1、Designation: D6600 00 (Reapproved 2013)Standard Practice forEvaluating Test Sensitivity for Rubber Test Methods1This standard is issued under the fixed designation D6600; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice covers testing to evaluate chemicalconstituents, chemical and physical properties of compoundingmaterial
3、s, and compounded and cured rubbers, which mayfrequently be conducted by one or more test methods. Whenmore than one test method is available, two questions arise:Which test method has the better (or best) response to ordiscrimination for the underlying fundamental property beingevaluated? and Which
4、 test method has the least error? Thesetwo characteristics collectively determine one type of technicalmerit of test methods that may be designated as test sensitivity.1.2 Although a comprehensive and detailed treatment, asgiven by this practice, is required for a full appreciation of testsensitivit
5、y, a simplified conceptual definition may be givenhere. Test sensitivity is the ratio of discrimination power for thefundamental property evaluated to the measurement error oruncertainty, expressed as a standard deviation. The greater thediscriminating power and the lower the test error, the better
6、isthe test sensitivity. Borrowing from the terminology inelectronics, this ratio has frequently been called the signal-to-noise ratio; the signal corresponding to the discriminationpower and the noise corresponding to the test measurementerror. Therefore, this practice describes how test sensitivity
7、,generically defined as the signal-to-noise ratio, may be evalu-ated for test methods used in the rubber manufacturingindustry, which measure typical physical and chemicalproperties, with exceptions as noted in 1.3.1.3 This practice does not address the topic of sensitivity forthreshold limits or mi
8、nimum detection limits (MDL) in suchapplications as (1) the effect of intentional variations ofcompounding materials on measured compound properties or(2) the evaluation of low or trace constituent levels. Minimumdetection limits are the subject of separate standards.1.4 This standard does not purpo
9、rt to address all of thesafety concerns, if any, associated with its use. It 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.1.5 The content of this practice is as follows:
10、SectionScope 1Referenced Documents 2Terminology 3Summary of Practice 4Significance and Use 5Measurement Process 6Development of Test Sensitivity Concepts(Absolute and Relative Test Sensitivity, Limited and ExtendedRange Test Sensitivity, Uniform and Nonuniform Test Sensitivity)7Steps in Conducting a
11、 Test Sensitivity Evaluation Program 8Report for Test Sensitivity Evaluation 9Keywords 10Annex A1Background on: Use of Linear Regression Analysis andPrecision of Test Sensitivity EvaluationAppendix X1Two Examples of Relative Test Sensitivity Evaluation:Relative Test Sensitivity: Limited RangeThree P
12、rocessabilityTestsRelative Test Sensitivity: Extended RangeCompliance versusModulusAppendix X2Background on: Transformation of Scale andDerivation of Absolute Sensitivity for a Simple Analytical Test2. Referenced Documents2.1 ASTM Standards:2D4483 Practice for Evaluating Precision for Test MethodSta
13、ndards in the Rubber and Carbon Black ManufacturingIndustries3. Terminology3.1 A number of specialized terms or definitions are re-quired for this practice. They are defined in a systematic orsequential order from simple terms to complex terms; thesimple terms may be used in the definition of the mo
14、re complexterms. This approach generates the most succinct and unam-biguous definitions. Therefore, the definitions do not appear inthe usual alphabetical sequence.3.2 Definitions:3.2.1 calibration material, CM,na material (or otherobject) selected to serve as a standard or benchmark referencemateri
15、al, with a fully documented FP reference value for a test1This practice is under the jurisdiction ofASTM Committee D11 on Rubber andis the direct responsibility of Subcommittee D11.16 on Application of StatisticalMethods.Current edition approved Nov. 1, 2013. Published January 2014. Originallyapprov
16、ed in 2000. Last previous edition approved in 2009 as D6600 00 (2009).DOI: 10.1520/D6600-00R13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Documen
17、t Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1method; the calibration material, along with several othersimilar materials with documented or FPreference values, maybe used to calibrate a particular
18、test method or may be used toevaluate test sensitivity.3.2.1.1 DiscussionA fully documented FP or FP referencevalue implies that an equally documented measured propertyvalue may be obtained from a MP = f (FP) relationship.However, unless f = 1, the numerical values for the MP and theFP are not equal
