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现行 ASTM D4678-15a(2023)
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Standard Practice for Rubber—Preparation, Testing, Acceptance, Documentation, and Use of Reference Materials 橡胶标准实施规程——标准物质的制备、试验、验收、文件编制和使用
发布日期: 2023-11-01
1.1 本规程涵盖了全行业范围内用作参考材料的材料,这些材料对橡胶行业的产品、规范和开发测试至关重要。本规程描述了确保任何有感知需求的候选材料都能成为参考材料所需的步骤。该实践规定了关于这些材料的准备步骤、为允许验收任何候选材料而应进行的测试以及如何记录验收所需的文件以供未来使用和审查的建议。 1.2 此规程应由ASTM D11委员会管理。 1.2.1 本规程的重要部分如下: 部分 意义和用途 3. 工业标准物质的制备 4. 工业标准物质测试概述 5. IRM的化学和物理规范 6. 参考资料文件 7. 典型参考材料使用 8. IRM的建议包大小 附件A1 均匀性测试的推荐抽样计划 IRM的 附件A2 IRM同质性的测试计划与分析 附件A3 评估合格产品的测试计划和分析 参考值 附件A4 IRM测试的统计模型 附件A5 典型IRM的附件计算示例 附录X1 计算方差的双向分析 Sr 附录X2 1.3 本标准并不旨在解决与其使用相关的所有安全问题(如有)。本标准的使用者有责任在使用前制定适当的安全、健康和环境实践,并确定监管限制的适用性。 1.4 本国际标准是根据世界贸易组织技术性贸易壁垒委员会发布的《关于制定国际标准、指南和建议的原则的决定》中确立的国际公认的标准化原则制定的。 ====意义和用途====== 3.1 标准物质在橡胶行业的产品和规格测试、研发工作、技术服务工作和质量控制操作中至关重要。它们对于裁判来说尤其有价值。 3.2 标准物质(RM)的类别、类别和类型: 3.2.1 参考资料分为两类: 3.2.1.1 行业参考资料(IRM)-- 根据规定的生产工艺制备的材料,以产生统一的批次; 通过指定的测量程序来评估定义批次质量的参数。 3.2.1.2 通用参考资料(CRM)-- 已制备为尽可能均匀但不具有既定特性(参数)值的材料;公共或单一来源的知识对于某些不太关键的应用是足够的。 3.2.2 根据评估批次参数的方法和生成批次材料的生产过程,工业参考材料(IRM)被划分为额外的类别和类型。对此进行了更全面的解释(请参阅 附件A3 和 附件A4 有关第节中讨论的更多详细信息 3. ). 3.2.3 以下批次参数对于参考材料的使用非常重要: 3.2.3.1 接受参考值(AR值)-- 通过指定的测试程序建立的平均IRM属性或参数值。 3.2.3.2 试验批限值(TL限值)-- 这些限值定义为定义批次质量的特性或参数的整个批次的单个IRM测试结果标准偏差的±3倍;测量是在产生IRM的组织的实验室中进行的。 3.2.3.3 尽管中定义的限制 3.2.3.2 以标准偏差的±3倍给出,在评估批次均匀性时,拒绝将批次的单个部分视为异常值或非典型部分是基于适当标准偏差的?倍,即基于95 % 置信区间。看见 附件A3 和 附件A4 了解更多信息和评估程序。 3.2.4 所有IRM都有AR值和TL限值;然而,可以通过两种方式中的一种来获得AR值,以产生两类AR值中的一类: 3.2.4.1 全球应收账款价值-- 该AR值是从实验室间测试程序中获得的,其中“全局”一词表示许多实验室的平均值。 3.2.4.2 本地AR值-- 这是在一个实验室或一个地点获得的AR值,通常是负责制备均质批次的实验室。 3.2.5 一个额外的参数对于具有全局AR值的IRM很重要: 3.2.5.1 实验室限值之间(BL)-- 进行实验室间测试以确定AR值的实验室组不等同于使用通常±3标准偏差限值的工业生产操作的典型系统或群体。 这种生产操作是指已经清除了所有可分配的变异原因的系统,并且处于“统计控制”状态,只有无法消除的随机变异。因此,所有IRM的建议限值为±2标准偏差限值,适用于95 % 置信水平。如果出于完全合理的严重原因,需要±3个标准偏差限值,则可以使用这些限值,前提是提供完整的文件来证明限值的合理性。 3.2.6 批次的均匀性或均匀性决定了TL极限的大小,可以指定为两个不同水平的均匀性之一。决定均匀性水平的关键因素是混合IRM部分或组成批次的零件的能力,以确保混合过程中的高度均匀性。 不能混合的IRM将具有额外的残余变化量(部分到部分),从而降低均匀性水平。 3.2.6.1 均匀性等级1(UL-1)-- 这是通过使用 指定的测试 用于测量定义批次质量的参数;它是通过使用混合材料获得的,被称为类型 B ( B = 混合)IRM。 3.2.6.2 均匀性等级2(UL-2)-- 这是通过使用 指定的测试 用于测量定义批次质量的参数;它通常用于非混合材料,被称为类型 NB (未混合)IRM。 3.3 IRM在技术领域有许多应用,如中所述 3.1 . 3.3.1 单个实验室自我评估-- IRM可以在给定的实验室(或与给定的测试系统)中使用,以将实验室内的测试结果与IRM的可接受参考值进行比较。IRM也可用于内部统计质量控制(SQC)操作。 3.3.2 多实验室评估-- IRM可在两个或多个实验室之间使用,以确定实验室中的测试系统是否在选定的控制范围内运行。 3.3.3 一种或多种IRM可用于制备用于评估化合物测试和性能中的非参考材料的化合物。 3.3.4 参考液体IRM可用于各种候选化合物或其他参考化合物的浸渍测试。由于浸没液体对橡胶化合物的有害影响,这种浸没测试是重要的。 3.3.5 IRM也可用于消除被称为“测试偏差”的实验室间测试变化:两个(或多个)实验室之间的差异,对于给定的测试性能水平,无论测试比较的时间如何,在实验室之间基本上是恒定的。在这样的应用中,差分测试测量值(IRM − 实验材料),成为校正的测试结果;该校正值被用作性能的测量,而不是感兴趣的实验材料的“实测”测试值。 3.4 平均值在该实践中的各种操作和决策中发挥着重要作用。在这种做法中,“平均数”被定义为算术平均数。 3.5 IRM和CRM的各种特征(类别、类别、类型)在中以摘要形式列出 表1 . (A) AR值  =  可接受的参考值。 TL限值  =  测试批次限制。 全球的  =  从实验室间试验程序中获得的AR值。 地方的  =  从一个实验室获得的AR值。 B类  =  已混合以确保高度一致性的IRM。 NB型  =  不能混合的IRM。 UL-1和UL-2  =  IRM批次的一致性水平;UL-1的均匀性高于UL-2。 看见 附件A3 和 附件A4 了解更多信息。 3.6 这一做法及其所描述的IRM计划是为了取代美国国家标准与技术研究所(NIST)于1948年开始实施的标准化计划而制定的,该计划已被逐步淘汰。 3.7 对于最终将成为IRM的各种材料,将所有必要的规范、制备模式、采样和测试协议写入该实践是不可行的。 因此,发布此实践是为了提供IRM的一般指南。 3.8 D11.20小组委员会内的常设IRM指导委员会应由D11.90小组委员会组成,以协助利用这一做法,并在必要时就IRM的准备和管理做出技术决策和政策决策。
