190 Organic compounds in soils, sediments & sludges
Takada and Ishimatari et al [4] extracted alkylbenzenes with normal C 10 −C 14
and branched C 11 −C 13 alkyl chains from marine and coastal sediment and suspended
matter in benzene methanol. The extract in benzene was then applied to a Florisil
column for removal of copper sulphide and polar materials, and then subjected to
silica gel column chromatography. Alkyl benzenes were quantified and identified using
gas chromatography with flame ionisation detection. The recoveries of alkyl benzenes
were 81−84%.
Whittle et al [5] has described a thin-layer chromatographic method for the
identification of hydrocarbon marker dyes in oil polluted waters.
McLeod et al [6] conducted inter-laboratory comparisons of methods for determining traces of aliphatic and aromatic hydrocarbons in marine sediments. Agreement
within a factor of 2 to 3 was obtained between the 12 participating laboratories.
Mark et al [7] has described an infrared method for the determination of the oil
content of marine sediments. He showed that the magnitude of the CH 2 stretching
band at 2925 cm
−1 , normally used to determine oil in a sediment, is enhanced when
biological matter is also present. The concentration of this material can generally be
estimated from the magnitude of the protein-NH band at 1650 cm
−1 with the use of a
calculated correction to the total absorption at 2925 cm
−1 , but the oil must contribute
less than 10% to the total absorption at 2925 cm
−1 . It is desirable, however, that
the nature of the organic matter be determined by means of a study of the complete
infrared spectrum.
Oil spills
Gas chromatography has also been used to distinguish between fossil fuels added to
sediments through oil pollution and those hydrocarbons present in low concentrations
as natural biogenic products (Blumer and Sass [13]; Farrington and Quinn [14]).
Page et al [15] used capillary gas chromatography and capillary gas
chromatography-mass spectrometry to determine aliphatic hydrocarbons in interstitial
sediments collected on the French coastline following the Amoco Cadiz disaster.
Brown et al [16] have described a rapid field method for detecting down to 2 µg
of oil in sediments associated with marine oil spills. The method was employed in
connection with the Argo Merchant oil spill off Nantuckett in December 1976.
In this method the sediment is mixed with sodium sulphate and extracted with
n-hexane. A portion of the extract is applied to a paper strip which is then eluted with
petroleum ether:benzene (35:65) for 60 seconds. Viewing of the strip under ultraviolet
light reveals a blue fluorescent spot indicating the presence of oil in the sediment.
Fluorescence spectroscopy has been adapted as an alternative analytical method
for estimating oil in sediments [23, 24, 8, 9].
Interlocutory, comparisons have been performed on a determination of selected
trace aliphatic and aromatic hydrocarbons in marine sediments [10–12].
8.1.1.2 Aromatic hydrocarbons
Henning et al [17] has applied ultraviolet spectroscopy to the determination of aromatic constituents of residual fuel oil in hexane extracts of marine sediment samples.
Examination of the ultraviolet spectra of samples of an oil pollutant from a beach
and of crude oil, at various concentrations, revealed strong absorption maxima at
Takada and Ishimatari et al [4] extracted alkylbenzenes with normal C 10 −C 14
and branched C 11 −C 13 alkyl chains from marine and coastal sediment and suspended
matter in benzene methanol. The extract in benzene was then applied to a Florisil
column for removal of copper sulphide and polar materials, and then subjected to
silica gel column chromatography. Alkyl benzenes were quantified and identified using
gas chromatography with flame ionisation detection. The recoveries of alkyl benzenes
were 81−84%.
Whittle et al [5] has described a thin-layer chromatographic method for the
identification of hydrocarbon marker dyes in oil polluted waters.
McLeod et al [6] conducted inter-laboratory comparisons of methods for determining traces of aliphatic and aromatic hydrocarbons in marine sediments. Agreement
within a factor of 2 to 3 was obtained between the 12 participating laboratories.
Mark et al [7] has described an infrared method for the determination of the oil
content of marine sediments. He showed that the magnitude of the CH 2 stretching
band at 2925 cm
−1 , normally used to determine oil in a sediment, is enhanced when
biological matter is also present. The concentration of this material can generally be
estimated from the magnitude of the protein-NH band at 1650 cm
−1 with the use of a
calculated correction to the total absorption at 2925 cm
−1 , but the oil must contribute
less than 10% to the total absorption at 2925 cm
−1 . It is desirable, however, that
the nature of the organic matter be determined by means of a study of the complete
infrared spectrum.
Oil spills
Gas chromatography has also been used to distinguish between fossil fuels added to
sediments through oil pollution and those hydrocarbons present in low concentrations
as natural biogenic products (Blumer and Sass [13]; Farrington and Quinn [14]).
Page et al [15] used capillary gas chromatography and capillary gas
chromatography-mass spectrometry to determine aliphatic hydrocarbons in interstitial
sediments collected on the French coastline following the Amoco Cadiz disaster.
Brown et al [16] have described a rapid field method for detecting down to 2 µg
of oil in sediments associated with marine oil spills. The method was employed in
connection with the Argo Merchant oil spill off Nantuckett in December 1976.
In this method the sediment is mixed with sodium sulphate and extracted with
n-hexane. A portion of the extract is applied to a paper strip which is then eluted with
petroleum ether:benzene (35:65) for 60 seconds. Viewing of the strip under ultraviolet
light reveals a blue fluorescent spot indicating the presence of oil in the sediment.
Fluorescence spectroscopy has been adapted as an alternative analytical method
for estimating oil in sediments [23, 24, 8, 9].
Interlocutory, comparisons have been performed on a determination of selected
trace aliphatic and aromatic hydrocarbons in marine sediments [10–12].
8.1.1.2 Aromatic hydrocarbons
Henning et al [17] has applied ultraviolet spectroscopy to the determination of aromatic constituents of residual fuel oil in hexane extracts of marine sediment samples.
Examination of the ultraviolet spectra of samples of an oil pollutant from a beach
and of crude oil, at various concentrations, revealed strong absorption maxima at