19、 for any CM.3.2.2 fundamental property, FP,nthe inherent or basicproperty (or constituent) that a test method is intended toevaluate.3.2.3 measured property, MP,nthe property that themeasuring instrument responds to; it is related to the FP by afunctional relationship, MP = f (FP), that is known or
20、that maybe readily evaluated by experiment.3.2.4 reference material, RM,na material (or other ob-ject) selected to serve as a common standard or benchmark forMP measurements for two or more test methods; the expectedmeasurement value for each of the test methods, designated asthe reference value, ma
21、y be known (from other sources) or itmay be unknown.3.2.5 testing domain, nthe operational conditions underwhich a test is conducted; it includes description of the testsample or specimen preparation, the instrument(s) used(calibration, adjustments, settings), the selected testtechnicians, and the s
22、urrounding environment.3.2.5.1 local testing, na testing domain comprised of onelocation or laboratory as typically used for quality control andinternal development or evaluation programs.3.2.5.2 global testing, na testing domain that encom-passes two or more locations or laboratories, domestic orin
23、ternational, typically used for producer-user testing, productacceptance, and interlaboratory test programs.3.2.6 Although a simplified conceptual definition of testsensitivity was given in the Scope, a more detailed but stillgeneral definition using quantitative terms is helpful forpreliminary disc
24、ussion.3.2.6.1 test sensitivity (generic),na derived quantity thatindicates the level of technical merit of a test method; it is theratio of the test discrimination power or signal, that is themagnitude of the change in the MP for some unit change in therelated FP of interest, to the noise or standa
25、rd deviation of theMP.3.2.6.2 DiscussionThis definition strictly applies to anabsolute sensitivity, see 7.2. The change in the FP may be anactual measurement unit or a selected FP difference. Therelation between the MP and the FP is of the form MP = f (FP).4. Summary of Practice4.1 This practice dev
26、elops the necessary terminology andthe required concepts for defining and evaluating test sensitiv-ity for test methods. Sufficient background information ispresented to place the standard on a firm conceptual andmathematical foundation. This allows for its broad applicationacross both chemical and
27、physical testing domains. The devel-opment of this practice draws heavily on the approach andtechniques as given in the referenced literature.3,44.2 After the introduction of some general definitions, abrief review of the measurement process is presented, suc-ceeded by a development of the basic tes
28、t sensitivity concepts.This is followed by defining two test sensitivity classifications,absolute and relative test sensitivity and two categories, (1) fora limited measured property range and (2) for an extendedproperty range evaluation. For an extended property range foreither classification, two
29、types of test sensitivity may exist, (1)uniform or equal sensitivity across a range of properties or (2)nonuniform sensitivity which depends on the value of themeasured properties across the selected range.4.3 Annex A1 is an important part of this practice. Itpresents recommendations for using linea
30、r regression analysisfor test sensitivity evaluation and recommendations for evalu-ating the precision of test sensitivity.4.4 Appendix X1 is also an important adjunct to thispractice. It gives two examples of relative test sensitivitycalculations: (1) for a limited range or spot check program and(2
31、) for an extended range test sensitivity program with adependent (nonuniform) test sensitivity. Appendix X2 givesbackground on transformation of scale often needed for ex-tended range sensitivity and for improved understanding, italso gives the derivation of the absolute test sensitivity for asimple
32、 analytical chemical test.5. Significance and Use5.1 Testing is conducted to make technical decisions onmaterials, processes, and products. With the continued growthin the available test methods for evaluating scientific andtechnical properties, a quantitative approach is needed to selecttest method
33、s that have high (or highest) quality or technicalmerit. The procedures as defined in this practice may be usedfor this purpose to make testing as cost effective as possible.5.2 One index of test method technical merit and impliedsensitivity frequently used in the past has been test methodprecision.
