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

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 — Partie 1: Méthode CLHP

General Information

Status
Published
Publication Date
18-Mar-2014
Current Stage
9092 - International Standard to be revised
Start Date
14-Mar-2025
Completion Date
13-Dec-2025
Ref Project

Overview

ISO 17293-1:2014 specifies an HPLC method for the determination of chloroacetic acids (chloroacetates) - specifically monochloroacetic acid and dichloroacetic acid - in surfactant products. The standard applies to a range of anionic surfactants (e.g., alkyl (phenyl) ethoxylated carboxylates, AEC) and amphoteric surfactants (e.g., alkyl imidazoline carboxylate, alkyl dimethyl betaine and fatty acetyl propyl dimethyl betaine). It describes sample preparation, chromatographic conditions, calibration, quantification limits and precision expectations for reliable analytical testing.

Key Topics

  • Analytes covered: monochloroacetic acid (monochloroacetate) and dichloroacetic acid (dichloroacetate).
  • Analytical technique: high-performance liquid chromatography (HPLC) with UV detection (typical detection at 214 nm).
  • Column & mobile phase: analysis uses a C‑bonded silicone gel column (5 µm, 250 × 4.6 mm) and a mobile phase prepared from acetonitrile and water with added phosphoric acid; conditions (flow 1.0 ml/min, injection 20 µl, room temperature) are provided as validated parameters.
  • Calibration: external standard calibration with prepared standard solutions; linearity requirement R ≥ 0.999.
  • Sensitivity:
    • LOD (standard solution): ≤ 0.3 µg/ml (monochloroacetic), ≤ 0.2 µg/ml (dichloroacetic).
    • LOQ (standard solution): ≤ 1.0 µg/ml (monochloroacetic), ≤ 0.75 µg/ml (dichloroacetic).
    • At 5 g sample: LOD ≤ 6 mg/kg (mono) and ≤ 4 mg/kg (di); LOQ ≤ 20 mg/kg (mono) and ≤ 15 mg/kg (di).
  • Sample prep notes: dissolve sample in mobile phase, adjust pH to match mobile phase with diluted HCl, filter prior to injection. For betaine-type samples, an informative annex describes a cation-exchange cleanup to remove interfering peaks.
  • Precision expectations: repeatability r ~10% (≥50 mg/kg) or 15% (<50 mg/kg); reproducibility R ≈ 40%.

Applications

Who uses ISO 17293-1:2014:

  • Quality control and R&D laboratories in detergent, personal care and chemical manufacturing for monitoring chloroacetate impurities.
  • Regulatory and compliance testing to confirm product safety and meet limits on chloroacetic acid contamination.
  • Environmental and analytical contract labs performing routine surfactant analysis.
    Practical benefits include standardized HPLC parameters, defined LOD/LOQ for trace-level monitoring, and documented sample cleanup for problematic matrices (e.g., betaines).

Related Standards

  • ISO 17293-2 - Surface active agents - Determination of chloroacetic acid in surfactants - Part 2: ionic chromatographic method.
  • Normative references within the standard: ISO 607 (sample division), ISO 3696 (water for analytical use), ISO 5725-2 (precision assessment).

Keywords: ISO 17293-1:2014, HPLC method, chloroacetic acid, chloroacetate, monochloroacetic acid, dichloroacetic acid, surfactants, anionic surfactants, betaine, LOD, LOQ, analytical method.

Standard
ISO 17293-1:2014 - Surface active agents — Determination of chloroacetic acid (chloroacetate) in surfactants — Part 1: HPLC method Released:3/19/2014
English language
8 pages
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Frequently Asked Questions

ISO 17293-1:2014 is a standard published by the International Organization for Standardization (ISO). Its full title is "Surface active agents - Determination of chloroacetic acid (chloroacetate) in surfactants - Part 1: HPLC method". This standard covers: 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.

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.

ISO 17293-1:2014 is classified under the following ICS (International Classification for Standards) categories: 71.100.40 - Surface active agents. The ICS classification helps identify the subject area and facilitates finding related standards.

