Surface active agents - Gas chromatographic trace determination of free ethylene oxide in ethoxylates

This European Standard specifies a test method for the determination of the content of free ethylene oxide in the range from 1 mg/kg to 100 mg/kg in polyglycols, ethoxylates of alcohols and alkylphenols and in fatty acid polyglycol esters.

Grenzflächenaktive Stoffe - Gaschromatographische Spurenbestimmung von freiem Ethylenoxid in Ethoxylaten

Diese Europäische Norm legt ein Verfahren zur Bestimmung von freiem Ethylenoxid im Bereich von 1 mg/kg bis 100 mg/kg in Polyglycolen, Ethoxylaten von Alkoholen und Alkylphenolen und in Fettsäurepolyglycolestern fest.

Agents de surface - Détermination de traces d'oxyde d'éthylene libre dans les éthoxylats par chromatographie en phase gazeuse

La présente Norme européenne spécifie une méthode de détermination de la teneur en oxyde d'éthylène libre comprise entre 1 mg/kg et 100 mg/kg dans les polyglycols, les éthoxylats d'alcools et d'alkylphénols ainsi que dans les esters de polyglycol d'acides gras.

Površinsko aktivne snovi - Določevanje sledov prostega etilen oksida v etoksilatih s plinsko kromatografijo

General Information

Status
Published
Publication Date
31-Aug-2002
ICS
71.100.40 - Surface active agents
Technical Committee
KDS - Cosmetics, chemical disinfectants and surface active agents
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
01-Sep-2002
Due Date
01-Sep-2002
Completion Date
01-Sep-2002
Ref Project
EN 13320:2002 - Surface active agents - Gas chromatographic trace determination of free ethylene oxide in ethoxylates

Overview

SIST EN 13320:2002 is a European Standard developed by CEN that defines a precise test method for determining the content of free ethylene oxide (EO) in surface active agents, specifically polyglycols, ethoxylates of alcohols and alkylphenols, and fatty acid polyglycol esters. The standard covers the quantitative trace determination of free ethylene oxide within the concentration range of 1 mg/kg to 100 mg/kg using gas chromatography with head-space sampling.

This method is vital for ensuring product safety and compliance in the manufacture and quality control of surfactants that include ethoxylated compounds, where residual free ethylene oxide can pose health and environmental hazards.

Key Topics

  • Scope and Applicability
    Specifies a gas chromatographic method to detect and quantify free ethylene oxide in ethoxylates and related compounds essential for controlling residual EO in industrial products.

  • Analytical Principle
    Analysis is conducted by head-space gas chromatography (GC) with flame ionization detection (FID). Free ethylene oxide in the sample is measured using the standard addition method for accuracy.

  • Reagents and Equipment
    Requires high purity water, ethylene oxide standards, N,N-dimethylformamide, and other analytical-grade reagents. Essential equipment includes a capillary gas chromatograph equipped with a head-space sampler and a fused silica column coated with crosslinked dimethylpolysiloxane.

  • Sample Preparation
    Laboratory samples must be handled following ISO 607 guidance. Samples can be liquids, pastes, or solids that may require gentle warming to liquefy without exceeding 50 °C to avoid decomposition of EO.

  • Calibration and Testing Procedures
    Employs carefully prepared ethylene oxide standard solutions and calibration solutions for method validation. Test samples are prepared with and without standard additions in vials sealed for head-space GC analysis.

  • Calculation and Expression of Results
    The EO content (micrograms per gram) is computed based on chromatographic peak areas adjusted by sample weight and calibration factors. Results are averaged for reproducibility.

  • Precision and Reliability
    Includes repeatability and reproducibility limits validated by interlaboratory ring tests to assure method consistency across labs.

  • Test Reporting Requirements
    Mandates detailed reporting on sample identification, test conditions, GC settings if altered, observed EO levels, and any deviations or issues encountered during testing.

Applications

  • Surfactant Quality Control
    Essential for manufacturers of surface active agents to monitor residual free ethylene oxide levels in products such as detergents, emulsifiers, and wetting agents.

  • Safety Compliance
    Helps ensure compliance with regulatory limits on ethylene oxide residues, minimizing health risks associated with EO exposure during product use or handling.

  • Research and Development
    Supports R&D activities aimed at optimizing ethoxylation processes and reducing residual EO in new or improved surfactant formulations.

