Water quality — Sampling — Part 25: Guideline on the validation of the storage time of water samples

The purpose of this document is to describe test plans and different operating methodologies of these test plans to define and verify the acceptable length of stability of a substance in a sample under specified conditions of preservation (temperature, matrix, light, addition of a stabilizer, where appropriate, type of preservation etc.) before starting analytical protocols (chemicals and physico-chemicals analysis). Biological and microbiological methods are excluded. It is necessary to have an analytical method with performances that have already been characterized (repeatability, intermediate precision, trueness, accuracy and uncertainty) in order to perform the stability study and implement its test plans.

Qualité de l'eau — Échantillonnage — Partie 25: Lignes directrices pour la validation de la durée de conservation des échantillons d'eau

Kakovost vode - Vzorčenje - 25. del: Smernice za validacijo roka uporabnosti vzorcev vode

Namen tega dokumenta je opisati testne načrte in različne metodologije delovanja teh testnih načrtov za opredelitev in preverjanje sprejemljivega trajanja stabilnosti snovi v vzorcu pod določenimi pogoji shranjevanja (temperatura, matrica, svetloba, dodatek stabilizatorja, kjer je to primerno, vrsta shranjevanja itd.) pred začetkom analitskih protokolov (kemijske in fizikalno-kemijske analize). Biološke in mikrobiološke metode so izključene.
Za izvedbo študije stabilnosti in izvajanje načrtov testiranja je treba imeti analitsko metodo z že opredeljenimi testi zmogljivosti (ponovljivost, vmesna natančnost, pravilnost, točnost in negotovost).

General Information

Status
Published
Publication Date
22-Feb-2022
Current Stage
9020 - International Standard under periodical review
Start Date
15-Jan-2025
Due Date
15-Jan-2025
Completion Date
15-Jan-2025

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SLOVENSKI STANDARD
01-april-2023
Kakovost vode - Vzorčenje - 25. del: Smernice za validacijo roka uporabnosti
vzorcev vode
Water quality - Sampling - Part 25: Guideline on the validation of the storage time of
water samples
Qualité de l'eau - Échantillonnage - Partie 25: Lignes directrices pour la validation de la
durée de conservation des échantillons d'eau
Ta slovenski standard je istoveten z: ISO/TS 5667-25:2022
ICS:
13.060.45 Preiskava vode na splošno Examination of water in
general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

TECHNICAL ISO/TS
SPECIFICATION 5667-25
First edition
2022-02
Water quality — Sampling —
Part 25:
Guideline on the validation of the
storage time of water samples
Qualité de l'eau — Échantillonnage —
Partie 25: Lignes directrices pour la validation de la durée de
conservation des échantillons d'eau
Reference number
© ISO 2022
All rights reserved. Unless otherwise specified, or required in the context of its implementation, 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
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions and symbols . 1
4 Principle . 5
5 Definition of the scope of the stability study . 6
5.1 Aim of the stability study . 6
5.2 Selection of the maximum acceptable delay before analysis and the acceptance
criteria . 6
5.3 Influence parameters of the maximum acceptable delay before analysis . 7
5.4 Duration of the study . 7
5.5 Concentration levels . 8
5.6 Definition of the matrices and selection of the representative samples . 8
5.7 Guidelines to the stability studies of transformation products . 9
6 Definition of the experimental plan .11
6.1 Determination of the value of the quantity of the material at T and at other times
during the study . 11
6.2 Test materials .12
6.2.1 Preparation .12
6.2.2 Characterization of the test materials . 13
6.2.3 MQD Evaluation . 14
6.3 Definition of the test plan . 14
6.3.1 Choice of the type of study . 14
6.3.2 Randomization . 14
7 Performance of the tests .15
7.1 General . 15
7.2 Chronological stability study . 15
7.3 Type 1 pseudo-isochronous stability study . 15
7.4 Type 2 pseudo-isochronous stability study . 16
7.5 Isochronous stability study . 17
8 Graphic representation of the data .17
9 Validation of the data .20
9.1 Initial validation of the study at T . 20
9.1.1 Calculation of the value assigned to T (VA ) . 20
0 T0
9.1.2 Verification of the accuracy . 21
9.2 Validation at times different from T . 22
10 Using the results . .22
10.1 Graphic view of all the data .22
10.2 Determination of the maximum acceptable delay before analysis by condition .23
10.3 Conclusion of the study . 33
11 Expression of stability .34
Annex A (informative) Measurement process .35
Annex B (informative) Fundamental notions.36
Annex C (informative) Study of stability and influence parameters .42
Annex D (informative) Example of study of atrazine stability in water . 44
Bibliography .50
iii
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 of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to
the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see
www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 6,
Sampling (general methods).
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
iv
Introduction
This document addresses the need for harmonized and reliable data on stability, which is essential
for the expression of recommendations for both normative and regulatory purposes. It describes
a methodological framework that enables laboratories to produce quality data that can be shared
[7]
and even monetized .
It enables laboratories to study the stability of parameters when using the physico-chemical parameters
measurement system: organic micropollutants, inorganic and organometallic micropollutants, nutrients
and macropollutants in aqueous matrices (surface water, ground water, residual urban and industrial
water and drinking water). It covers the sampling, transport and laboratory storage operations.
NOTE This document does not cover solid matrices from aquatic environments (suspended solids,
sediments).
v
TECHNICAL SPECIFICATION ISO/TS 5667-25:2022(E)
Water quality — Sampling —
Part 25:
Guideline on the validation of the storage time of water
samples
1 Scope
The purpose of this document is to describe test plans and different operating methodologies
of these test plans to define and verify the acceptable length of stability of a substance in a sample
under specified conditions of preservation (temperature, matrix, light, addition of a stabilizer, where
appropriate, type of preservation etc.) before starting analytical protocols (chemicals and physico-
chemicals analysis). Biological and microbiological methods are excluded.
It is necessary to have an analytical method with performances that have already been characterized
(repeatability, intermediate precision, trueness, accuracy and uncertainty) in order to perform
the stability study and implement
...


