SIST ISO 27108:2011
Water quality - Determination of selected plant treatment agents and biocide products - Method using solid-phase microextraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS)
Water quality - Determination of selected plant treatment agents and biocide products - Method using solid-phase microextraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS)
ISO 27108:2010 specifies a method for the determination of the dissolved amount of selected plant treatment agents and biocide products in drinking water, ground water and surface water by solid‑phase microextraction (SPME) followed by gas chromatography-mass spectrometry (GC‑MS). The limit of determination depends on the matrix, on the specific compound to be analysed and on the sensitivity of the mass spectrometer. For most plant treatment agents and biocides to which ISO 27108:2010 applies, it is at least 0,05 µg/l. Validation data related to a concentration range between 0,05 µg/l and 0,3 µg/l have been demonstrated in an interlaboratory trial.
This method may be applicable to other compounds not explicitly covered by ISO 27108:2010 or to other types of water. However, it is necessary to verify the applicability of this method for these special cases.
Qualité de l'eau - Détermination d'agents de traitement et de produits d'usine sélectionnés - Méthode utilisant une micro-extraction en phase solide (MEPS) suivie d'une chromatographie en phase gazeuse-spectrométrie de masse (CG-SM)
L'ISO 27108:2010 spécifie une méthode pour la détermination de la quantité d'agents de traitement et de produits d'usine sélectionnés dissous dans l'eau potable, les eaux souterraines et les eaux de surface par micro-extraction en phase solide (MEPS) suivie d'une chromatographie en phase gazeuse-spectrométrie de masse (CG-SM). La limite de la détermination dépend de la matrice, du composé spécifique à analyser et de la sensibilité du spectromètre de masse. Pour la plupart des agents de traitement et de produits d'usine auxquels l'ISO 27108:2010 s'applique, elle est d'au moins 0,05 µg/l. Les données de validation relatives à une gamme de concentrations comprises entre 0,05 µg/l et 0,3 µg/l ont été démontrées lors d'un essai interlaboratoires.
Cette méthode peut être applicable à d'autres composés qui ne sont pas explicitement traités dans l'ISO 27108:2010 ou à d'autres types d'eau. Toutefois, il est nécessaire de vérifier l'applicabilité de cette méthode à ces cas particuliers.
Kakovost vode - Določevanje izbranih sredstev za zaščito rastlin in biocidov - Metoda plinske kromatografije/masne spektrometrije (GC/MS) po mikroekstrakciji na trdni fazi (SPME)
Ta mednarodni standard opredeljuje metodo določevanja raztopljene količine izbranih sredstev za zaščito rastlin in biocidov v pitni vodi, podtalni vodi in površinski vodi z mikroekstrakcijo na trdni fazi (SPME), ki ji sledi plinska kromatografija - masna spektrometrija (GC-MS). Meja določevanja je odvisna od matrice, od določene spojine za analizo in od občutljivosti masnega spektrometra. Za večino sredstev za zaščito rastlin, za katere velja ta mednarodni standard, je ta vsaj 0,05 µg/l. Validacijski podatki, ki se nanašajo na razpon koncentracije med 0,05 µg/l in 0,3 µg/l, so bili izkazani v medlaboratorijskem preskusu.
Ta metoda se lahko uporablja za druge spojine, ki niso izrecno zajete v tem mednarodnem standardu, ali za druge vrste vode. Vendar je treba potrditi uporabo te metode za take posebne primere. OPOMBA: Določevanje po tem mednarodnem standardu se izvaja na majhni količini vzorca (npr. volumen vzorca med 8 ml in 16 ml).
