1、Designation: D4678 04 (Reapproved 2009)1Standard 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
2、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.1NOTEEditorially corrected A4.4.4 in October 2011.1. Scope1.1 This practice covers materials use
3、d on an industry-widebasis as reference materials, 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 Re
4、ference Material. Thepractice sets forth the recommendations 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 pr
5、actice shall be administered by ASTM Commit-tee D11 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 Physi
6、cal Specifications for IRM 6Reference Material Documentation 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
7、 an IRM Annex A3Test Plan and Analysis to Evaluate 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
8、X31.3 This standard does not purport 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.2. Referenced
9、 Documents2.1 ASTM Standards:2D4483 Practice for Evaluating 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 Co
10、nducting an Interlaboratory Study toDetermine the Precision 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 res
11、earch and development work, intechnical service work, 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
12、:3.2.1.1 Industry Reference Materials (IRM)Materials 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
13、 that have been prepared to be as uniform as possiblebut 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
14、 to the method ofevaluating the lot parameters and 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
15、2010. Originallyapproved in 1987. Last previous edition approved in 2004 as D4678 04. DOI:10.1520/D4678-04R09E01.2For 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
16、 standards Document Summary page onthe ASTM website.1Copyright 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 discuss
17、ion in Section 3).3.2.3 The following lot parameters are 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 t
18、he standard deviation of individual IRM testresults across 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 th
19、e standard deviation, the rejection ofindividual portions 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 mor
20、e information and the evaluation procedures.3.2.4 All 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”indi
21、cates an average value across many laboratories.3.2.4.2 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
22、Between-Laboratory Limits (BL)The group oflaboratories 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
23、been purged of all assignable causes ofvariation and are 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 total
24、ly justified, 63 standard deviation limits arerequired, 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
25、uniformity. The key factor thatdetermines the level of 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 port
26、ion) that lowers the level of unifor-mity.3.2.6.1 Uniformity 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
27、to as a Type B (B = blended) IRM.3.2.6.2 Uniformity Level 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) I
28、RM.3.3 IRMs have a number of use applications in the technicalareas, 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 a
29、lso be used forinternal statistical quality control (SQC) 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 preparat
30、ion ofcompounds to be used for evaluating non-reference 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 liquid
31、s on rubber compounds.3.3.5 IRMs may also be used to eliminate 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.
32、In such applications a differentialtest measurement value, (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 ro
33、le in various opera-tions and decisions in this practice. 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 beingdeve
34、loped to replace a standardization program conducted bythe 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
35、 in the “phase-outphase-in” operation, Appendix X3 lists 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)
36、(UL-2) Materialor (UL-1) or (UL-1)AAR value = accepted 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 b
37、lended.UL-1 and UL-2 = levels of uniformity in the IRM lot; UL-1 is higher uniformitythan UL-2.See Annex A3 and Annex A4 for more information.D4678 04 (2009)12Appendix 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 p
38、ractice all thenecessary specifications, modes of preparation, 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
39、shall be constituted by Subcommittee D11.90 inconsultation 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 D1
40、1 and D24.4. Preparation of Industry Reference Materials4.1 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
41、materials this implies athorough physical blending operation 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 t
42、he manufacturing steps or conductcertain blending operations 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
43、 Examples, as cited in 4.1.3.1, are such materials asaccelerators, 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
44、in small quantities or packages. The packages shall beconsecutively 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 suc
45、h minimum volume (mass) packages will of course vary,but 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
46、thereof, in normal storage. The stringency ofthis requirement 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 infor
47、mation:4.2.3.1 Name and number of the IRM,4.2.3.2 Name 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
48、:4.2.4.1 Accepted reference value,4.2.4.2 Test lot limits, 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
49、 information:4.3.1.1 Name and number of the CRM,4.3.1.2 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 Te
