Surface active agents -- Determination of free propylene oxide content in propylene oxide adduct surfactants -- GC method

ISO 19619:2018 specifies an analytical procedure for the determination of free propylene oxide in surfactants which are synthesized from propylene oxide copolymers. The method is appropriate for the qualitative and quantitative determination of propylene oxide groups in propylene oxide adducts, polyethers and polyglycol esters by headspace gas chromatography (HS-GC) with a flame ionization detector (FID) based on external procedure. Gas chromatography-mass spectrometry (GC-MS) is used for the confirmatory purposes.

Agents de surface tensioactifs -- Détermination de la teneur en oxyde de propylène libre dans les produits d'addition à base d'oxyde de propylène -- Méthode de chromatographie en phase gazeuse (GC)

General Information

Status
Published
Publication Date
09-Jan-2018
Current Stage
6060 - International Standard published
Start Date
22-Dec-2017
Completion Date
10-Jan-2018
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ISO 19619:2018 - Surface active agents -- Determination of free propylene oxide content in propylene oxide adduct surfactants -- GC method
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INTERNATIONAL ISO
STANDARD 19619
First edition
2018-01
Surface active agents —
Determination of free propylene oxide
content in propylene oxide adduct
surfactants — GC method
Agents de surface tensioactifs — Détermination de la teneur en oxyde
de propylène libre dans les produits d'addition à base d'oxyde de
propylène — Méthode de chromatographie en phase gazeuse (GC)
Reference number
ISO 19619:2018(E)
ISO 2018
---------------------- Page: 1 ----------------------
ISO 19619:2018(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2018, Published in Switzerland

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form

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ii © ISO 2018 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 19619:2018(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principles ..................................................................................................................................................................................................................... 1

5 Reagents ........................................................................................................................................................................................................................ 1

6 Apparatus ..................................................................................................................................................................................................................... 2

7 Preparation of calibration solutions ............................................................................................................................................... 3

7.1 Standard solutions ............................................................................................................................................................................... 3

7.1.1 General...................................................................................................................................................................................... 3

7.1.2 Difference weighing ...................................................................................................................................................... 3

7.1.3 Commercial standard vial ........................................................................................................................................ 3

7.2 Calibration solutions .......................................................................................................................................................................... 3

8 Sampling and preparation of the test sample ........................................................................................................................ 4

8.1 Preparation of the test sample .................................................................................................................................................. 4

8.2 Determination ......................................................................................................................................................................................... 4

8.3 Qualitative determination ............................................................................................................................................................. 4

8.4 Quantitative determination ......................................................................................................................................................... 4

9 Chromatographic and mass spectrometer conditions .................................................................................................. 5

10 Evaluation .................................................................................................................................................................................................................... 6

10.1 General ........................................................................................................................................................................................................... 6

10.2 Identification ............................................................................................................................................................................................ 6

10.3 Calculation .................................................................................................................................................................................................. 7

11 Precision ....................................................................................................................................................................................................................... 8

11.1 Repeatability ............................................................................................................................................................................................. 8

11.2 Reproducibility limit .......................................................................................................................................................................... 8

12 Test report ................................................................................................................................................................................................................... 8

Annex A (informative) Statistical data from the ring carried out ........................................................................................... 9

Bibliography .............................................................................................................................................................................................................................10

© ISO 2018 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 19619:2018(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

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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

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For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and

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URL: www.iso.org/iso/foreword.html.

This document was prepared by Technical Committee ISO/TC 91, Surface acting agents.

iv © ISO 2018 – All rights reserved
---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 19619:2018(E)
Surface active agents — Determination of free propylene
oxide content in propylene oxide adduct surfactants —
GC method

WARNING — The use of this document can involve hazardous materials, operations and

equipment. It does not purport to address all of the safety or environmental problems associated

with its use. It is the responsibility of users of this standard to take appropriate measures

to ensure the safety and health of personnel and the environment prior to application of the

standard, and fulfil statutory and regulatory requirements for this purpose.
1 Scope

This document specifies an analytical procedure for the determination of free propylene oxide in

surfactants which are synthesized from propylene oxide copolymers.

The method is appropriate for the qualitative and quantitative determination of propylene oxide groups

in propylene oxide adducts, polyethers and polyglycol esters by headspace gas chromatography (HS-

GC) with a flame ionization detector (FID) based on external procedure. Gas chromatography-mass

spectrometry (GC-MS) is used for the confirmatory purposes.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements 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
ISO 3696, Water for analytical laboratory use — Specification and test methods
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https://www.iso.org/obp
— IEC Electropedia: available at http://www.electropedia.org/
4 Principles

The sample is weighed into a headspace vial and 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 gas chromatography (GC). Qualitative detection is determined by retention

time of target compounds with FID or by relative abundance ratios of the fragment ions with MSD.

Quantification is achieved by external quantification method for GC-FID.
5 Reagents
During the analysis, use only reagents of recognized analytical grade.
© ISO 2018 – All rights reserved 1
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ISO 19619:2018(E)
5.1 Water, complying with grade 3 in accordance with ISO 3696.

5.2 Certain concentration of propylene oxide stock solution, prepared by either of the following

two methods:

a) Propylene oxide, C H O, with a purity of mass fraction ≥99,7 %, dissolved in acetonitrile, vials

3 6
containing 1,0 mg of propylene oxide dissolved in 1 ml of acetonitrile.

b) Commercial propylene oxide stock solutions of appropriate concentration if available may also be

used to simplify procedure and maintain the accuracy of solution concentration, e.g. 1 000 µg/mL

dissolved suitable solvent, or equivalent.
5.3 N, N-dimetylacetamide (DMAC), C H NO, with a purity ≥99,9 %.
3 7

DMAC may be substituted with other solvent which offers affordable safety and convenience.

Applicability of the solvent should be evaluated by appropriate validation. Possible substitutes are

including, but not limited to the following:
— Dimethyl formamide (DMF);
— Diethyl formamid
...

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