1.1本实施规程描述了基于实施规程D 6708统计原理的程序和方法，以验证总分析仪系统（或其子系统）产生的结果与旨在测量相同特性的独立测试方法产生的结果之间的一致程度是否符合用户规定的要求。这是一种基于性能的验证，将使用一组在开发所研究的两个测量系统之间的任何相关性时未事先使用的材料进行。独立试验方法的结果在本文中称为主要试验方法结果（PTMR）。 1.2本规程假设已将缓解分析仪系统和PTM之间系统偏差所需的任何相关性应用于分析仪结果。 1.3本规程要求对分析仪进行比较的主要方法和正在研究的分析仪系统进行统计控制。 应使用规程D 6299中描述的规程，以确保满足该条件。 1.4如果工艺流分析仪系统和主要试验方法基于相同的测量原理，或者如果工艺流分析仪系统使用与主要试验方法的测量原理类似的直接且易于理解的测量原理，则本规程适用。如果过程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PTMRs（见注释1中的情况1）。 1.5如果过程流分析仪系统使用间接或数学建模的测量原理，如化学计量学或多元分析技术，而化学计量学或多元模型开发需要PTMR，则本规程不适用。用户应参考实施规程D 6122了解这些类型分析仪系统的详细验证程序（见中的案例2）。 注释0 例如，对于火花点火燃料中苯的测量，基于试验方法D 6277的中红外过程分析仪系统与试验方法D 3606气相色谱一次试验方法的比较将被视为情况1，并且本规程将适用。对于每个样品，使用独立于主要测试方法（测试方法D 3606）的方法（测试方法D 6277）将中红外光谱转换为单个分析仪结果。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使用实施规程E 1655的方法测试方法D 3606参考值相关联时，视为情况2，实施规程D 6122适用。在本例2中，分析仪的直接输出是频谱，将该多变量输出转换为分析仪结果需要使用规程D 6122，因此它与主要测试方法无关。 1. 6性能验证是通过计算应用任何必要相关性后来自分析仪系统（或子系统）的结果与同一样本集的PTMR之间的差异的精度和偏差来进行的（此类结果在本文中称为预测的主要试验方法结果（PPTMR））。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分析仪系统应用的用户指定要求进行统计比较。 1.6.1对于产品放行或产品质量认证应用中使用的分析仪，一致程度的精度和偏差要求通常基于主要试验方法的现场或公布精度。 注释2 在这种类型的大多数应用中，PTM是引用规范的测试方法。 1.6.2本规程不描述为分析仪系统应用确定精度和偏差要求的程序。 此类要求必须基于结果对预期业务应用的重要性以及合同和监管要求。在启动本文所述的验证程序之前，用户必须确定精度和偏差要求。 1.7描述了两种验证程序:线性样品程序和验证标准物质（VRM）注射程序。 1.8本规程仅验证VRM注入点或线路样品提取点下游的分析仪系统或子系统。 1.9线路取样程序仅限于材料可以安全地从分析仪装置的取样点提取而不会显著改变相关特性的应用。 1.10本实施规程应用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。 1.11描述了两种类型的验证: 一般验证和级别特定验证。这些操作通常在安装时或在系统机械适用性确定后进行。 1.11.1一般验证基于实施规程D 6708的统计原则和方法。在大多数情况下，首选一般验证，但如果验证材料的变化不充分，则可能并不总是可行的。一般验证将在比级别特定验证更宽的操作范围内验证分析仪的操作。 1.11.2当可用验证材料的变化不足以满足实施规程D 6708的要求时，进行特定级别的验证，以验证分析仪在有限范围内的操作。 1.11.3验证结果仅在验证材料数据涵盖的范围内有效，来自多个不同验证（一般或特定级别）的验证材料数据可能组合用于一般验证。 1.12描述了持续验证系统性能的程序。这些程序通常以与应用的关键性相称的频率应用。 1.13本规程不涉及诊断验证失败原因的程序。 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和健康实践，并确定监管限制的适用性。

1.1 This practice describes procedures and methodologies based on the statistical principles of Practice D 6708 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). 1.2 This practice assumes any correlation necessary to mitigate systemic biases between the analyzer system and PTM have been applied to the analyzer results. 1.3 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 D 6299 should be used to ensure this condition is met. 1.4 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). 1.5 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 D 6122 for detailed validation procedures for these types of analyzer systems (see Case 2 in ). Note 0 For example, for the measurement of benzene in spark ignition fuels, comparison of a Mid-Infrared process analyzer system based on Test Method D 6277 to a Test Method D 3606 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 D 6277) that is independent of the primary test method (Test Method D 3606). However, when the same analyzer uses a multivariate model to correlate the measured Mid-Infrared spectrum to Test Method D 3606 reference values using the methodology of Practice E 1655, it is considered Case 2 and Practice D 6122 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 D 6122, hence it is not independent of the primary test method. 1.6 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. 1.6.1 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. 1.6.2 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. 1.7 Two procedures for validation are described: the line sample procedure and the validation reference material (VRM) injection procedure. 1.8 Only the analyzer system or subsystem downstream of the VRM injection point or the line sample extraction point is being validated by this practice. 1.9 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 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. 1.11 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. 1.11.1 General Validation is based on the statistical principles and methodology of Practice D 6708. 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. 1.11.2 When the variation in available validation materials is insufficient to satisfy the requirements of Practice D 6708, a Level Specific Validation is done to validate analyzer operation over a limited range. 1.11.3 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. 1.12 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. 1.13 This practice does not address procedures for diagnosing causes of validation failure. 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 and health practices and determine the applicability of regulatory limitations prior to use.