1、Designation: D4483 14Standard 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 or, in th
2、e 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 E691; a gene
3、ricstandard 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 over the
4、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 algorithms, the sa
5、me 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.First it ad
6、dresses 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 thatgive g
7、ood 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) outlierreplacement
8、. 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. Third, when
9、 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 data. This
10、is important since many ITPs are in the limited number of participatinglaboratories category.1. Scope1.1 This practice covers guidelines for evaluating precisionand serves as the governing practice for interlaboratory testprograms (ITP) used to evaluate precision for test methods asused in the rubbe
11、r manufacturing and the carbon black indus-tries. This practice uses the basic one way analysis of variancecalculation algorithms of Practice E691. Although bias is notevaluated in this practice, it is an essential concept in under-standing precision evaluation.1.2 This practice applies to test meth
12、ods that have testresults expressed in terms of a quantitative continuous variable.Although exceptions may occur, it is in general limited to testmethods that are fully developed and in routine use in a numberof laboratories.1.3 Two precision evaluation methods are given that aredescribed as robust
13、statistical procedures that attempt toeliminate or substantially decrease the influence of outliers.The first is a General Precision procedure intended for all testmethods in the rubber manufacturing industry, and the secondis a specific variation of the general precision proceduredesignated as Spec
14、ial Precision, that applies to carbon blacktesting. Both of these procedures use the same uniform levelexperimental design and the Mandel h and k statistics to reviewthe precision database for potential outliers. However, they use1This practice is under the jurisdiction ofASTM Committee D11 on Rubbe
15、r andis the direct responsibility of Subcommittee D11.16 on Application of StatisticalMethods.Current edition approved Jan. 1, 2014. Published February 2014. Originallyapproved in 1985. Last previous edition approved in 2011 as D4483 05a (2011).DOI: 10.1520/D4483-14.Copyright ASTM International, 100
16、 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1slight modifications in the procedure for rejecting incompatibledata values as outliers. The Special Precision procedure isspecific as to the number of replicates per database cell ormaterial-laboratory combination.1.4
17、This practice is divided into the following sections:SectionScope 1Referenced Documents 2Terminology 3Significance and Use 4Precision EvaluationGeneral Precision andSpecial Precision5Steps in Organizing an Interlaboratory Test Program(ITP)6Overview of the General Precision AnalysisProcedure7General
18、Precision: Analysis Step 1 8Preliminary Graphical Data Review 8.1Calculation of Precision for 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 9Ca
19、lculation of Precision for Revision 1 Database 9.1Detection of Outliers at 2 % Significance 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 Pre
20、cision AnalysisCarbon Black Testing 11Format for Precision Table and Clause in TestMethod Standards12Preparation of Report for Precision Analysis 13Definitions for Selected Terms Concerned withPrecision and TestingAnnex A1Statistical Model for Interlaboratory TestingProgramsAnnex A2Calculating the h
21、 and k Consistency Statistics forOutliersAnnex A3Spreadsheet Calculation Formulas, Table Layout,and Calculation SequenceAnnex A4Procedure for Calculating Replacement Values ofDeleted OutliersAnnex A5Example of General Precision EvaluationMooneyViscosity TestingAnnex A61.5 Six annexes are presented;
22、these serve as supplements tothe main body of this practice. Annex A1 and Annex A2 aregiven mainly as background information that is important for afull understanding of precision evaluation. Annex A3 AnnexA5 contain detailed instructions and procedures needed toperform the operations as called for
23、in various parts of thepractice. The use of these annexes in this capacity avoids longsections of involved instruction in the main body of thispractice. This allows for a better presentation and understand-ing of the central concepts involved in the evaluation ofprecision. Annex A6 is also important
24、; it gives a completeexample of precision evaluation that illustrates all of theprocedures 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 thesafety concerns, if any, associated with its use. It
25、 is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1646 Test Methods for RubberViscosity, StressRelaxation, and Pre-Vulcanization
26、Characteristics(Mooney Viscometer)D6600 Practice for Evaluating Test Sensitivity for RubberTest MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 ISO Standard:3ISO 289 Determination of Viscosity of Natural and Syn-thetic Rubbers by the Shearin
27、g Disk Viscometer3. Terminology3.1 Anumber of specialized terms or definitions are definedin a systematic sequential order, from simple terms to complexterms. This approach allows the simple terms to be used in thedefinition of the more complex terms; it generates unambigu-ous definitions. Thus the
28、definitions do not appear in the usualalphabetical sequence.3.1.1 This terminology section contains explanatory notesfor many of the definitions as well as discussion on theconnection between some of the terms and the various ways theterms are used in testing and precision evaluation. For specialemp
29、hasis, a few terms are defined in the main text of thispractice where certain precision concepts are discussed.3.1.2 Annex A1 is included as part of this practice with twoobjectives: (1) Annex A1 presents new more comprehensivedefinitions drafted with substantial tutorial content, and (2)Annex A1 pr