General Information
Buy Standard
Standards Content (Sample)
SLOVENSKI STANDARD
01-junij-2011
.DNRYRVWYRGH'RORþHYDQMHL]EUDQLKVUHGVWHY]D]DãþLWRUDVWOLQLQELRFLGRY
0HWRGDSOLQVNHNURPDWRJUDILMHPDVQHVSHNWURPHWULMH *&06 SRPLNURHNVWUDNFLML
QDWUGQLID]L 630(
Water quality - Determination of selected plant treatment agents and biocide products -
Method using solid-phase microextraction (SPME) followed by gas chromatography-
mass spectrometry (GC-MS)
Qualité de l'eau - Détermination d'agents de traitement et de produits d'usine
sélectionnés - Méthode utilisant une micro-extraction en phase solide (MEPS) suivie
d'une chromatographie en phase gazeuse-spectrométrie de masse (CG-SM)
Ta slovenski standard je istoveten z: ISO 27108:2010
ICS:
13.060.50 3UHLVNDYDYRGHQDNHPLþQH Examination of water for
VQRYL chemical substances
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
INTERNATIONAL ISO
STANDARD 27108
First edition
2010-04-15
Water quality — Determination of
selected plant treatment agents and
biocide products — Method using solid-
phase microextraction (SPME) followed
by gas chromatography-mass
spectrometry (GC-MS)
Qualité de l'eau — Détermination d'agents de traitement et de produits
d'usine sélectionnés — Méthode utilisant une micro-extraction en phase
solide (MEPS) suivie d'une chromatographie en phase gazeuse-
spectrométrie de masse (CG-SM)
Reference number
©
ISO 2010
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
© ISO 2010
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing 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 2010 – All rights reserved
Contents Page
Foreword .iv
Introduction.v
1 Scope.1
2 Normative references.1
3 Principle.1
4 Interferences .2
5 Reagents.4
6 Apparatus.5
7 Sampling and sample pretreatment .6
8 Procedure.6
9 Calibration.8
10 Calculation .11
11 Expression of results.11
12 Test report.11
Annex A (informative) Examples of gas chromatograms for compounds listed in Table 1 .12
Annex B (informative) Mass spectra of compounds of Table 1 (full-scan, EI, 70 eV).21
Annex C (informative) Precision data .35
Annex D (informative) General information about SPME .36
Bibliography.37
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 27108 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical,
chemical and biochemical methods.
iv © ISO 2010 – All rights reserved
Introduction
In recent years, ground water contamination as well as surface water contamination by pesticides has become
a matter of public concern. Identification and quantification of pesticides at trace level concentrations often
require both high sensitive chromatographic equipment and effective enrichment steps. In the analysis of
aqueous samples, sample preparation techniques including solid-phase extraction (SPE) are frequently the
most time-consuming steps and in many cases can be effectively replaced by solid-phase microextraction
(SPME).
When using this International Standard, it may be necessary in some cases to determine whether and to what
extent particular problems could require the specification of additional marginal conditions.
INTERNATIONAL STANDARD ISO 27108:2010(E)
Water quality — Determination of selected plant treatment
agents and biocide products — Method using solid-phase
microextraction (SPME) followed by gas chromatography-mass
spectrometry (GC-MS)
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.
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 the dissolved amount of selected plant
treatment agents and biocide products in drinking water, ground water and surface water by solid-phase
microextraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS). The limit of
determination depends on the matrix, on the specific compound to be analysed and on the sensitivity of the
mass spectrometer. For most plant treatment agents and biocides to which this International Standard applies,
it is at least 0,05 µg/l. Validation data related to a concentration range between 0,05 µg/l and 0,3 µg/l have
been demonstrated in an interlaboratory trial.
This method may be applicable to other compounds not explicitly covered by this International Standard or to
other types of water. However, it is necessary to verify the applicability of this method for these special cases.
NOTE Determinations by this International Standard are performed on small sample amounts (e.g. sample volumes
between 8 ml and 16 ml).
