ASTM E2617-08ae1
(Practice)Standard Practice for Validation of Empirically Derived Multivariate Calibrations
Standard Practice for Validation of Empirically Derived Multivariate Calibrations
SIGNIFICANCE AND USE
This practice outlines a universally applicable procedure to validate the performance of a quantitative or qualitative, empirically derived, multivariate calibration relative to an accepted reference method.
This practice provides procedures for evaluating the capability of a calibration to provide reliable estimations relative to an accepted reference method.
This practice provides purchasers of a measurement system that incorporates an empirically derived multivariate calibration with options for specifying validation requirements to ensure that the system is capable of providing estimations with an appropriate degree of agreement with an accepted reference method.
This practice provides the user of a measurement system that incorporates an empirically derived multivariate calibration with procedures capable of providing information that may be useful for ongoing quality assurance of the performance of the measurement system.
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 and only for the individual measurement system on which the practice is completely applied. It is the user's responsibility to select the property levels and the compositional characteristics of the validation samples such that they are suitable to the application. This practice allows the user to write a comprehensive validation statement for the analyzer system including specific limits for the validated range of application and specific restrictions to the permitted uses of the measurement system. Users are cautioned against extrapolation of validation results beyond the material type(s) and property range(s) used to obtain these results.
Users are cautioned that a validated empirically derived multivariate calibration is applicable only to samples that fall within the subset population represented in the validation set. The estimation from an empirically de...
SCOPE
1.1 This practice covers requirements for the validation of empirically derived calibrations (Note 1) such as calibrations derived by Multiple Linear Regression (MLR), Principal Component Regression (PCR), Partial Least Squares (PLS), Artificial Neural Networks (ANN), or any other empirical calibration technique whereby a relationship is postulated between a set of variables measured for a given sample under test and one or more physical, chemical, quality, or membership properties applicable to that sample.
Note 1—Empirically derived calibrations are sometimes referred to as “models” or “calibrations.” In the following text, for conciseness, the term “calibration” may be used instead of the full name of the procedure.
1.2 This practice does not cover procedures for establishing said postulated relationship.
1.3 This practice serves as an overview of techniques used to verify the applicability of an empirically derived multivariate calibration to the measurement of a sample under test and to verify equivalence between the properties calculated from the empirically derived multivariate calibration and the results of an accepted reference method of measurement to within control limits established for the prespecified statistical confidence level.
1.4 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.
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Designation:E2617–08a
Standard Practice for
1
Validation of Empirically Derived Multivariate Calibrations
This standard is issued under the fixed designation E 2617; 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
´ NOTE—Annex A1 was editorially corrected to be classified as Appendix X1 in February 2009.
1. Scope E 1655 Practices for Infrared Multivariate Quantitative
Analysis
1.1 This practice covers requirements for the validation of
E 1790 Practice for Near Infrared Qualitative Analysis
empirically derived calibrations (Note 1) such as calibrations
derived by Multiple Linear Regression (MLR), Principal Com-
3. Terminology
ponent Regression (PCR), Partial Least Squares (PLS), Artifi-
3.1 For terminology related to molecular spectroscopic
cial Neural Networks (ANN), or any other empirical calibra-
methods, refer to Terminology E 131. For terminology related
tion technique whereby a relationship is postulated between a
to multivariate quantitative modeling refer to PracticesE 1655.
setofvariablesmeasuredforagivensampleundertestandone
WhilePracticesE 1655iswritteninthecontextofmultivariate
or more physical, chemical, quality, or membership properties
spectroscopic methods, the terminology is also applicable to
applicable to that sample.
other multivariate technologies.
NOTE 1—Empirically derived calibrations are sometimes referred to as
3.2 Definitions of Terms Specific to This Standard:
“models”or“calibrations.”Inthefollowingtext,forconciseness,theterm
3.2.1 accuracy—the closeness of agreement between a test
“calibration” may be used instead of the full name of the procedure.
result and an accepted reference value.
1.2 This practice does not cover procedures for establishing
3.2.2 bias—the arithmetic average difference between the
said postulated relationship.
reference values and the values produced by the analytical
1.3 This practice serves as an overview of techniques used
method under test, for a set of samples.
to verify the applicability of an empirically derived multivari-
3.2.3 detection limit—the lowest level of a property in a
ate calibration to the measurement of a sample under test and
sample that can be detected, but not necessarily quantified, by
to verify equivalence between the properties calculated from
the measurement system.
the empirically derived multivariate calibration and the results
3.2.4 estimate—the constituent concentration, identifica-
of an accepted reference method of measurement to within
tion, or other property of a sample as determined by the
control limits established for the prespecified statistical confi-
analytical method being validated.
dence level.