30、esents some ancillary definitions that may pro-mote a better understanding of precision.3.2 Testing Terms:3.2.1 balanced uniform level design, nthe plan for aninterlaboratory test program for precision, where all laborato-ries test all the materials selected for the program and eachlaboratory conduc
31、ts the same number of repeated tests, on eachmaterial.3.2.2 element, nthe entity that is tested or observed, toevaluate a property or characteristic; it may be a single objectamong a group of objects (test pieces, and so forth) or anincrement or portion of a mass (or volume) of a material.3.2.2.1 Di
32、scussionThe generic term element has a numberof synonyms: test piece, test specimen, portion, aliquot part,subsample, and laboratory sample.3.2.3 element class (or class of elements), nthe categoryor descriptive name for a group of elements that have acommon origin or have nominally identical proper
33、ties.3.2.3.1 DiscussionThe term nominally identical impliesthat the elements come from a source that is as homogeneousas possible with regard to the property being measured.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For A
34、nnual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from International Organization for Standardization (ISO), 1, ch. dela Voie-Creuse, Case postale 56, CH-1211, Geneva 20, Switzerland, http:/www.iso.ch.D4483 1423.2.4 test result
35、, nthe value of a characteristic obtained bycarrying out a specified test method.3.2.4.1 DiscussionThe test method should specify thatone or a number of individual measurements, determinations,or observations be made and their average or another appro-priate function (median or other) be reported as
36、 the test result.3.2.5 testing domain, nthe location and operational con-ditions under which a test is conducted; it includes a descrip-tion of the element preparation (test sample or test piece), theinstrument(s) used (calibration, adjustments, and settings), theselected test technicians, and the s
37、urrounding environment.3.2.5.1 global testing domain, na domain that encom-passes two or more locations or laboratories, domestic orinternational, typically used for producer-user testing, productacceptance, and interlaboratory test programs.3.2.5.2 local testing domain, na domain comprised of onelo
38、cation or laboratory as typically used for quality control andinternal development or evaluation programs.3.3 Material and Sampling Terms:3.3.1 independent tests, na set of measurements (or ob-servations) for a defined testing domain, where, in relation tothe measurement process, there is no influen
39、ce of any selectedmeasurement on any other measurement in the set.3.3.1.1 DiscussionThe word independent is used through-out this practice as an adjective to indicate the concept ofindependence, for samples, test pieces, and so forth, as well astests.3.3.2 lot, na specified mass or volume of materia
40、l ornumber of objects; usually generated by an identifiableprocess, frequently with a recognized composition or propertyrange.3.3.2.1 DiscussionA lot may be generated by a commonproduction (or other natural) process in a restricted time periodand usually consists of a finite size or number. A lot ma
41、y be afractional part of a population (Interpretation 2 of population,see Annex A1). A recognized property range implies that somerough approximation is available.3.3.3 material, na specific entity or element class to betested; it usually exists in bulk form (solid, powder, or liquid).3.3.3.1 Discus
42、sionMaterial is used as a generic term todescribe the class of elements that is tested, that is, a materialmay be a rubber, a rubber compound, a carbon black, a rubberchemical, and so forth. A material may or may not behomogeneous. In product testing the term material may be usedto describe the clas
43、s of elements or type of rubber productssuch as O-rings, hose assemblies, motor mounts, and so forth.See also 5.1.4.1.3.3.4 sample (data), nthe number of test or observationvalues (n = 1, 2, 3, and so forth), obtained from (one or more)physical samples, by the application of a specific test (obser-v
44、ation) method.3.3.5 sample (physical), nthe number of elements or thespecified mass of a material, selected according to a particularprocedure, used to evaluate material, lot, or population char-acteristics.3.3.5.1 DiscussionThe term sample should not be used asa synonym for material, see 3.3.3,orta
45、rget material, see5.1.4.1. Ideally several materials are tested in any ITP witheach material being different (chemically, structurally, propertywise). From each material, some number of samples (allnominally identical) may be taken for testing. See 3.3.4.3.3.6 test sample, nthat part of a (physical)
46、 sample of anytype taken for chemical or other analytical testing, usually witha prescribed blending or other protocol.3.3.6.1 DiscussionA test sample is usually a mass orvolume that is some small fractional part of a bulk material.3.3.7 test specimen, nan object (appropriately shaped andprepared) t
47、aken from a sample for physical or mechanicaltesting.3.3.7.1 DiscussionOther terms for test specimen are: testportion, 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 meanobtained on the basis of n independe
48、nt replicate measurements;the greater n the better the approximation to the true orreference mean, provided there is no systematic deviation orbias.3.4.1.1 DiscussionThe words mean and estimated meanare frequent synonyms for estimated (true or reference) mean.The value for n in typical routine testi
49、ng programs is of theorder 1 to 10. When bias exists, the estimated (true orreference) mean so obtained estimates + Bi, where =true or reference mean and Bi = algebraic sum of all biasdeviation terms. Therefore, if bias exists and is unknown inmagnitude, the true value or cannot be approximated despiteincreased replication. See random and bias deviations inA1.2.5 and A1.2.6. See also Annex A2.3.4.2 outlier, na member of a set of values which isinconsistent with the other members of that set.3.4.3 reference value, na value (usually a mea
