SIST ISO 17280:2017

Surface active agents - Determination of 1,4-dioxan residues in surfactants obtained from epoxyethane by gas chromatography

ISO 17280:2015 provides a method for the determination of 1,4-dioxane residues in surfactants which are synthesized from epoxyethane, such as alkyl ether sulfates and alcohol ethoxylates.
The method is applicable for samples containing 1,4-dioxane more than 5 mg/kg. For samples containing 1,4-dioxane more than 100 mg/kg, the sample solutions should be diluted to appropriate concentration.

Agents de surface - Détermination de la teneur en résidus de 1,4-dioxane dans les agents tensioactifs obtenus à partir d'époxyéthane par chromatographie en phase gazeuse

Površinsko aktivne snovi - Določevanje ostankov 1,4-dioksana v površinsko aktivnih snoveh, pridobljenih iz epoksietana, s plinsko kromatografijo

Ta mednarodni standard podaja metodo za določevanje ostankov 1,4-dioksana v površinsko aktivnih snoveh, sintetiziranih iz epoksietana, kot so alkil eter sulfati in alkoholni etoksilati.
Metoda se uporablja za vzorce z vsebnostjo 1,4-dioksana več kot 5 mg/kg. Za vzorce z vsebnostjo 1,4-dioksana več kot 100 mg/kg je treba vzorčne raztopine razredčiti do ustrezne koncentracije.

General Information

• Status: Published
• Public Enquiry End Date: 03-Nov-2016
• Publication Date: 08-Oct-2017
• ICS: 71.040.50 - Physicochemical methods of analysis
• 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: 18-Sep-2017
• Due Date: 23-Nov-2017
• Completion Date: 09-Oct-2017
• Ref Project: ISO 17280:2015 - Surface active agents - Determination of 1,4-dioxan residues in surfactants obtained from epoxyethane by gas chromatography

Overview

ISO 17280:2015 specifies a validated analytical method for the determination of 1,4‑dioxane residues in surfactants synthesized from epoxyethane (for example, alcohol ethoxylates and alkyl ether sulfates). The method uses headspace sampling coupled with gas chromatography (GC) and flame ionization detection (FID). It is applicable to samples containing more than 5 mg/kg of 1,4‑dioxane; samples with >100 mg/kg should be diluted to an appropriate concentration before analysis.

Key topics and requirements

• Scope and applicability: Designed for surfactants produced from epoxyethane; lower applicability limit 5 mg/kg; dilution required above 100 mg/kg.
• Analytical principle: Weigh sample into a headspace vial, add calibration solution, equilibrate, and analyze vapour phase by temperature‑programmed GC‑FID. Quantification by internal standard or standard addition (and a relative response factor procedure).
• Reagents: High‑purity 1,4‑dioxane standard, 4‑methyl‑1,3‑dioxane as internal standard, and N,N‑dimethylformamide (DMF) as solvent (with validated alternatives such as DMA, DMSO, DEF or formamide).
• Apparatus: Headspace sampler, GC with temperature programming and FID, capillary column (e.g., polar PEG phase recommended), 20 ml crimp vials, gas‑tight syringes, and analytical balance.
• Calibration and preparation: Preparation of calibration solutions (A and B) and defined procedures for sample spiking, standard addition series, and calculation of results (graphical extrapolation or use of relative response factors).
• Quality and performance: The standard includes guidance on identification, calculation, precision (repeatability and reproducibility), and reporting requirements.
• Normative references: ISO 607 (sample division), ISO 3696 (water quality for analysis) and ISO 5725‑2 (accuracy and precision).

Applications and users

ISO 17280:2015 is intended for:

• Surfactant and detergent manufacturers performing routine quality control and batch release testing.
• Analytical testing laboratories assessing residual 1,4‑dioxane in ethoxylated products for safety and compliance.
• Regulatory and product‑safety teams verifying that consumer formulations meet residue limits or supplier specifications.
• R&D and process development groups optimizing ethoxylation and purification processes to reduce 1,4‑dioxane content.

Practical uses include compliance verification, supplier qualification, formulation safety assessment, and process optimization to minimize residual solvents.

