Petroleum and related products — Precision of measurement methods and results — Part 1: Determination of precision data in relation to methods of test

ISO 4259-1:2017 specifies the methodology for the design of an Interlaboratory Study (ILS) and calculation of precision estimates of a test method specified by the study. In particular, it defines the relevant statistical terms (Clause 3), the procedures to be adopted in the planning of ILS to determine the precision of a test method (Clause 4), and the method of calculating the precision from the results of such a study (Clauses 5 and 6). The procedures in ISO 4259-1:2017 have been designed specifically for petroleum and petroleum related products, which are normally considered as homogeneous. However, the procedures described in ISO 4259-1:2017 can also be applied to other types of homogeneous products. Careful investigations are necessary before applying ISO 4259-1:2017 to products for which the assumption of homogeneity can be questioned.

Produits pétroliers et connexes — Fidélité des méthodes de mesure et de leurs résultats — Partie 1: Détermination des valeurs de fidélité relatives aux méthodes d'essai

ISO 4259-1:2017 spécifié la méthodologie pour la conception d'un essai interlaboratoires (ILS) et pour le calcul des estimations de fidélité d'une méthode d'essai spécifié par cet ILS. En particulier, il définit les termes statistiques concernés (Article 3), les procédures à suivre dans l'organisation d'un ILS destiné à déterminer la fidélité d'une méthode d'essai (Article 4) et la méthode de calcul de la fidélité à partir des résultats d'un tel ILS (Articles 5 et 6). Les procédures de l' ISO 4259-1:2017 ont été conçues spécifiquement pour les produits pétroliers et leurs produits connexes qui sont normalement considérés homogènes. Les procédures décrites dans le présent document peuvent cependant aussi s'appliquer à d'autres types de produits homogènes. Il est nécessaire de procéder à des contrôles attentifs avant d'appliquer ce document à des produits pour lesquels la présomption d'homogénéité peut être mise en question.

General Information

Status
Published
Publication Date
31-Oct-2017
Current Stage
9092 - International Standard to be revised
Completion Date
14-Feb-2024
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INTERNATIONAL ISO
STANDARD 4259-1
First edition
2017-11
Petroleum and related products —
Precision of measurement methods
and results —
Part 1:
Determination of precision data in
relation to methods of test
Produits pétroliers — Fidélité des méthodes de mesure et des
résultats —
Partie 1: Détermination des valeurs de fidélité relatives aux
méthodes d'essai
Reference number
ISO 4259-1:2017(E)
©
ISO 2017

---------------------- Page: 1 ----------------------
ISO 4259-1:2017(E)

COPYRIGHT PROTECTED DOCUMENT
© ISO 2017, Published in Switzerland
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
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2017 – All rights reserved

---------------------- Page: 2 ----------------------
ISO 4259-1:2017(E)

Contents Page
Foreword .v
Introduction .vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Stages in the planning of an interlaboratory study for the determination of the
precision of a test method . 4
4.1 General . 4
4.2 Preparing a draft method of test . 5
4.3 Planning a pilot study with at least two laboratories . 5
4.4 Planning the ILS . 5
4.5 Executing the ILS . 6
5 Statistical treatment of ILS results . 7
5.1 General recommendation . 7
5.2 Pre-screen using GESD technique . 7
5.3 Transformation of data and outlier tests . 8
5.3.1 General. 8
5.3.2 Outlier identification after pre-screening .11
5.3.3 Uniformity of repeatability .11
5.3.4 Uniformity of reproducibility.
...

© ISO 2017 – All rights reserved
Style Definition
ISO/TC 28
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Formatted: English (U.S.)
Date: 2017‐10‐02
Field Code Changed
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ISO 4259-1:2017(E)
Formatted
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ISO/TC 28/WG 2
Formatted: Font: 12 pt, Bold, English
Secretariat: NEN (U.S.)
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Petroleum and related products — Precision of measurement methods and results —
Formatted
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Part 1: Determination of precision data in relation to methods of test
Formatted: Font: 12 pt, Bold,
German (Switzerland)
Produits pétroliers -- Fidélité des méthodes de mesure et des résultats -- Partie 1: Détermination
Deleted: /FDIS
des valeurs de fidélité relatives aux méthodes d'essai
Formatted
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Document type: International Standard
Document subtype:
Document stage: (50) Approval
Document language: E

