SIST ISO 16560:2017

Surface active agents - Determination of polyethylene glycol content in nonionic ethoxylated surfactants - HPLC method

ISO 16560:2015 specifies a method for the determination of the polyethylene glycol (PEG) content in aromatic and aliphatic non-ionic surface active agents of the type R-(O-C2H4) n OH; where n is the mean ethylene oxide (EO) value. It is applicable to all ethoxylated products soluble in methanol or methanol/water mixture. This method applies to PEG concentrations as mass fraction greater than or equal to 0,1 %. This International Standard is not applicable to PEG whose molar mass is lower than 400 g/mol. Monomeric ethylene glycol, diethylene glycol, triethylene glycol, and glycerol are not detected.

Agents de surface tensioactifs - Dosage de la teneur en polyéthylène glycol dans les surfactants éthoxylés non ioniques - Méthode par CLHP

Površinsko aktivne snovi - Določevanje polietilen glikola v neionskih etoksiliranih površinsko aktivnih snoveh - Metoda HPLC

Ta mednarodni standard določa metodo za določevanje vsebnosti polietilen glikola (PEG) v aromatskih in alifatskih neionskih površinsko aktivnih sredstvih tipa R-(O-C2H4) n OH; pri čemer se uporablja povprečna vrednost etilen oksida (EO). Uporablja se za vse etoksilirane proizvode, topne v metanolu ali mešanici metanola in vode. Ta metoda se uporablja za koncentracije PEG kot najmanj 0,1-odstotni masni delež. Ta mednarodni standard se ne uporablja za PEG z molsko maso manj kot 400 g/mol. Prisotnost monomernega etilen glikola, dietilen glikola, trietilen glikola in glicerola se ne ugotavlja.

General Information

• Status: Published
• Public Enquiry End Date: 03-Nov-2016
• Publication Date: 08-Oct-2017
• 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 16560:2015 - Surface active agents - Determination of polyethylene glycol content in nonionic ethoxylated surfactants - HPLC method

Overview

ISO 16560:2015 specifies a standardized HPLC method for the determination of polyethylene glycol (PEG) content in aromatic and aliphatic non‑ionic ethoxylated surfactants (R‑(O‑C2H4)n‑OH). The method uses reversed‑phase liquid chromatography with an Evaporative Light Scattering Detector (ELSD) or Charged Aerosol Detector (CAD) and external calibration (PEG molar mass = 1 000 g·mol‑1). It is applicable to ethoxylated products soluble in methanol or methanol/water and for PEG mass fractions ≥ 0.1%. PEGs with molar mass < 400 g·mol‑1 and small glycols/glycerol (monomeric ethylene glycol, di‑, tri‑ethylene glycol, glycerol) are not detected.

Key topics and technical requirements

• Scope & limits: PEG ≥ 0.1% (m/m); PEG molar mass ≥ 400 g·mol‑1; sample solubility in methanol or methanol/water.
• Separation principle: reversed‑phase HPLC where PEG elutes early and ethoxylated surfactants are retained.
• Detectors: ELSD or CAD are specified to avoid interference from volatile solvents.
• Calibration: external calibration with PEG 1 000 (typical calibration solutions 0.01, 0.05, 0.10, 0.25 g·L‑1) and a log–log calibration curve of peak area vs. PEG mass.
• Chromatographic conditions (as given): C18 column (5 µm, 250 × 4.6 mm), flow 1.0 mL·min‑1, injection 20 µL, gradient from methanol/water to 100% methanol (to elute ethoxylates), room temperature.
• Sample prep: dissolve weighed sample in mobile phase (e.g., 80/20 methanol/water), dilute appropriately per expected PEG content, filter (0.45 µm) if needed.
• Precision: repeatability limit ≤ 0.2% (95% probability); reproducibility limit ≤ 0.8% (95% probability).
• Reporting: include sample identification, reference to ISO 16560, analytical conditions (temperature, ELSD/CAD settings), deviations and incidents.

Applications

ISO 16560:2015 is intended for laboratories performing quantitative analysis of PEG contamination or formulation content in nonionic ethoxylated surfactants. Typical uses:

• Quality control in surfactant and detergent manufacturing
• Raw material verification and supplier testing
• Formulation development and R&D for personal care, industrial cleaners, agrochemical surfactants
• Regulatory or specification compliance testing
• Contract and third‑party analytical laboratories providing HPLC PEG determination

Who should use this standard

• Analytical and QC chemists in surfactant, detergent, cosmetics and chemical manufacturing
• Test laboratories and contract research organizations (CROs)
• Regulatory and compliance teams verifying product composition
• Method developers needing a validated HPLC procedure for PEG content

Related standards

• ISO 3696 - Water for analytical laboratory use
• ISO 607 - Sample division for surfactants and detergents
• ISO 5725‑2 - Precision (repeatability and reproducibility) of measurement methods
• EN 12582 - European standard on which ISO 16560 was developed

Keywords: ISO 16560:2015, polyethylene glycol, PEG content, nonionic ethoxylated surfactants, HPLC method, ELSD, CAD, reversed phase HPLC, surfactant quality control.

