1.1 本规程描述了基于《规程》统计原则的程序和方法 D6708 验证总分析仪系统（或其子系统）产生的结果与旨在测量相同性质的独立测试方法产生的结果之间的一致程度是否满足用户指定的要求。这是一种基于性能的验证，将使用一组材料进行，这些材料在开发所调查的两个测量系统之间的任何相关性时都没有先验使用。独立测试方法的结果在本文中被称为主要测试方法结果（PTMR）。 1.1.1 中描述的一致程度 1.1 可以用于在相同材料上测量的PPTMR和PTMR，也可以用于在恒定水平添加后在基料上测量的PPSMR和在这些相同基料上测得的PTMR。 1.1.2 在某些情况下，采用两步程序。在第一步中，将分析仪和PTM应用于相同混合料材料的测量。如果步骤1中使用的分析仪是多元分光光度分析仪，则实践 D6122 用于访问用于该第一步骤的PPTMR和PTMR之间的协议。否则，此做法用于将PPTMR与针对该混合料测量的PTMR进行比较，以确定一致程度。在第二步骤中，将步骤1中产生的PPTMR用作第二模型的输入，该第二模型预测当PTM应用于最终混合产品的分析时获得的结果。由于第二步不使用分析仪读数，因此第二步的验证是独立完成的。步骤2仅对有效的步骤1结果执行。请注意，第二个模型可能会为混合料添加不同级别或多种材料。 1.2 本规程假定，缓解分析仪系统和PTM之间系统偏差所需的任何相关性已应用于分析仪结果。请参阅指南 D7235 用于建立这种相关性的程序。 1.3 该实践假设所采用的任何建模技术都具有必要的调整，以减轻分析仪之间的系统偏差。PPTMR和PTMR已应用于模型结果。此实践不包括模型形式和调整，仅包括模型输出的验证。 1.4 该实践要求，与分析仪进行比较的主要方法和正在调查的分析仪系统都处于统计控制中。实践中描述的实践 D6299 应用于确保满足此条件。 1.5 如果工艺流分析仪系统和主要测试方法基于相同的测量原理，或者如果工艺流分析器系统使用直接且良好的- 理解的测量原理与主要测试方法的测量原理相似。如果工艺流分析仪系统使用与主要测试方法不同的测量技术，则本规程也适用，前提是分析仪直接输出的校准协议不需要使用PTMR（见 注1 )。 1.6 如果工艺流分析仪系统利用间接或数学建模的测量原理，如化学计量或多元分析技术，其中化学计量或多变量模型开发需要PTMR，则该实践不适用。用户应参考实践 D6122 有关这些类型分析仪系统的详细验证程序（请参阅 注1 )。 注1: 例如，对于火花点火式燃料中苯的测量- 基于测试方法的红外过程分析仪系统 D6277 测试方法 D3606 气相色谱法的主要测试方法将被视为案例1，该实践将适用。对于每个样品，使用方法将中红外光谱转换为单个分析仪结果（测试方法 D6277 )独立于主要测试方法（测试方法 D3606 )。然而，当同一分析仪使用多变量模型将测量的中红外光谱与测试方法相关联时 D3606 使用实践方法论的参考值 D8321 ，它被认为是案例2和实践 D6122 适用。在这种情况2的例子中，分析器的直接输出是频谱，并且将该多变量输出转换为分析器结果需要使用实践 D6122 ，因此它并不独立于主要测试方法。 1.7 性能验证是通过计算在应用任何必要的相关性后来自分析系统（或子系统）的结果之间的差异的精度和偏差来进行的（这些结果在本文中被称为预测的主要测试方法结果（PPTMR）），与同一样本集的PTMR相比。计算中使用的结果适用于相关性开发中未使用的样本。将计算的精度和偏差与用户指定的分析仪系统应用要求进行统计比较。 1.7.1 对于产品发布或产品质量认证申请中使用的分析仪，一致度的精度和偏差要求通常基于主要测试方法的现场或公布精度。 注2: 在大多数此类应用中，PTM是规范- 引用的试验方法。 1.7.2 本规程未描述分析仪系统应用的精度和偏差要求的制定程序。此类要求必须基于结果对预期业务应用程序的关键性以及合同和监管要求。用户必须在启动本文所述的验证程序之前确定精度和偏差要求。 1.8 描述了两种验证程序:线样品程序和验证参考物质（VRM）注射程序。 1.9 只有VRM注入点或线样本提取点下游的分析仪系统或子系统通过该实践进行验证。 1.10 线性采样程序仅限于可以安全地从分析仪单元的采样点提取材料而不会显著改变感兴趣的性质的应用。 1.10.1 当验证针对( 2b )材料，包括对材料进行额外处理的效果。 1.11 在应用本规程过程中获得的验证信息仅适用于用于进行验证的材料的类型和性能范围。 1.12 描述了两种类型的验证:一般验证和级别特定验证。这些通常在安装时或在系统机械适用性确定后进行主要维护。 1.12.1 一般验证基于统计原理和实践方法 D6708 在大多数情况下，一般验证是首选，但如果验证材料的变化不充分，则可能并不总是可行的。一般验证将在比特定级别验证更宽的操作范围内验证分析仪的操作。 1.12.2 当可用验证材料的变化不足以满足实践要求时 D6708 ，进行特定级别验证，以验证分析仪在有限范围内的操作。 1.12.3 验证结果仅在验证材料所涵盖的范围内有效。来自几种不同验证（一般或特定级别）的数据可能会组合用于一般验证。 1.13 描述了系统性能的持续验证程序。这些程序通常以与应用程序的关键性相称的频率应用。 1.14 本规程不涉及验证失败原因的诊断程序。 1.15 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。 1.16 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====== 5.1 该实践可用于量化工艺流分析仪系统或其子系统相对于感兴趣性质的主要测试方法的精度和偏差的性能。 5.2 该实践为工艺流分析仪系统的开发人员或制造商提供了有用的程序，用于评估新设计的工业应用系统的能力，这些工业应用需要通过流动部件或产品的主要测试方法对特定特性的测量进行可靠预测。 5.3 该实践为工艺流分析仪系统的购买者提供了一些可靠的选择，用于在调试时指定工艺流分析仪的验收测试要求，以确保系统能够以适当的精度或偏差规格或两者兼有的方式进行所需的性能测量。 5.4 如果实际的主要测试方法是在经过验证的性能范围和类型内的材料上进行的，则根据本规程验证的分析仪系统的PPTMR可用于以指定的置信度预测PTMR在指定的公差范围内。 5.5 该实践为工艺流分析仪系统的用户提供了来自正在进行的质量控制图的有用信息，以监测δ随时间的变化，并及时触发分析仪系统和主要测试方法之间的相关性更新。 5.6 在应用本规程过程中获得的验证信息仅适用于用于进行验证的材料的材料类型和性能范围。样品的性质水平和组成特征的选择必须适合分析仪系统的应用。这种做法允许用户为分析仪系统编写一份全面的验证声明，包括验证应用范围的具体限制。本规程不建议将验证结果外推到用于获得这些结果的材料类型和性能范围之外。此外，提醒用户，对于显示基质依赖性的测量系统，从纯化合物或纯化合物的简单混合物中确定的偏差信息可能不能代表在实际工艺或产品样品中获得的偏差信息。

1.1 This practice describes procedures and methodologies based on the statistical principles of Practice D6708 to validate whether the degree of agreement between the results produced by a total analyzer system (or its subsystem), versus the results produced by an independent test method that purports to measure the same property, meets user-specified requirements. This is a performance-based validation, to be conducted using a set of materials that are not used a priori in the development of any correlation between the two measurement systems under investigation. A result from the independent test method is herein referred to as a Primary Test Method Result (PTMR). 1.1.1 The degree of agreement described in 1.1 can be either for PPTMRs and PTMRs measured on the same materials, or for PPTMRs measured on basestocks and PTMRs measured on these same basestocks after constant level additivation. 1.1.2 In some cases, a two-step procedure is employed. In the first step, the analyzer and PTM are applied to the measurement of the same blendstock material. If the analyzer employed in Step 1 is a multivariate spectrophotometric analyzer, then Practice D6122 is used to access the agreement between the PPTMRs and the PTMRs for this first step. Otherwise, this practice is used to compare the PPTMRs to the PTMRs measured for this blendstock to determine the degree of agreement. In a second step, the PPTMRs produced in Step 1 are used as inputs to a second model that predicts the results obtained when the PTM is applied to the analysis of the finished blended product. Since this second step does not use analyzer readings, the validation of the second step is done independently. Step 2 is only performed on valid Step 1 results. Note that the second model might accommodate variable levels or multiple material additions to the blendstock. 