ISO 4259-1:2017
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.
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Foreword
Introduction
1 Scope
2 Normative references
3 Terms and definitions
4 Stages in the planning of an interlaboratory study for the determination of the precision of a test method
4.1 General
4.2 Preparing a draft method of test
4.3 Planning a pilot study with at least two laboratories
4.4 Planning the ILS
4.5 Executing the ILS
5 Statistical treatment of ILS results
5.1 General recommendation
5.2 Pre-screen using GESD technique
5.3 Transformation of data and outlier tests
5.3.1 General
5.3.2 Outlier identification after pre-screening
5.3.3 Uniformity of repeatability
5.3.4 Uniformity of reproducibility
5.4 Rejection of complete data (from all laboratories) for a sample
5.5 Estimating missing or rejected values
5.5.1 One of the two repeat values missing or rejected
5.5.2 Both repeat values missing or rejected
5.6 Rejection test for outlying laboratories
5.7 Confirmation of selected transformation
5.7.1 General
5.7.2 Identification of excessively influential sample(s)
6 Analysis of variance, calculation and expression of precision estimates
6.1 General
6.2 Analysis of variance
6.2.1 Forming the sums of squares for the laboratories × samples interaction sum of squares
6.2.2 Forming the sum of squares for the exact analysis of variance
6.2.3 Degrees of freedom
6.2.4 Mean squares and analysis of variance
6.3 Expectation of mean squares and calculation of precision estimates
6.3.1 Expectation of mean squares with no estimated values
6.3.2 Expectation of mean squares with estimated values
6.3.3 Calculation of precision estimates
6.4 Expression of precision estimates of a method of test
6.5 Specification of scope for the test method
7 R/r ratio
Annex A (normative) Determination of number of samples required
Annex B (informative) Derivation of formula for estimating the number of laboratories and samples required to meet minimum 30 degrees of freedom
Annex C (normative) Notation and tests
Annex D (normative) Illustration of procedures using ILS results for Bromine Number and statistical tables
Annex E (normative) Types of dependence and corresponding transformations
Annex F (normative) Weighted linear regression analysis
Annex G (normative) Rules for rounding
Annex H (normative) GESD technique to simultaneously identify multiple outliers in a data set
Annex I (informative) Glossary
Bibliography
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Foreword
Introduction
1 Scope
2 Normative references
3 Terms and definitions
4 Stages in the planning of an interlaboratory study for the determination of the precision of a test method
4.1 General
4.2 Preparing a draft method of test
4.3 Planning a pilot study with at least two laboratories
4.4 Planning the ILS
4.5 Executing the ILS
5 Statistical treatment of ILS results
5.1 General recommendation
5.2 Pre-screen using GESD technique
5.3 Transformation of data and outlier tests
5.3.1 General
5.3.2 Outlier identification after pre-screening
5.3.3 Uniformity of repeatability
5.3.4 Uniformity of reproducibility
5.4 Rejection of complete data (from all laboratories) for a sample
5.5 Estimating missing or rejected values
5.5.1 One of the two repeat values missing or rejected
5.5.2 Both repeat values missing or rejected
5.6 Rejection test for outlying laboratories
5.7 Confirmation of selected transformation
5.7.1 General
5.7.2 Identification of excessively influential sample(s)
6 Analysis of variance, calculation and expression of precision estimates
6.1 General
6.2 Analysis of variance
6.2.1 Forming the sums of squares for the laboratories × samples interaction sum of squares
6.2.2 Forming the sum of squares for the exact analysis of variance
6.2.3 Degrees of freedom
6.2.4 Mean squares and analysis of variance
6.3 Expectation of mean squares and calculation of precision estimates
6.3.1 Expectation of mean squares with no estimated values
6.3.2 Expectation of mean squares with estimated values
6.3.3 Calculation of precision estimates
6.4 Expression of precision estimates of a method of test
6.5 Specification of scope for the test method
7 R/r ratio
Annex A (normative) Determination of number of samples required
Annex B (informative) Derivation of formula for estimating the number of laboratories and samples required to meet minimum 30 degrees of freedom
Annex C (normative) Notation and tests
Annex D (normative) Illustration of procedures using ILS results for Bromine Number and statistical tables
Annex E (normative) Types of dependence and corresponding transformations
Annex F (normative) Weighted linear regression analysis
Annex G (normative) Rules for rounding
Annex H (normative) GESD technique to simultaneously identify multiple outliers in a data set
Annex I (informative) Glossary
Bibliography