1.1 This practice covers materials used on an industry-wide basis as reference materials, which are vitally important to conduct product, specification, and development testing in the rubber industry. This practice describes the steps necessary to ensure that any candidate material, that has a perceived need, can become a Reference Material. The practice sets forth the recommendations on the preparation 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 sections of this practice are as follows: Section Significance and Use 3 Preparation of Industry Reference Materials 4 Overview of Industry Reference Material Testing 5 Chemical and Physical Specifications for IRM 6 Reference Material Documentation 7 Typical Reference Material Use 8 Recommended Package Size for IRM Annex A1 Recommended Sampling Plans for Homogeneity Testing of an IRM Annex A2 Test Plan and Analysis for Homogeneity of an IRM Annex A3 Test Plan and Analysis to Evaluate an Accepted Reference Value Annex A4 Statistical Model(s) for IRM Testing Annex A5 Example of Annex Calculations for a Typical IRM Appendix X1 Two-Way Analysis of Variance for Calculating Sr Appendix X2 1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. 1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee. ====== Significance And Use ====== 3.1 Reference materials are vitally important in product and specification testing, in research and development work, in technical service work, and in quality control operations in the rubber industry. They are especially valuable 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)— Materials that have been prepared according to a specified production process to generate 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 not have established property (parameter) values; the knowledge of a common or single source is sufficient for certain less critical applications. 3.2.2 Industry reference materials (IRMs) are divided into additional classes and types according to the method of evaluating the lot parameters and according to the production process for generating the lot material. These are explained more fully (refer to 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 by way of a specified test program. 3.2.3.2 Test Lot Limits (TL Limits)— These are limits defined as ±3 times the standard deviation of individual IRM test results across the entire lot for the property or parameter(s) that defines lot quality; the measurements are conducted in the laboratory of the organization producing the IRM. 3.2.3.3 Although the limits as defined in 3.2.3.2 are given in terms of ±3 times the standard deviation, the rejection of individual portions of the lot as being outlier or non-typical portions in assessing the homogeneity of the lot is done on the basis of ±2 times the appropriate standard deviation, that is, on the basis of a 95 % confidence interval. See Annex A3 and Annex A4 for more information 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 one of two classes of AR values: 3.2.4.1 Global AR Value— This AR value is obtained from an interlaboratory test program where the word “global” indicates an average value across many laboratories. 3.2.4.2 Local AR Value— This is an AR value obtained in one laboratory or at one location, usually the laboratory responsible for preparation 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 an AR-value are not equivalent to a system or population typical of industrial production operations that use the usual ±3 standard deviation limits. Such production operations are systems that have been purged of all assignable causes of variation and are in a state of ‘statistical control’ with only random variations that cannot be removed. Thus, the recommended limits on all IRMs are the ±2 standard deviation limits that pertain to a 95 % confidence level. If for serious reasons that can be totally justified, ±3 standard deviation limits are required, these may be used provided that full and complete documentation is supplied to justify the limits. 