INTERNATIONAL ISO

STANDARD 4259

Third edition
2006-08-01

Petroleum products — Determination and

application of precision data in relation to
methods of test
Produits pétroliers — Détermination et application des valeurs de
fidélité relatives aux méthodes d'essai

Reference number
ISO 4259:2006(E)

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Copyright International Organization for Standardization © ISO 2006

Provided by IHS under license with ISO
No reproduction or networking permitted without license from IHS Not for Resale
 ISO 4259:2006(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 inter-laboratory test programme 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 programme with at least two laboratories.............................................................. 5
4.4 Planning the inter-laboratory programme.......................................................................................... 5
4.5 Executing the inter-laboratory programme........................................................................................ 5
5 Inspection of inter-laboratory results for uniformity and for outliers ............................................. 6
5.1 General................................................................................................................................................... 6
5.2 Transformation of data......................................................................................................................... 7
5.3 Tests for outliers................................................................................................................................... 8
5.4 Rejection of complete data from a sample ...................................................................................... 11
5.5 Estimating missing or rejected values ............................................................................................. 12
5.6 Rejection test for outlying laboratories............................................................................................ 13
5.7 Confirmation of selected transformation ......................................................................................... 14
6 Analysis of variance, calculation and expression of precision estimates ................................... 14
6.1 General................................................................................................................................................. 14
6.2 Analysis of variance ........................................................................................................................... 14
6.3 Expectation of mean squares and calculation of precision estimates ......................................... 17
6.4 Expression of precision estimates of a method of test .................................................................. 20
7 Significance of repeatability (r) and reproducibility (R) .................................................................. 21
7.1 General................................................................................................................................................. 21
7.2 Repeatability, r .................................................................................................................................... 21
7.3 Reproducibility, R................................................................................................................................ 22
8 Specifications...................................................................................................................................... 24
8.1 Aim of specifications.......................................................................................................................... 24
8.2 Construction of specifications limits in relation to precision........................................................ 24
9 Quality control against specifications.............................................................................................. 25
9.1 General................................................................................................................................................. 25
9.2 Testing margin at the supplier .......................................................................................................... 25
9.3 Testing margin at the recipient ......................................................................................................... 25
10 Dispute procedure .............................................................................................................................. 25
Annex A (normative) Determination of number of samples required......................................................... 28
Annex B (informative) Derivation of equation for calculating the number of samples required ............. 30
Annex C (normative) Notation and tests........................................................................................................ 31
Annex D (normative) Example results of test for determination of bromine number and statistical
tables.................................................................................................................................................... 36
Annex E (normative) Types of dependence and corresponding transformations .................................... 45
Annex F (normative) Weighted linear regression analysis.......................................................................... 49

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© ISO 2006 – All rights reserved

Copyright International Organization for Standardization iii
Provided by IHS under license with ISO
No reproduction or networking permitted without license from IHS Not for Resale