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ASTM E334-01(2021)

(Practice)

Standard Practice for General Techniques of Infrared Microanalysis

Standard Practice for General Techniques of Infrared Microanalysis

ABSTRACT
This practice establishes the standard techniques that are of general use in securing and analyzing samples in microgram quantities (microanalysis) by infrared spectrophotometry. These techniques include general microspectroscopy, analysis of gas chromatographic fractions, analysis of liquid chromatographic fractions, analysis of thin-layer chromatographic fractions, analysis of paper chromatographic fractions, analysis of gases evolved from a thermogravimetric analyzer, and infrared spectroscopy using a microscope.
SCOPE
1.1 This practice covers techniques that are of general use in securing and analyzing microgram quantities of samples by infrared spectrophotometric techniques. This practice makes repetition of description of specific techniques unnecessary in individual infrared methods.  
1.2 These recommendations are supplementary to Practices E168, E573, and E1252, which should be referred to for theory, general techniques of sample preparation, and calculations.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

General Information

Status
Published
Publication Date
31-Mar-2021
ICS
71.040.50 - Physicochemical methods of analysis
Technical Committee
E13 - Molecular Spectroscopy and Separation Science
Drafting Committee
E13.03 - Infrared and Near Infrared Spectroscopy
Current Stage
Ref Project

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ASTM E334-01(2021) - Standard Practice for General Techniques of Infrared Microanalysis
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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: E334 − 01 (Reapproved 2021)
Standard Practice for
1
General Techniques of Infrared Microanalysis
This standard is issued under the fixed designation E334; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope ric Analysis (TGA) Coupled With Infrared Analysis
(TGA/IR)
1.1 Thispracticecoverstechniquesthatareofgeneralusein
E2106 Practice for General Techniques of Liquid
securing and analyzing microgram quantities of samples by
Chromatography-Infrared (LC/IR) and Size Exclusion
infrared spectrophotometric techniques. This practice makes
Chromatography-Infrared (SEC/IR) Analyses
repetition of description of specific techniques unnecessary in
individual infrared methods.
3. Terminology
1.2 These recommendations are supplementary to Practices
3.1 Definitions and Symbols—For definitions of terms and
E168,E573,andE1252,whichshouldbereferredtofortheory,
symbols, refer to Terminology E131.
general techniques of sample preparation, and calculations.
3.2 Beam Condenser—Aspecializedaccessorydesignedfor
1.3 This standard does not purport to address all of the
analysis of samples of a microgram or less, comprising an
safety concerns, if any, associated with its use. It is the
analyte area or volume of 2.0 mm diameter or less.
responsibility of the user of this standard to establish appro-
4. Contamination
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use.
4.1 Although the presence of contaminants is a general
1.4 This international standard was developed in accor-
problem in any type of analysis, contamination can be particu-
dance with internationally recognized principles on standard-
larly severe in micro work. For example, minor impurities in a
ization established in the Decision on Principles for the
solvent can become major components of a residue remaining
Development of International Standards, Guides and Recom-
after solvent evaporation. Materials extracted from thin-layer
mendations issued by the World Trade Organization Technical
chromatographic materials, from the paper used in paper
Barriers to Trade (TBT) Committee.
chromatography, and from solid adsorbents in general, may
include particular contaminants of concern. It should also be
2. Referenced Documents
noted that the gas-chromatographic stationary phase may lead
2
2.1 ASTM Standards: to significant contamination. Consideration of these and other
E131Terminology Relating to Molecular Spectroscopy
sources of contamination must always enter interpretation of
E168Practices for General Techniques of Infrared Quanti- results in microanalysis. Erroneous results can be minimized
tative Analysis
by the use of pure reagents, extreme care in sample handling,
E573Practices for Internal Reflection Spectroscopy andthefrequentuseof“blanks”inthecourseofseparationand
E1252Practice for General Techniques for Obtaining Infra-
subsequent recording of spectra.
red Spectra for Qualitative Analysis
5. General Microspectroscopic Techniques
E1642Practice for General Techniques of Gas Chromatog-
raphy Infrared (GC/IR) Analysis
5.1 Spectroscopic techniques used for the examination of
E2105Practice for General Techniques of Thermogravimet-
microsamples are usually adaptations of comparable macro
techniques, and many have been described in the literature (1,
3
2).
1
This practice is under the jurisdiction ofASTM Committee E13 on Molecular
5.2 In computerized dispersive spectrometers or Fourier
Spectroscopy and Separation Science and is the direct responsibility of Subcom-
mittee E13.03 on Infrared and Near Infrared Spectroscopy.
transform-infrared (FT-IR) instruments, computer routines for
Current edition approved April 1, 2021. Published April 2021. Originally
multiple scanning, signal averaging, absorbance subtraction,
approved in 1990. Last previous edition approved in 2013 as E334–01 (2013).
andscaleexpansioncanbeusedveryeffectivelytoenhancethe
DOI: 10.1520/E0334-01R21.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The boldface numbers in parentheses refer to a list of references at the end of
the ASTM website. this practice.
Copyright © ASTM International, 100 Barr Har
...

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4.1 This practice permits an analyst to compare the performance of an instrument to the manufacturer's supplied performance specifications and to verify its suitability for continued routine use. It also provides generation of calibration monitoring data on a periodic basis, forming a base from which any changes in the performance of the instrument will be evident.
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Standard Practice for Using Flame Photometric Detectors in Gas Chromatography

ABSTRACT
This practice is intended as a guide for the use of a flame photometric detector (FPD) as the detection component of a gas chromatographic system. The different principles of flame photometric detectors, and detector construction are presented in details. The detector sensitivity, minimum detectability, dynamic range, power law of sulphur response, linear range-phosphorus mode, unipower response range, noise and drift, and specificity are presented in details. The photomultiplier dark current is the magnitude of the FPD output signal measured with the FPD flame off. Flame background current is the difference in FPD output signal with the flame on and with the flame off in the absence of phosphorus or sulfur compounds in the flame.
SCOPE
1.1 This practice is intended as a guide for the use of a flame photometric detector (FPD) as the detection component of a gas chromatographic system.  
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1.5 For general gas chromatographic procedures, Practice E260 should be followed except where specific changes are recommended herein for use of an FPD.  
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