1、Designation: D4483 14D4483 14aStandard Practice forEvaluating Precision for Test Method Standards in theRubber and Carbon Black Manufacturing Industries1This standard is issued under the fixed designation D4483; the number immediately following the designation indicates the year oforiginal adoption
2、or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.INTRODUCTIONThe primary precision standard for ASTM test method standards is Practice E69
3、1; a genericstandard that presents the fundamental statistical approach and calculation algorithms for evaluatingrepeatability and reproducibility precision. However, certain parts of Practice E691 are not compatiblewith precision as evaluated in the rubber manufacturing and carbon black industries
4、over the past fourdecades. Thus a separate standard is required for precision in these two industries. This practice isbeing issued as a major revision of Practice D4483, which has been used for precision evaluation byCommittee D11 since 1985. The basic Practice D4483 precision calculation algorithm
5、s, the same asin Practice E691, are unchanged. This new revised Practice D4483, organized to accommodate therequirements of the rubber and carbon black manufacturing industries, has three new features thatprovide for a more formal and structured analysis of interlaboratory test program (ITP) data.Fi
6、rst it addresses the overriding issues with precision evaluation over the past several decadesthefrequent discovery that reproducibility for many test methods is quite poor. Experience has shown thatfrequently poor reproducibility is caused by only a few laboratories that differ from the remainder t
7、hatgive good agreement. A new procedure designated as robust analysis provides an improved methodfor detecting outliers that cause poor precision, especially poor between laboratory agreement.Second, after outlier detection the new standard provides two options; (1) outlier deletion or (2) outlierre
8、placement. When outliers are deleted the revised standard provides a way to retain the non-outlierlaboratory data. This allows for a broader database for precision calculation. The current ASTMCommittee E11 computer program for calculating precision does not allow for outlier deletion in thisway. Th
9、ird, when exercising outlier Option 2, the standard gives a procedure for calculating specialreplacement values for deleted outliers in ITPs that have only a few participating laboratories. Thereplacement values are obtained in a way that preserves the observed data distribution of thenon-outlier da
10、ta. This is important since many ITPs are in the limited number of participatinglaboratories category.1. Scope1.1 This practice covers guidelines for evaluating precision and serves as the governing practice for interlaboratory testprograms (ITP) used to evaluate precision for test methods as used i
11、n 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 evaluatedin this practice, it is an essential concept in understanding precision evaluation.1.2 This practice applies to
12、test methods that have test results expressed in terms of a quantitative continuous variable.Althoughexceptions 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 describe
13、d as robust statistical procedures that attempt to eliminate orsubstantially decrease the influence of outliers.The first is a General Precision procedure intended for all test methods in the rubbermanufacturing industry, and the second is a specific variation of the general precision procedure desi
14、gnated as Special Precision,that applies to carbon black testing. Both of these procedures use the same uniform level experimental design and the Mandel hand k statistics to review the precision database for potential outliers. However, they use slight modifications in the procedure for1 This practi
15、ce is under the jurisdiction ofASTM Committee D11 on Rubber and is the direct responsibility of Subcommittee D11.16 on Application of Statistical Methods.Current edition approved Jan. 1, 2014May 1, 2014. Published February 2014May 2014. Originally approved in 1985. Last previous edition approved in
16、20112014 asD4483 05a (2011).D4483 14. DOI: 10.1520/D4483-14.10.1520/D4483-14A.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequate
17、ly depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken,
18、 PA 19428-2959. United States1rejecting incompatible data values as outliers. The Special Precision procedure is specific as to the number of replicates perdatabase cell or material-laboratory combination.1.4 This practice is divided into the following sections:SectionScope 1Referenced Documents 2Te
