This practice should be used by the developer of standard test methods that employ surrogate calibrations.

This practice assists the test method developer in setting and documenting requirements for the spectrometer/spectrophotometers that can perform the test method.

This practice assists the test method developer in setting and documenting spectral data collection and computation parameters for the test method.

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.

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.

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.

This practice describes how the user of a spectrometer/spectrophotometer can qualify the spectrometer/spectrophotometer to conduct the test method.

1. Scope

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 Practice 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.

2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

ASTM Standards

D6277 Test Method for Determination of Benzene in Spark-Ignition Engine Fuels Using Mid Infrared Spectroscopy

D6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and Lubricants

E131 Terminology Relating to Molecular Spectroscopy

E275 Practice for Describing and Measuring Performance of Ultraviolet and Visible Spectrophotometers

E387 Test Method for Estimating Stray Radiant Power Ratio of Dispersive Spectrophotometers by the Opaque Filter Method

E388 Test Method for Wavelength Accuracy and Spectral Bandwidth of Fluorescence Spectrometers

E579 Test Method for Limit of Detection of Fluorescence of Quinine Sulfate in Solution

E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method

E925 Practice for Monitoring the Calibration of Ultraviolet-Visible Spectrophotometers whose Spectral Bandwidth does not Exceed 2 nm

E932 Practice for Describing and Measuring Performance of Dispersive Infrared Spectrometers

E958 Practice for Measuring Practical Spectral Bandwidth of Ultraviolet-Visible Spectrophotometers

E1421 Practice for Describing and Measuring Performance of Fourier Transform Mid-Infrared (FT-MIR) Spectrometers: Level Zero and Level One Tests

E1655 Practices for Infrared Multivariate Quantitative Analysis

E1683 Practice for Testing the Performance of Scanning Raman Spectrometers

E1866 Guide for Establishing Spectrophotometer Performance Tests

E1944 Practice for Describing and Measuring Performance of Laboratory Fourier Transform Near-Infrared (FT-NIR) Spectrometers: Level Zero and Level One Tests

Keywords

fluorescence spectroscopy; infrared spectroscopy; molecular spectroscopy; multivariate analysis; quantitative analysis; Raman spectroscopy; spectrometer qualification; spectrophotometer qualification; ultraviolet-visible spectroscopy; Calibration--spectrochemical analysis instrumentation; Fluorescence spectrochemical analysis; Infrared spectroscopy; Molecular spectroscopy; Multivariate analyses; Performance--spectrochemical equipment; Qualifications; Quantitative analysis/measurement; Raman spectroscopy; Spectrometry; Spectrophotometry; Ultra-visible spectroscopy;

ICS Code

ICS Number Code 71.040.50 (Physicochemical methods of analysis)

Citing ASTM Standards

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