Related standards

• ISO 607 - Surface active agents and detergents: Methods of sample division
• ISO 3696 - Water for analytical laboratory use
• ISO 5725‑2 - Accuracy (trueness and precision) of measurement methods

Keywords: ISO 17280:2015, 1,4‑dioxane, surfactants, gas chromatography, headspace, FID, alcohol ethoxylates, alkyl ether sulfates, epoxyethane.

Standards Content (Sample)

SLOVENSKI STANDARD
01-november-2017
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Surface active agents - Determination of 1,4-dioxan residues in surfactants obtained
from epoxyethane by gas chromatography
Agents de surface - Détermination de la teneur en résidus de 1,4-dioxane dans les
agents tensioactifs obtenus à partir d'époxyéthane par chromatographie en phase
gazeuse
Ta slovenski standard je istoveten z: ISO 17280:2015
ICS:
71.040.50 Fizikalnokemijske analitske Physicochemical methods of
metode analysis
71.100.40 Površinsko aktivna sredstva Surface active agents
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

INTERNATIONAL ISO
STANDARD 17280
First edition
2015-05-15
Surface active agents — Determination
of 1,4-dioxan residues in surfactants
obtained from epoxyethane by gas
chromatography
Agents de surface — Détermination de la teneur en résidus
de 1,4-dioxane dans les agents tensioactifs obtenus à partir
d’époxyéthane par chromatographie en phase gazeuse
Reference number
©
ISO 2015
© ISO 2015, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. [phone]
Fax [phone]
[e-mail]
www.iso.org
ii © ISO 2015 – All rights reserved

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Reagents . 1
4.1 1,4-Dioxane, purity 99,5 % minimum. . 1
4.2 4-Methyl-1,3-dioxane, purity 98 % minimum. . 1
4.3 N, N-dimethylformamide (DMF). . 1
4.4 Carrier gas: nitrogen or helium, purity 99,99 % minimum. . 2
5 Apparatus . 2
5.1 Analytical balance, 0,1 mg readability. . 2
5.2 Gas chromatography system, attached with temperature programmed device and
flame ionization detector (FID). . 2
5.3 Head space sampling unit . 2
5.4 20 ml crimped top glass vials, sealing pliers and sealing clamp suitable for head
space unit. . 2
5.5 Septum and crimped tops, lined with aluminium or PTFE, for closing the vials. . 2
5.6 Sealing pliers, for the vials. . 2
5.7 Capillary column, capable of the separation characteristics shown in Figure 2. . 2
5.8 Volumetric flasks, 50 ml and 100 ml capacity. . 2
5.9 Gas tight syringes or glass pipettes, 1 ml ± 0,01 ml capacity. . 2
6 Preparation of calibration solutions . 2
6.1 Calibration solution A . 2
6.2 Calibration solution B . 3
7 Procedure. 3
7.1 Preparation of the test sample . 3
7.2 Standard addition procedure . 3
7.2.1 Preparation of test sample solutions . 3
7.2.2 Determination . 4
7.2.3 Expression of results . 4
7.3 Relative response factor procedure . 4
7.3.1 Determination of relative response factor . 4
7.3.2 Preparation of test sample solutions . 5
7.3.3 Determination . 5
7.3.4 Expression of results . 5
8 Chromatographic conditions . 5
9 Evaluation . 6
9.1 General . 6
9.2 Identification . 7
9.3 Calculation . 7
10 Precision . 7
10.1 Repeatability limit . 7
10.2 Reproducibility limit . 7
11 Test report . 7
Annex A (informative) Statistical data from the ring carried out . 8
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT), see the following URL: Foreword — Supplementary information.
The committee responsible for this document is ISO/TC 91, Surface active agents.
iv © ISO 2015 – All rights reserved

INTERNATIONAL STANDARD ISO 17280:2015(E)
Surface active agents — Determination of 1,4-dioxan
residues in surfactants obtained from epoxyethane by gas
chromatography
1 Scope
This International Standard provides a method for the determination of 1,4-dioxane residues in
surfactants which are synthesized from epoxyethane, such as alkyl ether sulfates and alcohol ethoxylates.
The method is applicable for samples containing 1,4-dioxane more than 5 mg/kg. For samples containing
1,4-dioxane more than 100 mg/kg, the sample solutions should be diluted to appropriate concentration.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. 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
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results — Part 2: Basic method
for the determination of repeatability and reproducibility of a standard measurement method
3 Principle
The sample is weighed into a head space vial and a calibration solution is added. The seal
...