19、rminology 3Significance and Use 4Precision EvaluationGeneral Precision andSpecial Precision5Steps in Organizing an Interlaboratory Test Program(ITP)6Overview of the General Precision AnalysisProcedure7General Precision: Analysis Step 1 8Preliminary Graphical Data Review 8.1Calculation of Precision f
20、or Original Database 8.2Detection of Outliers at 5 % Significance LevelUsing h and k Statistics8.3Generation of Revision 1 Database Using OutlierTreatment Option 1 or 28.4General Precision: Analysis Step 2 9Calculation of Precision for Revision 1 Database 9.1Detection of Outliers at 2 % Significance
21、 LevelUsing h and k Statistics9.1Generation of Revision 2 Database Using OutlierTreatment Option 1 or 29.1.2General Precision: Analysis Step 3 10Calculation of Precision Using Revision 2Database10.1Special Precision AnalysisCarbon Black Testing 11Format for Precision Table and Clause in TestMethod S
22、tandards12Preparation of Report for Precision Analysis 13Definitions for Selected Terms Concerned withPrecision and TestingAnnex A1Statistical Model for Interlaboratory TestingProgramsAnnex A2Calculating the h and k Consistency Statistics forOutliersAnnex A3Spreadsheet Calculation Formulas, Table La
23、yout,and Calculation SequenceAnnex A4Procedure for Calculating Replacement Values ofDeleted OutliersAnnex A5Example of General Precision EvaluationMooneyViscosity TestingAnnex A61.5 Six annexes are presented; these serve as supplements to the main body of this practice. AnnexA1 and AnnexA2 are given
24、mainly as background information that is important for a full understanding of precision evaluation. AnnexA3 AnnexA5 containdetailed instructions and procedures needed to perform the operations as called for in various parts of the practice. The use of theseannexes in this capacity avoids long secti
25、ons of involved instruction in the main body of this practice. This allows for a betterpresentation and understanding of the central concepts involved in the evaluation of precision. AnnexA6 is also important; it givesa complete example of precision evaluation that illustrates all of the procedures
26、and options likely to be encountered in anyprecision 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 responsibilityof the user of this standard to establish appropriate safety and hea
27、lth practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1646 Test Methods for RubberViscosity, Stress Relaxation, and Pre-Vulcanization Characteristics (Mooney Viscometer)D6600 Practice for Evaluating Test Sensitivity for Rubber
28、 Test MethodsE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method2.2 ISO Standard:3ISO 289 Determination of Viscosity of Natural and Synthetic Rubbers by the Shearing Disk Viscometer2 For referencedASTM standards, visit theASTM website, www.astm.org, or c
29、ontactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from International Organization for Standardization (ISO), 1, ch. de la Voie-Creuse, Case postale 56, CH-1211, Geneva 20,
30、Switzerland, http:/www.iso.ch.D4483 14a23. Terminology3.1 A number of specialized terms or definitions are defined in a systematic sequential order, from simple terms to complexterms. This approach allows the simple terms to be used in the definition of the more complex terms; it generates unambiguo
31、usdefinitions. Thus the definitions do not appear in the usual alphabetical sequence.3.1.1 This terminology section contains explanatory notes for many of the definitions as well as discussion on the connectionbetween some of the terms and the various ways the terms are used in testing and precision
32、 evaluation. For special emphasis, afew terms are defined in the main text of this practice where certain precision concepts are discussed.3.1.2 Annex A1 is included as part of this practice with two objectives: (1) Annex A1 presents new more comprehensivedefinitions drafted with substantial tutoria
33、l content, and (2) AnnexA1 presents some ancillary definitions that may promote a betterunderstanding of precision.3.2 Testing Terms:3.2.1 balanced uniform level design, nthe plan for an interlaboratory test program for precision, where all laboratories test allthe materials selected for the program
34、 and each laboratory conducts the same number of repeated tests, on each material.3.2.2 element, nthe entity that is tested or observed, to evaluate a property or characteristic; it may be a single object amonga group of objects (test pieces, and so forth) or an increment or portion of a mass (or vo
35、lume) of a material.3.2.2.1 DiscussionThe generic term element has a number of synonyms: test piece, test specimen, portion, aliquot part, subsample, and laboratorysample.3.2.3 element class (or class of elements), nthe category or descriptive name for a group of elements that have a commonorigin or