1.2 This practice assumes any correlation necessary to mitigate systemic biases between the analyzer system and PTM have been applied to the analyzer results. See Guide D7235 for procedures for establishing such correlations. 1.3 This practice assumes any modeling techniques employed have the necessary tuning to mitigate systemic biases between the analyzer PPTMR and PTMR have been applied to the model results. Model form and tuning is not covered by this practice, only the validation of the model output. 1.4 This practice requires that both the primary method against which the analyzer is compared to, and the analyzer system under investigation, are in statistical control. Practices described in Practice D6299 should be used to ensure this condition is met. 1.5 This practice applies if the process stream analyzer system and the primary test method are based on the same measurement principle(s), or, if the process stream analyzer system uses a direct and well-understood measurement principle that is similar to the measurement principle of the primary test method. This practice also applies if the process stream analyzer system uses a different measurement technology from the primary test method, provided that the calibration protocol for the direct output of the analyzer does not require use of the PTMRs (see Case 1 in Note 1 ). 1.6 This practice does not apply if the process stream analyzer system utilizes an indirect or mathematically modeled measurement principle such as chemometric or multivariate analysis techniques where PTMRs are required for the chemometric or multivariate model development. Users should refer to Practice D6122 for detailed validation procedures for these types of analyzer systems (see Case 2 in Note 1 ). Note 1: For example, for the measurement of benzene in spark ignition fuels, comparison of a Mid-Infrared process analyzer system based on Test Method D6277 to a Test Method D3606 gas chromatography primary test method would be considered Case 1, and this practice would apply. For each sample, the Mid-Infrared spectrum is converted into a single analyzer result using methodology (Test Method D6277 ) that is independent of the primary test method (Test Method D3606 ). However, when the same analyzer uses a multivariate model to correlate the measured Mid-Infrared spectrum to Test Method D3606 reference values using the methodology of Practice D8321 , it is considered Case 2 and Practice D6122 applies. In this case 2 example, the direct output of the analyzer is the spectrum, and the conversion of this multivariate output to an analyzer result require use of Practice D6122 , hence it is not independent of the primary test method. 1.7 Performance Validation is conducted by calculating the precision and bias of the differences between results from the analyzer system (or subsystem) after the application of any necessary correlation, (such results are herein referred to as Predicted Primary Test Method Results (PPTMRs)), versus the PTMRs for the same sample set. Results used in the calculation are for samples that are not used in the development of the correlation. The calculated precision and bias are statistically compared to user-specified requirements for the analyzer system application. 1.7.1 For analyzers used in product release or product quality certification applications, the precision and bias requirement for the degree of agreement are typically based on the site or published precision of the Primary Test Method. Note 2: In most applications of this type, the PTM is the specification-cited test method. 1.7.2 This practice does not describe procedures for establishing precision and bias requirements for analyzer system applications. Such requirements must be based on the criticality of the results to the intended business application and on contractual and regulatory requirements. The user must establish precision and bias requirements prior to initiating the validation procedures described herein. 1.8 Two procedures for validation are described: the line sample procedure and the validation reference material (VRM) injection procedure. 