1、Designation: D4678 11D4678 15Standard 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 the case of
2、 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-wide basis as reference materials, which are
3、 vitally important to conductproduct, specification, and development testing in the rubber industry. This practice describes the steps necessary to ensure thatany candidate material, that has a perceived need, can become a Reference Material. The practice sets forth the recommendationson the prepara
4、tion steps for these materials, on the testing that shall be conducted to permit acceptance of any candidate material,and on how the documentation needed for the acceptance shall be recorded for future use and review.1.2 This practice shall be administered by ASTM Committee D11.1.2.1 Important secti
5、ons 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 Documentation 7Assignment and Tabulation of Reference Material Numbers 8Typi
6、cal 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 an Accepted Reference Value Annex A4Statistical Model(s) for IRM Testing
7、 Annex A5Example of Annex Calculations for a Typical IRM Appendix X1Two-Way Analysis of Variance for Calculating Sr Appendix X21.3 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
8、appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D4483 Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing IndustriesD5900 Specification for Ph
9、ysical and Chemical Properties of Industry Reference Materials (IRM)E122 Practice for Calculating Sample Size to Estimate, With Specified Precision, the Average for a Characteristic of a Lot orProcessE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test MethodE82
10、6 Practice for Testing Homogeneity of a Metal Lot or Batch in Solid Form by Spark Atomic Emission Spectrometry3. Significance and Use3.1 Reference materials are vitally important in product and specification testing, in research and development work, intechnical service work, and in quality control
11、operations in the rubber industry. They are especially valuable for referee purposes.1 This practice is under the jurisdiction of ASTM Committee D11 on Rubber and is the direct responsibility of Subcommittee D11.20 on Compounding Materials andProcedures.Current edition approved Nov. 1, 2011June 1, 2
12、015. Published December 2011August 2015. Originally approved in 1987. Last previous edition approved in 20092011as D4678 04 (2009)D4678 11.1. DOI: 10.1520/D4678-11.10.1520/D4678-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org
13、. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.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 m
14、ay not be technically possible to adequately 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 Har
15、bor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.2 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)Materials that have been prepared according to a specified produc
16、tion process togenerate a uniform lot; the parameters that define the quality of 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 possible but do nothave established property (parameter) valu
17、es; the knowledge of a common or single source is sufficient for certain less criticalapplications.3.2.2 Industry reference materials (IRMs) are divided into additional classes and types according to the method of evaluatingthe lot parameters and according to the production process for generating th
18、e lot material. These are explained more fully (referto Annex A3 and Annex A4 for more details on the discussion in Section 3).3.2.3 The following lot parameters are important for reference material use:3.2.3.1 Accepted Reference Value (AR Value)An average IRM property or parameter value established
19、 by way of a specifiedtest program.3.2.3.2 Test Lot Limits (TL Limits)These are limits defined as 63 times the standard deviation of individual IRM test resultsacross the entire lot for the property or parameter(s) that defines lot quality; the measurements are conducted in the laboratory ofthe orga
20、nization producing the IRM.3.2.3.3 Although the limits as defined in 3.2.3.2 are given in terms of 63 times the standard deviation, the rejection of individualportions of the lot as being outlier or non-typical portions in assessing the homogeneity of the lot is done on the basis of 62 timesthe appr
21、opriate standard deviation, that is, on the basis of a 95 % confidence interval. See Annex A3 and Annex A4 for moreinformation and the evaluation procedures.3.2.4 All IRMs have an AR value and TL limits; however the AR value may be obtained in one of two ways to produce oneof two classes of AR value
22、s:3.2.4.1 Global AR ValueThis AR value is obtained from an interlaboratory test program where the word “global” indicatesan average value across many laboratories.3.2.4.2 Local AR ValueThis is an AR value obtained in one laboratory or at one location, usually the laboratory responsiblefor preparatio
23、n of the homogeneous lot.3.2.5 An additional parameter is of importance for IRMs that have a global AR value:3.2.5.1 Between-Laboratory Limits (BL)The group of laboratories that conduct interlaboratory testing to establish anAR-value are not equivalent to a system or population typical of industrial
24、 production operations that use the usual 63 standarddeviation limits. Such production operations are systems that have been purged of all assignable causes of variation and are in astate of statistical control with only random variations that cannot be removed. Thus, the recommended limits on all I
25、RMs arethe 62 standard deviation limits that pertain to a 95 % confidence level. If for serious reasons that can be totally justified, 63standard deviation limits are required, these may be used provided that full and complete documentation is supplied to justify thelimits.3.2.6 The homogeneity or u
26、niformity of the lot, which determines the magnitude of the TL limits, may be designated as oneof two different levels of uniformity. The key factor that determines the level of uniformity is the capability of blending the IRMportions or parts that constitute the lot, to ensure a high degree of unif
