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Standard Guide for Carbon Black—Validation of Test Method Precision and Bias 碳黑验证标准指南测试方法精度和偏差
发布日期: 2020-11-01
1.1 本指南涵盖了使用ASTM标准参考黑的程序 2. (SRBs)和HT和INR碘值标准,以连续监测已确定参考值的炭黑试验方法的精度。它还提供了各种测试方法的故障排除指南。 1.2 本指南定义了在D24管辖范围内对这些测试方法执行炭黑测试活动的实验室所需的环境条件。 1.3 本指南建立了使用x图连续监测第节中所列测试的程序 2. 用于实验室内精度(重复性)和实验室间精度(再现性)。 1.4 本指南提供了一种统计程序,用于当实验室无法在本指南给出的范围内对其仪器进行物理校准以获得ASTM参考黑的参考值时,提高测试再现性。 1.5 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 本指南深入了解了实验室运行所需的环境条件,或帮助设计使用D24管辖范围内的测试方法进行炭黑测试活动的新实验室。本指南不取代实验室可能选择制定的任何具体要求。 4.2 本指南建议使用统计x图,以图形方式监测第节中给出的试验方法的ASTM参考黑度测定的试验数据 2. . 鼓励所有实验室使用统计x图和ASTM参考图,因为这可以比较实验室内和实验室之间的测试精度。 本指南描述了使用重复性和再现性极限和x图的实践。 4.3 除了通过物理化学方法校准测试方法外,还提出了一种用于实现测试方法校准的统计方法(即, 规范化 ). 4.4 测试精度差可能是由于重复性差或再现性差或两者兼而有之。原因可能包括操作员培训不足、设备或实验室环境维护不当、样品制备或分析技术变化、仪器缺乏校准或标准化、仪器磨损、试剂不符合规范、仪器或设备的不同来源以及材料异质性。 所有测试误差源的总和对于单个实验室来说是唯一的。 4.5 ASTM参考黑的精度数据见 表1- 3. . 其中包括标准参考黑(SRB)系列8、HT和INR碘标准。建议使用HT或INR碘标准监测碘测试。 (A) 炭黑的碘吸附数随着炭黑老化而降低。通常,表面积越大,变化速度越快。因此,由于这种老化效应,可能无法获得表1A中给出的目标值或平均值。应使用HT或INR碘标准及其参考值(见表2和表3)监测碘值测试。 参见第节 10 了解更多信息。 注1: 首选精度值以粗体显示 表1- 3. .
1.1 This guide covers procedures for using the ASTM Standard Reference Blacks 2 (SRBs) and the HT and INR Iodine Number Standards to continuously monitor the precision of those carbon black test methods for which reference values have been established. It also offers guidelines for troubleshooting various test methods. 1.2 This guide defines the environmental conditions that are required for laboratories that perform carbon black testing activities for those test methods under D24’s jurisdiction. 1.3 This guide establishes procedures for the use of x-charts to continuously monitor those tests listed in Section 2 for within-lab precision (repeatability) and between-lab accuracy (reproducibility). 1.4 This guide provides a statistical procedure for improving test reproducibility when a laboratory cannot physically calibrate its apparatus to obtain the reference values of the ASTM reference blacks, within the ranges given in this guide. 1.5 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 This guide provides insight into the environmental conditions required for operation of laboratories or to aid in the design of new laboratories that perform carbon black testing activities using those test methods that are under D24’s jurisdiction. This guide does not supersede any specific requirements a laboratory may choose to establish. 4.2 This guide recommends the use of statistical x-charts to graphically monitor test data determined for the ASTM reference blacks for those test methods given in Section 2 . All laboratories are encouraged to utilize statistical x-charts and ASTM reference blacks because this enables a comparison of testing precision within and between laboratories. The guide describes practices for the use of repeatability and reproducibility limits and x-charts. 4.3 In addition to the calibration of a test method by physicochemical means, a statistical method for achieving calibration of a test method is presented (that is, normalization ). 4.4 Poor test precision can be the result of poor repeatability or poor reproducibility or both. Causes may include inadequate operator training, improperly maintained equipment or laboratory environment, variation in sample preparation or analysis techniques, the lack of calibration or standardization of instrumentation, worn-out apparatus, reagents that do not meet specifications, different sources of instrumentation or equipment, and material heterogeneity. The sum of all sources of testing error is unique for an individual laboratory. 4.5 Precision data for ASTM Reference Blacks are found in Tables 1- 3 . These include standard reference blacks (SRB’s) Series 8, HT and INR Iodine Standards. The HT or INR Iodine standards are recommended for monitoring iodine testing. (A) The iodine adsorption number of carbon black has been shown to decrease in value as the carbon black ages. Generally, the higher the surface area the faster the rate of change. Therefore, the target or mean values given in Table 1A may not be obtained due to this aging effect. Iodine Number testing should be monitored using HT or INR iodine standards and their reference values found in Table 2 and Table 3. See Section 10 for additional information. Note 1: Preferred precision values are bolded in Tables 1- 3 .
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归口单位: D24.61
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