Surface active agents - Determination of hydroxyl value - p-Toluensulfonyl isocyanate (TSI) method and potentiometric titration with tetrabutylammonium hydroxide

This European Standard specifies a method for the determination of hydroxyl value of aliphatic and cyclic hydroxyl compounds with hydroxyl groups attached to primary and secondary carbon atoms.
This European Standard is applicable to polyacetals, temperature sensitive materials, high solids polymer polyols and rigid polyols and phenols.
This European Standard is not suitable for determination of hydroxyl groups attached to tertiary carbon atoms.
NOTE   This method is currently recommended for neutral refined products. However for products that contain an excess of acidic species a validation should be carried out to show that the acidic species either does not interfere or that the acidic species interference has been obviated.

Grenzflächenaktive Stoffe - Bestimmung der Hydroxylzahl - p-Toluolsulfonylisocyanat-(TSI-) Verfahren und potentiometrische Titration mit Tetrabutylammoniumhydroxid

Dieses Dokument legt ein Verfahren zur Bestimmung der Hydroxylzahl von aliphatischen und zyklischen Hydroxylverbindungen fest, deren Hydroxylgruppen an primäre und sekundäre Kohlenstoffatome gebunden sind.
Dieses Dokument gilt für Polyacetale, temperaturempfindliche Substanzen, hochpolymere Polyole, feste Polyole und Phenole.
Dieses Dokument ist nicht zur Bestimmung von an tertiäre Kohlenstoffatome gebundenen Hydroxylgruppen geeignet.
ANMERKUNG   Gegenwärtig wird dieses Verfahren für neutral raffinierte Produkte empfohlen. Bei Produkten jedoch, die einen Überschuss an sauren Bestandteilen enthalten, sollte eine Überprüfung erfolgen, um den Nachweis zu erbringen, dass die sauren Bestandteile nicht stören oder dass die durch die sauren Bestandteile bewirkte Beeinträchtigung beseitigt wurde.

Agents de surface - Détermination de l'indice d'hydroxyle - Méthode au p-toluènesulfonylisocyanate (TSI) et dosage potentiomètrique avec l'hydroxyde de tétrabutylammonium

Le présent document spécifie une méthode de détermination de l’indice d’hydroxyle des composés hydroxylés cycliques et aliphatiques dont les groupes hydroxyles sont liés aux atomes de carbone primaires ou secondaires.
Ce document s’applique aux polyacétals, aux matériaux sensibles à la température, aux hauts polymères solides de polyol et aux phénols et polyols rigides.
Ce document ne s’applique pas à la détermination des groupes hydroxyles liées aux atomes de carbone tertiaires.
NOTE   Cette méthode est actuellement recommandée pour les produits neutres et purifiés. Une validation est cependant nécessaire pour les produits contenant un excès d’espèces acides afin de montrer que ces dernières n’interfèrent pas ou que cette interférence a été prise en compte.

Površinsko aktivne snovi - Določevanje hidroksilne vrednosti - Metoda s p-toluen sulfonil izocianatom (metoda s TSI) in potenciometrijsko titracijo s tetrabutilamonijevim hidroksidom

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Status
Published
Publication Date
28-Nov-2006
Current Stage
9060 - Closure of 2 Year Review Enquiry - Review Enquiry
Due Date
04-Mar-2019
Completion Date
04-Mar-2019

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Surface active agents - Determination of hydroxyl value - p-Toluensulfonyl isocyanate (TSI) method and potentiometric titration with tetrabutylammonium hydroxideAgents de surface - Détermination de l'indice d'hydroxyle - Méthode au p-toluenesulfonylisocyanate (TSI) et dosage potentiometrique avec l'hydroxyde de tétrabutylammoniumGrenzflächenaktive Stoffe - Bestimmung der Hydroxylzahl - p-Toluolsulfonylisocyanat-(TSI-) Verfahren und potentiometrische Titration mit TetrabutylammoniumhydroxidTa slovenski standard je istoveten z:EN 15168:2006SIST EN 15168:2007en71.100.40Površinsko aktivna sredstvaSurface active agentsICS:SLOVENSKI

STANDARDSIST EN 15168:200701-april-2007

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 15168November 2006ICS 71.100.40 English VersionSurface active agents - Determination of hydroxyl value - p-Toluensulfonyl isocyanate (TSI) method and potentiometrictitration with tetrabutylammonium hydroxideAgents de surface - Détermination de l'indice d'hydroxyle -Méthode à la p-toluènesulfonylisocyanate (TSI) et titragepotentiomètrique avec l'hydroxyde de tétrabutylammoniumGrenzflächenaktive Stoffe - Bestimmung der Hydroxylzahl -p-Toluolsulfonylisocyanat-(TSI-) Verfahren undpotentiometrische Titration mitTetrabutylammoniumhydroxidThis European Standard was approved by CEN on 6 October 2006.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 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 translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.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, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36

B-1050 Brussels© 2006 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15168:2006: E

EN 15168:2006 (E) 2 Contents

Page Foreword..............................................................................................................................................................3 1 Scope......................................................................................................................................................4 2 Normative references............................................................................................................................4 3 Terms and definitions...........................................................................................................................4 4 Principle..................................................................................................................................................4 5 Reagents.................................................................................................................................................5 6 Apparatus...............................................................................................................................................5 7 Sampling.................................................................................................................................................6 8 Procedure...............................................................................................................................................6 9 Calculation and expression of results.................................................................................................8 10 Precision.................................................................................................................................................8 11 Test report..............................................................................................................................................8 Annex A (informative)

