EN 14667:2005

Surface active agents - Determination of low boiling solvents in liquid formulations - Gas chromatographic method

This European standard specifies a method for the determination of the content of low boiling solvents, e. g. methanol, ethanol propan-1-ol and propan-2-ol in liquid detergents.
The method is applicable to liquid detergents containing low boiling solvents in the range from 0,5 g/100 g to 10 g/100 g.

Grenzflächenaktive Stoffe - Bestimmung des Gehaltes an leichtsiedenden Lösemitteln in flüssigen Formulierungen - Gaschromatographisches Verfahren

Diese Europäische Norm legt ein Verfahren zur Bestimmung des Gehaltes an leichtsiedenden Lösemitteln,
z. B. Methanol, Ethanol, Propan-1-ol und Propan-2-ol, in flüssigen Detergenzien fest. Gewöhnlich ist nur ein
Lösemittel in dieser Probenart vorhanden.
Dieses Verfahren gilt für flüssige Detergenzien, die leichtsiedende Lösemittel in einem Massenanteil-Bereich
von 0,5 % bis 10 % enthalten.

Agents de surface - Détermination des solvants à faible point d'ébullition dans les formulations liquides - Méthode par chromatographie en phase gazeuse

La présente Norme européenne spécifie une méthode de détermination de la teneur en solvants à faible point d'ébullition, par exemple le méthanol, l'éthanol, le propan-1-ol et le propan-2-ol dans les détergents liquides. Généralement, un seul solvant est présent dans ce type d'échantillons.
Cette méthode est applicable aux détergents liquides contenant des solvants à faible point d'ébullition à des teneurs comprises entre 0,5 % et 10 % en masse.

Površinsko aktivne snovi – Določevanje topil z nizkim vreliščem v tekočih formulacijah – Metoda plinske kromatografije

General Information

• Status: Published
• Publication Date: 21-Jun-2005
• Withdrawal Date: 30-Dec-2005
• ICS: 71.100.40 - Surface active agents
• Technical Committee: CEN/TC 276 - Surface active agents
• Drafting Committee: CEN/TC 276/WG 1 - Methods of analysis
• Current Stage: 9093 - Decision to confirm - Review Enquiry
• Start Date: 31-Oct-2024
• Completion Date: 14-Apr-2025
• Ref Project: SIST EN 14667:2005 - Surface active agents - Determination of low boiling solvents in liquid formulations - Gas chromatographic method

Overview

EN 14667:2005 (CEN) - "Surface active agents - Determination of low boiling solvents in liquid formulations - Gas chromatographic method" specifies a validated gas chromatographic (GC) procedure for measuring low boiling solvents (for example methanol, ethanol, propan‑1‑ol, propan‑2‑ol) in liquid detergents and surfactant formulations. The method is applicable to formulations containing such solvents in the range 0.5 g/100 g to 10 g/100 g (0.5–10 % w/w). It is intended for quality control, regulatory testing and formulation verification where accurate solvent quantification is required.

Key topics and technical requirements

• Principle: Dissolve the liquid detergent in butan‑1‑ol (higher boiling, water‑miscible diluent) and determine solvent content by GC with flame ionization detection (FID).
• Instrumentation: Fused silica capillary column (recommendation: 30 m × 0.53 mm ID, 0.25 μm film, 5 % phenyl/95 % methyl polysiloxane), split injector, autosampler or manual injection, and electronic integrator. Typical injection volume 1 μL.
• Calibration: Multi‑level calibration using weighed standards (ethanol, propan‑1‑ol, propan‑2‑ol ≥ 99.5 %), linear regression (no forced origin). Calibration solutions are prepared in butan‑1‑ol and injected to establish slope and intercept for each solvent.
• Sample prep: Weigh sample (≈ 400 mg to 10 mL with butan‑1‑ol), sonicate if necessary, filter (0.45 μm) to remove particulates.
• Calculation: Use peak area, calibration slope and intercept to calculate solvent content in g/100 g. Formula and reporting requirements are specified.
• Performance & precision: Precision data (repeatability r and reproducibility R) are given in Annex B (examples: for propan‑2‑ol in a softener sample mean 1.17 g/100 g, r = 0.07 g/100 g, R = 0.25 g/100 g; for ethanol in a dishwashing liquid mean 3.09 g/100 g, r = 0.21 g/100 g, R = 0.37 g/100 g).

