ASTM E1655-17
(Practice)Standard Practices for Infrared Multivariate Quantitative Analysis
Standard Practices for Infrared Multivariate Quantitative Analysis
SIGNIFICANCE AND USE
5.1 These practices can be used to establish the validity of the results obtained by an infrared (IR) spectrometer at the time the calibration is developed. The ongoing validation of estimates produced by analysis of unknown samples using the calibration model should be covered separately (see for example, Practice D6122).
5.2 These practices are intended for all users of infrared spectroscopy. Near-infrared spectroscopy is widely used for quantitative analysis. Many of the general principles described in these practices relate to the common modern practices of near-infrared spectroscopic analysis. While sampling methods and instrumentation may differ, the general calibration methodologies are equally applicable to mid-infrared spectroscopy. New techniques are under study that may enhance those discussed within these practices. Users will find these practices to be applicable to basic aspects of the technique, to include sample selection and preparation, instrument operation, and data interpretation.
5.3 The calibration procedures define the range over which measurements are valid and demonstrate whether or not the sensitivity and linearity of the analysis outputs are adequate for providing meaningful estimates of the specific physical or chemical characteristics of the types of materials for which the calibration is developed.
SCOPE
1.1 These practices cover a guide for the multivariate calibration of infrared spectrometers used in determining the physical or chemical characteristics of materials. These practices are applicable to analyses conducted in the near infrared (NIR) spectral region (roughly 780 to 2500 nm) through the mid infrared (MIR) spectral region (roughly 4000 to 400 cm−1).
Note 1: While the practices described herein deal specifically with mid- and near-infrared analysis, much of the mathematical and procedural detail contained herein is also applicable for multivariate quantitative analysis done using other forms of spectroscopy. The user is cautioned that typical and best practices for multivariate quantitative analysis using other forms of spectroscopy may differ from practices described herein for mid- and near-infrared spectroscopies.
1.2 Procedures for collecting and treating data for developing IR calibrations are outlined. Definitions, terms, and calibration techniques are described. Criteria for validating the performance of the calibration model are described.
1.3 The implementation of these practices require that the IR spectrometer has been installed in compliance with the manufacturer's specifications. In addition, it assumes that, at the times of calibration and of validation, the analyzer is operating at the conditions specified by the manufacturer.
1.4 These practices cover techniques that are routinely applied in the near and mid infrared spectral regions for quantitative analysis. The practices outlined cover the general cases for coarse solids, fine ground solids, and liquids. All techniques covered require the use of a computer for data collection and analysis.
1.5 These practices provide a questionnaire against which multivariate calibrations can be examined to determine if they conform to the requirements defined herein.
1.6 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 herein, they do not conform to procedures described herein, specifically with respect to the handling of outliers. Surrogate methods may indicate that they make use of the mathematics described herein, but they should not claim to follow the procedures described herein.
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are...
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Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E1655 − 17
Standard Practices for
1
Infrared Multivariate Quantitative Analysis
This standard is issued under the fixed designation E1655; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope analyzed. While these surrogate methods generally make use
of the multivariate mathematics described herein, they do not
1.1 These practices cover a guide for the multivariate
conform to procedures described herein, specifically with
calibration of infrared spectrometers used in determining the
respect to the handling of outliers. Surrogate methods may
physical or chemical characteristics of materials. These prac-
indicate that they make use of the mathematics described
tices are applicable to analyses conducted in the near infrared
herein, but they should not claim to follow the procedures
(NIR) spectral region (roughly 780 to 2500 nm) through the
described herein.
mid infrared (MIR) spectral region (roughly 4000 to 400
−1
cm ). 1.7 The values stated in SI units are to be regarded as
NOTE 1—While the practices described herein deal specifically with
standard. No other units of measurement are included in this
mid-andnear-infraredanalysis,muchofthemathematicalandprocedural
standard.
detail contained herein is also applicable for multivariate quantitative
1.8 This standard does not purport to address all of the
analysisdoneusingotherformsofspectroscopy.Theuseriscautionedthat
typicalandbestpracticesformultivariatequantitativeanalysisusingother safety concerns, if any, associated with its use. It is the
formsofspectroscopymaydifferfrompracticesdescribedhereinformid-
responsibility of the user of this standard to establish appro-
and near-infrared spectroscopies.
priate safety, health, and environmental practices and deter-
1.2 Procedures for collecting and treating data for develop-
mine the applicability of regulatory limitations prior to use.
ing IR calibrations are outlined. Definitions, terms, and cali-
1.9 This international standard was developed in accor-
bration techniques are described. Criteria for validating the
dance with internationally recognized principles on standard-
performance of the calibration model are described.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
1.3 The implementation of these practices require that the
mendations issued by the World Trade Organization Technical
IR spectrometer has been installed in compliance with the
Barriers to Trade (TBT) Committee.
manufacturer’s specifications. In addition, it assumes that, at
the times of calibration and of validation, the analyzer is
2. Referenced Documents
operating at the conditions specified by the manufacturer.
