Surface active agents -- Determination of chloroacetic acid (chloroacetate) in surfactants

ISO 17283-1:2014 specifies a method for the determination of monochloroacetic acid (monochloroacetate) and dichloroacetic acid (dichloroacetate) in surfactants by HPLC method. The method applies for anionic surfactants such as alkyl (phenyl) ethoxylated carboxylate (AEC) or amphoteric surfactants such as alkyl imidazoline carboxylate, alkyl dimethyl betaine, and fatty acetyl propyl dimethyl betaine. The limit of detection (LOD) is ≤0,3 µg/ml for monochloroacetic acid and ≤0,2 µg/ml for dichloroacetic acid; the limit of quantification (LOQ) is ≤1,0 µg/ml for monochloroacetic acid and ≤0,75 µg/ml for dichloroacetic acid (using a standard solution). The LOD, at 5 g of sample weight, is ≤6 mg/kg for monochloroacetic acid and ≤4 mg/kg for dichloroacetic acid; and the LOQ is ≤20 mg/kg for monochloroacetic acid and ≤15 mg/kg for dichloroacetic acid.

Agents de surface -- Détermination de l'acide chloroacétique (chloroacétate) dans les agents tensioactifs

General Information

Status
Published
Publication Date
18-Mar-2014
Current Stage
6060 - International Standard published
Start Date
12-Feb-2014
Completion Date
19-Mar-2014
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INTERNATIONAL ISO
STANDARD 17293-1
First edition
2014-04-01
Surface active agents — Determination
of chloroacetic acid (chloroacetate) in
surfactants —
Part 1:
HPLC method
Agents de surface — Détermination de l’acide chloroacétique
(chloroacétate) dans les agents tensioactifs —
Partie 1: Méthode CLHP
Reference number
ISO 17293-1:2014(E)
ISO 2014
---------------------- Page: 1 ----------------------
ISO 17293-1:2014(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2014

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
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2014 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 17293-1:2014(E)
Contents Page

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

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

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

3 Principle ........................................................................................................................................................................................................................ 1

4 Reagents ........................................................................................................................................................................................................................ 1

4.1 General ........................................................................................................................................................................................................... 1

5 Apparatus ..................................................................................................................................................................................................................... 2

6 Procedures .................................................................................................................................................................................................................. 2

6.1 HPLC conditions ..................................................................................................................................................................................... 2

6.2 Calibration .................................................................................................................................................................................................. 3

6.3 Sampling and analysis ...................................................................................................................................................................... 3

7 Results and calculation .................................................................................................................................................................................. 3

7.1 General ........................................................................................................................................................................................................... 3

7.2 The content of monochloroacetic acid ............................................................................................................................... 4

7.3 The content of dichloroacetic acid ......................................................................................................................................... 4

8 Precision ....................................................................................................................................................................................................................... 4

8.1 Repeatability limit ................................................................................................................................................................................ 4

8.2 Reproducibility limit .......................................................................................................................................................................... 4

9 Test report ................................................................................................................................................................................................................... 4

Annex A (informative) Preliminary treatment of betaine sample ......................................................................................... 6

Annex B (informative) Typical chromatogram .......................................................................................................................................... 8

© ISO 2014 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 17293-1:2014(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.

ISO 17293 consists of the following parts, under the general title Surface active agents — Determination

of chloroacetic acid (chloroacetate) in surfactants:
— Part 1: HPLC method
— Part 2: Ionic chromatographic method
iv © ISO 2014 – All rights reserved
---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 17293-1:2014(E)
Surface active agents — Determination of chloroacetic acid
(chloroacetate) in surfactants —
Part 1:
HPLC method
1 Scope

This part of ISO 17293 specifies a method for the determination of monochloroacetic acid

(monochloroacetate) and dichloroacetic acid (dichloroacetate) in surfactants by HPLC method.

The method applies for anionic surfactants such as alkyl (phenyl) ethoxylated carboxylate (AEC) or

amphoteric surfactants such as alkyl imidazoline carboxylate, alkyl dimethyl betaine, and fatty acetyl

propyl dimethyl betaine.

The limit of detection (LOD) is ≤0,3 µg/ml for monochloroacetic acid and ≤0,2 µg/ml for dichloroacetic

acid; the limit of quantification (LOQ) is ≤1,0 µg/ml for monochloroacetic acid and ≤0,75 µg/ml for

dichloroacetic acid (using a standard solution).

The LOD, at 5 g of sample weight, is ≤6 mg/kg for monochloroacetic acid and ≤4 mg/kg for dichloroacetic

acid; and the LOQ is ≤20 mg/kg for monochloroacetic acid and ≤15 mg/kg for dichloroacetic acid.

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 dissolved in the mobile phase in order to analyse by high performance liquid chromatography

(HPLC). After injection, it flows through a C -bonded silicone gel column. The monochloroacetic acid

(monochloroacetate) and dichloroacetic acid (dichloroacetate) are separated in the column

...

DRAFT INTERNATIONAL STANDARD ISO/DIS 17293-1
ISO/TC 91 Secretariat: ISIRI
Voting begins on Voting terminates on
2013-04-29 2013-07-29

INTERNATIONAL ORGANIZATION FOR STANDARDIZATION • МЕЖДУНАРОДНАЯ ОРГАНИЗАЦИЯ ПО СТАНДАРТИЗАЦИИ • ORGANISATION INTERNATIONALE DE NORMALISATION

Surface active agents — Determination of chloroacetic acid
(chloroacetate) in surfactants —
Part 1:
HPLC method

Agents de surface — Détermination de l'acide chloroacétique (chloroacétate) dans les agents tensioactifs —

Partie 1
ICS 71.100.40

To expedite distribution, this document is circulated as received from the committee

secretariat. ISO Central Secretariat work of editing and text composition will be undertaken at

publication stage.

