ISO 19619:2018

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
• ICS: 71.100.40 - Surface active agents
• Technical Committee: ISO/TC 91 - Surface active agents
• Drafting Committee: ISO/TC 91 - Surface active agents
• Current Stage: 9093 - International Standard confirmed
• Start Date: 16-Jan-2024
• Completion Date: 13-Dec-2025

Overview - ISO 19619:2018 (Surface active agents, propylene oxide)

ISO 19619:2018 specifies an analytical procedure for determining free propylene oxide in surfactants produced from propylene oxide copolymers. The method uses headspace gas chromatography (HS‑GC) with GC‑FID for quantitative analysis (external calibration) and GC‑MS for confirmatory qualitative identification. It is applicable to propylene oxide adducts, polyethers and polyglycol esters.

Key topics and technical requirements

• Principle: equilibrate sealed headspace vials and analyze the vapor phase by temperature‑programmed GC. Quantification by GC‑FID (external calibration); confirmation by GC‑MS (ion abundance ratios).
• Sample preparation: typical procedure - weigh ~1.0 g sample into headspace vials, add 5 mL N,N‑dimethylacetamide (DMAC), vortex, equilibrate and analyze (three replicate vials recommended).
• Calibration: prepare propylene oxide working solutions by difference weighing or commercial certified vials; generate multi‑point calibration (0 to 100 µg/mL example). For standard addition, calibration must be linear with correlation coefficient ≥ 0.995 and intercept SD ≤ 10% of mean.
• Identification criteria: match retention time with standard and confirm by MS relative ion abundances (propyl oxide detect ions m/z 28, 58, 27, 31 with established relative ratios and allowed deviations as specified).
• Reagents & apparatus: analytical‑grade reagents, DMAC (or validated solvent alternatives such as DMF/DMSO), high‑purity carrier gases (N2 for GC‑FID, He for GC‑MS), analytical balance, HS autosampler, capillary GC column (example: 30 m × 0.32 mm, 6% cyanopropylphenyl/94% dimethylpolysiloxane), FID and MSD.
• Quality and statistical requirements: precision, repeatability and reproducibility are addressed (statistical data and ring trial results included in annexes).
• Safety: the standard warns about hazardous materials and requires users to observe appropriate safety and environmental controls.

Applications - who uses ISO 19619:2018

• Surfactant and specialty chemical manufacturers - routine quality control of propylene‑oxide‑based adducts.
• Analytical and contract testing laboratories - validated HS‑GC methods for determining residual monomer.
• R&D teams - method development and confirmation testing for polyether and polyglycol ester products.
• Regulatory and compliance groups - documentation of free propylene oxide content for safety and product specifications.

Keywords: ISO 19619:2018, propylene oxide, headspace GC, HS‑GC, GC‑FID, GC‑MS, surfactants, propylene oxide adducts, polyethers, analytical procedure, calibration.

Related standards

• ISO 607 - Surface active agents and detergents - Methods of sample division
• ISO 3696 - Water for analytical laboratory use - Specification and test methods

This summary highlights practical use, instrumentation, calibration and qualification requirements from ISO 19619:2018 for laboratories implementing residual propylene oxide testing in surfactant products.

Standards Content (Sample)

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 2018
© 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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written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of
the requester.
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ii © ISO 2018 – All rights reserved

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
Foreword
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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

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.
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
...