Applications and users

• Quality control laboratories in detergent and surfactant manufacturing.
• Formulation and R&D teams verifying residual or added volatile solvents.
• Regulatory and compliance testing where limits for low‑boiling alcohols must be demonstrated.
• Contract analytical labs offering GC‑FID testing of consumer and industrial liquid formulations.

Related standards

• ISO 607 (sample division for surfactants and detergents) - referenced for sampling.
• ISO 5725‑2 - used for inter‑laboratory precision evaluation methodology.
• Developed by CEN/TC 276 (Surface Active Agents).

Keywords: EN 14667:2005, gas chromatographic method, low boiling solvents, liquid detergents, GC‑FID, solvent determination, surfactant analysis, butan‑1‑ol, calibration, precision.

Standards Content (Sample)

SLOVENSKI STANDARD
01-november-2005
3RYUãLQVNRDNWLYQHVQRYL±'RORþHYDQMHWRSLO]QL]NLPYUHOLãþHPYWHNRþLK
IRUPXODFLMDK±0HWRGDSOLQVNHNURPDWRJUDILMH
Surface active agents - Determination of low boiling solvents in liquid formulations - Gas
chromatographic method
Grenzflächenaktive Stoffe - Bestimmung des Gehaltes an leichtsiedenden Lösemitteln in
flüssigen Formulierungen - Gaschromatographisches Verfahren
Agents de surface - Détermination des solvants a faible point d'ébullition dans les
formulations liquides - Méthode par chromatographie en phase gazeuse
Ta slovenski standard je istoveten z: EN 14667:2005
ICS:
71.100.40 Površinsko aktivna sredstva Surface active agents
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN 14667
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2005
ICS 71.100.40
English version
Surface active agents - Determination of low boiling solvents in
liquid formulations - Gas chromatographic method
Agents de surface - Détermination des solvants à faible Grenzflächenaktive Stoffe - Bestimmung des Gehaltes an
point d'ébullition dans les formulations liquides - Méthode leichtsiedenden Lösemitteln in flüssigen Formulierungen -
par chromatographie en phase gazeuse Gaschromatographisches Verfahren
This European Standard was approved by CEN on 19 May 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 Ref. No. EN 14667:2005: E
worldwide for CEN national Members.

Contents
Page
Foreword .3
1 Scope .4
2 Normative references .4
3 Terms and definitions.4
4 Principle.4
5 Reagents.4
6 Apparatus .4
7 Sampling and preparation of the sample .5
8 Procedure .5
9 Calculation and expression of results.6
10 Precision.6
11 Test report .7
Annex A (informative) Typical gas chromatogram.8
Annex B (informative) Results of inter-laboratory test .9

Foreword
This European Standard (EN 14667:2005) 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 December 2005, and conflicting national standards shall be withdrawn at the latest
by December 2005.
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.
1 Scope
This European Standard specifies a method for the determination of the content of low boiling solvents, e.g.
methanol, ethanol propan-1-ol and propan-2-ol in liquid detergents. Typically only one solvent is present in these
kinds of samples.
The method is applicable to liquid detergents containing low boiling solvents in the range from 0,5 % to 10 % by
weight.
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 Terms and definitions
For the purposes of this European Standard, the following terms and definitions apply.
low boiling solvent
alcohol with a boiling point below 100 °C
NOTE For example ethanol, propan-1-ol and propan-2-ol.
4 Principle
The liquid detergent is dissolved in butan-1-ol, which is a water miscible solvent with higher boiling point than the
solvents to be determined. The content of low boiling solvents is determined with gas chrom
...