ASTM D4483 - 14a

    Standard Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing Industries

    Active Standard ASTM D4483 | Developed by Subcommittee: D11.16

    Book of Standards Volume: 09.01


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    Significance and Use

    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. Scope

    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

    Scope

    1

    Referenced Documents

    2

    Terminology

    3

    Significance and Use

    4

    Precision Evaluation—General Precision and Special Precision

    5

    Steps in Organizing an Interlaboratory Test Program (ITP)

    6

    Overview of the General Precision Analysis Procedure

    7

    General 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

    8.4

    General 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

    9.1.2

    General Precision: Analysis Step 3

    10

     Calculation of Precision Using Revision 2 Database

    10.1

    Special Precision Analysis—Carbon Black Testing

    11

    Format for Precision Table and Clause in Test Method Standards

    12

    Preparation of Report for Precision Analysis

    13

    Definitions for Selected Terms Concerned with Precision and Testing

    Annex A1

    Statistical Model for Interlaboratory Testing Programs

    Annex A2

    Calculating the h and k Consistency Statistics for Outliers

    Annex A3

    Spreadsheet Calculation Formulas, Table Layout, and Calculation Sequence

    Annex A4

    Procedure for Calculating Replacement Values of Deleted Outliers

    Annex A5

    Example of General Precision Evaluation—Mooney Viscosity Testing

    Annex A6


    1.5 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 and health practices and determine the applicability of regulatory limitations prior to use.


    2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

    ASTM Standards

    D1646 Test Methods for Rubber--Viscosity, Stress Relaxation, and Pre-Vulcanization Characteristics (Mooney Viscometer)

    D6600 Practice for Evaluating Test Sensitivity for Rubber Test Methods

    E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method

    ISO Standard

    ISO289 Determination of Viscosity of Natural and Synthetic Rubbers by the Shearing Disk Viscometer


    ICS Code

    ICS Number Code 83.060 (Rubber)

    UNSPSC Code

    UNSPSC Code 13101700(Elastomers); 12171603(Carbon black)


    Referencing This Standard

    DOI: 10.1520/D4483

    ASTM International is a member of CrossRef.

    Citation Format

    ASTM D4483-14a, Standard Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing Industries, ASTM International, West Conshohocken, PA, 2014, www.astm.org

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