EN ISO 23631:2006

SLOVENSKI STANDARD
01-julij-2006
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Water quality - Determination of dalapon, trichloroacetic acid and selected haloacetic
acids - Method using gas chromatography (GC-ECD and/or GC-MS detection) after
liquid-liquid extraction and derivatization (ISO 23631:2006)
Wasserbeschaffenheit - Bestimmung von Dalapon, Trichloressigsäure und ausgewählten
Halogenessigsäuren - Verfahren mittels Gaschromatographie (GC-ECD und/oder GC-
MS-Detektion) nach Flüssig-Flüssig-Extraktion und Derivatisierung (ISO 23631:2006)
Qualité de l'eau - Dosage du dalapon, de l'acide trichloroacétique et d'acides
haloacétiques selectionnés - Méthode par chromatographie en phase gazeuse (détection
CG-DCE et/ou CG-SM) apres extraction liquide-liquide et dérivatisation (ISO
23631:2006)
Ta slovenski standard je istoveten z: EN ISO 23631:2006
ICS:
13.060.50
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EUROPEAN STANDARD
EN ISO 23631
NORME EUROPÉENNE
EUROPÄISCHE NORM
February 2006
ICS 13.060.50
English Version
Water quality - Determination of dalapon, trichloroacetic acid
and selected haloacetic acids - Method using gas
chromatography (GC-ECD and/or GC-MS detection) after liquid-
liquid extraction and derivatization (ISO 23631:2006)
Qualité de l'eau - Dosage du dalapon, de l'acide Wasserbeschaffenheit - Bestimmung von Dalapon,
trichloroacétique et d'acides haloacétiques selectionnés - Trichloressigsäure und ausgewählten Halogenessigsäuren
Méthode par chromatographie en phase gazeuse - Verfahren mittels Gaschromatographie (GC-ECD
(détection CG-DCE et/ou CG-SM) après extraction liquide- und/oder GC-MS-Detektion) nach Flüssig-Flüssig-
liquide et dérivatisation (ISO 23631:2006) Extraktion und Derivatisierung (ISO 23631:2006)
This European Standard was approved by CEN on 16 January 2006.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards may be obtained on application to the Central Secretariat or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation
under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,
Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 23631:2006: E
worldwide for CEN national Members.

Foreword
This document (EN ISO 23631:2006) has been prepared by Technical Committee ISO/TC 147
"Water quality" in collaboration with Technical Committee CEN/TC 230 "Water analysis", the
secretariat of which is held by DIN.

This European Standard shall be given the status of a national standard, either by publication of
an identical text or by endorsement, at the latest by August 2006, and conflicting national
standards shall be withdrawn at the latest by August 2006.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to implement this European Standard: Austria, Belgium,
Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary,
Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.

Endorsement notice
The text of ISO 23631:2006 has been approved by CEN as EN ISO 23631:2006 without any
modifications.
INTERNATIONAL ISO
STANDARD 23631
First edition
2006-02-01
Water quality — Determination of
dalapon, trichloroacetic acid and selected
haloacetic acids — Method using gas
chromatography (GC-ECD and/or GC-MS
detection) after liquid-liquid extraction
and derivatization
Qualité de l'eau — Dosage du dalapon, de l'acide trichloroacétique et
d'acides haloacétiques sélectionnés — Méthode par chromatographie
en phase gazeuse (détection CG-DCE et/ou CG-SM) après extraction
liquide-liquide et dérivatisation

Reference number
ISO 23631:2006(E)
©
ISO 2006
ISO 23631:2006(E)
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ii © ISO 2006 – All rights reserved

ISO 23631:2006(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope . 1
2 Normative references . 2
3 Principle. 2
4 Interferences . 2
5 Reagents. 2
6 Apparatus . 5
7 Sampling and sample pre-treatment. 7
8 Procedure . 7
9 Calibration . 10
10 Calculation. 13
11 Expression of results . 14
12 Test report . 15
Annex A (informative) Examples of gas chromatograms . 16
Annex B (informative) Mass spectra of methylated dalapon and haloacetic acids. 19
Annex C (informative) Precision data. 23
Bibliography . 24

ISO 23631:2006(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.
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 23631 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical,
chemical and biochemical methods.
iv © ISO 2006 – All rights reserved

ISO 23631:2006(E)
Introduction
The user should be aware the particular problems could require the specifications of additional marginal
conditions.
INTERNATIONAL STANDARD ISO 23631:2006(E)

Water quality — Determination of dalapon, trichloroacetic acid
and selected haloacetic acids — Method using gas
chromatography (GC-ECD and/or GC-MS detection) after liquid-
liquid extraction and derivatization
WARNING — Persons using this International Standard should be familiar with normal laboratory
practice. This International Standard does not purport to address all of the safety problems, if any,
associated with its use. It is the responsibility of the user to establish appropriate safety and health
practices and to ensure compliance with any national regulatory conditions.
Diazomethane is explosive, extremely toxic and severely irritating, causing pulmonary oedema when
inhaled in high concentrations. Long-term, low-level exposure may lead to sensitization, resulting in
asthma-like symptoms. Also, diazomethane and several of its chemical precursors have been cited as
carcinogens.
IMPORTANT — It is absolutely essential that tests conducted according to this International Standard
be carried out by suitably trained staff.
1 Scope
This International Standard specifies a method for the determination of dalapon, trichloroacetic acid (TCA) and
selected haloacetic acids (see Table 1) in ground water and drinking water by gas chromatography (GC-ECD
and/or GC-MS detection) after liquid-liquid-extraction and derivatization using diazomethane. Depending on
the matrix, the method is applicable to a concentration range from 0,5 µg/l to 10 µg/l. The validated reporting
limit of TCA and dalapon is about 0,05 µg/l (see Table C.1). Detection by electron-capture detector (ECD) in
general leads to lower detection limits. Detection by mass spectrometry (MS) allows analyte identification.
This method may be applicable as well to compounds not mentioned in Table 1 or to other types of water.
However, it is necessary to verify the applicability of this method for these special cases.
Table 1 — Haloacetic acids determined by this method
Name Molecular formula Relative molecular mass CAS registry No.
Bromochloroacetic acid C H BrClO 173,4 5589-96-8
2 2 2
a
Dalapon C H Cl O 143,0 75-99-0
3 4 2 2
Dibromoacetic acid C H Br O 217,8 631-64-1
2 2 2 2
Dichloroacetic acid C H Cl O 128,9 79-43-6
2 2 2 2
Monobromoacetic acid C H BrO 138,9 79-08-3
2 3 2
Monochloroacetic acid C H ClO 94,5 79-11-8
2 3 2
Trichloroacetic acid (TCA) C HCl O 163,4 76-03-9
2 3 2
a
2,2-Dichloropropionic acid.
ISO 23631:2006(E)
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 3696:1987, Water for analytical laboratory use — Specification and test methods
ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes
ISO 5667-2, Water quality — Sampling — Part 2: Guidance on sampling techniques
ISO 5667-3, Water quality — Sampling — Part 3: Guidance on the preservation and handling of water
samples
3 Principle
Dalapon, trichloroacetic acid (TCA) and selected haloacetic acids are extracted from the acidified water
sample with methyl-tert-bu
...