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, Water for analytical laboratory use — Specification and test methods
ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and
sampling techniques
ISO 5667-3, Water quality — Sampling — Part 3: Guidance on the preservation and handling of water
samples
3 Principle
Substances under investigation are extracted from the water sample by solid-phase microextraction (SPME)
according to their equilibrium of distribution. The extraction is performed by a chemically modified fused-silica
fibre, the surface of which is coated with a suitable adsorbent polymer. During extraction, the fibre is
immersed in the liquid sample. After completion of the extraction procedure, the fibre is drawn back into the
needle, removed from the sample vial, and introduced directly into the GC injector. The analytes are
transferred to the GC column by thermal desorption.
The analytes are separated, identified and quantified by means of capillary gas chromatography with mass
spectrometric detection (GC-MS) using electron impact (EI) ionisation mode.
Table 1 — Plant treatment agents and biocide products determined by this method
Reference No. in example
Molar mass
chromatograms of Figure
Name Molecular formula CAS registry No.
g/mol A.1 A.2 A.3
Dichlobenil C H ClN 1194-65-6 172,0 1 1 1
7 3 2
Desethylatrazine C H ClN 6190-65-4 187,6 2 2 3
6 10 5
Desethylterbutylazine C H ClN 30125-63-4 201,7 3 3 2
7 12 5
Simazine C H ClN 122-34-9 201,7 4 4 7
7 12 5
Atrazine C H ClN 1912-24-9 215,7 6 5 5
8 14 5
Lindane C H Cl 58-89-9 290,8 7 6 8
6 6 6
Terbutylazine C H ClN 5915-41-3 229,7 8 7 6
9 16 5
Metribuzine C H NOS 21087-64-9 214,3 9 8 14
8 14 4
Parathion-methyl C H NOPS 298-00-0 263,2 10 9 11
8 10 5
Heptachlor C H Cl 76-44-8 373,3 11 10 9
10 5 7
Terbutryn C H NS 886-50-0 241,4 12 11 12
10 19 5
Aldrin C H Cl 309-00-2 364,9 13 12 10
12 8 6
Metolachlor C H ClNO 51218-45-2 283,8 14 13 13
15 22 2
Parathion-ethyl C H NOPS 56-38-2 291,3 15 14 15
10 14 5
exo-Heptachlorepoxide C H ClO 1024-57-3 389,3 16 16 16
10 5 7
Pendimethalin C H N O 40487-42-1 281,3 17 15 17
13 19 3 4
endo-Heptachlorepoxide C H ClO 28044-83-9 389,3 18 17 18
10 5 7
Triclosan C H Cl O 3380-34-5 289,5 19 18 19
12 7 3 2
Dieldrin C H ClO 60-57-1 380,9 20 19 20
12 8 6
Carfentrazone-ethyl C H Cl F N O 128639-02-1 412,2 21 20 21
15 14 2 3 3 3
Diflufenican C H F N O 83164-33-4 394,3 22 21 22
19 11 5 2 2
Mefenpyr-diethyl C H Cl N O 135590-91-9 373,2 23 22 23
16 18 2 2 4
4 Interferences
4.1 Interferences during sampling
To avoid interference, collect samples as specified in Clause 7, observing the instructions specified in
ISO 5667-1 and ISO 5667-3.
2 © ISO 2010 – All rights reserved
4.2 Interferences during extraction procedure
Commercially available SPME fibres differ frequently in quality. Variations in the selectivity of the materials
also frequently occur from batch to batch, thus possibly causing significant deviations in extraction yield. This
does not basically impair their suitability, apart from a resulting higher detection limit of individual substances.
Inadequately conditioned fibres frequently result in lower extraction yields and poorly reproducible results;
therefore precondition new fibres according to Clause 8. Also condition used fibres by performing the whole
SPME process using at least two sampling vials containing only water (5.1) prior to starting with the first
sample of a new sample sequence.
Sensitivity of fibres gradually decreases throughout a sequence of samples. Therefore regular measurements
of the reference solution within the sample sequence (see 9.1) are recommended. The fibre is still usable if
the method shows required sensitivity for substances under investigation.