3.2.5 initial validation—validation that is performed when
1.4 This standard does not purport to address all of the
an analyzer system is initially installed or after major mainte-
safety concerns, if any, associated with its use. It is the
nance.
responsibility of the user of this standard to establish appro-
3.2.6 Negative Fraction Identified—the fraction of samples
priate safety and health practices and determine the applica-
not having a particular characteristic that is identified as not
bility of regulatory limitations prior to use.
having that characteristic.
3.2.6.1 Discussion—Negative Fraction Identified assumes
2. Referenced Documents
that the characteristic that the test measures either is or is not
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2.1 ASTM Standards:
present. It is not applicable to tests with multiple possible
E 131 Terminology Relating to Molecular Spectroscopy
outcomes.
3.2.7 ongoing periodic revalidation—the quality assurance
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This practice is under the jurisdiction of ASTM Committee E13 on Molecular process by which, in the case of quantitative calibrations, the
Spectroscopy and Separation Science and is the direct responsibility of Subcom-
bias and precision or, in the case of qualitative calibrations, the
mittee E13.11 on Multivariate Analysis.
Positive Fraction Identified and Negative Fraction Identified
Current edition approved Oct. 1, 2008. Published October 2008. Originally
performance determined during initial validation are shown to
approved in 2008. Last previous edition approved in 2008 as E 2617 – 08.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
be sustained.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
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Designation:E2617–08 Designation:E2617–08a
Standard Practice for
1
Validation of Empirically Derived Multivariate Calibrations
This standard is issued under the fixed designation E 2617; 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
´ NOTE—Annex A1 was editorially corrected to be classified as Appendix X1 in February 2009.
1. Scope
1.1 Thispracticecoversrequirementsforthevalidationofempiricallyderivedcalibrations(Note1)suchascalibrationsderived
by Multiple Linear Regression (MLR), Principal Component Regression (PCR), Partial Least Squares (PLS), Artificial Neural
Networks (ANN), or any other empirical calibration technique whereby a relationship is postulated between a set of variables
measured for a given sample under test and one or more physical, chemical, quality, or membership properties applicable to that
sample.
NOTE 1—Empirically derived calibrations are sometimes referred to as “models” or “calibrations.” In the following text, for conciseness, the term
“calibration” may be used instead of the full name of the procedure.
1.2 This practice does not cover procedures for establishing said postulated relationship.
1.3 This practice serves as an overview of techniques used to verify the applicability of an empirically derived multivariate
calibration to the measurement of a sample under test and to verify equivalence between the properties calculated from the
empirically derived multivariate calibration and the results of an accepted reference method of measurement to within control
limits established for the prespecified statistical confidence level.
1.4 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.
2. Referenced Documents
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2.1 ASTM Standards:
E 131 Terminology Relating to Molecular Spectroscopy
E 1655 Practices for Infrared Multivariate Quantitative Analysis
E 1790 Practice for Near Infrared Qualitative Analysis
3. Terminology
3.1 For terminology related to molecular spectroscopic methods, refer to Terminology E 131. For terminology related to
multivariate quantitative modeling refer to Practices E 1655. While Practices E 1655 is written in the context of multivariate
spectroscopic methods, the terminology is also applicable to other multivariate technologies.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 accuracy—the closeness of agreement between a test result and an accepted reference value.
3.2.2 bias—the arithmetic average difference between the reference values and the values produced by the analytical method
under test, for a set of samples.
3.2.3 detection limit—the lowest level of a property in a sample that can be detected, but not necessarily quantified, by the
measurement system.
3.2.4 estimate—the constituent concentration, identification, or other property of a sample as determined by the analytical
method being validated.
3.2.5 initial validation—validation that is performed when an analyzer system is initially installed or after major maintenance.
3.2.6 Negative Fraction Identified—the fraction of samples not having a particular characteristic that is identified as not having
that characteristic.
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This practice is under the jurisdiction of ASTM Committee E13 on Molecular Spectroscopy and Separation Science and is the direct responsibility of Subcommittee
E13.11 on Multivariate Analysis.
Current edition approved May 15, 2008. Published June 2008.
Current edition approved Oct. 1, 2008. Published October 2008. Originally approved in 2008. Last previous edition approved in 2008 as E 2617 – 08.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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E2617–08a
3.2.6.1 Discussion—NegativeFractionIdentifiedassumesthatthecharacteristicthatthetestmeasureseitherisorisnotpresent.
It is not applicable to tests with
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