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ASTM E1642-00(2010)

(Practice)

Standard Practice for General Techniques of Gas Chromatography Infrared (GC/IR) Analysis

Standard Practice for General Techniques of Gas Chromatography Infrared (GC/IR) Analysis

SIGNIFICANCE AND USE
This practice provides general guidelines for the proper practice of gas chromatography coupled with infrared spectrophotometric detection and analysis (GC/IR). This practice assumes that the chromatography involved in the practice is adequate to separate the compounds of interest. It is not the intention of this practice to instruct the user how to perform gas chromatography properly.
SCOPE
1.1 This practice covers techniques that are of general use in analyzing qualitatively multicomponent samples by using a combination of gas chromatography (GC) and infrared (IR) spectrophotometric techniques. The mixture is separated into its individual components by GC and then these individual components are analyzed by IR spectroscopy. Types of GC-IR techniques discussed include eluent trapping, flowcell, and eluite deposition.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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 and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
28-Feb-2010
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

Relations

Replaces
ASTM E1642-00(2005) - Standard Practice for General Techniques of Gas Chromatography Infrared (GC/IR) Analysis
Effective Date
01-Mar-2010
Replaced By
ASTM E1642-00(2016) - Standard Practice for General Techniques of Gas Chromatography Infrared (GC/IR) Analysis
Effective Date
01-Apr-2016
Referred By
ASTM F2150-19 - Standard Guide for Characterization and Testing of Biomaterial Scaffolds Used in Regenerative Medicine and Tissue-Engineered Medical Products
Effective Date
01-Mar-2010
Referred By
ASTM E1252-98(2021) - Standard Practice for General Techniques for Obtaining Infrared Spectra for Qualitative Analysis
Effective Date
01-Mar-2010
Referred By
ASTM E334-01(2021) - Standard Practice for General Techniques of Infrared Microanalysis
Effective Date
01-Mar-2010
Referred By
ASTM E2310-04(2015) - Standard Guide for Use of Spectral Searching by Curve Matching Algorithms with Data Recorded Using Mid-Infrared Spectroscopy
Effective Date
01-Mar-2010

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ASTM E1642-00(2010) - Standard Practice for General Techniques of Gas Chromatography Infrared (GC/IR) AnalysisASTM E1642-00(2010) - Standard Practice for General Techniques of Gas Chromatography Infrared (GC/IR) Analysis
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ASTM E1642-00(2010) - Standard Practice for General Techniques of Gas Chromatography Infrared (GC/IR) Analysis
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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: E1642 − 00 (Reapproved2010)
Standard Practice for
General Techniques of Gas Chromatography Infrared (GC/
1
IR) Analysis
This standard is issued under the fixed designation E1642; 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 E1421Practice for Describing and Measuring Performance
of Fourier Transform Mid-Infrared (FT-MIR) Spectrom-
1.1 Thispracticecoverstechniquesthatareofgeneralusein
eters: Level Zero and Level One Tests
analyzing qualitatively multicomponent samples by using a
E1510Practice for Installing Fused Silica Open Tubular
combination of gas chromatography (GC) and infrared (IR)
Capillary Columns in Gas Chromatographs
spectrophotometric techniques. The mixture is separated into
its individual components by GC and then these individual
3. Terminology
components are analyzed by IR spectroscopy. Types of GC-IR
techniques discussed include eluent trapping, flowcell, and
3.1 Definitions—Fordefinitionsoftermsandsymbols,refer
eluite deposition. to Terminology E131 and Practice E355.
1.2 The values stated in SI units are to be regarded as
4. Significance and Use
standard. No other units of measurement are included in this
standard.
4.1 This practice provides general guidelines for the proper
practice of gas chromatography coupled with infrared spectro-
1.3 This standard does not purport to address all of the
photometric detection and analysis (GC/IR). This practice
safety concerns, if any, associated with its use. It is the
assumes that the chromatography involved in the practice is
responsibility of the user of this standard to establish appro-
adequate to separate the compounds of interest. It is not the
priate safety and health practices and determine the applica-
intentionofthispracticetoinstructtheuserhowtoperformgas
bility of regulatory limitations prior to use.
chromatography properly.
2. Referenced Documents
2
5. General GC/IR Techniques
2.1 ASTM Standards:
E131Terminology Relating to Molecular Spectroscopy
5.1 Three different types of GC/IR technique have been
E168Practices for General Techniques of Infrared Quanti-
used to analyze samples. These consist of analyte trapping,
tative Analysis
flowcell, or lightpipe, and direct eluite deposition and are
E260Practice for Packed Column Gas Chromatography
presented in the order that they were first used.
E334Practice for General Techniques of Infrared Micro-
5.2 The GC eluent must not be routed to a destructive GC
analysis
detector (such as a flame ionization detector) prior to reaching
E355PracticeforGasChromatographyTermsandRelation-
the IR detector as this will destroy or alter the individual
ships
components. It is acceptable to split the eluent so that part of
E932PracticeforDescribingandMeasuringPerformanceof
the stream is directed to such a detector or to pass the stream
Dispersive Infrared Spectrometers
back to the detector after infrared analysis if such techniques
E1252Practice for General Techniques for Obtaining Infra-
are feasible.
red Spectra for Qualitative Analysis
5.3 Eluent Trapping Techniques—Analyte trapping tech-
niques are the least elaborate means for obtaining GC/IR data.
1
This practice is under the jurisdiction ofASTM Committee E13 on Molecular
In these techniques, the sample eluting from the chromato-
Spectroscopy and Separation Science and is the direct responsibility of Subcom-
graph is collected in discrete aliquots to be analyzed. In
mittee E13.03 on Infrared and Near Infrared Spectroscopy.
utilizing such techniques, it is essential that a GC detector be
Current edition approved March 1, 2010. Published April 2010. Originally
employed to allow definition of component elution. If a
approved in 1994. Last previous edition approved in 2005 as E1642–00(2005).
DOI: 10.1520/E1642-00R10.
destructive detector is employed, then post-column splitting to
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
that detector is required. GC fractions can be trapped in the
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
condensed phase by passing the GC effluent through a solvent,
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. a powdered solid, or a cold trap for subsequent analysis (see
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E1642 − 00 (2010)
3
Practice E1252) (1). Vapor phase samples can be trapped in a a safe level as soon as possible. It must be noted that repeated
heated low-volume
...