You can purchase ISO 17293-1:2014 directly from iTeh Standards. The document is available in PDF format and is delivered instantly after payment. Add the standard to your cart and complete the secure checkout process. iTeh Standards is an authorized distributor of ISO standards.

Standards Content (Sample)


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 2014
© 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

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
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

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
...

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記事タイトル:ISO 17293-1:2014-表面活性剤-界面活性剤における塩酸(塩酸エステル)の測定-パート1:HPLC法 記事の内容:ISO 17283-1:2014は、HPLC法を使用して、界面活性剤中の塩化モノアセチン酸(モノクロロアセテート)および二塩化アセチン酸(ジクロロアセテート)の濃度を測定するための方法を規定しています。この方法は、アニオン性界面活性剤(アルキル(フェニル)エトキシカルボン酸エステル(AEC)など)やアンフォテリック界面活性剤(アルキルイミダゾリンカルボン酸エステル、アルキルジメチルベタイン、脂肪酸アセチルプロピルジメチルベタインなど)に適用されます。モノクロロアセチン酸の検出限界(LOD)は、≤0.3µg/mlであり、ジクロロアセチン酸のLODは≤0.2µg/mlです。モノクロロアセチン酸の定量限界(LOQ)は、≤1.0µg/mlであり、ジクロロアセチン酸のLOQは≤0.75µg/mlです(標準溶液を使用)。また、5gの試料重量でのモノクロロアセチン酸のLODは≤6mg/kgであり、ジクロロアセチン酸のLODは≤4mg/kgです。モノクロロアセチン酸のLOQは≤20mg/kgであり、ジクロロアセチン酸のLOQは≤15mg/kgです。

ISO 17293-1:2014 is a standard that specifies a method for determining the levels of monochloroacetic acid (monochloroacetate) and dichloroacetic acid (dichloroacetate) in surfactants using a high-performance liquid chromatography (HPLC) method. The method is applicable to anionic surfactants like alkyl (phenyl) ethoxylated carboxylate (AEC) and amphoteric surfactants like alkyl imidazoline carboxylate, alkyl dimethyl betaine, and fatty acetyl propyl dimethyl betaine. The limit of detection (LOD) for monochloroacetic acid is ≤0.3 µg/ml and for dichloroacetic acid is ≤0.2 µg/ml. The limit of quantification (LOQ) for monochloroacetic acid is ≤1.0 µg/ml and for dichloroacetic acid is ≤0.75 µg/ml (using a standard solution). When determining the levels of these acids in a sample of 5 g weight, the LOD is ≤6 mg/kg for monochloroacetic acid and ≤4 mg/kg for dichloroacetic acid, while the LOQ is ≤20 mg/kg for monochloroacetic acid and ≤15 mg/kg for dichloroacetic acid.

記事のタイトル:ISO 17293-1:2014 - 表面活性剤- 表面活性剤中のクロロ酢酸(クロロアセテート)の測定− 第1部:HPLC法 記事内容:ISO 17283-1:2014は、HPLC法による表面活性剤中の一塩基クロロ酢酸(一塩基クロロアセテート)および二塩基クロロ酢酸(二塩基クロロアセテート)の濃度を測定するための方法を指定しています。この方法は、アルキル(フェニル)エトキシカルボキシレート(AEC)などの陰イオン性の表面活性剤や、アルキルイミダゾリンカルボキシレート、アルキルジメチルベタイン、脂肪酸アセチルプロピルジメチルベタインなどの両性表面活性剤に適用されます。一塩基クロロ酢酸の検出限界(LOD)は≤0.3µg/mLであり、二塩基クロロ酢酸のLODは≤0.2µg/mLです。一塩基クロロ酢酸の定量限界(LOQ)は≤1.0µg/mLであり、二塩基クロロ酢酸のLOQは≤0.75µg/mLです(標準溶液を使用した場合)。サンプルの重量が5gの場合、一塩基クロロ酢酸のLODは≤6mg/kgであり、二塩基クロロ酢酸のLODは≤4mg/kgです。また、一塩基クロロ酢酸のLOQは≤20mg/kgであり、二塩基クロロ酢酸のLOQは≤15mg/kgです。