...
INTERNATIONAL ISO
STANDARD 27108
First edition
2010-04-15
Water quality — Determination of
selected plant treatment agents and
biocide products — Method using solid-
phase microextraction (SPME) followed
by gas chromatography-mass
spectrometry (GC-MS)
Qualité de l'eau — Détermination d'agents de traitement et de produits
d'usine sélectionnés — Méthode utilisant une micro-extraction en phase
solide (MEPS) suivie d'une chromatographie en phase gazeuse-
spectrométrie de masse (CG-SM)
Reference number
©
ISO 2010
PDF disclaimer
This PDF file may contain embedded typefaces. In accordance with Adobe's licensing policy, this file may be printed or viewed but
shall not be edited unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In
downloading this file, parties accept therein the responsibility of not infringing Adobe's licensing policy. The ISO Central Secretariat
accepts no liability in this area.
Adobe is a trademark of Adobe Systems Incorporated.
Details of the software products used to create this PDF file can be found in the General Info relative to the file; the PDF-creation
parameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In
the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below.
© ISO 2010
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing 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 2010 – All rights reserved
Contents Page
Foreword .iv
Introduction.v
1 Scope.1
2 Normative references.1
3 Principle.1
4 Interferences .2
5 Reagents.4
6 Apparatus.5
7 Sampling and sample pretreatment .6
8 Procedure.6
9 Calibration.8
10 Calculation .11
11 Expression of results.11
12 Test report.11
Annex A (informative) Examples of gas chromatograms for compounds listed in Table 1 .12
Annex B (informative) Mass spectra of compounds of Table 1 (full-scan, EI, 70 eV).21
Annex C (informative) Precision data .35
Annex D (informative) General information about SPME .36
Bibliography.37
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 27108 was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 2, Physical,
chemical and biochemical methods.
iv © ISO 2010 – All rights reserved
Introduction
In recent years, ground water contamination as well as surface water contamination by pesticides has become
a matter of public concern. Identification and quantification of pesticides at trace level concentrations often
require both high sensitive chromatographic equipment and effective enrichment steps. In the analysis of
aqueous samples, sample preparation techniques including solid-phase extraction (SPE) are frequently the
most time-consuming steps and in many cases can be effectively replaced by solid-phase microextraction
(SPME).
When using this International Standard, it may be necessary in some cases to determine whether and to what
extent particular problems could require the specification of additional marginal conditions.
INTERNATIONAL STANDARD ISO 27108:2010(E)
Water quality — Determination of selected plant treatment
agents and biocide products — Method using solid-phase
microextraction (SPME) followed by gas chromatography-mass
spectrometry (GC-MS)
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.
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 the dissolved amount of selected plant
treatment agents and biocide products in drinking water, ground water and surface water by solid-phase
microextraction (SPME) followed by gas chromatography-mass spectrometry (GC-MS). The limit of
determination depends on the matrix, on the specific compound to be analysed and on the sensitivity of the
mass spectrometer. For most plant treatment agents and biocides to which this International Standard applies,
it is at least 0,05 µg/l. Validation data related to a concentration range between 0,05 µg/l and 0,3 µg/l have
been demonstrated in an interlaboratory trial.
This method may be applicable to other compounds not explicitly covered by this International Standard or to
other types of water. However, it is necessary to verify the applicability of this method for these special cases.
NOTE Determinations by this International Standard are performed on small sample amounts (e.g. sample volumes
between 8 ml and 16 ml).
