Surface active agents - Determination of content of high boiling solvents in liquid detergents by GLC

This European Standard specifies a method for the identifying and quantifying of high boiling point solvents in finished liquid detergents and raw materials.

Grenzflächenaktive Stoffe - Bestimmung des Gehaltes an hochsiedenden Lösemitteln in flüssigen Reinigungsmitteln durch GLC

Diese Europäische Norm legt ein Verfahren zur qualitativen und quantitativen Analyse von hochsiedenden
Lösemitteln in flüssigen Reinigungsmitteln und Rohstoffen fest.

Agents de surface - Détermination de la teneur en solvants a point d'ébullition élevé dans les détergents liquides par chromatographie en phase gazeuse

La présente Norme européenne décrit une méthode permettant l’identification et la détermination quantitative des solvants a point d’ébullition élevé dans les détergents liquides formulés et les matieres premieres.

Površinsko aktivne snovi - Določevanje topil z visokim vreliščem v tekočih detergentih s plinsko tekočinsko kromatografijo (GLC)

General Information

Status
Published
Publication Date
31-Mar-2007
Withdrawal Date
31-Mar-2007
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-Apr-2007
Due Date
01-Apr-2007
Completion Date
01-Apr-2007

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Standard
SIST EN 14981:2007
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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Surface active agents - Determination of content of high boiling solvents in liquid detergents by GLCAgents de surface - Détermination de la teneur en solvants a point d'ébullition élevé dans les détergents liquides par chromatographie en phase gazeuseGrenzflächenaktive Stoffe - Bestimmung des Gehaltes an hochsiedenden Lösemitteln in flüssigen Reinigungsmitteln durch GLCTa slovenski standard je istoveten z:EN 14981:2006SIST EN 14981:2007en71.100.40Površinsko aktivna sredstvaSurface active agentsICS:SLOVENSKI

STANDARDSIST EN 14981:200701-april-2007

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 14981October 2006ICS 71.100.40 English VersionSurface active agents - Determination of content of high boilingsolvents in liquid detergents by GLCAgents de surface - Détermination de la teneur en solvantsà point d'ébullition élevé dans les détergents liquides parchromatographie en phase gazeuseGrenzflächenaktive Stoffe - Bestimmung des Gehaltes anhochsiedenden Lösemitteln in flüssigen Reinigungsmittelndurch GLCThis European Standard was approved by CEN on 28 August 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 14981:2006: E

EN 14981:2006 (E) 2 Contents Page Foreword..............................................................................................................................................................3 1 Scope......................................................................................................................................................4 2 Normative references............................................................................................................................4 3 Terms and Definitions...........................................................................................................................4 4 Principle..................................................................................................................................................4 5 Reagents.................................................................................................................................................4 6 Apparatus...............................................................................................................................................5 7 Sampling and preparation of the sample............................................................................................5 8 Procedure...............................................................................................................................................5 8.1 Gas chromatographic conditions........................................................................................................5 8.2 Preparation of solutions.......................................................................................................................5 8.2.1 Solvent reference solution 1.................................................................................................................5 8.2.2 Solvent reference solution 2.................................................................................................................5 8.2.3 Stock solution for calibrations.............................................................................................................6 8.2.4 Carvone internal standard solution.....................................................................................................6 8.3 Calibration..............................................................................................................................................6 8.4 Sample analysis.....................................................................................................................................7 8.4.1 Solvent identification............................................................................................................................7 8.4.2 Solvent quantification...........................................................................................................................7 9 Calculation and expression of results.................................................................................................7 10 Precision.................................................................................................................................................8 10.1 Repeatability limit..................................................................................................................................8 10.2 Reproducibility limit..............................................................................................................................8 11 Test report..............................................................................................................................................8 Annex A (informative)

Examples of chromatogram.......................................................................................9 A.1 Solvent identification............................................................................................................................9 A.2 Solvent quantification.........................................................................................................................12 Annex B (informative)

Statistical and other data derived from the results of inter-laboratory tests.....13 Bibliography......................................................................................................................................................14

EN 14981:2006 (E) 3 Foreword This document (EN 14981:2006) 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 April 2007, and conflicting national standards shall be withdrawn at the latest by April 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 14981:2006 (E) 4 1 Scope This European Standard specifies a method for the identifying and quantifying of high boiling point solvents in finished liquid detergents and raw materials. 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 607, Surface active agents and detergents - Methods of sample division 3 Term and Definition For the purposes of this European Standard, the following term and definition applies. high boiling solvent solvent, mainly a glycol and glycol ether product, with a boiling point significantly higher than water (100° C) 4 Principle The organic solvents are determined by gas chromatography. The sample is dissolved in ethanol and injected into a polar phase capillary column and the unknown solvent is identified by its retention time. After qualitative determination, the solvent is quantified using (-) Carvone (2-Methyl-5-(1-methylethenyl)-2-cyclohexene-1-one) as internal standard. 5 Reagents During the analysis, unless otherwise specified, use only reagents of recognized analytical grade that have been checked in advance so as not to interfere with the analytical results. WARNING Some reagents used throughout this procedure are toxic. Care should be taken not to inhale the vapours. Contact with the skin should also be avoided. Safety glasses and gloves should be worn when handling the reagents. Waste solvent disposal should be carried out in accordance with safety and environmental regulations. 5.1 Ethanol (CAS number: 64-17-5). 5.2 (-) Carvone (2-Methyl-5-(1-methylethenyl)-2-cyclohexene-1-one), minimum purity 99,5 % (CAS number : 6485-40-1) 5.3 Solvents to be determined (see example in Annex A) WARNING Some solvents may exist as different isomers. 5.4 Carrier gas for gas chromatography 5.5 Auxiliary gas for gas chromatography

EN 14981:2006 (E) 5 6 Apparatus Ordinary laboratory apparatus and the following: 6.1 Gas chromatograph equipped with split/splitless injection port and flame ionization detector (FID). 6.2 Electronic integrator or, preferably, a suitable data acquisition system. 6.3 Capillary column, capable of the separation characteristics shown in Figures A.1 and A.2. 6.4 Glass tube, with a capacity of at least 40 ml.

NOTE A 30 m x 0,25 mm internal diameter, fused silica capillary column (film thickness 0,25 µm) with 100 % polyethylene glycol stationary phase is advisable. 7 Sampling and preparation of the sample The laboratory sample shall be prepared and stored in accordance with ISO 607. 8 Procedure 8.1 Gas chromatographic conditions The following GC conditions have been found to be suitable. At least the quality of separation shown in Figures A.1 and A.2 shall be achieved.  Oven temperature programs:

 qualitative analysis: 60°C (5 min) to 240°C (5 min) at 5°C/min;  qu
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