기사 제목: ISO 17293-1:2014 - 표면활성제 - 표면활성제 내 클로로아세트산 (클로로아세테이트)의 결정 - 파트 1: HPLC 방법 기사 내용: ISO 17283-1:2014는 HPLC 방법을 통해 표면활성제 내의 모노클로로아세트산 (모노클로로아세테이트) 및 이클로로아세트산 (이클로로아세테이트)의 함량을 결정하기 위한 방법을 규정합니다. 이 방법은 알킬 (페닐) 에톡시카복실레이트 (AEC)와 같은 음이온 표면활성제, 알킬 이미다졸린 카복실레이트, 알킬 디메틸 베타인, 지방산 아세틸 프로필 디메틸 베타인과 같은 양이온 표면활성제에 적용됩니다. 모노클로로아세트산의 검출 한계 (LOD)는 ≤0.3 µg/ml이며 이클로로아세트산의 LOD는 ≤0.2 µg/ml입니다. 모노클로로아세트산의 측정 한계 (LOQ)는 ≤1.0 µg/ml이며 이클로로아세트산의 LOQ는 ≤0.75 µg/ml입니다 (표준용액 사용). 또한, 5g의 샘플 중 모노클로로아세트산의 LOD는 ≤6 mg/kg이고 이클로로아세트산의 LOD는 ≤4 mg/kg입니다. 모노클로로아세트산의 LOQ는 ≤20 mg/kg이며 이클로로아세트산의 LOQ는 ≤15 mg/kg입니다.

제목: ISO 17293-1:2014 - 표면활성제 - 표면활성제 내의 염소아세트산 (클로로아세트산)의 정량 결정 - 제1부: HPLC 방법 내용: ISO 17283-1:2014는 HPLC 방법을 사용하여 표면활성제 내의 단클로로아세트산 (단클로로아세테이트) 및 이클로로아세트산 (이클로로아세테이트)의 수준을 결정하기 위한 방법을 명시하고 있다. 이 방법은 알킬 (페닐) 에톡시카복실레이트 (AEC)와 같은 음이온 표면활성제, 알킬 이미다졸린 카복실레이트, 알킬 디메틸 베타인, 지방산 아세틸 프로필 디메틸 베타인과 같은 양이온 표면활성제에 적용된다. 단클로로아세트산의 검출 한계 (LOD)는 ≤0.3 µg/ml이고 이클로로아세트산은 ≤0.2 µg/ml이다. 단클로로아세트산의 정량 한계 (LOQ)는 ≤1.0 µg/ml이고 이클로로아세트산은 ≤0.75 µg/ml이다 (표준 용액을 사용할 경우). 샘플 중 5 g의 무게로 이산화클로로아세트산의 농도를 결정할 때 LOD는 ≤6 mg/kg이고 이클로로아세트산은 ≤4 mg/kg이며, LOQ는 ≤20 mg/kg의 단클로로아세트산과 ≤15 mg/kg의 이클로로아세트산이다.

기사 제목: ISO 17293-1:2014 - 표면활성제 - 계면활성제에서 클로로아세트산(클로로아세테이트)의 정량 결정 - 제1부: HPLC 방법 기사 내용: ISO 17293-1:2014는 HPLC 방법을 사용하여 계면활성제에서 단클로로아세트산(단클로로아세테이트) 및 이중클로로아세트산(이중클로로아세테이트)의 함량을 결정하기 위한 방법을 명시합니다. 이 방법은 알킬(페닐) 에톡시카보실레이트(AEC)와 같은 음이온성 계면활성제, 알킬 피톤일카복실레이트, 알킬 디메틸베타인 및 지방산 아세틸 프로필 디메틸베타인과 같은 양성계면활성제에 적용될 수 있습니다. 단클로로아세트산의 검출한계는 ≤0.3 µg/ml이고, 이중클로로아세트산의 검출한계는 ≤0.2 µg/ml입니다. 단클로로아세트산의 정량한계는 ≤1.0 µg/ml이고, 이중클로로아세트산의 정량한계는 ≤0.75 µg/ml입니다(표준 용액을 사용할 경우). 또한, 표본 중량이 5 g인 경우, 단클로로아세트산의 검출한계는 ≤6 mg/kg이고, 이중클로로아세트산의 검출한계는 ≤4 mg/kg입니다. 표본 중량이 5 g인 경우, 단클로로아세트산의 정량한계는 ≤20 mg/kg이고, 이중클로로아세트산의 정량한계는 ≤15 mg/kg입니다.

