1、Designation: D4678 04 (Reapproved 2009)Standard Practice forRubberPreparation, Testing, Acceptance, Documentation,and Use of Reference Materials1This standard is issued under the fixed designation D4678; the number immediately following the designation indicates the year oforiginal adoption or, in t
2、he 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.1. Scope1.1 This practice covers materials used on an industry-widebasis as reference materials,
3、which are vitally important toconduct product, specification, and development testing in therubber and carbon black industry. This practice describes thesteps necessary to ensure that any candidate material, that hasa perceived need, can become a Reference Material. Thepractice sets forth the recomm
4、endations on the preparationsteps for these materials, on the testing that shall be conductedto permit acceptance of any candidate material, and on how thedocumentation needed for the acceptance shall be recorded forfuture use and review.1.2 This practice shall be administered by ASTM Commit-tee D11
5、 in consultation on all matters with Committee D24.1.2.1 Important sections of this practice are as follows:SectionSignificance and Use 3Preparation of Industry Reference Materials 4Overview of Industry Reference Material Testing 5Chemical and Physical Specifications for IRM 6Reference Material Docu
6、mentation 7Assignment and Tabulation of Reference Material Numbers 8Typical Reference Material Use 9Recommended Package Size for IRM Annex A1Recommended Sampling Plans for Homogeneity Testing of anIRMAnnex A2Test Plan and Analysis for Homogeneity of an IRM Annex A3Test Plan and Analysis to Evaluate
7、an Accepted Reference ValueAnnex A4Statistical Model(s) for IRM Testing Annex A5Example of Annex Calculations for a Typical IRM Appendix X1Two-Way Analysis of Variance for Calculating Sr Appendix X2Inventory of NIST Rubber Compounding SRMs Appendix X31.3 This standard does not purport to address all
8、 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.2. Referenced Documents2.1 ASTM Standards:2D4483 Practice for Ev
9、aluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesE122 Practice for Calculating Sample Size to Estimate,With Specified Precision, the Average for a Characteristicof a Lot or ProcessE691 Practice for Conducting an Interlaboratory Study toDetermine the P
10、recision of a Test MethodE826 Practice for Testing Homogeneity of a Metal Lot orBatch in Solid Form by SparkAtomic Emission Spectrom-etry3. Significance and Use3.1 Reference materials are vitally important in product andspecification testing, in research and development work, intechnical service wor
11、k, and in quality control operations in therubber and carbon black industries. They are especially valu-able for referee purposes.3.2 Categories, Classes, and Types of Reference Materials(RM):3.2.1 Reference materials are divided into two categories:3.2.1.1 Industry Reference Materials (IRM)Material
12、s thathave been prepared according to a specified production processto generate a uniform lot; the parameters that define the qualityof the lot are evaluated by a specified measurement program.3.2.1.2 Common-Source Reference Materials (CRM)Materials that have been prepared to be as uniform as possib
13、lebut do not have established property (parameter) values; theknowledge of a common or single source is sufficient forcertain less critical applications.3.2.2 Industry reference materials (IRMs) are divided intoadditional classes and types according to the method ofevaluating the lot parameters and
14、according to the production1This practice is under the jurisdiction ofASTM Committee D11 on Rubber andis the direct responsibility of Subcommittee D11.20 on Compounding Materials andProcedures.Current edition approved Sept. 1, 2009. Published March 2010. Originallyapproved in 1987. Last previous edi
15、tion approved in 2004 as D4678 04. DOI:10.1520/D4678-04R09.2For 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 Document Summary page onthe ASTM website.1C
16、opyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.process for generating the lot material. These are explainedmore fully (refer to Annex A3 and Annex A4 for more detailson the discussion in Section 3).3.2.3 The following lot parameters a
17、re important for refer-ence material use:3.2.3.1 Accepted Reference Value (AR Value)An averageIRM property or parameter value established by way of aspecified test program.3.2.3.2 Test Lot Limits (TL Limits)These are limits de-fined as 63 times the standard deviation of individual IRM testresults ac
18、ross the entire lot for the property or parameter(s) thatdefines lot quality; the measurements are conducted in thelaboratory of the organization producing the IRM.3.2.3.3 Although the limits as defined in 3.2.3.2 are given interms of 63 times the standard deviation, the rejection ofindividual porti
19、ons of the lot as being outlier or non-typicalportions in assessing the homogeneity of the lot is done on thebasis of 62 times the appropriate standard deviation, that is, onthe basis of a 95 % confidence interval. See Annex A3 andAnnexA4 for more information and the evaluation procedures.3.2.4 All
20、IRMs have an AR value and TL limits; howeverthe AR value may be obtained in one of two ways to produceone of two classes of AR values:3.2.4.1 Global AR ValueThis AR value is obtained froman interlaboratory test program where the word “global”indicates an average value across many laboratories.3.2.4.
