Organic compounds in soils 47
Neumayr et al [124] has discussed methods for sampling soil atmospheres and
gives a detailed account of gas chromatographic methods employing electron capture
and flame ionization detectors for detecting and estimating specific components of the
soil atmosphere.
Krock and Wilkins et al [229] have used multi-dimensional gas chromatography
with infrared and mass spectrometric detection to determine organics in soil. Direct
acetylation followed by gas chromatography with flame ionisation, electron capture
and mass spectrometric detectors has been used to determine phenolic residues in soil
[119]. Llopart-Visoso et al [118] have used direct acetylation followed by headspace
gas chromatography to determine mixtures of phenolic and cresolic components of soil.
2.9.2 Pyrolysis-gas chromatography-mass spectrometry
De Leeuw et al [32] have described a method for the screening in soils and sediments of
anthropogenic compounds including polycyclic aromatic hydrocarbons, haloorganics,
aliphatic hydrocarbons, heteroaromatics, elemental sulphur and pyrolysis products of
synthetic polymers. Elimination of wet chemical sample preparation enables a complete
analysis to be performed and data to be quickly analysed. The detection limits are in the
low part-per-million range using mass spectrometric detection. Alternatively, detection
of compounds can be achieved by all common gas chromatography detectors (flame
ionisation detector, electron capture detector and flame photometric detector) and
detection limits are determined by the method of detection employed.
The polyaromatic hydrocarbons in the soil sample were quantitated by using an
external standard of anthracene. The results reportedly for a polluted soil and sediment sample indicate that this flash evaporated-pyrolysis technique combined with gas
chromatography-mass spectrometry is a valuable tool for rapidly screening polluted
samples for virtually all types of anthropogenic contaminants except for heavy metals.
This method allows for the simultaneous detection of highly volatile (e.g. dioxane), volatile (e.g. polyaromatic hydrocarbons) and non-volatile (e.g. polystyrene)
substances. The sensitivity of the method depends of course on the detector(s) used.
Pyrolysis-gas chromatography has been reported for the analysis of soil samples
by several investigators [197, 292, 295]. Barrio et al [295] used pyrolysis gas chromatography to study organic matter evolution in sewage sludge-amended soils by
using nitrogen-phosphorus, flame ionisation and mass spectrometric detection. Two
methylation reagents and two pyrolysis gas chromatographic techniques have been
used by Schulten et al [292] for organics in soil. Both methylation procedures studied gave valuable additional information on the occurrence of aliphatic and aromatic
carboxylic acids, substituted phenols, benzenediols, benzenetriols, phenolic acids and
amides in soil organic matter. Pyrolysis products of explosives in soil have been studied
by using pyrolysis-gas chromatography with a turnable infrared laser detector [197].
Schnitzer and Shulten et al [296] have reviewed the analysis of organic matter in soil
extracts and whole soils using pyrolysis mass spectrometry.
2.9.3 Purge and trap gas chromatography
The use of capillary columns in gas chromatography coupled with purge and trap
concentrations has been accelerated by the publication of methods for the analysis of
Neumayr et al [124] has discussed methods for sampling soil atmospheres and
gives a detailed account of gas chromatographic methods employing electron capture
and flame ionization detectors for detecting and estimating specific components of the
soil atmosphere.
Krock and Wilkins et al [229] have used multi-dimensional gas chromatography
with infrared and mass spectrometric detection to determine organics in soil. Direct
acetylation followed by gas chromatography with flame ionisation, electron capture
and mass spectrometric detectors has been used to determine phenolic residues in soil
[119]. Llopart-Visoso et al [118] have used direct acetylation followed by headspace
gas chromatography to determine mixtures of phenolic and cresolic components of soil.
2.9.2 Pyrolysis-gas chromatography-mass spectrometry
De Leeuw et al [32] have described a method for the screening in soils and sediments of
anthropogenic compounds including polycyclic aromatic hydrocarbons, haloorganics,
aliphatic hydrocarbons, heteroaromatics, elemental sulphur and pyrolysis products of
synthetic polymers. Elimination of wet chemical sample preparation enables a complete
analysis to be performed and data to be quickly analysed. The detection limits are in the
low part-per-million range using mass spectrometric detection. Alternatively, detection
of compounds can be achieved by all common gas chromatography detectors (flame
ionisation detector, electron capture detector and flame photometric detector) and
detection limits are determined by the method of detection employed.
The polyaromatic hydrocarbons in the soil sample were quantitated by using an
external standard of anthracene. The results reportedly for a polluted soil and sediment sample indicate that this flash evaporated-pyrolysis technique combined with gas
chromatography-mass spectrometry is a valuable tool for rapidly screening polluted
samples for virtually all types of anthropogenic contaminants except for heavy metals.
This method allows for the simultaneous detection of highly volatile (e.g. dioxane), volatile (e.g. polyaromatic hydrocarbons) and non-volatile (e.g. polystyrene)
substances. The sensitivity of the method depends of course on the detector(s) used.
Pyrolysis-gas chromatography has been reported for the analysis of soil samples
by several investigators [197, 292, 295]. Barrio et al [295] used pyrolysis gas chromatography to study organic matter evolution in sewage sludge-amended soils by
using nitrogen-phosphorus, flame ionisation and mass spectrometric detection. Two
methylation reagents and two pyrolysis gas chromatographic techniques have been
used by Schulten et al [292] for organics in soil. Both methylation procedures studied gave valuable additional information on the occurrence of aliphatic and aromatic
carboxylic acids, substituted phenols, benzenediols, benzenetriols, phenolic acids and
amides in soil organic matter. Pyrolysis products of explosives in soil have been studied
by using pyrolysis-gas chromatography with a turnable infrared laser detector [197].
Schnitzer and Shulten et al [296] have reviewed the analysis of organic matter in soil
extracts and whole soils using pyrolysis mass spectrometry.
2.9.3 Purge and trap gas chromatography
The use of capillary columns in gas chromatography coupled with purge and trap
concentrations has been accelerated by the publication of methods for the analysis of