TECHNICAL ISO/TS
SPECIFICATION 5667-25
First edition
2022-02
Water quality — Sampling —
Part 25:
Guideline on the validation of the
storage time of water samples
Qualité de l'eau — Échantillonnage —
Partie 25: Lignes directrices pour la validation de la durée de
conservation des échantillons d'eau
Reference number
© ISO 2022
All rights reserved. Unless otherwise specified, or required in the context of its implementation, 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
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms, definitions and symbols . 1
4 Principle . 5
5 Definition of the scope of the stability study . 6
5.1 Aim of the stability study . 6
5.2 Selection of the maximum acceptable delay before analysis and the acceptance
criteria . 6
5.3 Influence parameters of the maximum acceptable delay before analysis . 7
5.4 Duration of the study . 7
5.5 Concentration levels . 8
5.6 Definition of the matrices and selection of the representative samples . 8
5.7 Guidelines to the stability studies of transformation products . 9
6 Definition of the experimental plan .11
6.1 Determination of the value of the quantity of the material at T and at other times
during the study . 11
6.2 Test materials .12
6.2.1 Preparation .12
6.2.2 Characterization of the test materials . 13
6.2.3 MQD Evaluation . 14
6.3 Definition of the test plan . 14
6.3.1 Choice of the type of study . 14
6.3.2 Randomization . 14
7 Performance of the tests .15
7.1 General . 15
7.2 Chronological stability study . 15
7.3 Type 1 pseudo-isochronous stability study . 15
7.4 Type 2 pseudo-isochronous stability study . 16
7.5 Isochronous stability study . 17
8 Graphic representation of the data .17
9 Validation of the data .20
9.1 Initial validation of the study at T . 20
9.1.1 Calculation of the value assigned to T (VA ) . 20
0 T0
9.1.2 Verification of the accuracy . 21
9.2 Validation at times different from T . 22
10 Using the results . .22
10.1 Graphic view of all the data .22
10.2 Determination of the maximum acceptable delay before analysis by condition .23
10.3 Conclusion of the study . 33
11 Expression of stability .34
Annex A (informative) Measurement process .35
Annex B (informative) Fundamental notions.36
Annex C (informative) Study of stability and influence parameters .42
Annex D (informative) Example of study of atrazine stability in water . 44
Bibliography .50
iii
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 of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to
the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see
www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 147, Water quality, Subcommittee SC 6,
Sampling (general methods).
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www.iso.org/members.html.
iv
Introduction
This document addresses the need for harmonized and reliable data on stability, which is essential
for the expression of recommendations for both normative and regulatory purposes. It describes
a methodological framework that enables laboratories to produce quality data that can be shared
[7]
and even monetized .
It enables laboratories to study the stability of parameters when using the physico-chemical parameters
measurement system: organic micropollutants, inorganic and organometallic micropollutants, nutrients
and macropollutants in aqueous matrices (surface water, ground water, residual urban and industrial
water and drinking water). It covers the sampling, transport and laboratory storage operations.
NOTE This document does not cover solid matrices from aquatic environments (suspended solids,
sediments).
v
TECHNICAL SPECIFICATION ISO/TS 5667-25:2022(E)
Water quality — Sampling —
Part 25:
Guideline on the validation of the storage time of water
samples
1 Scope
The purpose of this document is to describe test plans and different operating methodologies
of these test plans to define and verify the acceptable length of stability of a substance in a sample
under specified conditions of preservation (temperature, matrix, light, addition of a stabilizer, where
appropriate, type of preservation etc.) before starting analytical protocols (chemicals and physico-
chemicals analysis). Biological and microbiological methods are excluded.
It is necessary to have an analytical method with performances that have already been characterized
(repeatability, intermediate precision, trueness, accuracy and uncertainty) in order to perform
the stability study and implement its test plans.
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/TS 21231, Water quality — Characterization of analytical methods — Guidelines for the selection of a
representative matrix
3 Terms, definitions and symbols
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
3.1
analytical process
detailed description of a measurement according to one or more measurement principles and to one
given measurement method, and including any calculations intended to obtain a measurement result
3.2
batch
...

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