INTERNATIONAL ISO
STANDARD 17280
First edition
2015-05-15
Surface active agents — Determination
of 1,4-dioxan residues in surfactants
obtained from epoxyethane by gas
chromatography
Agents de surface — Détermination de la teneur en résidus
de 1,4-dioxane dans les agents tensioactifs obtenus à partir
d’époxyéthane par chromatographie en phase gazeuse
Reference number
©
ISO 2015
© ISO 2015, Published in Switzerland
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form
or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior
written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. [phone]
Fax [phone]
[e-mail]
www.iso.org
ii © ISO 2015 – All rights reserved

Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Principle . 1
4 Reagents . 1
4.1 1,4-Dioxane, purity 99,5 % minimum. . 1
4.2 4-Methyl-1,3-dioxane, purity 98 % minimum. . 1
4.3 N, N-dimethylformamide (DMF). . 1
4.4 Carrier gas: nitrogen or helium, purity 99,99 % minimum. . 2
5 Apparatus . 2
5.1 Analytical balance, 0,1 mg readability. . 2
5.2 Gas chromatography system, attached with temperature programmed device and
flame ionization detector (FID). . 2
5.3 Head space sampling unit . 2
5.4 20 ml crimped top glass vials, sealing pliers and sealing clamp suitable for head
space unit. . 2
5.5 Septum and crimped tops, lined with aluminium or PTFE, for closing the vials. . 2
5.6 Sealing pliers, for the vials. . 2
5.7 Capillary column, capable of the separation characteristics shown in Figure 2. . 2
5.8 Volumetric flasks, 50 ml and 100 ml capacity. . 2
5.9 Gas tight syringes or glass pipettes, 1 ml ± 0,01 ml capacity. . 2
6 Preparation of calibration solutions . 2
6.1 Calibration solution A . 2
6.2 Calibration solution B . 3
7 Procedure. 3
7.1 Preparation of the test sample . 3
7.2 Standard addition procedure . 3
7.2.1 Preparation of test sample solutions . 3
7.2.2 Determination . 4
7.2.3 Expression of results . 4
7.3 Relative response factor procedure . 4
7.3.1 Determination of relative response factor . 4
7.3.2 Preparation of test sample solutions . 5
7.3.3 Determination . 5
7.3.4 Expression of results . 5
8 Chromatographic conditions . 5
9 Evaluation . 6
9.1 General . 6
9.2 Identification . 7
9.3 Calculation . 7
10 Precision . 7
10.1 Repeatability limit . 7
10.2 Reproducibility limit . 7
11 Test report . 7
Annex A (informative) Statistical data from the ring carried out . 8
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT), see the following URL: Foreword — Supplementary information.
The committee responsible for this document is ISO/TC 91, Surface active agents.
iv © ISO 2015 – All rights reserved

INTERNATIONAL STANDARD ISO 17280:2015(E)
Surface active agents — Determination of 1,4-dioxan
residues in surfactants obtained from epoxyethane by gas
chromatography
1 Scope
This International Standard provides a method for the determination of 1,4-dioxane residues in
surfactants which are synthesized from epoxyethane, such as alkyl ether sulfates and alcohol ethoxylates.
The method is applicable for samples containing 1,4-dioxane more than 5 mg/kg. For samples containing
1,4-dioxane more than 100 mg/kg, the sample solutions should be diluted to appropriate concentration.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. 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
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results — Part 2: Basic method
for the determination of repeatability and reproducibility of a standard measurement method
3 Principle
The sample is weighed into a head space vial and a calibration solution is added. The sealed vial is
placed in a head space sampling instrument and allowed to reach thermal equilibrium. A portion of the
vapour phase is then analysed by temperature programmed GC with flame ionization detection. Either
an internal standard or standard addition method of quantification are employed.
4 Reagents
During the analysis, use only reagents of recognized analytical grade and the water used shall conform
to grade 3 in accordance with ISO 3696.
4.1 1,4-Dioxane, purity 99,5 % minimum.
4.2 4-Methyl-1,3-dioxane, purity 98 % minim
...