27、ormity from the blending process. IRMs that cannot beblended will have an extra residual amount of variation (portion to portion) that lowers the level of uniformity.3.2.6.1 Uniformity Level 1 (UL-1)This is the most uniform or highest level of homogeneity that can be attained by the useof a specifie
28、d test for measuring the parameter that defines lot quality; it is obtained by the use of a blended material and is referredto as a Type B (B = blended) IRM.3.2.6.2 Uniformity Level 2 (UL-2)This is the lesser degree of uniformity that is attained by the use ofa specified test formeasuring the parame
29、ter that defines lot quality; it is normally obtained for non-blended materials and is referred to as a Type NB(not blended) IRM.3.3 IRMs have a number of use applications in the technical areas, as cited in 3.1.3.3.1 Single Laboratory Self EvaluationThe IRM may be used in a given laboratory (or wit
30、h a given test system) to comparethe test results within the laboratory to the accepted reference value for the IRM. An IRM can also be used for internal statisticalquality control (SQC) operations.3.3.2 Multi-Laboratory EvaluationThe IRM may be used between two or more laboratories to determine if
31、the test systemsin the laboratories are operating within selected control limits.3.3.3 One or more IRMs may be used in the preparation of compounds to be used for evaluating non-reference materials incompound testing and performance.3.3.4 Reference liquid IRMs may be used for immersion testing of va
32、rious candidate or other reference compounds. Suchimmersion testing is important due to the deleterious influences of immersion liquids on rubber compounds.3.3.5 IRMs may also be used to eliminate interlaboratory testing variation known as “test bias:” a difference between two (ormore) laboratories
33、that is essentially constant between the laboratories for a given test property level, irrespective of the time ofD4678 152the test comparisons. In such applications a differential test measurement value, (IRM experimental material), becomes acorrected test result; this corrected value is used as th
34、e measure of performance rather than the “as-measured” test value on theexperimental material of interest.3.4 Average values play an important role in various operations and decisions in this practice. For this practice, “average” isdefined as the arithmetic mean.3.5 The various characteristics of I
35、RMs and CRMs (categories, classes, types) are listed in summary form in Table 1.3.6 This practice and the IRM program it describes was developed to replace a standardization program conducted by theNational Institute of Standards and Technology (NIST) that began in 1948 and has been phased out.3.7 I
36、t is not feasible to write into this practice all the necessary specifications, modes of preparation, sampling, and testingprotocols, for the wide variety of materials that will eventually become IRM. Therefore this practice is published to give generalguidelines for IRMs.3.8 Apermanent IRM Steering
37、 Committee within Subcommittee D11.20 shall be constituted by Subcommittee D11.90 to assistin the utilization of this practice and to make technical and, where required, policy decisions regarding the preparation andadministration of IRM.4. Preparation of Industry Reference Materials4.1 Basic Prepar
38、ation Steps:4.1.1 An IRM should be prepared in a way that ensures that the 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 a thorough physical blending operation during or
39、 after the manufacturingsteps, 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 materials that are required in the manufacturing steps or conduct certainblending operations at interm
40、ediate manufacturing steps to ensure maximum homogeneity.4.1.3.2 Use intensive statistical quality control procedures to ensure a specified degree of homogeneity among the packets,bales, or other discrete units of the material.4.1.4 Examples, as cited in 4.1.3.1, are such materials as accelerators,
41、antioxidants, sulfur, and reference test (liquid) fuels.4.1.5 Examples, as cited in 4.1.3.2, are various synthetic rubbers.4.2 Packaging of Industry Reference Materials:4.2.1 Industry reference materials should be packaged preferably in small quantities or packages. The packages shall beconsecutivel
42、y numbered as they are filled. Nominally the size should be the smallest amount that the average user of the materialwould require for normal volume testing. High volume users could therefore order multiple package lots.The use of such minimumvolume (mass) packages will of course vary, but Annex A1
43、gives recommended masses or volumes.4.2.2 Industry reference materials shall be suitably packaged to prevent or retard the change of IRM values with the passageof time or inadvertent exposure to heat, light, moisture, or combinations thereof, in normal storage. The stringency of thisrequirement vari
44、es with the type of IRM. All precautions shall be taken to make IRMs as stable as possible.4.2.3 Packages shall be dispensed by the manufacturing or distribution 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 of the ma
45、nufacturer,4.2.3.3 Date of manufacture or preparation,4.2.3.4 Storage conditions, andTABLE 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)A AR value = accep
46、ted 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
47、IRM lot; UL-1 is higher uniformitythan UL-2.See Annex A3 and Annex A4 for more information.D4678 1534.2.3.5 Reference to ASTM research report for documentation of testing.4.2.4 For each test property measured to assess lot quality report the following:4.2.4.1 Accepted reference value,4.2.4.2 Test lo
48、t 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 same manner as for IRMs. Each CRM package shall be furnished with adocumentation sheet with the following information:4.3.1.1 Name and number of the CRM,
49、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 uniformity of the IRM lot to some selected limits and evaluate the test lot limits,and (2) to establish an accepted reference value for the lot and as a secondary goal to evaluate the between-laboratory limits forinterlaboratory testing of the IRM where this is applicable.5.2 Testing for Homogeneity:5.2.1 Homogeneity tes
