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ASTM E1642-00(2005)

(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 the standard. The values given in parentheses are for information only.
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
31-Aug-2005
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 - Standard Practice for General Techniques of Gas Chromatography Infrared (GC/IR) Analysis
Effective Date
01-Sep-2005
Replaced By
ASTM E1642-00(2010) - Standard Practice for General Techniques of Gas Chromatography Infrared (GC/IR) Analysis
Effective Date
01-Mar-2010
Referred By
ASTM E334-01(2021) - Standard Practice for General Techniques of Infrared Microanalysis
Effective Date
01-Sep-2005
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-Sep-2005
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-Sep-2005
Referred By
ASTM E1252-98(2021) - Standard Practice for General Techniques for Obtaining Infrared Spectra for Qualitative Analysis
Effective Date
01-Sep-2005

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ASTM E1642-00(2005) - Standard Practice for General Techniques of Gas Chromatography Infrared (GC/IR) AnalysisASTM E1642-00(2005) - Standard Practice for General Techniques of Gas Chromatography Infrared (GC/IR) Analysis
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ASTM E1642-00(2005) - 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(Reapproved2005)
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 E1421 Practice 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
E1510 Practice 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
3.1 Definitions—Fordefinitionsoftermsandsymbols,refer
techniques discussed include eluent trapping, flowcell, and
to Terminology E131 and Practice E355.
eluite deposition.
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
4.1 This practice provides general guidelines for the proper
standard.
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
5. General GC/IR Techniques
2
2.1 ASTM Standards:
5.1 Three different types of GC/IR technique have been
E131 Terminology Relating to Molecular Spectroscopy
used to analyze samples. These consist of analyte trapping,
E168 Practices for General Techniques of Infrared Quanti-
flowcell, or lightpipe, and direct eluite deposition and are
tative Analysis
presented in the order that they were first used.
E260 Practice for Packed Column Gas Chromatography
5.2 The GC eluent must not be routed to a destructive GC
E334 Practice for General Techniques of Infrared Mi-
detector (such as a flame ionization detector) prior to reaching
croanalysis
the IR detector as this will destroy or alter the individual
E355 Practice for Gas Chromatography Terms and Rela-
components. It is acceptable to split the eluent so that part of
tionships
the stream is directed to such a detector or to pass the stream
E932 Practice for Describing and Measuring Performance
back to the detector after infrared analysis if such techniques
of Dispersive Infrared Spectrometers
are feasible.
E1252 PracticeforGeneralTechniquesforObtainingInfra-
5.3 Eluent Trapping Techniques—Analyte trapping tech-
red Spectra for Qualitative Analysis
niques are the least elaborate means for obtaining GC/IR data.
In these techniques, the sample eluting from the chromato-
1
This practice is under the jurisdiction ofASTM Committee E13 on Molecular
graph is collected in discrete aliquots to be analyzed. In
Spectroscopy and Separation Science and is the direct responsibility of Subcom-
utilizing such techniques, it is essential that a GC detector be
mittee E13.03 on Infrared and Near Infrared Spectroscopy.
employed to allow definition of component elution. If a
Current edition approved Sept. 1, 2005. Published September 2005. Originally
approved in 1994. Last previous edition approved in 2000 as E1642–00. DOI: destructive detector is employed, then post-column splitting to
10.1520/E1642-00R05.
that detector is required. GC fractions can be trapped in the
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
condensed phase by passing the GC effluent through a solvent,
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E1642–00 (2005)
a powdered solid, or a cold trap for subsequent analysis (see thecase,thetemperatureofthelight-pipeshouldbereducedto
3
Practice E1252) (1). Vapor phase samples can be trapped in a a safe level as soo
...

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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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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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