21、2 Local AR ValueThis is an AR value obtained inone laboratory or at one location, usually the laboratoryresponsible for preparation of the homogeneous lot.3.2.5 An additional parameter is of importance for IRMsthat have a global AR value:3.2.5.1 Between-Laboratory Limits (BL)The group oflaboratories
22、 that conduct interlaboratory testing to establish anAR-value are not equivalent to a system or population typicalof industrial production operations that use the usual 63standard deviation limits. Such production operations aresystems that have been purged of all assignable causes ofvariation and a
23、re in a state of statistical control with onlyrandom variations that cannot be removed. Thus, the recom-mended limits on all IRMs are the 62 standard deviation limitsthat pertain to a 95 % confidence level. If for serious reasonsthat can be totally justified, 63 standard deviation limits arerequired
24、, these may be used provided that full and completedocumentation is supplied to justify the limits.3.2.6 The homogeneity or uniformity of the lot, whichdetermines the magnitude of the TL limits, may be designatedas one of two different levels of uniformity. The key factor thatdetermines the level of
25、 uniformity is the capability of blendingthe IRM portions or parts that constitute the lot, to ensure ahigh degree of uniformity from the blending process. IRMsthat cannot be blended will have an extra residual amount ofvariation (portion to portion) that lowers the level of unifor-mity.3.2.6.1 Unif
26、ormity Level 1 (UL-1)This is the most uni-form or highest level of homogeneity that can be attained bythe use of a specified test for measuring the parameter thatdefines lot quality; it is obtained by the use of a blendedmaterial and is referred to as a Type B (B = blended) IRM.3.2.6.2 Uniformity Le
27、vel 2 (UL-2)This is the lesser degreeof uniformity that is attained by the use ofa specified test formeasuring the parameter that defines lot quality; it is normallyobtained for non-blended materials and is referred to as a TypeNB (not blended) IRM.3.3 IRMs have a number of use applications in the t
28、echnicalareas, as cited in 3.1.3.3.1 Single Laboratory Self EvaluationThe IRM may beused in a given laboratory (or with a given test system) tocompare the test results within the laboratory to the acceptedreference value for the IRM. An IRM can also be used forinternal statistical quality control (S
29、QC) operations.3.3.2 Multi-Laboratory EvaluationThe IRM may be usedbetween two or more laboratories to determine if the testsystems in the laboratories are operating within selectedcontrol limits.3.3.3 One or more IRMs may be used in the preparation ofcompounds to be used for evaluating non-referenc
30、e materialsin compound testing and performance.3.3.4 Reference liquid IRMs may be used for immersiontesting of various candidate or other reference compounds.Such immersion testing is important due to the deleteriousinfluences of immersion liquids on rubber compounds.3.3.5 IRMs may also be used to e
31、liminate interlaboratorytesting variation known as “test bias:” a difference between two(or more) laboratories that is essentially constant between thelaboratories for a given test property level, irrespective of thetime of the test comparisons. In such applications a differentialtest measurement va
32、lue, (IRM experimental material), be-comes a corrected test result; this corrected value is used as themeasure of performance rather than the “as-measured” testvalue on the experimental material of interest.3.4 Average values play an important role in various opera-tions and decisions in this practi
33、ce. For this practice, “average”is defined as the arithmetic mean.3.5 The various characteristics of IRMs and CRMs (catego-ries, classes, types) are listed in summary form in Table 1.3.6 This practice and the IRM program it describes is beingdeveloped to replace a standardization program conducted b
34、ythe National Institute of Standards and Technology (NIST) thatwas begun in 1948 and is being phased out. The standardmaterials developed by the NIST program are referred to asStandard Reference Materials or SRM.3.7 To provide for some continuity in the “phase-outphase-in” operation, Appendix X3 lis
35、ts the rubber and com-pounding materials still carried by NIST on an interim basis.TABLE 1 Categories of Reference MaterialsAIRM CRMAR Value Global Local NoneHomogeneity Type B Type NB Type B Type NB Single Source(TL Limits) (UL-1) (UL-2) (UL-1) (UL-2) Materialor (UL-1) or (UL-1)AAR value = accepted
