Organic compounds in saline marine and estuarine sediments 191
approximately 228 nm and 256 nm. The ratio of the peak heights at these wavelengths
is constant for a particular oil, and is independent of concentration. These permit
quantitative analysis of sediment samples many months after an oil spill.
Hargrave and Phillips et al [18] have used fluorescence spectroscopy to evaluate
concentrations of aromatic constituents in aquatic sediments. The oil concerned, a
Venezuelan crude, contained about 35% by weight of aromatic constituents. Aromatic
substances were extracted with n-hexane and fluorescence spectroscopy was used to
produce a series of contour diagrams of fluorescence intensity at various excitation
and emission wavelengths in order to compare fluorescence spectral pattern of sample
extracts and standard oils. Petroleum residues were determined and it was found that
total oil concentrations ranged from 10 to 3000 µg g
−1 wet sediment, with the highest
concentrations occurring in sedimenting particles.
Krahn et al [19] have described a high performance liquid chromatographic
method for the determination of 127 aromatic hydrocarbons and 21 chlorinated
hydrocarbons in solvent extracts of marine sediments.
Vowles and Mantoura et al [20] determined sediment-water partition coefficients
and the high-performance liquid chromatography capacity factors for 14 alkylbenzene and polyaromatic hydrocarbons. The partition coefficient correlated well with
the alkyl-cyano capacity factors, and it was concluded that this phase gave a better
indication of sorption on sediment than either the octanol or octadecylsilane phases.
8.1.1.3 Polycyclic aromatic hydrocarbons
Saber et al [21] used high resolution Shpol’skii spectrofluorimetry at 10
◦ K to quantitatively determine polyaromatic hydrocarbons in lacustral sediments. Polyaromatic
hydrocarbons incorporated into n-alkane matrix at low temperature yielded high resolution fluorescence spectra of quasi lines with a multiplet structure related to several
insertion sites. Samples required extraction and purification, and the choice of sample
treatment, which depended on the total organic pollution levels, is discussed.
A high-performance liquid chromatographic procedure [38] has been applied to
the determination of polyaromatic hydrocarbons in saline sediments.
Dunn and Stich et al [22] and Dunn et al [23] have described a monitoring procedure for polyaromatic hydrocarbons, particularly benzo[a]pyrene in marine sediments.
The procedures involve extraction and purification of hydrocarbon fractions from the
sediments and determination of compounds by thin layer chromatography and fluorometry, or gas chromatography. In this procedure, the sediment was refluxed with
ethanolic potassium hydroxide, then filtered and the filtrate extracted with isooctane.
The isooctane extract was cleaned up on a florisil column, then the polyaromatic hydrocarbons were extracted from the isoactive extract with pure dimethyl sulphoxide. The
latter phase was contacted with water, then extracted with isooctane to recover polyaromatic hydrocarbons. The overall recovery of polyaromatic hydrocarbons in this
extract by fluorescence spectroscopy was 50–70%.
Karakas and Pekey et al [24] carried out a source apportionment of polycyclic
aromatic hydrocarbons in surface sediments of Izmit Bay, Turkey. Thirty five surface
sediment samples were collected from the north eastern coast of the Izmit Bay to apportion the sources of polycyclic aromatic hydrocarbons entering the Bay. Samples were
collected in February and June 2002 and they were analysed for 16 polycyclic aromatic
approximately 228 nm and 256 nm. The ratio of the peak heights at these wavelengths
is constant for a particular oil, and is independent of concentration. These permit
quantitative analysis of sediment samples many months after an oil spill.
Hargrave and Phillips et al [18] have used fluorescence spectroscopy to evaluate
concentrations of aromatic constituents in aquatic sediments. The oil concerned, a
Venezuelan crude, contained about 35% by weight of aromatic constituents. Aromatic
substances were extracted with n-hexane and fluorescence spectroscopy was used to
produce a series of contour diagrams of fluorescence intensity at various excitation
and emission wavelengths in order to compare fluorescence spectral pattern of sample
extracts and standard oils. Petroleum residues were determined and it was found that
total oil concentrations ranged from 10 to 3000 µg g
−1 wet sediment, with the highest
concentrations occurring in sedimenting particles.
Krahn et al [19] have described a high performance liquid chromatographic
method for the determination of 127 aromatic hydrocarbons and 21 chlorinated
hydrocarbons in solvent extracts of marine sediments.
Vowles and Mantoura et al [20] determined sediment-water partition coefficients
and the high-performance liquid chromatography capacity factors for 14 alkylbenzene and polyaromatic hydrocarbons. The partition coefficient correlated well with
the alkyl-cyano capacity factors, and it was concluded that this phase gave a better
indication of sorption on sediment than either the octanol or octadecylsilane phases.
8.1.1.3 Polycyclic aromatic hydrocarbons
Saber et al [21] used high resolution Shpol’skii spectrofluorimetry at 10
◦ K to quantitatively determine polyaromatic hydrocarbons in lacustral sediments. Polyaromatic
hydrocarbons incorporated into n-alkane matrix at low temperature yielded high resolution fluorescence spectra of quasi lines with a multiplet structure related to several
insertion sites. Samples required extraction and purification, and the choice of sample
treatment, which depended on the total organic pollution levels, is discussed.
A high-performance liquid chromatographic procedure [38] has been applied to
the determination of polyaromatic hydrocarbons in saline sediments.
Dunn and Stich et al [22] and Dunn et al [23] have described a monitoring procedure for polyaromatic hydrocarbons, particularly benzo[a]pyrene in marine sediments.
The procedures involve extraction and purification of hydrocarbon fractions from the
sediments and determination of compounds by thin layer chromatography and fluorometry, or gas chromatography. In this procedure, the sediment was refluxed with
ethanolic potassium hydroxide, then filtered and the filtrate extracted with isooctane.
The isooctane extract was cleaned up on a florisil column, then the polyaromatic hydrocarbons were extracted from the isoactive extract with pure dimethyl sulphoxide. The
latter phase was contacted with water, then extracted with isooctane to recover polyaromatic hydrocarbons. The overall recovery of polyaromatic hydrocarbons in this
extract by fluorescence spectroscopy was 50–70%.
Karakas and Pekey et al [24] carried out a source apportionment of polycyclic
aromatic hydrocarbons in surface sediments of Izmit Bay, Turkey. Thirty five surface
sediment samples were collected from the north eastern coast of the Izmit Bay to apportion the sources of polycyclic aromatic hydrocarbons entering the Bay. Samples were
collected in February and June 2002 and they were analysed for 16 polycyclic aromatic