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, Water for analytical laboratory use — Specification and test methods
ISO 5667-1, Water quality — Sampling — Part 1: Guidance on the design of sampling programmes and
sampling techniques
ISO 5667-3, Water quality — Sampling — Part 3: Guidance on the preservation and handling of water
samples
3 Principle
Substances under investigation are extracted from the water sample by solid-phase microextraction (SPME)
according to their equilibrium of distribution. The extraction is performed by a chemically modified fused-silica
fibre, the surface of which is coated with a suitable adsorbent polymer. During extraction, the fibre is
immersed in the liquid sample. After completion of the extraction procedure, the fibre is drawn back into the
needle, removed from the sample vial, and introduced directly into the GC injector. The analytes are
transferred to the GC column by thermal desorption.
The analytes are separated, identified and quantified by means of capillary gas chromatography with mass
spectrometric detection (GC-MS) using electron impact (EI) ionisation mode.
Table 1 — Plant treatment agents and biocide products determined by this method
Reference No. in example
Molar mass
chromatograms of Figure
Name Molecular formula CAS registry No.
g/mol A.1 A.2 A.3
Dichlobenil C H ClN 1194-65-6 172,0 1 1 1
7 3 2
Desethylatrazine C H ClN 6190-65-4 187,6 2 2 3
6 10 5
Desethylterbutylazine C H ClN 30125-63-4 201,7 3 3 2
7 12 5
Simazine C H ClN 122-34-9 201,7 4 4 7
7 12 5
Atrazine C H ClN 1912-24-9 215,7 6 5 5
8 14 5
Lindane C H Cl 58-89-9 290,8 7 6 8
6 6 6
Terbutylazine C H ClN 5915-41-3 229,7 8 7 6
9 16 5
Metribuzine C H NOS 21087-64-9 214,3 9 8 14
8 14 4
Parathion-methyl C H NOPS 298-00-0 263,2 10 9 11
8 10 5
Heptachlor C H Cl 76-44-8 373,3 11 10 9
10 5 7
Terbutryn C H NS 886-50-0 241,4 12 11 12
10 19 5
Aldrin C H Cl 309-00-2 364,9 13 12 10
12 8 6
Metolachlor C H ClNO 51218-45-2 283,8 14 13 13
15 22 2
Parathion-ethyl C H NOPS 56-38-2 291,3 15 14 15
10 14 5
exo-Heptachlorepoxide C H ClO 1024-57-3 389,3 16 16 16
10 5 7
Pendimethalin C H N O 40487-42-1 281,3 17 15 17
13 19 3 4
endo-Heptachlorepoxide C H ClO 28044-83-9 389,3 18 17 18
10 5 7
Triclosan C H Cl O 3380-34-5 289,5 19 18 19
12 7 3 2
Dieldrin C H ClO 60-57-1 380,9 20 19 20
12 8 6
Carfentrazone-ethyl C H Cl F N O 128639-02-1 412,2 21 20 21
15 14 2 3 3 3
Diflufenican C H F N O 83164-33-4 394,3 22 21 22
19 11 5 2 2
Mefenpyr-diethyl C H Cl N O 135590-91-9 373,2 23 22 23
16 18 2 2 4
4 Interferences
4.1 Interferences during sampling
To avoid interference, collect samples as specified in Clause 7, observing the instructions specified in
ISO 5667-1 and ISO 5667-3.
2 © ISO 2010 – All rights reserved
4.2 Interferences during extraction procedure
Commercially available SPME fibres differ frequently in quality. Variations in the selectivity of the materials
also frequently occur from batch to batch, thus possibly causing significant deviations in extraction yield. This
does not basically impair their suitability, apart from a resulting higher detection limit of individual substances.
Inadequately conditioned fibres frequently result in lower extraction yields and poorly reproducible results;
therefore precondition new fibres according to Clause 8. Also condition used fibres by performing the whole
SPME process using at least two sampling vials containing only water (5.1) prior to starting with the first
sample of a new sample sequence.
Sensitivity of fibres gradually decreases throughout a sequence of samples. Therefore regular measurements
of the reference solution within the sample sequence (see 9.1) are recommended. The fibre is still usable if
the method shows required sensitivity for substances under investigation.