Pour accélérer la distribution, le présent document est distribué tel qu'il est parvenu du

secrétariat du comité. Le travail de rédaction et de composition de texte sera effectué au

Secrétariat central de l'ISO au stade de publication.

THIS DOCUMENT IS A DRAFT CIRCULATED FOR COMMENT AND APPROVAL. IT IS THEREFORE SUBJECT TO CHANGE AND MAY NOT BE

REFERRED TO AS AN INTERNATIONAL STANDARD UNTIL PUBLISHED AS SUCH.

IN ADDITION TO THEIR EVALUATION AS BEING ACCEPTABLE FOR INDUSTRIAL, TECHNOLOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT

INTERNATIONAL STANDARDS MAY ON OCCASION HAVE TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL TO BECOME STANDARDS TO

WHICH REFERENCE MAY BE MADE IN NATIONAL REGULATIONS.

RECIPIENTS OF THIS DRAFT ARE INVITED TO SUBMIT, WITH THEIR COMMENTS, NOTIFICATION OF ANY RELEVANT PATENT RIGHTS OF WHICH

THEY ARE AWARE AND TO PROVIDE SUPPORTING DOCUMENTATION.
© International Organization for Standardization, 2013
---------------------- Page: 1 ----------------------
ISO/DIS 17293-1
COPYRIGHT PROTECTED DOCUMENT
© ISO 2013

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
Case postale 56 • CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland
ii © ISO 2013 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/DIS 17293-1
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.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards Draft. International Standards

adopted by the technical committees are circulated to the member bodies for voting. Publication as an

International Standard requires approval by at least 75 % of the member bodies casting a vote.

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.

ISO 17293-1 was prepared by Technical Committee ISO/TC 91 Surface active agents.
© ISO 2002 – All rights reserved iii
---------------------- Page: 3 ----------------------
DRAFT INTERNATIONAL STANDARD ISO/DIS 17293-1
Surface active agents - Determination of chloroacetic acids
(chloroacetates) in surfactants-Part 1: HPLC method
1 Scope

This International Standard specifies a method for the determination of mono-chloroacetic acid (mono-

chloroacetate) and di-chloroacetic acid (di-chloroacetate) in surfactants by HPLC method.

The method applies for anionic surfactants such as alkyl (phenyl) ethoxylated carboxylate (AEC) or

amphoteric surfactants such as alkyl imidazoline carboxylate , alkyl dimethyl betaine and fatty acetyl propyl

dimethyl betaine.

The limit of detection (LOD) should be ≤0,3 µg/ml for mono-chloroacetic acid and ≤0,2 µg/ml for di-

chloroacetic acid; and the limit of quantification (LOQ) should be ≤1,0 µg/ml for mono-chloroacetic acid and

≤0,75 µg/ml for di-chloroacetic acid (using a standard solution), respectively.

The LOD, at 5g of sample weight, should be ≤6 mg/kg for mono-chloroacetic acid and ≤4 mg/kg for di-

chloroacetic acid; and the LOQ should be ≤20 mg/kg for mono-chloroacetic acid and ≤15 mg/kg for di-

chloroacetic acid, respectively.
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 3696, Water for analytical laboratory use — Specification and test methods
ISO 607, Surface active agents and detergents — Methods of sample division.

ISO 5725-2, Accuracy (trueness and precision) 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 dissolved in the mobile phase in order to analyze by high performance liquid chromatography

(HPLC). After injection, it flows through an C -bonded silicone gel column. The mono-chloroacetic acid

(mono-chloroacetate) and di-chloroacetic acid (di-chloroacetate) are separated in the column and detected by

an UV detector.

The contents of mono-chloroacetic acid and di-chloroacetic acid in the sample are achieved by external

calibration method.
4 Reagents
4.1 General

During the analysis, use only reagents of recognized analytical grade and the water used shall conform to

grade 1 in accordance with ISO 3696, unless otherwise specified.
4.2 Mono-chloroacetic acid (ClCH COOH ): purity >99 % ( w/w )
© ISO 2002 – All rights reserved 1
---------------------- Page: 4 ----------------------
ISO/DIS 17293-1
4.3 Di-chloroacetic acid (Cl CHCOOH ): purity >99 % ( w/w )

4.4 Acetonitrile (CH CN ): HPLC grade, filtered before use with filter unit ( 5.7 )

4.5 Phosphoric acid (H PO )
3 4
4.6 Hydrochloric acid (HCl )
4.7 Hydrochloric acid solution, 1:1 ( V/V )

Add to about 10 ml of Hydrochloric acid (4.6) and 10 ml of water in portions, mix well.

5 Apparatus
Use usual laboratory apparatus and, in particular, the following.

5.1 HPLC instrument, equipped with pump and a high resolution UV detector or photo diode array detector, of

-5 -3

which the noise and the drift of base line at 254 nm <2×10 AU/s (blank cell) and at 254 nm <1×10 AU/h

( blank cell, after stabilizing for 60 minutes), respectively.

5.2 HPLC column: C -bonded phase silicone gel (particle size 5μm) , 250 mm  4,6 mm(ID), pH range from

1 to 8; or equivalent
5.3 Filter syringe, of capacity 2 ml or 5 ml
5.4 Injection syringe, of capacity 25 µl
5.5 Analytical balance, accurate to 0,1 mg
5.6 Ultra sonic device for the degassing of reagents

5.7 Filters with suitable porosity (0,2 µm or 0,45 µm) for the filtration of reagents and

...

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