1、BSI Standards PublicationWB11885_BSI_StandardCovs_2013_AW.indd 1 15/05/2013 15:06Petroleum and related products Precision of measurement methods and resultsPart 1: Determination of precision data in relation to methods of testBS EN ISO 42591:2017EUROPEANSTANDARDNORME EUROPENNE EUROPISCHE NORMENISO42
2、59-1December 2017ICS 75.080 Supersedes EN ISO 4259:2006EnglishVersionPetroleum and related products - Precision ofmeasurement methods and results - Part 1: Determination of precision data in relation to methods of test (ISO 4259-1:2017)Produits ptrolierset connexes- Fidlit des mthodesde mesure et de
3、 leurs rsultats - Partie 1:Dtermination desvaleursde fidlit relativesauxmthodes dessai (ISO4259-1:2017)Minerallerzeugnisse -Przision vonMessverfahrenund Ergebnissen - Teil 1: Bestimmung der Werte fr die Przision von Prfverfahren(ISO 4259-1:2017)This European Standard was approved by CEN on 27 Octobe
4、r2017.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving thisEuropean Standard the status of a national standard without any alteration.Up-to-date lists and bibliographical referencesconcerning such national standards may be obtained o
5、n application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made bytranslation under the responsibility of a CEN member into its own language and notified to the CEN-CENEL
6、EC ManagementCentre has the same status as the officialversions.CEN members are the nationalstandards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, La
7、tvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGCEN-CENELEC Management Centre: Rue d
8、e la Science 23, B-1040 Brussels 2017 CEN All rights of exploitation in any form and by any means reservedworldwide for CENnational Members.Ref. No. EN ISO 4259-1:2017 ENational forewordThis British Standard is the UK implementation of EN ISO 42591:2017. It is identical to ISO 42591:2017. Together w
9、ith BS EN ISO 42592:2017, it supersedes BS EN ISO 4259:2006, which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee PTI/13, Petroleum Testing and Terminology.A list of organizations represented on this committee can be obtained on request to its secretary.Thi
10、s publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2018 Published by BSI Standards Limited 2018ISBN 978 0 580 85639 6ICS 75.080Compliance with a British Standard cannot confer immu
11、nity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 January 2018.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN ISO 42591:2017EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM
12、EN ISO 4259-1 December 2017 ICS 75.080 Supersedes EN ISO 4259:2006English Version 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) Produits ptroliers et connexes - Fidlit des mthod
13、es de mesure et de leurs rsultats - Partie 1: Dtermination des valeurs de fidlit relatives aux mthodes dessai (ISO 4259-1:2017) Minerallerzeugnisse - Przision von Messverfahren und Ergebnissen - Teil 1: Bestimmung der Werte fr die Przision von Prfverfahren (ISO 4259-1:2017) This European Standard wa
14、s approved by CEN on 27 October 2017. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such n
15、ational standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own la
16、nguage and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Gree
17、ce, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR
18、NORMUNG CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels 2017 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 4259-1:2017 EBS EN ISO 42591:2017EN ISO 4259-1:2017 (E) 3 European foreword This document (EN ISO
19、 4259-1:2017) has been prepared by Technical Committee ISO/TC 28 “Petroleum and related products, fuels and lubricants from natural or synthetic sources“ in collaboration with Technical Committee CEN/TC 19 “Gaseous and liquid fuels, lubricants and related products of petroleum, synthetic and biologi
20、cal origin” the secretariat of which is held by NEN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by June 2018, and conflicting national standards shall be withdrawn at the latest by June 2018. At
21、tention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 4259:2006. According to the CEN-CENELEC Internal Regulations, the natio
22、nal standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lith
23、uania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 4259-1:2017 has been approved by CEN as EN ISO 4259-1:2017 without any modification. BS EN ISO 42591:201
24、7ISO 4259-1:2017(E)Foreword vIntroduction vi1 Scope . 12 Normative references 13 Terms and definitions . 14 Stages in the planning of an interlaboratory study for the determination of the precision of a test method 44.1 General . 44.2 Preparing a draft method of test . 54.3 Planning a pilot study wi
25、th at least two laboratories 54.4 Planning the ILS . 54.5 Executing the ILS . 65 Statistical treatment of ILS results . 75.1 General recommendation 75.2 Pre-screen using GESD technique 75.3 Transformation of data and outlier tests . 85.3.1 General 85.3.2 Outlier identification after pre-screening .1
26、15.3.3 Uniformity of repeatability 115.3.4 Uniformity of reproducibility. 115.4 Rejection of complete data (from all laboratories) for a sample 115.5 Estimating missing or rejected values . 125.5.1 One of the two repeat values missing or rejected 125.5.2 Both repeat values missing or rejected .125.6
