ASTM E2056-04(2010)
(Practice)Standard Practice for Qualifying Spectrometers and Spectrophotometers for Use in Multivariate Analyses, Calibrated Using Surrogate Mixtures
Standard Practice for Qualifying Spectrometers and Spectrophotometers for Use in Multivariate Analyses, Calibrated Using Surrogate Mixtures
SIGNIFICANCE AND USE
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.
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 r...
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Standards Content (Sample)
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Designation: E2056 − 04 (Reapproved2010)
Standard Practice for
Qualifying Spectrometers and Spectrophotometers for Use
in Multivariate Analyses, Calibrated Using Surrogate
1
Mixtures
This standard is issued under the fixed designation E2056; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 1.3 For surrogate test methods, this practice recommends
limitations that should be placed on calibration options that are
1.1 This practice relates to the multivariate calibration of
allowed in the test method. Specifically, this practice recom-
spectrometers and spectrophotometers used in determining the
mends that the test method developer demonstrate that all
physical and chemical characteristics of materials. A detailed
calibrations that are allowed in the test method produce
description of general multivariate analysis is given in Practice
statistically indistinguishable results.
E1655. This standard refers only to those instances where
surrogate mixtures can be used to establish a suitable calibra- 1.4 For surrogate test methods that reference spectrometer/
tion matrix.This practice specifies calibration and qualification spectrophotometer performance practices, such as Practices
data set requirements for interlaboratory studies (ILSs), that is, E275, E925, E932, E958, E1421, E1683,or E1944; Test
round robins, of standard test methods employing surrogate Methods E387, E388,or E579; or Guide E1866, this practice
calibration techniques that do not conform exactly to Practices recommends that instrument performance data be collected as
E1655. part of the ILS to establish the relationship between
spectrometer/spectrophotometer performance and test method
NOTE 1—For some multivariate spectroscopic analyses, interferences
precision.
andmatrixeffectsaresufficientlysmallthatitispossibletocalibrateusing
mixtures that contain substantially fewer chemical components than the
2. Referenced Documents
samples that will ultimately be analyzed. While these surrogate methods
generally make use of the multivariate mathematics described in Practices 2
2.1 ASTM Standards:
E1655, they do not conform to procedures described therein, specifically
D6277 Test Method for Determination of Benzene in Spark-
with respect to the handling of outliers.
Ignition Engine Fuels Using Mid Infrared Spectroscopy
1.2 This practice specifies how the ILS data is treated to
D6300 Practice for Determination of Precision and Bias
establish spectrometer/spectrophotometer performance qualifi-
Data for Use in Test Methods for Petroleum Products and
cation requirements to be incorporated into standard test
Lubricants
methods.
E131 Terminology Relating to Molecular Spectroscopy
NOTE 2—Spectrometer/spectrophotometer qualification procedures are
E275 Practice for Describing and Measuring Performance of
intended to allow the user to determine if the performance of a specific
Ultraviolet and Visible Spectrophotometers
spectrometer/spectrophotometer is adequate to conduct the analysis so as
E387 TestMethodforEstimatingStrayRadiantPowerRatio
to obtain results consistent with the published test method precision.
of Dispersive Spectrophotometers by the Opaque Filter
1.2.1 The spectroscopies used in the surrogate test methods
Method
would include but not be limited to mid- and near-infrared,
E388 Test Method for Wavelength Accuracy and Spectral
ultraviolet/visible, fluorescence and Raman spectroscopies.
Bandwidth of Fluorescence Spectrometers
1.2.2 The surrogate calibrations covered in this practice are:
E579 Test Method for Limit of Detection of Fluorescence of
multilinearregression(MLR),principalcomponentsregression
Quinine Sulfate in Solution
(PCR) or partial least squares (PLS) mathematics. These
E691 Practice for Conducting an Interlaboratory Study to
calibration procedures are described in detail in Practices
Determine the Precision of a Test Method
E1655.
E925 Practice for Monitoring the Calibration of Ultraviolet-
Visible Spectrophotometers whose Spectral Bandwidth
1
This practice is under the jurisdiction of ASTM Committee E13 on Molecular
Spectroscopy and Separation Science and is the direct responsibility of Subcom-
2
mittee E13.11 on Multivariate Analysis. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved March 1, 2010. Published May 2010. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1999. Last previous edition approved in 2004 as E2056 – 04. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E2056-04R10. the ASTM
...
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