The article discusses ISO 17293-1:2014, which is a standard that specifies a method for determining the presence of monochloroacetic acid and dichloroacetic acid in surfactants using high-performance liquid chromatography (HPLC). The method is applicable to anionic surfactants like alkyl (phenyl) ethoxylated carboxylate (AEC) as well as amphoteric surfactants like alkyl imidazoline carboxylate, alkyl dimethyl betaine, and fatty acetyl propyl dimethyl betaine. The limit of detection for monochloroacetic acid is ≤0.3 µg/ml and ≤0.2 µg/ml for dichloroacetic acid. The limit of quantification for monochloroacetic acid is ≤1.0 µg/ml and ≤0.75 µg/ml for dichloroacetic acid when using a standard solution. Additionally, the limits of detection at a sample weight of 5 g are ≤6 mg/kg for monochloroacetic acid and ≤4 mg/kg for dichloroacetic acid. The limits of quantification at that sample weight are ≤20 mg/kg for monochloroacetic acid and ≤15 mg/kg for dichloroacetic acid.

記事のタイトル:ISO 17293-1:2014 - 表面活性剤-界面活性剤中のクロロ酢酸(クロロアセテート)の定量に関する方法- 第1部:HPLC法 記事の内容:ISO 17293-1:2014は、HPLC法を用いて表面活性剤中のモノクロロ酢酸(モノクロロアセテート)とジクロロ酢酸(ジクロロアセテート)の含有量を定量するための方法を規定しています。この方法は、アルキル(フェニル)エトキシカルボキシレート(AEC)などのアニオン性界面活性剤や、アルキルイミダゾリンカルボキシレート、アルキルジメチルベタイン、脂肪酰アセチルプロピルジメチルベタインなどのアンフォテリック界面活性剤に適用されます。モノクロロ酢酸の検出限界は≤0.3 µg/mlであり、ジクロロ酢酸の検出限界は≤0.2 µg/mlです。モノクロロ酢酸の定量限界は≤1.0 µg/mlであり、ジクロロ酢酸の定量限界は≤0.75 µg/mlです(標準溶液を使用)。また、サンプル重量が5 gの場合、モノクロロ酢酸の検出限界は≤6 mg/kgであり、ジクロロ酢酸の検出限界は≤4 mg/kgです。同様に、サンプル重量が5 gの場合、モノクロロ酢酸の定量限界は≤20 mg/kgであり、ジクロロ酢酸の定量限界は≤15 mg/kgです。

The article discusses ISO 17293-1:2014, which is a standard that specifies a method for determining the levels of monochloroacetic acid and dichloroacetic acid in surfactants using high-performance liquid chromatography (HPLC). This method is applicable to anionic surfactants like alkyl (phenyl) ethoxylated carboxylate (AEC) and amphoteric surfactants like alkyl imidazoline carboxylate, alkyl dimethyl betaine, and fatty acetyl propyl dimethyl betaine. The limit of detection (LOD) for monochloroacetic acid is ≤0.3 µg/ml and for dichloroacetic acid is ≤0.2 µg/ml. The limit of quantification (LOQ) for monochloroacetic acid is ≤1.0 µg/ml and for dichloroacetic acid is ≤0.75 µg/ml, using a standard solution. Additionally, the LOD for monochloroacetic acid is ≤6 mg/kg and for dichloroacetic acid is ≤4 mg/kg, with a sample weight of 5 g. The LOQ is ≤20 mg/kg for monochloroacetic acid and ≤15 mg/kg for dichloroacetic acid.