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ASTM E334-01(2013)

(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.

General Information

Status
Historical
Publication Date
31-Dec-2012
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(2013) - Standard Practice for General Techniques of Infrared MicroanalysisASTM E334-01(2013) - Standard Practice for General Techniques of Infrared Microanalysis
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ASTM E334-01(2013) - Standard Practice for General Techniques of Infrared Microanalysis
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: E334 − 01 (Reapproved 2013)
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 3.2 Beam Condenser—Aspecializedaccessorydesignedfor
analysis of samples of a microgram or less, comprising an
1.1 Thispracticecoverstechniquesthatareofgeneralusein
analyte area or volume of 2.0 mm diameter or less.
securing and analyzing microgram quantities of samples by
infrared spectrophotometric techniques. This practice makes
4. Contamination
repetition of description of specific techniques unnecessary in
4.1 Although the presence of contaminants is a general
individual infrared methods.
problem in any type of analysis, contamination can be particu-
1.2 These recommendations are supplementary to Practices
larly severe in micro work. For example, minor impurities in a
E168,E573,andE1252,whichshouldbereferredtofortheory,
solvent can become major components of a residue remaining
general techniques of sample preparation, and calculations.
after solvent evaporation. Materials extracted from thin-layer
chromatographic materials, from the paper used in paper
2. Referenced Documents
chromatography, and from solid adsorbents in general, may
2
2.1 ASTM Standards: include particular contaminants of concern. It should also be
E131Terminology Relating to Molecular Spectroscopy
noted that the gas-chromatographic stationary phase may lead
E168Practices for General Techniques of Infrared Quanti- to significant contamination. Consideration of these and other
3
tative Analysis (Withdrawn 2015)
sources of contamination must always enter interpretation of
E573Practices for Internal Reflection Spectroscopy
results in microanalysis. Erroneous results can be minimized
E1252Practice for General Techniques for Obtaining Infra-
by the use of pure reagents, extreme care in sample handling,
red Spectra for Qualitative Analysis
andthefrequentuseof“blanks”inthecourseofseparationand
E1642Practice for General Techniques of Gas Chromatog-
subsequent recording of spectra.
raphy Infrared (GC/IR) Analysis
5. General Microspectroscopic Techniques
E2105Practice for General Techniques of Thermogravimet-
ric Analysis (TGA) Coupled With Infrared Analysis
5.1 Spectroscopic techniques used for the examination of
(TGA/IR)
microsamples are usually adaptations of comparable macro
E2106 Practice for General Techniques of Liquid
techniques, and many have been described in the literature (1,
4
Chromatography-Infrared (LC/IR) and Size Exclusion
2).
Chromatography-Infrared (SEC/IR) Analyses
5.2 In computerized dispersive spectrometers or Fourier
transform-infrared (FT-IR) instruments, computer routines for
3. Terminology
multiple scanning, signal averaging, absorbance subtraction,
3.1 Definitions and Symbols—For definitions of terms and
andscaleexpansioncanbeusedveryeffectivelytoenhancethe
symbols, refer to Terminology E131.
observed signal-to-noise ratio of weak bands and increase
sensitivity (3, 4). Absorbance subtraction is also commonly
usedtoeliminateinterferingbandsfromthesamplematrixand
1
This practice is under the jurisdiction ofASTM Committee E13 on Molecular
thus lower the limits of detection (see Practice E168).
Spectroscopy and Separation Science and is the direct responsibility of Subcom-
5.3 Use of Masking Apertures—The aperture of sample
mittee E13.03 on Infrared and Near Infrared Spectroscopy.
Current edition approved Jan. 1, 2013. Published January 2013. Originally
holders used for microspectroscopic study (without the use of
approved in 1990. Last previous edition approved in 2007 as E334–01 (2007).
an infrared microscope) are usually significantly smaller than
DOI: 10.1520/E0334-01R13.
the beam at the sample position of the instrument. As a
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
consequenceofthesesmallapertures,stepsneedtobetakento
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.
3 4
The last approved version of this historical standard is referenced on The boldface numbers in parentheses refer to a list of references at the end of
www.astm.org. this practice.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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E334 − 01 (2013)
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