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

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.

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
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
18-Sep-2017
Due Date
23-Nov-2017
Completion Date
09-Oct-2017

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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 17280:2015(E)
ISO 2015
---------------------- Page: 1 ----------------------
ISO 17280:2015(E)
COPYRIGHT PROTECTED DOCUMENT
© 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. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2015 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 17280:2015(E)
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

© ISO 2015 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 17280:2015(E)
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
---------------------- Page: 4 ----------------------
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
...

SLOVENSKI STANDARD
SIST ISO 17280:2017
01-november-2017
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DNWLYQLKVQRYHKSULGREOMHQLKL]HSRNVLHWDQDVSOLQVNRNURPDWRJUDILMR

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
SIST ISO 17280:2017 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST ISO 17280:2017
---------------------- Page: 2 ----------------------
SIST ISO 17280:2017
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 17280:2015(E)
ISO 2015
---------------------- Page: 3 ----------------------
SIST ISO 17280:2017
ISO 17280:2015(E)
COPYRIGHT PROTECTED DOCUMENT
© 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. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2015 – All rights reserved
---------------------- Page: 4 ----------------------
SIST ISO 17280:2017
ISO 17280:2015(E)
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

© ISO 2015 – All rights reserved iii
---------------------- Page: 5 ----------------------
SIST ISO 17280:2017
ISO 17280:2015(E)
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
---------------------- Page: 6 ----------------------
SIST ISO 17280:2017
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

...

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