Adding sodium chloride to the sample results in a clear improvement of the extraction yield for most
substances listed in Table 1. The addition of common salt (near saturation) is therefore recommended. Some
substances listed in Table 1 show a reverse effect, which in most cases is weaker. Salt additions of < 20 % of
the saturation concentration (e.g. about 0,5 g of NaCl in an 8 ml water sample) cause a deterioration in
reproducibility. It is important to keep to exactly the same salt additions for all samples of a calibration
sequence and/or sample sequence.
Salt deposits may accumulate in the metal syringe needle of the fibre holder after extended use. Salt deposits
always occur when the syringe needle of the fibre holder is immersed in the water sample during extraction.
This may damage the fibres and the injector liner. Therefore adjust the immersion depth precisely, and, if
necessary, rinse out the SPME syringe needle to dissolve any encrusted salt.
To ensure that the measurements are of high accuracy and precision, keep extraction time constant (e.g.
60 min) within a sample sequence for all samples. It is highly preferable to use an automatic sampler with an
SPME option.
For automatic operation, preferably use sampling vials with a thin septum (e.g. 0,9 mm to 1,3 mm thickness)
in order to avoid
...
NORME ISO
INTERNATIONALE 27108
Première édition
2010-04-15
Qualité de l’eau — Détermination
d’agents de traitement et de produits
d’usine sélectionnés — Méthode
utilisant une micro-extraction en
phase solide (MEPS) suivie d’une
chromatographie en phase gazeuse-
spectrométrie de masse (CG-SM)
Water quality — Determination of selected plant treatment agents
and biocide products — Method using solid-phase microextraction
(SPME) followed by gas chromatography-mass spectrometry (GC-MS)
Numéro de référence
©
ISO 2010
DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2010
Droits de reproduction réservés. Sauf indication contraire, aucune partie de cette publication ne peut être reproduite ni utilisée
sous quelque forme que ce soit et par aucun procédé, électronique ou mécanique, y compris la photocopie, l’affichage sur
l’internet ou sur un Intranet, sans autorisation écrite préalable. Les demandes d’autorisation peuvent être adressées à l’ISO à
l’adresse ci-après ou au comité membre de l’ISO dans le pays du demandeur.
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
Version française parue en 2013
Publié en Suisse
ii © ISO 2010 – Tous droits réservés
Sommaire Page
Avant-propos .iv
Introduction .v
1 Domaine d’application . 1
2 Références normatives . 1
3 Principe . 1
4 Interférences . 2
4.1 Interférences lors de l’échantillonnage . 2
4.2 Interférences lors du mode opératoire d’extraction . 2
4.3 Interférences lors du mode opératoire de chromatographie en phase gazeuse et
spectrométrie de masse . 3
5 Réactifs . 4
6 Appareillage . 6
7 Échantillonnage et prétraitement de l’échantillon . 7
8 Mode opératoire. 7
8.1 Préparation des échantillons et extraction . 7
8.2 Chromatographe en phase gazeuse . 8
8.3 Identification des composés individuels par CG-SM . 8
8.4 Mesurage des valeurs à blanc . 9
9 Étalonnage . 9
9.1 Exigences générales . 9
9.2 Étalonnage avec un étalon interne couvrant le mode opératoire total .10
10 Calcul .11
11 Expression des résultats.12
12 Rapport d’essai .12
Annexe A (informative) Exemples de chromatogrammes en phase gazeuse pour les composés
énumérés dans le Tableau 1 .13
Annexe B (informative) Spectres de masse des composés du Tableau 1 (balayage complet, impact
électronique, 70 eV) .23
Annexe C (informative) Données de fidélité .36
Annexe D (informative) Informations générales sur la micro-extraction en phase solide (MEPS) .38
Bibliographie .39
Avant-propos
L’ISO (Organisation internationale de normalisation) est une fédération mondiale d’organismes
nationaux de normalisation (comités membres de l’ISO). L’élaboration des Normes internationales est
en général confiée aux comités techniques de l’ISO. Chaque comité membre intéressé par une étude
a le droit de faire partie du comité technique créé à cet effet. Les organisations internationales,
gouvernementales et non gouvernementales, en liaison avec l’ISO participent également aux travaux.