3.2.6 The homogeneity or uniformity of the lot, which determines the magnitude of the TL limits, may be designated as one of two different levels of uniformity. The key factor that determines the level of uniformity is the capability of blending the IRM portions or parts that constitute the lot, to ensure a high degree of uniformity from the blending process. IRMs that cannot be blended 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 use of a specified test for measuring the parameter that defines lot quality; it is obtained by the use of a blended material and is referred to 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 of a specified test for measuring the parameter 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 Evaluation— The IRM may be used in a given laboratory (or with a given test system) to compare the test results within the laboratory to the accepted reference value for the IRM. An IRM can also be used for internal statistical quality control (SQC) operations. 3.3.2 Multi-Laboratory Evaluation— The IRM may be used between two or more laboratories to determine if the test systems in 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 in compound testing and performance. 3.3.4 Reference liquid IRMs may be used for immersion testing of various candidate or other reference compounds. Such immersion 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 (or more) laboratories that is essentially constant between the laboratories for a given test property level, irrespective of the time of the test comparisons. In such applications a differential test measurement value, (IRM − experimental material), becomes a corrected test result; this corrected value is used as the measure of performance rather than the “as-measured” test value on the experimental material of interest. 3.4 Average values play an important role in various operations and decisions in this practice. For this practice, “average” is defined as the arithmetic mean. 3.5 The various characteristics of IRMs and CRMs (categories, classes, types) are listed in summary form in Table 1 . (A) AR 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 blended. UL-1 and UL-2  =  levels of uniformity in the IRM lot; UL-1 is higher uniformity than UL-2. See Annex A3 and Annex A4 for more information. 3.6 This practice and the IRM program it describes was developed to replace a standardization program conducted by the National Institute of Standards and Technology (NIST) that began in 1948 and has been phased out. 3.7 It is not feasible to write into this practice all the necessary specifications, modes of preparation, sampling, and testing protocols, for the wide variety of materials that will eventually become IRM. Therefore this practice is published to give general guidelines for IRMs. 3.8 A permanent IRM Steering Committee within Subcommittee D11.20 shall be constituted by Subcommittee D11.90 to assist in the utilization of this practice and to make technical and, where required, policy decisions regarding the preparation and administration of IRM.
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归口单位: D11.20
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