【国外标准】 Standard Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing Industries

4.1 Tests are conducted using standard test methods to generate test data that are used to make decisions for commercial, technical, and scientific purposes. It follows that the precision of a particular test method is an important quality characteristic or figure of merit for a test method and a decision process.4.2 An evaluation of the precision of a test method is normally conducted with (1) some selected group of materials as typically used with that method and (2) with a group of volunteer laboratories that have experience with the test method. The evaluation represents an event in time for the test method for these materials and laboratories. Another ITP precision evaluation with somewhat different materials or even with the same materials with the same laboratories at a different time, may generate precision results that differ from the initial ITP.4.3 Experience as indicated in Refs (1-4)4 and elsewhere has shown that the poor reproducibility among the laboratories of a typical ITP is almost always due to interlaboratory bias. Certain laboratories are always low or high compared to a reference as well as other laboratories in all tests. This usual outcome for many ITPs is addressed in this practice by the use of the three-step robust analysis procedures as described in Section 7.4.4 Caution is urged in applying precision results of a particular test method to product testing for consumer-producer product acceptance. Product acceptance procedures should be developed on the basis of precision data obtained in special programs that are specific to the commercial products and to the laboratories of the interested parties for this type of testing.1.1 This practice covers guidelines for evaluating precision and serves as the governing practice for interlaboratory test programs (ITP) used to evaluate precision for test methods as used in the rubber manufacturing and the carbon black industries. This practice uses the basic one way analysis of variance calculation algorithms of Practice E691. Although bias is not evaluated in this practice, it is an essential concept in understanding precision evaluation.1.2 This practice applies to test methods that have test results expressed in terms of a quantitative continuous variable. Although exceptions may occur, it is in general limited to test methods that are fully developed and in routine use in a number of laboratories.1.3 Two precision evaluation methods are given that are described as robust statistical procedures that attempt to eliminate or substantially decrease the influence of outliers. The first is a General Precision procedure intended for all test methods in the rubber manufacturing industry, and the second is a specific variation of the general precision procedure designated as Special Precision, that applies to carbon black testing. Both of these procedures use the same uniform level experimental design and the Mandel h and k statistics to review the precision database for potential outliers. However, they use slight modifications in the procedure for rejecting incompatible data values as outliers. The Special Precision procedure is specific as to the number of replicates per database cell or material-laboratory combination.1.4 This practice is divided into the following sections:  Section  1Referenced Documents  2Terminology  3  4Precision Evaluation—General Precision and Special Precision  5Steps in Organizing an Interlaboratory Test Program (ITP)  6Overview of the General Precision Analysis Procedure  7General Precision: Analysis Step 1  8 Preliminary Graphical Data Review  8.1 Calculation of Precision for Original Database  8.2 Detection of Outliers at 5 % Significance Level Using h and k Statistics  8.3 Generation of Revision 1 Database Using Outlier Treatment Option 1 or 2  8.4General Precision: Analysis Step 2  9 Calculation of Precision for Revision 1 Database  9.1 Detection of Outliers at 2 % Significance Level Using h and k Statistics  9.1 Generation of Revision 2 Database Using Outlier Treatment Option 1 or 2  9.1.2General Precision: Analysis Step 3  10 Calculation of Precision Using Revision 2 Database  10.1Special Precision Analysis—Carbon Black Testing  11Format for Precision Table and Clause in Test Method Standards  12Preparation of Report for Precision Analysis  13Definitions for Selected Terms Concerned with Precision and Testing Annex A1Statistical Model for Interlaboratory Testing Programs Annex A2Calculating the h and k Consistency Statistics for Outliers Annex A3Spreadsheet Calculation Formulas, Table Layout, and Calculation Sequence Annex A4Procedure for Calculating Replacement Values of Deleted Outliers Annex A5Example of General Precision Evaluation—Mooney Viscosity Testing Annex A61.5 Six annexes are presented; these serve as supplements to the main body of this practice. Annex A1 and Annex A2 are given mainly as background information that is important for a full understanding of precision evaluation. Annex A3 – Annex A5 contain detailed instructions and procedures needed to perform the operations as called for in various parts of the practice. The use of these annexes in this capacity avoids long sections of involved instruction in the main body of this practice. This allows for a better presentation and understanding of the central concepts involved in the evaluation of precision. Annex A6 is also important; it gives a complete example of precision evaluation that illustrates all of the procedures and options likely to be encountered in any precision evaluation, from the simple to the most complex.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.