L’ISO collabore étroitement avec la Commission électrotechnique internationale (CEI) en ce qui concerne
la normalisation électrotechnique.
Les Normes internationales sont rédigées conformément aux règles données dans les Directives
ISO/CEI, Partie 2.
La tâche principale des comités techniques est d’élaborer les Normes internationales. Les projets de
Normes internationales adoptés par les comités techniques sont soumis aux comités membres pour vote.
Leur publication comme Normes internationales requiert l’approbation de 75 % au moins des comités
membres votants.
L’attention est appelée sur le fait que certains des éléments du présent document peuvent faire l’objet de
droits de propriété intellectuelle ou de droits analogues. L’ISO ne saurait être tenue pour responsable de
ne pas avoir identifié de tels droits de propriété et averti de leur existence.
L’ISO 27108 a été élaborée par le comité technique ISO/TC 147, Qualité de l’eau, sous-comité SC 2, Méthodes
physiques, chimiques et biochimiques.
iv © ISO 2010 – Tous droits réservés
Introduction
Au cours de ces dernières années, la contamination des eaux souterraines et des eaux de surface par
les pesticides est devenue un sujet de préoccupation d’ordre public. L’identification et la quantification
des pesticides à des concentrations présentes à l’état de traces nécessitent souvent des équipements
chromatographiques de grande sensibilité et des étapes d’enrichissement effectives. Dans l’analyse
d’échantillons aqueux, les techniques de préparation des échantillons, y compris l’extraction en phase
solide (EPS), constituent souvent les étapes les plus chronophages et peuvent, dans un grand nombre de
cas, être efficacement remplacées par la micro-extraction en phase solide (MEPS).
Lors de l’utilisation de la présente Norme internationale, il est possible que l’on soit amené, dans certains
cas, à déterminer si et dans quelle mesure des problèmes particuliers nécessiteront la spécification de
conditions particulières.
NORME INTERNATIONALE ISO 27108:2010(F)
Qualité de l’eau — Détermination d’agents de traitement
et de produits d’usine sélectionnés — Méthode utilisant
une micro-extraction en phase solide (MEPS) suivie d’une
chromatographie en phase gazeuse-spectrométrie de
masse (CG-SM)
AVERTISSEMENT — Il convient que l’utilisateur de la présente Norme internationale connaisse
bien les pratiques courantes de laboratoire. La présente Norme internationale n’a pas pour but
de traiter tous les problèmes de sécurité qui sont, le cas échéant, liés à son utilisation. Il incombe
à l’utilisateur d’établir des pratiques appropriées en matière d’hygiène et de sécurité, et de
s’assurer de la conformité à la réglementation nationale en vigueur.
IMPORTANT — Il est absolument essentiel que les essais réalisés conformément à la présente
Norme internationale soient exécutés par du personnel ayant reçu une formation adéquate.
1 Domaine d’application
La présente Norme internationale spécifie une méthode pour la détermination de la quantité d’agents
de traitement et de produits d’usine sélectionnés dissous dans l’eau potable, les eaux souterraines et
les eaux de surface par micro-extraction en phase solide (MEPS) suivie d’une chromatographie en
phase gazeuse-spectrométrie de masse (CG-SM). La limite de la détermination dépend de la matrice, du
composé spécifique à analyser et de la sensibilité du spectromètre de masse. Pour la plupart des agents
de traitement et de produits d’usine auxquels la présente Norme internationale s’applique, elle est d’au
moins 0,05 µg/l. Les données de validation relatives à une gamme de concentrations comprises entre
0,05 µg/l et 0,3 µg/l ont été démontrées lors d’un essai interlaboratoires.