34、 The precision is usually expressed as some multipleof the test measurement standard deviation for a defined testingdomain. Although precision is a required quantity for testsensitivity, it is an incomplete characteristic (only one half ofthe necessary information) since it does not consider thedisc
35、rimination power for the FP (or constituent) being evalu-ated.5.3 Any attempt to evaluate relative test sensitivity for twodifferent test methods on the basis of test measurementstandard deviation ratios or variance ratios, which lack anydiscrimination power information content, constitutes an in-va
36、lid quantitative basis for sensitivity, or technical merit3Mandel, J., and Stiehler, R.D., Journal of Research of National Bureau ofStandards, Vol 53, No. 3, September 1954. See also “Precision Measurement andCalibrationStatistical Concepts and Procedures,” Special Publication 300, Vol 1,National Bu
37、reau of Standards, 1969, pp. 179155). (The National Bureau ofStandards is now the National Institute for Standards and Technology.)4“The Statistical Analysis of Experimental Data,” Chapters 13 and 14, J.Mandel, Interscience Publishers (John Wiley for every value of MP theremust be a unique single va
38、lue for FP. The relationship must bespecific for any particular measuring process or test, and, ifthere are two different processes or tests for evaluating the FP,the relationship is generally different for each test.7. Development of Test Sensitivity Concepts7.1 Test DomainThe scope of any potentia
39、l test sensitivityevaluation program should be established. Is the evaluation fora limited local testing situation, that is, one laboratory or testlocation? Or are the results to be applied on a global basisacross numerous domestic or worldwide laboratories or loca-tions? If local testing is the iss
40、ue, the test measurements areconducted in one laboratory or location. For global testing, aninterlaboratory test program (ITP) must be conducted. Two ormore replicate test sensitivity evaluations are conducted ineach participating laboratory and an overall or average testsensitivity is obtained acro
41、ss all laboratories. In the context ofan ITP for global evaluation, each replicate sensitivity evalu-ation is defined as the entire set of operations that is requiredto calculate one estimated value for the test sensitivity. Foradditional background on the assessment of precision for thetest sensiti
42、vity values attained, see A1.2 and also PracticeD4483.7.2 Test Sensitivity ClassificationThere are two classifica-tions for test sensitivity.7.2.1 Class 1 is absolute test sensitivity, or ATS, where theword absolute is used in the sense that the measured propertycan be related to the FP by a relatio
43、nship that gives absolute ordirect values for FP from a knowledge of the MP. In evaluatingtest sensitivity for this class, two or more CMs are used eachhaving documented values for the FP.7.2.2 Class 2 is relative test sensitivity, or RTS, where thetest sensitivity of Test Method 1 is compared to Te
44、st Method 2,on the basis of a ratio, using two or more RMs with differentMP values. This class is used for physical test methods whereno FPs can be evaluated.7.3 Absolute Test SensitivityIn this section absolute ordirect test sensitivity is defined in a simplified manner by theuse of Fig. 1.7.3.1 De
45、velopment of Absolute Test SensitivityFig. 1 isconcerned with two types of properties: (1) an FP (or singlecriterion or constituent), the value of which is established bythe use of a CM and (2) an MP obtained by applying the testmethod to the CM. A relationship or functionality existsbetween the MP
46、and FP that may be nonlinear. In theapplication of a particular test, FP1corresponds to MP1andFP2corresponds to MP2. Over a selected region of therelationship, designed by points a and b, the slope, K, of theillustrated curve is approximated by the relationship K =(MP)/(FP). If the test measurement
47、standard deviation forMP denoted as SMP, is constant over this a to b range, theabsolute test sensitivity designated as Ais defined by Eq 1.A5?K ?/SMP(1)The equation indicates that for the selected region of interest,test sensitivity will increase with the increase of the numerical(absolute) value o
48、f the slope,|K|andsensitivity will increasethe more precise the MP measurement. Thus, Amay be usedas a criterion of technical merit to select one of a number of testmethods to measure the FP provided that a functionalrelationship, MP = f (FP), can be established for each testmethod.7.3.2 Absolute te
49、st sensitivity may not be uniform orconstant across a broad range of MPor FPvalues. It is constantacross a specified range, only if the direct (not transformed)MP versus FP relationship is linear and the test error SMPisFIG. 1 Measured Versus Fundamental Property RelationshipD6600 00 (2013)3constant. With an assumed monotonic relationship between FPand MP, absolute test sensitivity, A, may be evaluated on thebasis of (1) two or more CMs, (or objects) with differentknown FP values or (2) a theoretical relationship between MPand FP.7.3.3 Formal Development f