Gcms
Gcms
Analytical Letters
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To cite this article: J. Sneddon , S. Masuram & J. C. Richert (2007): Gas ChromatographyMass
SpectrometryBasic Principles, Instrumentation and Selected Applications for Detection of Organic
Compounds, Analytical Letters, 40:6, 1003-1012
To link to this article: http://dx.doi.org/10.1080/00032710701300648
MINI-REVIEW
Abstract: This mini-review discusses the analytical technique of gas chromatographymass spectrometry (GC-MS), specifically basic principles and instrumentations. The
applications of GC-MS to a number of studies for determining organic compounds
from around the world are presented and highlight its universal use and acceptance.
Selected applications show that GC-MS is an integral and complimentary part of
many field studies involving organic compound detection and determination.
Keywords: Gas chromatography-mass spectrometry, organic compounds, environmental samples
INTRODUCTION
Since its development in the mid-1950s, gas chromatography-mass spectrometry (GC-MS) has become indispensable in the chemical analysts laboratory. While it can be used to determine drugs and metabolites in the
Received 12 February 2007; accepted 24 February 2007
The authors acknowledge, with thanks, the support of Environmental Protection
Agency, EPA-R-82958401-1. One of us (SM) is a Coastal Restoration and Enhancement through Science and Technology (CREST) Graduate Scholars Fellow. We
thank the Board of Regents (BoR) of Louisiana for a Louisiana Education Quality
Science Fund (LEQSF) Research Teachers Graduate Fellowship for JCR.
Address correspondence to J. Sneddon, Department of Chemistry, McNeese State
University, PO. Box 90455, Lake Charles, Louisiana 70609. E-mail: jsneddon@
mcneese.edu
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cross-polarization magic angle spinning (CP-MAS) 13C NMR, Curie-pointpyrolysis-gas chromatograph-mass spectrometry (Cp-Py-GC-MS), and by
pyrolysis-field ionization mass spectrometry (Py-FIMS). Long-term cultivation resulted in a large significant decrease in total soil organic matter
(SOM), as represented by total soil organic carbon. There were significant
increases in aromaticity of the SOM as a result of long-term cultivation as
indicated by CP-MAS 13C NMR spectroscopy. This was mainly attributable
to the result of cultivation-enhanced degradation of aliphatic carbon relative
to aromatic carbon. Organic compounds identified in the Cp-Py-GC-MS
spectra of the virgin and cultivated soils at site No. 4 consisted of n-alkanes
(ranging from C11 to C22) and alkenes (ranging from C7:1 to C21:1), with
the virgin soil being richer in alkenes than the cultivated soil. Other components identified were cyclic aromatics, carbo-cyclics, N-containing
aromatics, N-heterocyclics, benzene and substituted benzenes, phenols and
substituted phenols, and substituted furans. The compounds identified
appeared to originate from long-chain aliphatics, lignins, polyphenols,
aromatics, polysaccharides, and N-containing compounds in the two soils.
While similar compounds were identified by Py-FIMS in the two soils, the
total ion intensity (TII) of the virgin soil was almost 2.5 times as high as
that of the cultivated soil. This suggests that cultivation made the organic
matter less volatile, either by favoring the formation of higher molecular
weight organic matter or by promoting the formation of non-volatile metalorganic matter complexes. The Py-FIMS spectra showed that the virgin soil
contained relatively more lignin dimers, lipids, sterols, and n-C16 to n-C34
fatty acids than the cultivated soil. Thus, conversely, the cultivated soil was
richer in carbohydrates, phenols and lignin monomers, alkyl aromatics and
N-containing compounds, including peptides, than the virgin soil.
Soil organic matter (SOM) in five soil horizons from Arctic tundra and one
soil horizon from a temperate region was collected and separated into an extractable fraction (EF) and a non-extractable fraction (NEF) by dilute alkali (Dai
et al. 2002). The modified classical fractionation method was applied to characterize SOM in the EF; and the wet chemistry fractionation scheme, cross-polarization magic angle spinning (CP-MAS) 13C NMR, and pyrolysis-gas
chromatography-mass spectrometry (Py-GC-MS) techniques were used to
characterize SOM in the NEF. Each of these methods provided information
on the chemical compounds of SOM at varying angles. The NEF comprises a
large amount of SOM in these Arctic tundra soils and has great potential to
influence carbon cycling in these ecosystems with climate warming.
The relationship between the chemistry, biochemistry, and spectroscopic
characteristics of humic substances and clay mineralogy was studied (Laird
et al. 2001). Clay-humic complexes were separated from a Webster soil
(fine-loamy, mixed, superactive Typic Endoaquoll) by an invasive sonication-centrifugation technique. The samples were analyzed for mineralogy
by XRD (X-ray diffraction), chemical composition by inductively coupled
plasma-optical emission spectroscopy (ICP-OES), C and N by thermal
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different types of sample. The use of fast gas chromatography with a mass
spectrometer detector coupled to the headspace sampler allows identification
of the major hydrocarbons present in the mineral and organic polluted
samples; interpretation of the results obtained, and demonstrates the analytical
potential of headspace-mass spectrometry coupling.
Four recent applications of analytical pyrolysis in environmental science
and engineering are discussed (White et al. 2004). In all applications, samples
were analyzed to provide information about the origin of organic matter or
changes to an organic matrix. In the first application, GC/MS and
pyrolysis-GC/flame ionization detection (FID) were used to classify the
origin of natural organic matter (NOM) buried in the Antarctic. In the
second application, pyrolysis-GC-MS was used to compare the recalcitrance
of NOM to biodegradation. In the third application, pyrolysis-GC-FID was
used to quantatively differentiate between lipogenic NOM and petroleum
pollution in highly organic soil. In the fourth application, pyrolysis-GC-MS
was used to fingerprint organic matter in water samples to describe the
relationship between surface water, groundwater, and springs in a complex
watershed. In all applications, the benefits of pyrolysis analysis are still
being discovered.
A method for determining of all phenols, alkylphenols, and chlorophenols
in organic matter extracted from bottom sediments is presented (Czaplicka
2001). The analytical procedure comprises extraction with dichloromethane
in an ultrasonic field, separation of acidic compounds using acid-basic extraction, and determination of the phenols and chlorophenols using GC-MS. The
method has demonstrated the presence of phenol, its alkyl derivatives, and
chlorophenols, the last in insignificant amounts.
Collection and analysis of organic pollutants at depth without bringing
soil to the surface is described (Robbat 2001). A thermal extraction cone
penetrometer (TECP) probe was used to extract soil-bound semi-volatile
organics, transferring them to the surface for ultra-fast GC-MS analysis.
Findings showed that polychlorinated biphenyls, polycyclic aromatic hydrocarbons, chlorinated pesticides, and explosives could be collected and
analyzed in 5 min when soil water content was , 20% and in 15 min when
soil water content was 20 35%. When the TECP was directly connected to
the GC-MS, TNT and four of its synthetic precursors were speciated in 20
s. Moreover, 51 volatile organic compounds were detected by membraneinlet mass spectrometry in approximately 10 s. Organics were sniffed from
a vial and were identified using ion fingerprint detection software. The algorithms provide the means to untangle complex mass spectra making real-time,
electronic nose detection, and identification by MS possible.
A method of using headspace-GC-MS system to detect volatile organic
compounds in water is described (Cantu et al. 2004). This method corresponds
to the performance requirements for the analysis of drinking water. The
equipment setup and parameters are given along with a list of successfully
detected compounds.
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