Cette méthode peut être applicable à d’autres composés qui ne sont pas explicitement traités dans
la présente Norme internationale ou à d’autres types d’eau. Toutefois, il est nécessaire de vérifier
l’applicabilité de cette méthode à ces cas particuliers.
NOTE Les déterminations selon la présente Norme internationale sont effectuées sur des petites quantités
d’échantillon (par exemple, volumes d’échantillon compris entre 8 ml et 16 ml).
2 Références normatives
Les documents suivants, en tout ou partie, sont référencés de manière normative dans le présent
document et sont indispensables pour son application. Pour les références datées, seule l’édition citée
s’applique. Pour les références non datées, la dernière édition du document de référence s’applique (y
compris les éventuels amendements).
ISO 3696, Eau pour laboratoire à usage analytique — Spécification et méthodes d’essai
ISO 5667-1, Qualité de l’eau — Échantillonnage — Partie 1: Lignes directrices pour la conception des
programmes et des techniques d’échantillonnage
ISO 5667-3, Qualité de l’eau — Échantillonnage — Partie 3: Lignes directrices pour la conservation et la
manipulation des échantillons d’eau
3 Principe
Les substances étudiées sont extraites de l’échantillon d’eau par micro-extraction en phase solide (MEPS)
selon leur équilibre de distribution. L’extraction est effectuée par une fibre de silice fondue chimiquement
modifiée dont la surface est revêtue d’un adsorbant polymère approprié. Durant l’extraction, la fibre est
immergée dans l’échantillon liquide. À l’issue de la procédure d’extraction, la fibre est ramenée dans
l’aiguille, retirée du flacon à échantillon, puis introduite directement dans l’injecteur du chromatographe
en phase gazeuse. Les analytes sont transférés vers la colonne CG par désorption thermique.
Les analytes sont séparés, identifiés et quantifiés par chromatographie en phase gazeuse sur capillaire
avec détection par spectrométrie de masse (CG-SM) utilisant un mode d’ionisation par impact
électronique.
Tableau 1 — Agents de traitement et produits d’usine déterminés par cette méthode
Numéro de référence dans
Masse
les exemples de chromato-
Formule molécu-
molaire
Nom Numéro CAS
grammes de la Figure
laire
g/mol A.1 A.2 A.3
Dichlobénil C H Cl N 1194-65-6 172,0 1 1 1
7 3 2
Déséthylatrazine C H ClN 6190-65-4 187,6 2 2 3
6 10 5
Déséthylterbuthylazine C H ClN 30125-63-4 201,7 3 3 2
7 12 5
Simazine C H ClN 122-34-9 201,7 4 4 7
7 12 5
Atrazine C H ClN 1912-24-9 215,7 6 5 5
8 14 5
Lindane C H Cl 58-89-9 290,8 7 6 8
6 6 6
Terbuthylazine C H ClN 5915-41-3 229,7 8 7 6
9 16 5
Métribuzine C H N OS 21087-64-9 214,3 9 8 14
8 14 4
Parathion-méthyl C H NO PS 298-00-0 263,2 10 9 11
8 10 5
Heptachlore C H Cl 76-44-8 373,3 11 10 9
10 5 7
Terbutryne C H N S 886-50-0 241,4 12 11 12
10 19 5
Aldrine C H Cl 309-00-2 364,9 13 12 10
12 8 6
Métolachlore C H ClNO 51218-45-2 283,8 14 13 13
15 22 2
Parathion-éthyl C H NO PS 56-38-2 291,3 15 14 15
10 14 5
exo-Heptachlore-époxyde C H Cl O 1024-57-3 389,3 16 16 16
10 5 7
Pendiméthaline C H N O 40487-42-1 281,3 17 15 17
13 19 3 4
endo-Heptachlore-époxyde C H Cl O 28044-83-9 38
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.