1.9 Only the analyzer system or subsystem downstream of the VRM injection point or the line sample extraction point is being validated by this practice. 1.10 The line sample procedure is limited to applications where material can be safely withdrawn from the sampling point of the analyzer unit without significantly altering the property of interest. 1.10.1 The line sample procedure is the primary option for when the validation is for ( 2b ) materials including effect from additional treatment to the material. 1.11 Validation information obtained in the application of this practice is applicable only to the type and property range of the materials used to perform the validation. 1.12 Two types of validation are described: General Validation, and Level Specific Validation. These are typically conducted at installation or after major maintenance once the system mechanical fitness-for-use has been established. 1.12.1 General Validation is based on the statistical principles and methodology of Practice D6708 . In most cases, General Validation is preferred, but may not always be possible if the variation in validation materials is insufficient. General Validation will validate analyzer operation over a wider operating range than Level Specific Validation. 1.12.2 When the variation in available validation materials is insufficient to satisfy the requirements of Practice D6708 , a Level Specific Validation is done to validate analyzer operation over a limited range. 1.12.3 The validation outcome are considered valid only within the range covered by the validation material Data from several different Validations (general or level-specific) can potentially be combined for use in a General Validation. 1.13 Procedures for the continual validation of system performance are described. These procedures are typically applied at a frequency commensurate with the criticality of the application. 1.14 This practice does not address procedures for diagnosing causes of validation failure. 1.15 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. 1.16 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 ====== 5.1 This practice can be used to quantify the performance of a process stream analyzer system or its subsystem in terms of precision and bias relative to those of a primary test method for the property of interest. 5.2 This practice provides developers or manufacturers of process stream analyzer systems with useful procedures for evaluating the capability of newly designed systems for industrial applications that require reliable prediction of measurements of a specific property by a primary test method of a flowing component or product. 5.3 This practice provides purchasers of process stream analyzer systems with some reliable options for specifying acceptance test requirements for process stream analyzer systems at the time of commissioning to ensure the system is capable of making the desired property measurement with the appropriate precision or bias specifications, or both. 5.4 PPTMR from Analyzer Systems validated in accordance with this practice can be used to predict, with a specified confidence, what the PTMR would be, to within a specified tolerance, if the actual primary test method was conducted on the materials that are within the validated property range and type. 5.5 This practice provides the user of a process stream analyzer system with useful information from on-going quality control charts to monitor the variation in δ over time, and trigger update of correlation relationship between the analyzer system and primary test method in a timely manner. 5.6 Validation information obtained in the application of this practice is applicable only to the material type and property range of the materials used to perform the validation. Selection of the property levels and the compositional characteristics of the samples must be suitable for the application of the analyzer system. This practice allows the user to write a comprehensive validation statement for the analyzer system including specific limits for the validated range of application. This practice does not recommend extrapolation of validation results beyond the material type and property range used to obtain these results. In addition, users are cautioned that for measurement systems that show matrix dependencies, bias information determined from pure compounds or simple mixtures of pure compounds may not be representative of that achieved on actual process or product samples.