36、 reference value.TL limits = test lot limits.Global = AR value obtained from an interlaboratory test program.Local = AR value obtained from one laboratory.Type-B = IRM that has been blended to ensure high uniformity.Type-NB = IRM that cannot be blended.UL-1 and UL-2 = levels of uniformity in the IRM
37、 lot; UL-1 is higher uniformitythan UL-2.See Annex A3 and Annex A4 for more information.D4678 04 (2009)2Appendix X3 will be retained in this practice until such time asNIST materials are no longer used.3.8 It is not feasible to write into this practice all thenecessary specifications, modes of prepa
38、ration, sampling, andtesting protocols, for the wide variety of materials that willeventually become IRM. Therefore this practice is published togive general guidelines for IRMs.3.9 A permanent IRM Steering Committee within Subcom-mittee D11.20 shall be constituted by Subcommittee D11.90 inconsultat
39、ion with Committee D24 to assist in the utilization ofthis practice and to make technical and, where required, policydecisions regarding the preparation and administration of IRM.The IRM Steering Committee shall have members of bothCommittees D11 and D24.4. Preparation of Industry Reference Material
40、s4.1 Basic Preparation Steps:4.1.1 An IRM should be prepared in a way that ensures thatthe entire quantity or lot of the material is as homogeneous, incomposition and vital performance properties, as is possible.4.1.2 For particulate and liquid materials this implies athorough physical blending oper
41、ation during or after themanufacturing steps, or both.4.1.3 For materials not easily blended after manufacture,two options to ensure homogeneity are recommended:4.1.3.1 Use highly homogeneous components or other ma-terials that are required in the manufacturing steps or conductcertain blending opera
42、tions at intermediate manufacturingsteps to ensure maximum homogeneity.4.1.3.2 Use intensive statistical quality control proceduresto ensure a specified degree of homogeneity among thepackets, bales, or other discrete units of the material.4.1.4 Examples, as cited in 4.1.3.1, are such materials asac
43、celerators, antioxidants, sulfur, and reference test (liquid)fuels.4.1.5 Examples, as cited in 4.1.3.2, are various syntheticrubbers.4.2 Packaging of Industry Reference Materials:4.2.1 Industry reference materials should be packaged pref-erably in small quantities or packages. The packages shall bec
44、onsecutively numbered as they are filled. Nominally the sizeshould be the smallest amount that the average user of thematerial would require for normal volume testing. High vol-ume users could therefore order multiple package lots. The useof such minimum volume (mass) packages will of course vary,bu
45、t Annex A1 gives recommended masses or volumes.4.2.2 Industry reference materials shall be suitably pack-aged to prevent or retard the change of IRM values with thepassage of time or inadvertent exposure to heat, light, moisture,or combinations thereof, in normal storage. The stringency ofthis requi
46、rement varies with the type of IRM. All precautionsshall be taken to make IRMs as stable as possible.4.2.3 Packages shall be dispensed by the manufacturing ordistribution organization with a document that shall furnish thefollowing general information:4.2.3.1 Name and number of the IRM,4.2.3.2 Name
47、of the manufacturer,4.2.3.3 Date of manufacture or preparation,4.2.3.4 Storage conditions, and4.2.3.5 Reference to ASTM research report for documenta-tion of testing.4.2.4 For each test property measured to assess lot qualityreport the following:4.2.4.1 Accepted reference value,4.2.4.2 Test lot limi
48、ts, and4.2.4.3 Between-laboratory limits.4.3 Packaging of CommonSource Reference Materials:4.3.1 CRMs shall be packaged and dispensed in the samemanner as for IRMs. Each CRM package shall be furnishedwith a documentation sheet with the following information:4.3.1.1 Name and number of the CRM,4.3.1.2
49、 Name of manufacturer,4.3.1.3 Date of manufacture or preparation,4.3.1.4 Storage conditions, and4.3.1.5 Reference to ASTM research report.5. Overview of Industry Reference Material Testing5.1 Testing is conducted to (1) demonstrate the uniformityof the IRM lot to some selected limits and evaluate the test lotlimits, and (2) to establish an accepted reference value for thelot and as a secondary goal to evaluate the between-laboratorylimits for interlaboratory testing of the IRM where this isapplicable.5.2 Testing for Homogeneity:5.2.1 Homogeneity testing is ideally