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4.1 Generally, Raman spectra measured using grating-based dispersive or Fourier transform Raman spectrometers have not been corrected for the instrumental response (spectral responsivity of the detection system). Raman spectra obtained with different instruments may show significant variations in the measured relative peak intensities of a sample compound. This is mainly as a result of differences in their wavelength-dependent optical transmission and detector efficiencies. These variations can be particularly large when widely different laser excitation wavelengths are used, but can occur when the same laser excitation is used and spectra of the same compound are compared between instruments. This is illustrated in Fig. 1, which shows the uncorrected luminescence spectrum of SRM 2241, acquired upon four different commercially available Raman spectrometers operating with 785 nm laser excitation. Instrumental response variations can also occur on the same instrument after a component change or service work has been performed. Each spectrometer, due to its unique combination of filters, grating, collection optics and detector response, has a very unique spectral response. The spectrometer dependent spectral response will of course also affect the shape of Raman spectra acquired upon these systems. The shape of this response is not to be construed as either “good or bad” but is the result of design considerations by the spectrometer manufacturer. For instance, as shown in Fig. 1, spectral coverage can vary considerably between spectrometer systems. This is typically a deliberate tradeoff in spectrometer design, where spectral coverage is sacrificed for enhanced spectral resolution.
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1.1 This guide is designed to enable the user to correct a Raman spectrometer for its relative spectral-intensity response function using NIST Standard Reference Materials2 in the 224X series (currently SRMs 2241, 2242, 2243, 2244, 2245, 2246), or a calibrated irradiance source. This relative intensity correction procedure will enable the intercomparison of Raman spectra acquired from differing instruments, excitation wavelengths, and laboratories.  
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Standard Practices for General Techniques of Infrared Quantitative Analysis

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4.1 These practices are intended for all infrared spectroscopists. For novices, these practices will serve as an overview of preparation, operation, and calculation techniques. For experienced persons, these practices will serve as a review when seldom-used techniques are needed.
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1.5 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.

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SIGNIFICANCE AND USE
4.1 A scanning Raman spectrometer should be checked regularly to determine if its condition is adequate for routine measurements or if it has changed. This practice is designed to facilitate that determination and, if performance is unsatisfactory, to identify the part of the system that needs attention. These tests apply for single-, double-, or triple-monochromator scanning Raman instruments commercially available. They do not apply for multichannel or Fourier transform instruments, or for gated integrator systems requiring a pulsed laser source. Use of this practice is intended only for trained optical spectroscopists and should be used in conjunction with standard texts.
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4.1 Assessment of the spectrometer resolution and instrument line shape (ILS) function of a Raman spectrometer is important for intercomparability of spectra obtained among widely varying spectrometer systems, if spectra are to be transferred among systems, if various sampling accessories are to be used, or if the spectrometer can be operated at more than one laser excitation wavelength.  
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4.3.1 First, it may be difficult to align the lamps properly with the sample position leading to distortion of the line, especially if the entrance slit of the spectrometer is underfilled or not symmetrically illuminated.  
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5.1 This technique is designed for on-site rapid screening and characterization of environmental soil and water samples resulting in significant cost savings for environmental remediation projects. Remote analysis can be made with optical fibers when situations warrant or demand use of this option.  
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1.1 This test method covers a rapid method for the screening of environmental samples for aromatic hydrocarbons (AHs) and polycyclic aromatic hydrocarbons (PAHs). The screening takes place in the field and provides immediate feedback on limits of contamination by substances containing AHs and PAHs. Quantification is obtained by the use of appropriately characterized, site-specific calibration curves. Remote sensing by use of optical fibers is useful for accessing difficult to reach areas or potentially dangerous materials or situations. When contamination of field personnel by dangerous materials is a possibility, use of remote sensors may minimize or eliminate the likelihood of such contamination taking place.  
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ASTM E334-01(2021)(Practice)
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.

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