226 Organic compounds in soils, sediments & sludges
high-performance liquid chromatography gave information on structure and concentration of alkylphenol polyethoxylates surfactants in sewage and sewage sludges.
Nonylphenol ethoxylates with 1–18 ethoxy units were found in untreated wastes at
0.8–2 3 mg per litre. Boyd-Boland and Pawliszyn et al [74] have used solid-phase
microextraction coupled with high-performance liquid chromatography to determine
alkylphenol ethoxylate (Triton X-100) surface active agent in sewage effluent samples. These workers used normal phase gradient elution and detection by ultraviolet
absorbance at 220nm to determine alkylphenol ethyloxylates (Triton ×100) surface
active agent in sewage effluent samples. Carbowax-templates resin or Carbowaxdivinylbenzene coatings on the column allowed successful analysis of the ethoxylates
with a linear range of 100–1 mg L
−1 . Limits of detection were in the low microgram
per litre range.
Crozier et al [75] reported a rapid screening procedure for nonylphenol ethoxylates in sewage treatment plant samples based on flow injection liquid chromatography
(APCI-MS). By using precursor scanning and multiple reaction monitoring total
nonyl phenolethyoxylate in samples could be determined at concentrations as low
as 50 ng L
−1 .
Holt et al [49] have described a high performance liquid chromatographic method
with fluorimetric detection for the determination of down to 0.2 µg L
−1 of alkyl phenol
mono and diethyoxylates in sewage sludge.
Spectrophotometric methods
Dozanska et al [76] has described a spectrophotometric method involving reaction
with cobalt thiocyanate or tungstophosphoric acid for the determination of non-ionic
detergents in sewage. Stephanou and Giger et al [77] carried out quantitative determinations of nonylphenolethoxylates and nonylphenol in sewage effluents by capillary
gas chromatography.
Waters et al [78] investigated the scope and limitations of the Wickbold active
substances procedure for the determination of non-ionic substances in sewage. The
method was found to be unsuitable for sewage which gives low recoveries.
10.3 CHLORINE CONTAINING COMPOUNDS
10.3.1 Chlorinated hydrocarbons
Gas Chromatography
Von Duzzeln et al [79] and Henderson and Glaze et al [80] have discussed the gas
chromatographic determination of chlorinated hydrocarbons in sewage. Henderson
and Glaze et al [80] used a gas chromatography-mass spectrometry computer program
to manipulate the data to produce a limited cluster search, the resulting chromatogram
indicates the peaks on the total ion chromatogram which possess a specific number of
chlorine or bromine atoms.
H. M. Stationery Office (UK) [81] have described methods for the determination
of chlorinated hydrocarbons, organochlorine pesticides and polychlorinated biphenols
in sewage sludge.
high-performance liquid chromatography gave information on structure and concentration of alkylphenol polyethoxylates surfactants in sewage and sewage sludges.
Nonylphenol ethoxylates with 1–18 ethoxy units were found in untreated wastes at
0.8–2 3 mg per litre. Boyd-Boland and Pawliszyn et al [74] have used solid-phase
microextraction coupled with high-performance liquid chromatography to determine
alkylphenol ethoxylate (Triton X-100) surface active agent in sewage effluent samples. These workers used normal phase gradient elution and detection by ultraviolet
absorbance at 220nm to determine alkylphenol ethyloxylates (Triton ×100) surface
active agent in sewage effluent samples. Carbowax-templates resin or Carbowaxdivinylbenzene coatings on the column allowed successful analysis of the ethoxylates
with a linear range of 100–1 mg L
−1 . Limits of detection were in the low microgram
per litre range.
Crozier et al [75] reported a rapid screening procedure for nonylphenol ethoxylates in sewage treatment plant samples based on flow injection liquid chromatography
(APCI-MS). By using precursor scanning and multiple reaction monitoring total
nonyl phenolethyoxylate in samples could be determined at concentrations as low
as 50 ng L
−1 .
Holt et al [49] have described a high performance liquid chromatographic method
with fluorimetric detection for the determination of down to 0.2 µg L
−1 of alkyl phenol
mono and diethyoxylates in sewage sludge.
Spectrophotometric methods
Dozanska et al [76] has described a spectrophotometric method involving reaction
with cobalt thiocyanate or tungstophosphoric acid for the determination of non-ionic
detergents in sewage. Stephanou and Giger et al [77] carried out quantitative determinations of nonylphenolethoxylates and nonylphenol in sewage effluents by capillary
gas chromatography.
Waters et al [78] investigated the scope and limitations of the Wickbold active
substances procedure for the determination of non-ionic substances in sewage. The
method was found to be unsuitable for sewage which gives low recoveries.
10.3 CHLORINE CONTAINING COMPOUNDS
10.3.1 Chlorinated hydrocarbons
Gas Chromatography
Von Duzzeln et al [79] and Henderson and Glaze et al [80] have discussed the gas
chromatographic determination of chlorinated hydrocarbons in sewage. Henderson
and Glaze et al [80] used a gas chromatography-mass spectrometry computer program
to manipulate the data to produce a limited cluster search, the resulting chromatogram
indicates the peaks on the total ion chromatogram which possess a specific number of
chlorine or bromine atoms.
H. M. Stationery Office (UK) [81] have described methods for the determination
of chlorinated hydrocarbons, organochlorine pesticides and polychlorinated biphenols
in sewage sludge.