27、 Rejection test for outlying laboratories 125.7 Confirmation of selected transformation 135.7.1 General. 135.7.2 Identification of excessively influential sample(s) 136 Analysis of variance, calculation and expression of precision estimates .146.1 General 146.2 Analysis of variance . 146.2.1 Forming
28、 the sums of squares for the laboratories samples interaction sum of squares 146.2.2 Forming the sum of squares for the exact analysis of variance 156.2.3 Degrees of freedom .156.2.4 Mean squares and analysis of variance .156.3 Expectation of mean squares and calculation of precision estimates 156.3
29、.1 Expectation of mean squares with no estimated values 156.3.2 Expectation of mean squares with estimated values 166.3.3 Calculation of precision estimates .176.4 Expression of precision estimates of a method of test 186.5 Specification of scope for the test method . 197 R/r ratio 20Annex A (normat
30、ive) Determination of number of samples required.21Annex B (informative) Derivation of formula for estimating the number of laboratories and samples required to meet minimum 30 degrees of freedom 23Annex C (normative) Notation and tests .25Annex D (normative) Illustration of procedures using ILS res
31、ults for Bromine Number and statistical tables .30 ISO 2017 All rights reserved iiiContents PageBS EN ISO 42591:2017ISO 4259-1:2017(E)Annex E (normative) Types of dependence and corresponding transformations.49Annex F (normative) Weighted linear regression analysis 55Annex G (normative) Rules for ro
32、unding 62Annex H (normative) GESD technique to simultaneously identify multiple outliers in a data set .64Annex I (informative) Glossary72Bibliography .75iv ISO 2017 All rights reservedBS EN ISO 42591:2017ISO 4259-1:2017(E)ForewordISO (the International Organization for Standardization) is a worldwi
33、de 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 tha
34、t 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 docu
35、ment 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 Directiv
36、es, 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 developmen
37、t 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 on the voluntary nature of
38、standards, the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following URL: www.iso.org/iso/foreword.html.This document was
39、prepared by Technical Committee ISO/TC 28, Petroleum and related products, fuels and lubricants from natural or synthetic sources.This first edition of ISO 4259-1, together with ISO 4259-2, cancels and replaces ISO 4259, which has been technically revised. A list of all parts in the ISO 4259 series
40、can be found on the ISO website. ISO 2017 All rights reserved vBS EN ISO 42591:2017ISO 4259-1:2017(E)IntroductionFor purposes of quality control and to check compliance with specifications, the properties of commercial petroleum products are assessed by standard laboratory test methods. Two or more
41、measurements of the same property of a specific sample by a specific test method, or, by different test methods that purport to measure the same property, will not usually give exactly the same result. It is, therefore, necessary to take proper account of this fact, by arriving at statistically base
42、d estimates of the precision for a method, i.e. an objective measure of the degree of agreement expected between two or more results obtained in specified circumstances.This document makes reference to ISO 3534-21, which gives a different definition of true value (see 3.23). This document also refer
43、s to ISO 5725-2. The latter is required in particular and unusual circumstances (see 5.3.1) for the purpose of estimating precision.The two parts of ISO 4259 encompass both the derivation of precision estimates and the application of precision data. They combine the information in ASTM D63002regardi
44、ng the determination of the precision estimates and the information in ASTM D32443for the utilization of test data.A glossary of the variables used in this document and ISO 4259-2 is included as Annex I in this document.vi ISO 2017 All rights reservedBS EN ISO 42591:2017Petroleum and related product
45、s Precision of measurement methods and results Part 1: Determination of precision data in relation to methods of test1 ScopeThis document 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 part
46、icular, 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 this document hav
47、e been designed specifically for petroleum and petroleum related products, which are normally considered as homogeneous. However, the procedures described in this document can also be applied to other types of homogeneous products. Careful investigations are necessary before applying this document t
48、o products for which the assumption of homogeneity can be questioned.2 Normative referencesThe 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
49、references, the latest edition of the referenced document (including any amendments) applies.ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.ISO and IEC maintain terminological databases for use in standardization at the following addresses: ISO Online browsing pla
