ASTM E1655-05(2012)
(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 inc...
General Information
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: E1655 − 05 (Reapproved 2012)
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 and health practices and determine the applica-
1.2 Procedures for collecting and treating data for develop-
bility of regulatory limitations prior to use.
ing IR calibrations are outlined. Definitions, terms, and cali-
bration techniques are described. Criteria for validating the
2. Referenced Documents
performance of the calibration model are described.
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2.1 ASTM Standards:
1.3 The implementation of these practices require that the
D1265Practice for Sampling Liquefied Petroleum (LP)
IR spectrometer has been installed in compliance with the
Gases, Manual Method
manufacturer’s specifications. In addition, it assumes that, at
D4057Practice for Manual Sampling of Petroleum and
the times of calibration and of validation, the analyzer is
Petroleum Products
operating at the conditions specified by the manufacturer.
D4177Practice for Automatic Sampling of Petroleum and
Petroleum Products
1.4 These practices cover techniques that are routinely
D4855Practice for Comparing Test Methods (Withdrawn
applied in the near and mid infrared spectral regions for
3
2008)
quantitative analysis. The practices outlined cover the general
D6122Practice for Validation of the Performance of Multi-
cases for coarse solids, fine ground solids, and liquids. All
variate Online,At-Line, and Laboratory Infrared Spectro-
techniques covered require the use of a computer for data
photometer Based Analyzer Systems
collection and analysis.
D6299Practice for Applying Statistical Quality Assurance
1.5 These practices provide a questionnaire against which
and Control Charting Techniques to Evaluate Analytical
multivariate calibrations can be examined to determine if they
Measurement System Performance
conform to the requirements defined herein.
D6300Practice for Determination of Precision and Bias
1.6 For some multivariate spectroscopic analyses, interfer-
Data for Use in Test Methods for Petroleum Products and
encesandmatrixeffectsaresufficientlysmallthatitispossible
Lubricants
to calibrate using mixtures that contain substantially fewer
E131Terminology Relating to Molecular Spectroscopy
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 edition approved April 1, 2012. Published May 2012. Originally the ASTM website.
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approved in 1997. Last previous edition approved in 2005 as E1655–05. DOI: The last approved version of this historical standard is referenced on
10.1520/E1655-05R12. www.astm.org.
Copyright © ASTM Inter
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