36、 have nominally identical properties.3.2.3.1 DiscussionThe term nominally identical implies that the elements come from a source that is as homogeneous as possible with regard to theproperty being measured.3.2.4 test result, nthe value of a characteristic obtained by carrying out a specified test me
37、thod.3.2.4.1 DiscussionThe test method should specify that one or a number of individual measurements, determinations, or observations be made andtheir average or another appropriate function (median or other) be reported as the test result.3.2.5 testing domain, nthe location and operational conditi
38、ons under which a test is conducted; it includes a description of theelement preparation (test sample or test piece), the instrument(s) used (calibration, adjustments, and settings), the selected testtechnicians, and the surrounding environment.3.2.5.1 global testing domain, na domain that encompass
39、es two or more locations or laboratories, domestic or international,typically used for producer-user testing, product acceptance, and interlaboratory test programs.3.2.5.2 local testing domain, na domain comprised of one location or laboratory as typically used for quality control andinternal develo
40、pment or evaluation programs.3.3 Material and Sampling Terms:3.3.1 independent tests, na set of measurements (or observations) for a defined testing domain, where, in relation to themeasurement process, there is no influence of any selected measurement on any other measurement in the set.3.3.1.1 Dis
41、cussionThe word independent is used throughout this practice as an adjective to indicate the concept of independence, for samples, testpieces, and so forth, as well as tests.3.3.2 lot, na specified mass or volume of material or number of objects; usually generated by an identifiable process,frequent
42、ly with a recognized composition or property range.3.3.2.1 DiscussionA lot may be generated by a common production (or other natural) process in a restricted time period and usually consists of aD4483 14a3finite size or number. A lot may be a fractional part of a population (Interpretation 2 of popu
43、lation, see Annex A1). A recognizedproperty range implies that some rough approximation is available.3.3.3 material, na specific entity or element class to be tested; it usually exists in bulk form (solid, powder, or liquid).3.3.3.1 DiscussionMaterial is used as a generic term to describe the class
44、of elements that is tested, that is, a material may be a rubber, a rubbercompound, a carbon black, a rubber chemical, and so forth. A material may or may not be homogeneous. In product testing theterm material may be used to describe the class of elements or type of rubber products such as O-rings,
45、hose assemblies, motormounts, and so forth. See also 5.1.4.1.3.3.4 sample (data), nthe number of test or observation values (n = 1, 2, 3, and so forth), obtained from (one or more) physicalsamples, by the application of a specific test (observation) method.3.3.5 sample (physical), nthe number of ele
46、ments or the specified mass of a material, selected according to a particularprocedure, used to evaluate material, lot, or population characteristics.3.3.5.1 DiscussionThe term sample should not be used as a synonym for material, see 3.3.3, or target material, see 5.1.4.1. Ideally several materialsa
47、re tested in any ITPwith each material being different (chemically, structurally, property wise). From each material, some numberof samples (all nominally identical) may be taken for testing. See 3.3.4.3.3.6 test sample, nthat part of a (physical) sample of any type taken for chemical or other analy
48、tical testing, usually with aprescribed blending or other protocol.3.3.6.1 DiscussionA test sample is usually a mass or volume that is some small fractional part of a bulk material.3.3.7 test specimen, nan object (appropriately shaped and prepared) taken from a sample for physical or mechanical test
49、ing.3.3.7.1 DiscussionOther terms for test specimen are: test portion, test item, and test piece (used in ISO standards).3.4 Statistical Terms Relating to Precision:3.4.1 estimated (true or reference) mean, nthe mean obtained on the basis of n independent replicate measurements; thegreater n the better the approximation to the true or reference mean, provided there is no systematic deviation or bias.3.4.1.1 DiscussionThe words mean and estimated mean are frequent synonyms for estimated (true or reference) mean. The value for n in typicalroutine
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