232 Organic compounds in soils, sediments & sludges
Roe et al [143] has discussed the determination of volatile compounds (methandiol,
dimethyl sulphide) and also hydrogen sulphide and sulphur dioxide in sewage samples.
Konig et al [141] using gas chromatography-mass spectrometry, have identified
dimethyl di-, tri- and tetrasulphides in sewage works samples. These substances can
be used by microorganisms as precursors of sulphuric acid, which would explain
unexpectedly high corrosion rates of concrete pipes.
Winter et al [142] employed purge and trap sampling of sewage sludge samples
followed by GC-MS to identify various sulphides, particularly dimethyl trisulphide.
10.5.2 Thiosteroids
Mejia et al [144] identified and determined thiosteroids and their post treatment
products in sewage sludge. These include steroid thiols: 5α-chloestane-3-thiol, 2.4methyl-5α-cholestane-3-thiol and 2.4-ethyl-5α-cholestane-3-thiol were detected in the
gas chromatography with mass spectrometry detector (GC-MS) analysis. These three
compounds, related to the thiostanol family, have only been encountered in previous
studies in sea sediments. Gas chromatography with sulphur-selective flame photometric detector was used with the objective of detecting other related compounds in sludge.
It allowed the detection of other compounds whose mass spectra could correspond
with the one of steroid enethiols. The research focused on detecting the formation
point of these sulphur compounds in the sludge treatment process, as well as their
biodegradation resistance in the post-treatment processes. The amount of these products in the sludge was quantified using gas chromatography with flame ionisation
detector (GC-FID). This study confirmed that the identified compounds are not easily
biodegradable.
10.6 PHOSPHORUS COMPOUNDS
McIntyre et al [145] investigated methods for determining organophosphorus compounds in sewage sludge and made a survey of sewage sludges from 12 different UK
sewage treatment works. Highest recoveries were achieved using the disperser method,
together with an alumina column clean-up step, and analysis by flame photometric gasliquid chromatography. The survey results indicate that organophosphorus compounds
are not very common micropollutants of sewage sludges.
10.7 INSECTICIDES PESTICIDES HERBICIDES
10.7.1 Organochlorine insecticides
Gas chromatography
Various workers [146–158] have reported methods for the determination of polychlorobiphenyls and organochlorine insecticides in sewage and sewage sludges.
Mattson and Mugren et al [153] have described the chromatographic procedure
for the determination of polychlorobiphenyls and some chlorinated insecticides in
sewage sludge. The capillary column is coated with silicone oil SF96.
The sample is extracted with a mixture of hexane, acetone and water. After separation, the hexane phase is reduced in volume and divided into two aliquots, one
Roe et al [143] has discussed the determination of volatile compounds (methandiol,
dimethyl sulphide) and also hydrogen sulphide and sulphur dioxide in sewage samples.
Konig et al [141] using gas chromatography-mass spectrometry, have identified
dimethyl di-, tri- and tetrasulphides in sewage works samples. These substances can
be used by microorganisms as precursors of sulphuric acid, which would explain
unexpectedly high corrosion rates of concrete pipes.
Winter et al [142] employed purge and trap sampling of sewage sludge samples
followed by GC-MS to identify various sulphides, particularly dimethyl trisulphide.
10.5.2 Thiosteroids
Mejia et al [144] identified and determined thiosteroids and their post treatment
products in sewage sludge. These include steroid thiols: 5α-chloestane-3-thiol, 2.4methyl-5α-cholestane-3-thiol and 2.4-ethyl-5α-cholestane-3-thiol were detected in the
gas chromatography with mass spectrometry detector (GC-MS) analysis. These three
compounds, related to the thiostanol family, have only been encountered in previous
studies in sea sediments. Gas chromatography with sulphur-selective flame photometric detector was used with the objective of detecting other related compounds in sludge.
It allowed the detection of other compounds whose mass spectra could correspond
with the one of steroid enethiols. The research focused on detecting the formation
point of these sulphur compounds in the sludge treatment process, as well as their
biodegradation resistance in the post-treatment processes. The amount of these products in the sludge was quantified using gas chromatography with flame ionisation
detector (GC-FID). This study confirmed that the identified compounds are not easily
biodegradable.
10.6 PHOSPHORUS COMPOUNDS
McIntyre et al [145] investigated methods for determining organophosphorus compounds in sewage sludge and made a survey of sewage sludges from 12 different UK
sewage treatment works. Highest recoveries were achieved using the disperser method,
together with an alumina column clean-up step, and analysis by flame photometric gasliquid chromatography. The survey results indicate that organophosphorus compounds
are not very common micropollutants of sewage sludges.
10.7 INSECTICIDES PESTICIDES HERBICIDES
10.7.1 Organochlorine insecticides
Gas chromatography
Various workers [146–158] have reported methods for the determination of polychlorobiphenyls and organochlorine insecticides in sewage and sewage sludges.
Mattson and Mugren et al [153] have described the chromatographic procedure
for the determination of polychlorobiphenyls and some chlorinated insecticides in
sewage sludge. The capillary column is coated with silicone oil SF96.
The sample is extracted with a mixture of hexane, acetone and water. After separation, the hexane phase is reduced in volume and divided into two aliquots, one