Organic compounds in non-saline sediments 137
Guiney et al [88] showed that fused silica capillary gas chromatography offered
high resolution and precision and provided reasonable detection limits for analysing
kerosene range hydrocarbons in non-saline sediments isolated from rivers and streams.
GC MS has been used for the rapid determination of total anthropogenic petroleum
hydrocarbons in sediment [89 90].
Miscellaneous
Another technique that has been used to determine anthropogenic polycyclicaromatic hydrocarbon in sediments include fluorescence spectrometry [91]. Broman et al
[92] have discussed methods of fingerprinting petroleum hydrocarbons in bottom
sediments.
Petroleum pollution monitoring laboratories in the Mediterranean region participated (1984–1986) in two intercalibration exercises (METCAL I and II) to evaluate the
International Oceanographic Commission (IOC) Manual for petroleum hydrocarbon
determination in sediment (IOC, Manuals and Guides, No. 11). The main source of
error in the analysis was the extraction/partition step.
6.2 OXYGEN CONTAINING COMPOUNDS
6.2.1 Phenols
Goldberg and Weiner et al [93] have described methods for the extraction and concentration of phenolic compounds from sediment. Lopez Avila et al [94] have described a
microwave assisted extraction procedure for the separation of phenols from sediments.
Ding and Fang et al [95] achieved quantitative extraction of 4-nonylphenol from
sediments with shorter extraction times and with less solvent use by employing
pressurised liquid extraction.
Ale et al [96] have discussed the performance of different extraction media for the
ultrasonic-assisted extraction of nonylphenol and nonyphenol mono and di ethoxylates from sediments. A systematic study was undertaken to optimise and compare
the performance of different extraction media employing ultrasonic-assisted extraction for the recovery of nonylphenol and nonylphenol mono- and diethoxylates
(NP 1 EO and NP 2 EO respectively) from different spiked sediments (sand, clay and soil).
Dichloromethane and ethyl acetate were used alone or with methanol. Normal phase
high performance liquid chromatography with fluorescence detection (HPLC-FL) was
used for separation and quantification. In a first stage, a screening Plackett-Burman
experimental design was used as a multivariate strategy to evaluate the effect of three
variables (solvent polarity, analytes concentrations and sonication time), at two levels each, on spiked clay. Solvent polarity was found to be the most influential factor,
especially on the recovery of NP 2 EO. In a second stage, based on the screening results,
time was set at 5 minutes to evaluate the performance of a: and a methyl alcohol
1:1 dichloromethane and a 1:1 methyl alcohol: ethyl acetate mixture on spiked sand,
clay and soil. The 1:1 methyl alcohol ethyl acetate mixture led to highly satisfactory
recoveries for every analyte, statistically comparable to those yielded by a 1:1 methyl
alcohol ethyl mixture (NP > 85%, NP 1 EO and NP 2 > 90%). Due to similar interaction observed between each single sediment and the 1:1 methyl alcohol ethyl acetate
Guiney et al [88] showed that fused silica capillary gas chromatography offered
high resolution and precision and provided reasonable detection limits for analysing
kerosene range hydrocarbons in non-saline sediments isolated from rivers and streams.
GC MS has been used for the rapid determination of total anthropogenic petroleum
hydrocarbons in sediment [89 90].
Miscellaneous
Another technique that has been used to determine anthropogenic polycyclicaromatic hydrocarbon in sediments include fluorescence spectrometry [91]. Broman et al
[92] have discussed methods of fingerprinting petroleum hydrocarbons in bottom
sediments.
Petroleum pollution monitoring laboratories in the Mediterranean region participated (1984–1986) in two intercalibration exercises (METCAL I and II) to evaluate the
International Oceanographic Commission (IOC) Manual for petroleum hydrocarbon
determination in sediment (IOC, Manuals and Guides, No. 11). The main source of
error in the analysis was the extraction/partition step.
6.2 OXYGEN CONTAINING COMPOUNDS
6.2.1 Phenols
Goldberg and Weiner et al [93] have described methods for the extraction and concentration of phenolic compounds from sediment. Lopez Avila et al [94] have described a
microwave assisted extraction procedure for the separation of phenols from sediments.
Ding and Fang et al [95] achieved quantitative extraction of 4-nonylphenol from
sediments with shorter extraction times and with less solvent use by employing
pressurised liquid extraction.
Ale et al [96] have discussed the performance of different extraction media for the
ultrasonic-assisted extraction of nonylphenol and nonyphenol mono and di ethoxylates from sediments. A systematic study was undertaken to optimise and compare
the performance of different extraction media employing ultrasonic-assisted extraction for the recovery of nonylphenol and nonylphenol mono- and diethoxylates
(NP 1 EO and NP 2 EO respectively) from different spiked sediments (sand, clay and soil).
Dichloromethane and ethyl acetate were used alone or with methanol. Normal phase
high performance liquid chromatography with fluorescence detection (HPLC-FL) was
used for separation and quantification. In a first stage, a screening Plackett-Burman
experimental design was used as a multivariate strategy to evaluate the effect of three
variables (solvent polarity, analytes concentrations and sonication time), at two levels each, on spiked clay. Solvent polarity was found to be the most influential factor,
especially on the recovery of NP 2 EO. In a second stage, based on the screening results,
time was set at 5 minutes to evaluate the performance of a: and a methyl alcohol
1:1 dichloromethane and a 1:1 methyl alcohol: ethyl acetate mixture on spiked sand,
clay and soil. The 1:1 methyl alcohol ethyl acetate mixture led to highly satisfactory
recoveries for every analyte, statistically comparable to those yielded by a 1:1 methyl
alcohol ethyl mixture (NP > 85%, NP 1 EO and NP 2 > 90%). Due to similar interaction observed between each single sediment and the 1:1 methyl alcohol ethyl acetate