1.1 本规程涉及用于测定材料物理和化学特性的光谱仪和分光光度计的多元校准。在实践中对一般多元分析进行了详细描述 E1655 . 本标准仅适用于替代混合物可用于建立合适校准矩阵的情况。本规程规定了使用不完全符合规程的替代校准技术的标准试验方法的实验室间研究（ILS）的校准和鉴定数据集要求，即round robins E1655 . 注1: 对于一些多变量光谱分析，干扰和基质效应足够小，因此可以使用含有比最终分析的样品少得多的化学成分的混合物进行校准。而这些替代方法通常使用实践中描述的多元数学 E1655 ，它们不符合其中描述的程序，特别是关于异常值的处理。 1.2 本规程规定了如何处理ILS数据，以建立光谱仪/分光光度计性能鉴定要求，并将其纳入标准试验方法。 注2: 光谱仪/分光光度计鉴定程序旨在允许用户确定特定光谱仪/分光光度计的性能是否足以进行分析，以获得与公布的测试方法精度一致的结果。 1.2.1 替代测试方法中使用的光谱仪包括但不限于中红外和近红外、紫外/可见光、荧光和拉曼光谱仪。 1.2.2 本实践中涵盖的替代校准包括:多线性回归（MLR）、主成分回归（PCR）或偏最小二乘（PLS）数学。实践中详细描述了这些校准程序 E1655 . 1.3 对于替代试验方法，本规程建议对试验方法中允许的校准选项施加限制。具体而言，本规程建议测试方法开发人员证明测试方法中允许的所有校准都会产生统计上无法区分的结果。 1.4 对于参考光谱仪/分光光度计性能实践的替代测试方法，例如实践 E275 , E925 , E932 , E958 , E1421 , E1683 或 E1944年 ; 试验方法 E387 , E388 或 E579元 ; 或指南 E1866 ，本规程建议收集仪器性能数据，作为ILS的一部分，以建立光谱仪/分光光度计性能与测试方法精度之间的关系。 ====意义和用途====== 5.1 采用替代校准的标准测试方法的开发人员应使用本规程。 5.1.1 本规程有助于测试方法开发人员设置和记录可执行测试方法的光谱仪/分光光度计的要求。 5.1.2 本规程帮助测试方法开发人员设置和记录测试方法的光谱数据收集和计算参数。 5.1.3 本规程有助于测试方法开发人员在可能的多元分析程序中进行选择，这些程序可用于建立替代校准。本规程描述了应进行的统计测试，以确保测试方法范围内允许的所有多元分析程序产生统计上无法区分的结果。 5.1.4 本规程描述了测试方法开发人员应对校准和鉴定数据进行的统计计算，这些数据应作为建立测试方法精度的ILS的一部分收集。这些计算确定了光谱仪/分光光度计必须满足的性能水平，以便执行测试方法。 5.2 本规程描述了校准光谱仪/分光光度计的人员如何测试所述光谱仪/分光光度计的性能，以确定性能是否足以进行测试方法。 5.3 本规程描述了光谱仪/分光光度计的用户如何使光谱仪/分光光度计有资格进行试验方法。

1.1 This practice relates to the multivariate calibration of spectrometers and spectrophotometers used in determining the physical and chemical characteristics of materials. A detailed description of general multivariate analysis is given in Practices E1655 . This standard refers only to those instances where surrogate mixtures can be used to establish a suitable calibration matrix. This practice specifies calibration and qualification data set requirements for interlaboratory studies (ILSs), that is, round robins, of standard test methods employing surrogate calibration techniques that do not conform exactly to Practices E1655 . Note 1: For some multivariate spectroscopic analyses, interferences and matrix effects are sufficiently small that it is possible to calibrate using mixtures that contain substantially fewer chemical components than the samples that will ultimately be analyzed. While these surrogate methods generally make use of the multivariate mathematics described in Practices E1655 , they do not conform to procedures described therein, specifically with respect to the handling of outliers. 1.2 This practice specifies how the ILS data is treated to establish spectrometer/spectrophotometer performance qualification requirements to be incorporated into standard test methods. Note 2: Spectrometer/spectrophotometer qualification procedures are intended to allow the user to determine if the performance of a specific spectrometer/spectrophotometer is adequate to conduct the analysis so as to obtain results consistent with the published test method precision. 1.2.1 The spectroscopies used in the surrogate test methods would include but not be limited to mid- and near-infrared, ultraviolet/visible, fluorescence and Raman spectroscopies. 1.2.2 The surrogate calibrations covered in this practice are: multilinear regression (MLR), principal components regression (PCR) or partial least squares (PLS) mathematics. These calibration procedures are described in detail in Practices E1655 . 1.3 For surrogate test methods, this practice recommends limitations that should be placed on calibration options that are allowed in the test method. Specifically, this practice recommends that the test method developer demonstrate that all calibrations that are allowed in the test method produce statistically indistinguishable results. 1.4 For surrogate test methods that reference spectrometer/spectrophotometer performance practices, such as Practices E275 , E925 , E932 , E958 , E1421 , E1683 , or E1944 ; Test Methods E387 , E388 , or E579 ; or Guide E1866 , this practice recommends that instrument performance data be collected as part of the ILS to establish the relationship between spectrometer/spectrophotometer performance and test method precision. ====== Significance And Use ====== 5.1 This practice should be used by the developer of standard test methods that employ surrogate calibrations. 5.1.1 This practice assists the test method developer in setting and documenting requirements for the spectrometer/spectrophotometers that can perform the test method. 5.1.2 This practice assists the test method developer in setting and documenting spectral data collection and computation parameters for the test method. 5.1.3 This practice assists the test method developer in selecting among possible multivariate analysis procedures that could be used to establish the surrogate calibration. The practice describes statistical tests that should be performed to ensure that all multivariate analysis procedures that are allowed within the scope of the test method produce statistically indistinguishable results. 5.1.4 This practice describes statistical calculations that the test method developer should perform on the calibration and qualification data that should be collected as part of the ILS that establishes the test method precision. These calculations establish the level of performance that spectrometers/spectrophotometers must meet in order to perform the test method. 5.2 This practice describes how the person who calibrates a spectrometer/spectrophotometer can test the performance of said spectrometer/spectrophotometer to determine if the performance is adequate to conduct the test method. 5.3 This practice describes how the user of a spectrometer/spectrophotometer can qualify the spectrometer/spectrophotometer to conduct the test method.