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Standard Practice for Evaluating Precision for Test Method Standards in the Rubber and Carbon Black Manufacturing Industries 橡胶和炭黑制造业试验方法标准精度评定的标准实施规程
发布日期: 2020-06-01
1.1 本规程涵盖精度评估指南,并作为实验室间测试程序(ITP)的管理规程,用于评估橡胶制造和炭黑行业中使用的测试方法的精度。本实践使用了基本的单向方差分析实践计算算法 E691 . 虽然在本实践中未评估偏差,但它是理解精度评估的一个基本概念。 1.2 本规程适用于试验结果以定量连续变量表示的试验方法。 尽管可能会出现例外情况,但通常仅限于在许多实验室中充分开发和常规使用的测试方法。 1.3 给出了两种精度评估方法,描述如下: 稳健统计 试图消除或大幅减少异常值影响的程序。第一个是 一般精度 该程序适用于橡胶制造业的所有试验方法,第二个是一般精度程序的具体变体,指定为 特殊精度 ,这适用于炭黑测试。这两种程序使用相同的均匀水平实验设计和Mandel h 和 k 统计数据以审查精度数据库中的潜在异常值。然而,他们在拒绝不兼容数据值作为异常值的过程中使用了轻微修改。这个 特殊精度 程序针对每个数据库单元或材料实验室组合的复制次数而定。 1.4 本规程分为以下几节: 部分 范围 1. 参考文件 2. 术语 3. 意义和用途 4. 精度评定一般精度和特殊精度 5. 组织实验室间测试计划(ITP)的步骤 6. 一般精度分析程序概述 7. 一般精度:分析步骤1 8. 初步图形数据审查 8.1 原始数据库的精度计算 8.2 在5时检测异常值 % 显著性水平使用 h 和 k 统计数字 8.3 生成 修订版1 使用离群值处理选项1或2的数据库 8.4 一般精度:分析步骤2 9 精度计算 修订版1 数据库 9.1 检测2处的异常值 % 显著性水平使用 h 和 k 统计数字 9.1 生成 修订版2 使用离群值处理选项1或2的数据库 9.1.2 一般精度:分析步骤3 10 使用计算精度 修订版2 数据库 10.1 特殊精度分析炭黑测试 11 试验方法标准中精度表和条款的格式 12 准备精度分析报告 13 与精度和测试有关的选定术语的定义 附件A1 实验室间测试程序的统计模型 附件A2 计算 h 和 k 异常值的一致性统计 附件A3 电子表格计算公式、表格布局和计算顺序 附件A4 计算已删除异常值的替换值的程序 附件A5 通用精度评估示例穆尼粘度测试 附录A6 1.5 提出了六个附件;这些是对本实践主体的补充。 附录A1和 附件A2 主要作为背景信息提供,这对于全面理解精度评估非常重要。 附件A3– 附件A5 包含执行实践中各部分要求的操作所需的详细说明和程序。以这种身份使用这些附件可以避免本实践主体中涉及的长节说明。这样可以更好地表示和理解精度评估中涉及的核心概念。 附录A6 也是重要的;它给出了精度评估的完整示例,说明了任何精度评估中可能遇到的所有程序和选项,从简单到最复杂。 1.6 本标准并非旨在解决与其使用相关的所有安全问题(如有)。本标准的用户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。 1.7 本国际标准是根据世界贸易组织技术性贸易壁垒(TBT)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》中确立的国际公认标准化原则制定的。 ====意义和用途====== 4.1 测试使用标准测试方法进行,以生成用于商业、技术和科学目的决策的测试数据。 因此,特定测试方法的精度是测试方法和决策过程的重要质量特征或优值。 4.2 测试方法的精度评估通常通过以下方式进行:( 1. )一些选定的材料组通常与该方法一起使用,以及( 2. )与一组具有测试方法经验的志愿者实验室合作。评估代表了 及时的事件 这些材料和实验室的试验方法。 使用稍有不同的材料或甚至在不同时间使用相同实验室的相同材料进行ITP精度评估,可能会产生不同于初始ITP的精度结果。 4.3 经验如参考文献所示 ( 1- 4. ) 4. 其他地方的研究表明,典型ITP的实验室间再现性差几乎总是由于实验室间的偏见。在所有测试中,与参考实验室以及其他实验室相比,某些实验室总是低或高。 许多ITP的这一常见结果在本实践中通过使用第节所述的三步稳健分析程序来解决 7. . 4.4 在将特定测试方法的精度结果应用于消费品-生产者产品验收的产品测试时应谨慎。产品验收程序应基于在特定于商业产品和此类测试相关方实验室的特殊程序中获得的精度数据制定。
1.1 This practice covers guidelines for evaluating precision and serves as the governing practice for interlaboratory test programs (ITP) used to evaluate precision for test methods as used in the rubber manufacturing and the carbon black industries. This practice uses the basic one way analysis of variance calculation algorithms of Practice E691 . Although bias is not evaluated in this practice, it is an essential concept in understanding precision evaluation. 1.2 This practice applies to test methods that have test results expressed in terms of a quantitative continuous variable. Although exceptions may occur, it is in general limited to test methods that are fully developed and in routine use in a number of laboratories. 1.3 Two precision evaluation methods are given that are described as robust statistical procedures that attempt to eliminate or substantially decrease the influence of outliers. The first is a General Precision procedure intended for all test methods in the rubber manufacturing industry, and the second is a specific variation of the general precision procedure designated as Special Precision , that applies to carbon black testing. Both of these procedures use the same uniform level experimental design and the Mandel h and k statistics to review the precision database for potential outliers. However, they use slight modifications in the procedure for rejecting incompatible data values as outliers. The Special Precision procedure is specific as to the number of replicates per database cell or material-laboratory combination. 