Standards Content (Sample)

SLOVENSKI STANDARD
01-november-2017
3RYUãLQVNRDNWLYQHVQRYL'RORþHYDQMHSROLHWLOHQJOLNRODYQHLRQVNLKHWRNVLOLUDQLK
SRYUãLQVNRDNWLYQLKVQRYHK0HWRGD+3/&
Surface active agents - Determination of polyethylene glycol content in nonionic
ethoxylated surfactants - HPLC method
Agents de surface tensioactifs - Dosage de la teneur en polyéthylène glycol dans les
surfactants éthoxylés non ioniques - Méthode par CLHP
Ta slovenski standard je istoveten z: ISO 16560:2015
ICS:
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 16560
First edition
2015-04-15
Surface active agents —
Determination of polyethylene glycol
content in nonionic ethoxylated
surfactants — HPLC method
Agents de surface tensioactifs — Dosage de la teneur en polyéthylène
glycol dans les surfactants éthoxylés non ioniques — Méthode par CLHP
Reference number
©
ISO 2015
© ISO 2015
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 [e-mail]
Web www.iso.org
Published in Switzerland
ii © ISO 2015 – All rights reserved

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 1
6 Apparatus . 2
7 Sampling . 2
7.1 Preparation of the test sample . 2
7.2 Preparation of test solutions . 2
8 Procedure. 3
8.1 Apparatus settings . 3
8.2 Calibration . 3
8.2.1 Preparation of calibration solutions . 3
8.2.2 Calibration curve . 4
8.3 Determination . 4
9 Expression of results . 5
10 Precision . 5
10.1 Repeatability . 5
10.2 Reproducibility . 5
11 Test report . 5
Annex A (informative) Results of interlaboratory tests for fatty alcohol ethoxylate .6
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

Introduction
This International Standard was developed based on EN 12582.
INTERNATIONAL STANDARD ISO 16560:2015(E)
Surface active agents — Determination of polyethylene glycol
content in nonionic ethoxylated surfactants — HPLC method
1 Scope
This International Standard specifies a method for the determination of the polyethylene glycol (PEG)
content in aromatic and aliphatic non-ionic surface active agents of the type R-(O-C H ) OH; where n
2 4 n
is the mean ethylene oxide (EO) value. It is applicable to all ethoxylated products soluble in methanol
or methanol/water mixture. This method applies to PEG concentrations as mass fraction greater than
or equal to 0,1 %. This International Standard is not applicable to PEG whose molar mass is lower than
400 g/mol. Monomeric ethylene glycol, diethylene glycol, triethylene glycol, and glycerol are not detected.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensab
...

INTERNATIONAL ISO
STANDARD 16560
First edition
2015-04-15
Surface active agents —
Determination of polyethylene glycol
content in nonionic ethoxylated
surfactants — HPLC method
Agents de surface tensioactifs — Dosage de la teneur en polyéthylène
glycol dans les surfactants éthoxylés non ioniques — Méthode par CLHP
Reference number
©
ISO 2015
© ISO 2015
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 [e-mail]
Web www.iso.org
Published in Switzerland
ii © ISO 2015 – All rights reserved

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 1
5 Reagents . 1
6 Apparatus . 2
7 Sampling . 2
7.1 Preparation of the test sample . 2
7.2 Preparation of test solutions . 2
8 Procedure. 3
8.1 Apparatus settings . 3
8.2 Calibration . 3
8.2.1 Preparation of calibration solutions . 3
8.2.2 Calibration curve . 4
8.3 Determination . 4
9 Expression of results . 5
10 Precision . 5
10.1 Repeatability . 5
10.2 Reproducibility . 5
11 Test report . 5
Annex A (informative) Results of interlaboratory tests for fatty alcohol ethoxylate .6
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

Introduction
This International Standard was developed based on EN 12582.
INTERNATIONAL STANDARD ISO 16560:2015(E)
Surface active agents — Determination of polyethylene glycol
content in nonionic ethoxylated surfactants — HPLC method
1 Scope
This International Standard specifies a method for the determination of the polyethylene glycol (PEG)
content in aromatic and aliphatic non-ionic surface active agents of the type R-(O-C H ) OH; where n
2 4 n
is the mean ethylene oxide (EO) value. It is applicable to all ethoxylated products soluble in methanol
or methanol/water mixture. This method applies to PEG concentrations as mass fraction greater than
or equal to 0,1 %. This International Standard is not applicable to PEG whose molar mass is lower than
400 g/mol. Monomeric ethylene glycol, diethylene glycol, triethylene glycol, and glycerol are not detected.
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 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
...