K) = 99
% dried at (105 ± 1) °C.SIST EN 13926:2003



EN 13926:2003 (E)55.6Ethanol, C2H5OH.5.7Potassium hydroxide standard volumetric solution in ethanol, c(KOH) = 0,5 mol/l.Weigh 66,0 g of potassium hydroxide with a purity of 85
% (m/m) to the nearest 0,1 g and dissolve it in 250 mlfreshly boiled water. Then transfer the solution into a 2 l volumetric flask and complete to the mark with ethanol(5.6). Allow the solution to stand for 24 h before standardization.5.8Acetylation reagentCarefully mix 92 ml of tetrahydrofuran (5.2) and 8 ml of acetic anhydride (5.3). This solution is stable for up to onemon
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