2
2.1 ASTM Standards:
1.4 These practices cover techniques that are routinely
D1265Practice for Sampling Liquefied Petroleum (LP)
applied in the near and mid infrared spectral regions for
Gases, Manual Method
quantitative analysis. The practices outlined cover the general
D4057Practice for Manual Sampling of Petroleum and
cases for coarse solids, fine ground solids, and liquids. All
Petroleum Products
techniques covered require the use of a computer for data
D4177Practice for Automatic Sampling of Petroleum and
collection and analysis.
Petroleum Products
1.5 These practices provide a questionnaire against which
D4855Practice for Comparing Test Methods (Withdrawn
3
multivariate calibrations can be examined to determine if they
2008)
conform to the requirements defined herein.
D6122Practice for Validation of the Performance of Multi-
variate Online,At-Line, and Laboratory Infrared Spectro-
1.6 For some multivariate spectroscopic analyses, interfer-
photometer Based Analyzer Systems
encesandmatrixeffectsaresufficientlysmallthatitispossible
D6299Practice for Applying Statistical Quality Assurance
to calibrate using mixtures that contain substantially fewer
and Control Charting Techniques to Evaluate Analytical
chemical components than the samples that will ultimately be
1 2
These practices are under the jurisdiction of ASTM Committee E13 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Molecular Spectroscopy and Separation Science and are the direct responsibility of contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Subcommittee E13.11 on Multivariate Analysis. Standards volume information, refer to the standard’s Document Summary page on
Current editi
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
Designation: E1655 − 05 (Reapproved 2012) E1655 − 17
Standard Practices for
1
Infrared Multivariate Quantitative Analysis
This standard is issued under the fixed designation E1655; 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
1.1 These practices cover a guide for the multivariate calibration of infrared spectrometers used in determining the physical or
chemical characteristics of materials. These practices are applicable to analyses conducted in the near infrared (NIR) spectral
−1
region (roughly 780 to 2500 nm) through the mid infrared (MIR) spectral region (roughly 4000 to 400 cm ).
NOTE 1—While the practices described herein deal specifically with mid- and near-infrared analysis, much of the mathematical and procedural detail
contained herein is also applicable for multivariate quantitative analysis done using other forms of spectroscopy. The user is cautioned that typical and
best practices for multivariate quantitative analysis using other forms of spectroscopy may differ from practices described herein for mid- and
near-infrared spectroscopies.
1.2 Procedures for collecting and treating data for developing IR calibrations are outlined. Definitions, terms, and calibration
techniques are described. Criteria for validating the performance of the calibration model are described.
1.3 The implementation of these practices require that the IR spectrometer has been installed in compliance with the
manufacturer’s specifications. In addition, it assumes that, at the times of calibration and of validation, the analyzer is operating
at the conditions specified by the manufacturer.
1.4 These practices cover techniques that are routinely applied in the near and mid infrared spectral regions for quantitative
analysis. The practices outlined cover the general cases for coarse solids, fine ground solids, and liquids. All techniques covered
require the use of a computer for data collection and analysis.
1.5 These practices provide a questionnaire against which multivariate calibrations can be examined to determine if they
conform to the requirements defined herein.
1.6 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 herein, they do not conform to
procedures described herein, specifically with respect to the handling of outliers. Surrogate methods may indicate that they make
use of the mathematics described herein, but they should not claim to follow the procedures described herein.
1.7 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.8 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.9 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2
2.1 ASTM Standards:
D1265 Practice for Sampling Liquefied Petroleum (LP) Gases, Manual Method
D4057 Practice for Manual Sampling of Petroleum and Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and Petroleum Products
1
These practices are under the jurisdiction of ASTM Committee E13 on Molecular Spectroscopy and Separation Science and are the direct responsibility of Subcommittee
E13.11 on Multivariate Analysis.
Current edition approved April 1, 2012Dec. 1, 2017. Published May 2012January 2018. Originally approved in 1997. Last previous edition approved in 20052012 as
E1655 – 05.E1655 – 05(2012). DOI: 10.1520/E1655-05R12.10.1520/E1655-17.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For A
...
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