160 Organic compounds in soils, sediments & sludges
times with a methanol-benzene (1:1) mixture. After the solvent was evaporated the
residue was dissolved in hot water and this solution used for analysis of (MBAS)
alkyl benzene-sulphonate (ABS) and fluorescent whitening agent (FWA) in bottom
sediments.
Stroll and Giger et al [199] have described a reverse phase high-performance liquid chromatographic method for the determination of detergent derived fluorescent
whitening agent isomers in lake sediments.
Sterioisomers of two main laundry detergent fluorescent whitening agents of the
diaminostilbene type (DAS 1) and the distyrylbiphenyl type (DSBP), as well as total BLS
were quanititated in sediments and water from Greifensee, a lake in Switzerland. The
freeze-dried sediments were extracted in an ultrasonic bath using methanol with tetrabutylammonium hydrogen sulphate as an ion-pairing reagent. Aqueous samples were
extracted with C 18 extraction disks, which were subsequently eluted by methanol with
tetrabutylammonium hydrogen sulphate. Extracts from solid samples were analysed
by reversed-phase high-performance liquid chromatography. Fluorescence detection
was applied after post-column UV irradiation. Analytical reproducibility ranged from
1 to 12% (Relative standard deviation) was 1–11 g/kg of dry matter. Recoveries ranged
from 93 to 100% in solid samples. Concentrations of DAS-1 and DSBP ranged from
0.4 to 1.4 mg/kg of dry matter on top matter sediment layers. Concentrations of BLS
were between 0.02 and 0.08 mg/kg of dry mater in top sediment layers.
6.8.4 Carbohydrates
McQuaker and Fung et al [65] determined carbohydrates in sediments spectrophotometrically at 485 nm by reacting with phenol and concentrated sulphuric acid.
Mopper and Regeus et al [200] determined monosaccharides in lake sediments with
a sensitivity of 0.1 nmol, using an automated chromatographic sugar analyser. The test
solution is forced by nitrogen pressure into a nylon column (110 cm × 2.8 mm) packed
with Echnicon type S resin (sulphate form) and maintained at 76
◦ C. The sugars are
separated by pumping 89% ethanol through the column and the eluate is mixed with
an alkaline solution of tetrazolium blue which is considerably more sensitive and less
corrosive than other dyes. The extinction is monitored at 520 nm.
6.8.5 Uronic acids and aldoses
These substances can be determined by a procedure [201] involving preliminary
hydrolysis with hydrofluoric acid at 135
◦ C producing N-alkyl aldonamide and
alditolacetates. These substances are then determined by capillary column gas
chromatography.
6.8.6 Pharmaceuticals
Himmelsbach et al [202] determined pharmaceutical drug residues in particulate
material in surface water. In this paper a gas chromatographic method with mass spectrometric detection is presented which allows the determination of the particle-bound
fraction of some pharmaceuticals commonly found in surface water. Determination
limits are between 2 and 12 ng/g particles. Results from surface water samples indicate
times with a methanol-benzene (1:1) mixture. After the solvent was evaporated the
residue was dissolved in hot water and this solution used for analysis of (MBAS)
alkyl benzene-sulphonate (ABS) and fluorescent whitening agent (FWA) in bottom
sediments.
Stroll and Giger et al [199] have described a reverse phase high-performance liquid chromatographic method for the determination of detergent derived fluorescent
whitening agent isomers in lake sediments.
Sterioisomers of two main laundry detergent fluorescent whitening agents of the
diaminostilbene type (DAS 1) and the distyrylbiphenyl type (DSBP), as well as total BLS
were quanititated in sediments and water from Greifensee, a lake in Switzerland. The
freeze-dried sediments were extracted in an ultrasonic bath using methanol with tetrabutylammonium hydrogen sulphate as an ion-pairing reagent. Aqueous samples were
extracted with C 18 extraction disks, which were subsequently eluted by methanol with
tetrabutylammonium hydrogen sulphate. Extracts from solid samples were analysed
by reversed-phase high-performance liquid chromatography. Fluorescence detection
was applied after post-column UV irradiation. Analytical reproducibility ranged from
1 to 12% (Relative standard deviation) was 1–11 g/kg of dry matter. Recoveries ranged
from 93 to 100% in solid samples. Concentrations of DAS-1 and DSBP ranged from
0.4 to 1.4 mg/kg of dry matter on top matter sediment layers. Concentrations of BLS
were between 0.02 and 0.08 mg/kg of dry mater in top sediment layers.
6.8.4 Carbohydrates
McQuaker and Fung et al [65] determined carbohydrates in sediments spectrophotometrically at 485 nm by reacting with phenol and concentrated sulphuric acid.
Mopper and Regeus et al [200] determined monosaccharides in lake sediments with
a sensitivity of 0.1 nmol, using an automated chromatographic sugar analyser. The test
solution is forced by nitrogen pressure into a nylon column (110 cm × 2.8 mm) packed
with Echnicon type S resin (sulphate form) and maintained at 76
◦ C. The sugars are
separated by pumping 89% ethanol through the column and the eluate is mixed with
an alkaline solution of tetrazolium blue which is considerably more sensitive and less
corrosive than other dyes. The extinction is monitored at 520 nm.
6.8.5 Uronic acids and aldoses
These substances can be determined by a procedure [201] involving preliminary
hydrolysis with hydrofluoric acid at 135
◦ C producing N-alkyl aldonamide and
alditolacetates. These substances are then determined by capillary column gas
chromatography.
6.8.6 Pharmaceuticals
Himmelsbach et al [202] determined pharmaceutical drug residues in particulate
material in surface water. In this paper a gas chromatographic method with mass spectrometric detection is presented which allows the determination of the particle-bound
fraction of some pharmaceuticals commonly found in surface water. Determination
limits are between 2 and 12 ng/g particles. Results from surface water samples indicate