  • Environmental Monitoring
    Enables monitoring of EO emissions and residues in environmental samples related to industrial surfactant production facilities.

Related Standards

  • EN ISO 3696 – Water for Analytical Laboratory Use: Specifies quality requirements for water used in analytical procedures critical to EN 13320.

  • ISO 607 – Surface Active Agents and Detergents: Deals with sample preparation and division methods relevant to surfactant analysis.

  • Additional CEN/TC 276 standards relating to surface active agents may complement the procedures and quality requirements outlined in EN 13320.

Keywords: SIST EN 13320:2002, free ethylene oxide determination, ethoxylates analysis, gas chromatography, surface active agents, polyglycols, ethoxylates, residual ethylene oxide, standard addition method, GC-FID, head-space sampling, surfactant quality control, CEN standards, analytical chemistry, trace determination

Frequently Asked Questions

SIST EN 13320:2002 is a standard published by the Slovenian Institute for Standardization (SIST). Its full title is "Surface active agents - Gas chromatographic trace determination of free ethylene oxide in ethoxylates". This standard covers: This European Standard specifies a test method for the determination of the content of free ethylene oxide in the range from 1 mg/kg to 100 mg/kg in polyglycols, ethoxylates of alcohols and alkylphenols and in fatty acid polyglycol esters.

This European Standard specifies a test method for the determination of the content of free ethylene oxide in the range from 1 mg/kg to 100 mg/kg in polyglycols, ethoxylates of alcohols and alkylphenols and in fatty acid polyglycol esters.

SIST EN 13320:2002 is classified under the following ICS (International Classification for Standards) categories: 71.100.40 - Surface active agents. The ICS classification helps identify the subject area and facilitates finding related standards.

You can purchase SIST EN 13320:2002 directly from iTeh Standards. The document is available in PDF format and is delivered instantly after payment. Add the standard to your cart and complete the secure checkout process. iTeh Standards is an authorized distributor of SIST standards.

Standards Content (Sample)


2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Grenzflächenaktive Stoffe - Gaschromatographische Spurenbestimmung von freiem Ethylenoxid in EthoxylatenAgents de surface - Détermination de traces d'oxyde d'éthylene libre dans les éthoxylats par chromatographie en phase gazeuseSurface active agents - Gas chromatographic trace determination of free ethylene oxide in ethoxylates71.100.40Površinsko aktivna sredstvaSurface active agentsICS:Ta slovenski standard je istoveten z:EN 13320:2002SIST EN 13320:2002en01-september-2002SIST EN 13320:2002SLOVENSKI
STANDARD
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13320February 2002ICS 71.100.40English versionSurface active agents - Gas chromatographic tracedetermination of free ethylene oxide in ethoxylatesAgents de surface - Détermination de traces d'oxyded'éthylène libre dans les éthoxylats par chromatographie enphase gazeuseGrenzflächenaktive Stoffe - GaschromatographischeSpurenbestimmung von freiem Ethylenoxid in EthoxylatenThis European Standard was approved by CEN on 16 November 2001.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,Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2002 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13320:2002 ESIST EN 13320:2002

Ring test results.9Annex B (informative)
Titration of ethylene oxide stock solution.11SIST EN 13320:2002

99,5 %.4.3Ethylene oxide, C2H4O, dissolved in dichloromethane, vials containing 50 mg of ethylene oxide dissolvedin 1 ml of dichloromethane.4.4N,N-dimethylformamide, C3H7NO.5 ApparatusOrdinary laboratory apparatus and the following.5.1Capillary gas chromatograph, with flame ionisation detector (FID) and head-space sampling accessory. Theapparatus shall be equipped with a split system. The head-space sampling accessory shall be designed such thateach head-space bottle can be thermostated for a defined time.NOTESince ethylene oxide is easily decomposed by traces of impurities such as acids and transition metals, (catalyseddecomposition), a meticulously clean sampling accessory is necessary.5.2Fused silica capillary column, coating: crosslinked dimethylpolysiloxanes, column length 30 m, internaldiameter 0,25 mm, film thickness 1,0 .5.3Vials, closable by means of a septum, 20 ml, suitable for head-space sampling accessory.5.4Septums and aluminium caps, lined with aluminium or polytetrafluoroethylene (PTFE) for closing the vials.SIST EN 13320:2002
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