STD Version 2.3

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Deleted: Copyright notice¶
This ISO document is a Draft International
Standard and is copyright‐protected by ISO.
Except as permitted under the applicable
laws of the user's country, neither this ISO
draft nor any extract from it may be
reproduced, stored in a retrieval system or
transmitted in any form or by any means,
electronic, photocopying, recording or
otherwise, without prior written permission
being secured.¶
Requests for permission to reproduce should
be addressed to either ISO at the address
below or ISO's member body in the country of
the requester.¶
ISO copyright office¶
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Tel. + 41 22 749 01 11¶
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Reproduction may be subject to royalty
payments or a licensing agreement.¶
Violators may be prosecuted.¶
© ISO 2017 – All rights reserved
ii

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Deleted: 1 Scope 1¶
2 Normative references 1¶
3 Terms and definitions 1¶
Stages in the planning of an
4
Contents Page
Interlaboratory Study for the
determination of the precision of
a test method 4¶
4.1 General 4¶
4.2 Preparing a draft method of
test 4¶
4.3 Planning a pilot study with
at least two laboratories 4¶
4.4 Planning the ILS 5¶
4.5 Executing the ILS 5¶
5 Statistical treatment of ILS
results 6¶
5.1 General recommendation 6¶
5.2 Pre-screen using GESD
technique 7¶
5.3 Transformation of data and
outlier tests 8¶
5.4 Rejection of complete data
(from all laboratories) for a
sample 10¶
5.5 Estimating missing or
rejected values 10¶
5.6 Rejection test for outlying
laboratories 11¶
Confirmation of selected
5.7
transformation 11¶
6 Analysis of variance,
calculation and expression of
precision estimates 12¶
6.1 General 12¶
6.2 Analysis of variance 12¶
6.3 Expectation of mean squares
and calculation of precision
estimates 14¶
6.4 Expression of precision
estimates of a method of test 16¶
6.5 Specification of scope for the
test method 17¶
7 R / r ratio 18¶
Annex A (normative)
Determination of number of
samples required 19¶
Annex B (informative) Derivation
of formula for estimating the
number of labs and samples
required to meet minimum 30
degrees of freedom (Table
A.1) 21¶
B.1 Degrees of freedom 21¶
B.2 Explanation for choice of 30
as Minimum degrees of
freedom 22¶
Annex C (normative) Notation and
tests 23¶
C.1 Introduction 23¶
C.2 Array of duplicate
results 23¶
C.3 Array of sums of duplicate
results 24¶
C.4 Sums of squares and
variances 24¶
C.5 Cochran's test 25¶
C.6 Hawkins' test 25¶
C.7 Variance ratio test (F-
test) 27¶
Annex D (normative) Illustration
of procedures using ILS results
... [8]
© ISO 2017 – All rights reserved
iii

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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). Deleted: 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 right
...

NORME ISO
INTERNATIONALE 4259-1
Première édition
2017-11
Produits pétroliers et connexes —
Fidélité des méthodes de mesure et de
leurs résultats —
Partie 1:
Détermination des valeurs de fidélité
relatives aux méthodes d'essai
Petroleum and related products — Precision of measurement
methods and results —
Part 1: Determination of precision data in relation to methods of test
Numéro de référence
ISO 4259-1:2017(F)
©
ISO 2017

---------------------- Page: 1 ----------------------
ISO 4259-1:2017(F)

DOCUMENT PROTÉGÉ PAR COPYRIGHT
© ISO 2017, Publié en Suisse
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
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2017 – Tous droits réservés

---------------------- Page: 2 ----------------------
ISO 4259-1:2017(F)

Sommaire Page
Avant-propos .v
Introduction .vi
1 Domaine d'application . 1
2 Références normatives . 1
3 Termes et définitions . 1
4 Étapes de l'organisation d'un essai interlaboratoires pour la détermination de la
fidélité d'une méthode d'essai . 4
4.1 Généralités . 4
4.2 Préparation d'un projet de méthode d'essai . 5
4.3 Organisation d'un ILS pilote avec au moins deux laboratoires . 5
4.4 Organisation de l’ILS . 5
4.5 Exécution de l’ILS . 6
5 Traitement statistique des résultats de l’ILS. 7
5.1 Recommandation . 7
5.2 Prévisualisation selon la technique GESD . 8
5.3 Transformation des données et recherche des valeurs aberrantes . 9
5.3.1 Généralités . 9
5.3.2 Identification des valeurs aberrantes après prévisualisation .11
5.3.3 Uniformité de la répétabilité .11
5.3.4 Uniformité de la reproductibilité .11
5.4 Rejet de tous les résultats (de tous les laboratoires) concernant un échanti
...

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