1.4 This practice is divided into the following sections: Section Scope 1 Referenced Documents 2 Terminology 3 Significance and Use 4 Precision Evaluation—General Precision and Special Precision 5 Steps in Organizing an Interlaboratory Test Program (ITP) 6 Overview of the General Precision Analysis Procedure 7 General Precision: Analysis Step 1 8 Preliminary Graphical Data Review 8.1 Calculation of Precision for Original Database 8.2 Detection of Outliers at 5 % Significance Level Using h and k Statistics 8.3 Generation of Revision 1 Database Using Outlier Treatment Option 1 or 2 8.4 General Precision: Analysis Step 2 9 Calculation of Precision for Revision 1 Database 9.1 Detection of Outliers at 2 % Significance Level Using h and k Statistics 9.1 Generation of Revision 2 Database Using Outlier Treatment Option 1 or 2 9.1.2 General Precision: Analysis Step 3 10 Calculation of Precision Using Revision 2 Database 10.1 Special Precision Analysis—Carbon Black Testing 11 Format for Precision Table and Clause in Test Method Standards 12 Preparation of Report for Precision Analysis 13 Definitions for Selected Terms Concerned with Precision and Testing Annex A1 Statistical Model for Interlaboratory Testing Programs Annex A2 Calculating the h and k Consistency Statistics for Outliers Annex A3 Spreadsheet Calculation Formulas, Table Layout, and Calculation Sequence Annex A4 Procedure for Calculating Replacement Values of Deleted Outliers Annex A5 Example of General Precision Evaluation—Mooney Viscosity Testing Annex A6 1.5 Six annexes are presented; these serve as supplements to the main body of this practice. Annex A1 and Annex A2 are given mainly as background information that is important for a full understanding of precision evaluation. Annex A3 – Annex A5 contain detailed instructions and procedures needed to perform the operations as called for in various parts of the practice. The use of these annexes in this capacity avoids long sections of involved instruction in the main body of this practice. This allows for a better presentation and understanding of the central concepts involved in the evaluation of precision. Annex A6 is also important; it gives a complete example of precision evaluation that illustrates all of the procedures and options likely to be encountered in any precision evaluation, from the simple to the most complex. 1.6 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. 1.7 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 ====== 4.1 Tests are conducted using standard test methods to generate test data that are used to make decisions for commercial, technical, and scientific purposes. It follows that the precision of a particular test method is an important quality characteristic or figure of merit for a test method and a decision process. 4.2 An evaluation of the precision of a test method is normally conducted with ( 1 ) some selected group of materials as typically used with that method and ( 2 ) with a group of volunteer laboratories that have experience with the test method. The evaluation represents an event in time for the test method for these materials and laboratories. Another ITP precision evaluation with somewhat different materials or even with the same materials with the same laboratories at a different time, may generate precision results that differ from the initial ITP. 4.3 Experience as indicated in Refs ( 1- 4 ) 4 and elsewhere has shown that the poor reproducibility among the laboratories of a typical ITP is almost always due to interlaboratory bias. Certain laboratories are always low or high compared to a reference as well as other laboratories in all tests. This usual outcome for many ITPs is addressed in this practice by the use of the three-step robust analysis procedures as described in Section 7 . 4.4 Caution is urged in applying precision results of a particular test method to product testing for consumer-producer product acceptance. Product acceptance procedures should be developed on the basis of precision data obtained in special programs that are specific to the commercial products and to the laboratories of the interested parties for this type of testing.
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归口单位: D11.16
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