Interferences..................................................................................................................9 Annex B (informative)

Titration apparatus settings.......................................................................................10 Annex C (informative)

Example for a typical potentiometric titration curve...............................................11 Annex D (informative)

Statistical and other data derived from the results of inter-laboratory tests.......12 Bibliography......................................................................................................................................................13

EN 15168:2006 (E) 3 Foreword This document (EN 15168:2006) 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 or by endorsement, at the latest by May 2007, and conflicting national standards shall be withdrawn at the latest by May 2007. 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, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

EN 15168:2006 (E) 4 1 Scope This European Standard specifies a method for the determination of hydroxyl value of aliphatic and cyclic hydroxyl compounds with hydroxyl groups attached to primary and secondary carbon atoms. This European Standard is applicable to polyacetals, temperature sensitive materials, high solids polymer polyols and rigid polyols and phenols. This European Standard is not suitable for determination of hydroxyl groups attached to tertiary carbon atoms. NOTE This method is currently recommended for neutral refined products. However for products that contain an excess of acidic species a validation should be carried out to show that the acidic species either does not interfere or that the acidic species interference has been obviated. 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. EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987) ISO 607, Surface active agents and detergents — Methods of sample division 3 Terms and definitions For the purposes of this document, the following term and definition applies. 3.1 hydroxyl value, OHV number of milligrams of potassium hydroxide corresponding to the hydroxyl groups in 1 g of material 4 Principle A known mass of test sample is reacted with an excess of p-toluenesulfonyl isocyanate to form an acidic carbamate. Water is added to convert un-reacted isocyanate to sulfonamide followed by direct potentiometric titration of the acidic carbamate with tetra-n-butyl ammonium hydroxide in non-aqueous medium. The reactions occurring are as follows: a) formation of acidic carbamate; CH3

SO2-NCO + R-OH → CH3
SO2-NHCOOR b) hydrolysis of the excess of isocyanate; CH3
SO2-NCO + H2O → CH3
SO2 NH2 + CO2
EN 15168:2006 (E) 5 c) titration of the acidic carbamate formed. CH3
SO2-NH COOR + OH- → CH3

SO2-N- - COOR + H2O 5 Reagents During the analysis, unless otherwise specified, use only reagents of recognized analytical grade that have been checked in advance as to not interfere with the analytical results. WARNING — Acetonitrile, p-toluenesulfonyl isocyanate and tetrabutylammonium hydroxide being hazardous chemicals: conduct all the operations under a well-ventilated fume hood. 5.1 Water complying with grade 3 as defined in EN ISO 3696. 5.2 Acetonitrile, with water content < 0,01 % (m/m) (CAS number : 75-05-8). 5.3 Toluene, minimum purity 99 % (m/m) (CAS number : 108-88-3). 5.4 Tetrahydrofurane (THF), minimum purity 99 % (m/m) (CAS number : 109-99-9). 5.5 p-Toluenesulfonyl isocyanate (TSI), minimum purity 96 % (m/m) (CAS number : 4083-64-1). Maintain a nitrogen pad above this reagent after opening the flask. 5.6 p-Toluenesulfonyl isocyanate (TSI) reagent solution. Pipette 20 ml of TSI (5.5) into a dry 500 ml volumetric flask half filled with acetonitrile. Make up to the mark with acetonitrile and mix well. This reagent shall be prepared fresh monthly. 5.7 Potassium hydrogen phthalate, primary standard minimum purity 99 %(m/m) dried 2 h at 120 °C (CAS number : 877-24-7). 5.8 Tetra-n-butyl ammonium hydroxide standard volumetric solution, c([CH3 (CH2) 3] 4NOH) = 0,1 mol/l (CAS number : 2052-49-5). in 2-propanol/methanol. 5.9 Electrolyte: 0,4

mol/l tetraethyl ammonium bromide solution (CAS number : 71-91-0) in ethylene glycol (CAS number:107-21-1). 5.10 Electrolyte: saturated LiCl solution (CAS number : 7447-41-8) in ethanol (CAS number : 64-17-5). 6 Apparatus Normal laboratory apparatus, and the following. 6.1 Automatic potentiometer, with drift-controlled data acquisition and dynamic titrimetric dosing equipped with an automatic burette assembly and a magnetic stirrer. 6.2 Electrodes: There are two options for the electrodes definition. 6.2.1 Two electrodes system 6.2.1.1 Glass pH electrode. 6.2.1.2 Ag/AgCl double-junction ground joint diaphragm reference electrode, inner and outer chambers filled with 0,4 mol/l

solution of tetraethyl ammonium bromide in ethylene glycol (5.9). or

EN 15168:2006 (E) 6 6.2.2 One electrode system Combined glass pH electrode for titrations in non aqueous media (e.g. Solvotrode1)), filled with 0,4 mol/l solution of tetraethyl ammonium bromide in ethylene glycol (5.9). NOTE For electrode maintenance it is recommended to follow the manufacturer instructions. A saturated lithium chloride solution in ethanol (5.10) can also be used as electrolyte to fill the electrodes. 7 Sampling The sample shall be taken and stored in accordance with ISO 607. Samples that are solids at room temperature shall be heated prior to weighing to obtain a clear liquid, at the lowest possible temperature (50 °C to 70 °C) to avoid any undesirable changes in the sample. If higher temperatures are required to melt the sample, for example 110 °C, then the sample shall be removed from the oven as soon as a clear liquid is obtained. After heating, invert the sample

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