Surface active agents -- Detergents -- Determination of alkylphenol ethoxylates

This document provides a method for the determination of alkylphenol ethoxylates (APEOs) in surfactants using high performance liquid chromatography (HPLC) and detected with diode array detector (DAD) or fluorescence detector (FLD). This method is appropriate for the detection and quantification of APEOs in surfactants.

Agents de surface -- Détergents -- Dosage des alkylphénols éthoxylés

General Information

Status
Published
Publication Date
23-Jul-2019
Current Stage
6060 - International Standard published
Start Date
04-Jul-2019
Completion Date
24-Jul-2019
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ISO 21264:2019 - Surface active agents -- Detergents -- Determination of alkylphenol ethoxylates
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INTERNATIONAL ISO
STANDARD 21264
First edition
2019-07
Surface active agents — Detergents
— Determination of alkylphenol
ethoxylates
Agents de surface — Détergents — Dosage des alkylphénols éthoxylés
Reference number
ISO 21264:2019(E)
ISO 2019
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ISO 21264:2019(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2019

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

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Published in Switzerland
ii © ISO 2019 – All rights reserved
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ISO 21264:2019(E)
Contents Page

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

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

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

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

4 Principle ........................................................................................................................................................................................................................ 1

5 Reagents and materials ................................................................................................................................................................................. 1

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

7 Procedure..................................................................................................................................................................................................................... 2

7.1 Standard preparation ........................................................................................................................................................................ 2

7.2 Sample preparation ............................................................................................................................................................................ 2

7.3 Analysis.......................................................................................................................................................................................................... 3

7.3.1 Chromatographic condition ................................................................................................................................... 3

7.3.2 Qualitative determination ........................................................................................................................................ 3

7.3.3 Calibration curve ............................................................................................................................................................. 3

7.3.4 Quantitative determination .................................................................................................................................... 4

8 Expression of results ........................................................................................................................................................................................ 4

8.1 Calculation .................................................................................................................................................................................................. 4

8.2 E valuation .................................................................................................................................................................................................... 4

8.3 Precision ....................................................................................................................................................................................................... 5

8.3.1 Repeatability ....................................................................................................................................................................... 5

8.3.2 Reproducibility limit..................................................................................................................................................... 5

9 Test report ................................................................................................................................................................................................................... 5

Annex A (informative) Chromatogram of alkylphenol ethoxylates (APEOs) ..............................................................6

Annex B (informative) Identification test ........................................................................................................................................................ 7

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

© ISO 2019 – All rights reserved iii
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ISO 21264:2019(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 of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso

.org/iso/foreword .html.

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

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/members .html.
iv © ISO 2019 – All rights reserved
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INTERNATIONAL STANDARD ISO 21264:2019(E)
Surface active agents — Detergents — Determination of
alkylphenol ethoxylates
1 Scope

This document provides a method for the determination of alkylphenol ethoxylates (APEOs) in

surfactants using high performance liquid chromatography (HPLC) and detected with diode array

detector (DAD) or fluorescence detector (FLD).

This method is appropriate for the detection and quantification of APEOs in surfactants.

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
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 Principle

The sample is weighed into a vial and extracted in methanol using an ultrasonic bath. Subsequently

the extract is filtered and analysed using high performance chromatography system with diode array

detector (DAD) or fluorescence detector (FLD). Quantification is achieved by external quantification

method and using the relationship chromatographic peak through its unique its retention time.

5 Reagents and materials

During the analysis, use only reagents of recognized analytical grade and the water of quality for HPLC

analysis.
5.1 Methanol, HPLC Grade.

5.2 Octylphenol ethoxylates (OPEO, 2 ≤ n ≤ 12), for example, Triton X-100 , CAS no. 9002-93-1,

Sigma-Aldrich Part Number T9284.

1) Triton X-1000 ®, CAS no. 9002-93-1, Sigma Aldrich Part Number T9284 is an example of products. This

information is given for the convenience of users of this document and does not constitute an endorsement by ISO

of the product named. Equivalent products may be used if they can be shown to lead to the same results.

© ISO 2019 – All rights reserved 1
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ISO 21264:2019(E)

5.3 Nonylphenol ethoxylates (NPEO, 3 ≤ n ≤ 18), for example, IGEPAL CO-630 , CAS no. 9016-45-

9, Sigma-Aldrich Part Number 542334.

NOTE There is a possibility that reagents of the grade of OPEO and NPEO are not available.

6 Apparatus
Normal laboratory apparatus and, in particular, the following:
6.1 Analytical balance, weighing to an accuracy of 0,1 mg.
6.2 Ultrasonic bath, 40 kHz, with thermostat.
6.3 Membrane filter, polyamide, 0,45 μm.
6.4 Volumetric flasks, 10 ml, 50 and 100 ml capacity.
6.5 High-performance Liquid Chromatography (HPLC) with DAD or FLD detector.

6.6 Reverse phase column with guard column, a stainless-steel column 150 mm and 2,1 mm in

internal diameter filled with 3,5 µm ODS (C ) as stationary phases.
7 Procedure
7.1 Standard preparation

7.1.1 Prepare 1 000 mg/l stock solutions of each APEOs from standard materials or certified solutions in

methanol. 100 mg of the OP EO (5.2) and NP EO (5.3) are dissolved in different 100 ml volumetric flasks

n n
with methanol and filled up to the mark respectively.

Depending on the stock concentrations prepared, the solubility at that concentration will have to be

ensured.

7.1.2 Prepare calibration curve for samples of each APEO stock standard solution at required

concentrations by adding aliquots of stock solutions to a 100 ml volumetric flask and then diluted with

methanol to the desired calibration level. If lower reporting limit is required, lower concentration of

calibration standard shall be prepared to cover the reporting limit. Each calibration curve is prepared

using the respective stock solution. The preparation of the Level 5 standard can be accomplished using

different volumes and concentrations of stock solutions as is accustomed in the individual laboratory.

The calibration vials shall be used within 24 h to ensure optimum results. Stock calibration standards

are routinely repla
...

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