234 Organic compounds in soils, sediments & sludges
insecticides emerged in the diethyl ether-hexane eluate. A standard solution containing
Aroclor 1260, p, p
-DDE, γ-HCH and Dieldrin was carried through this separation
procedure in order to assess recovery. The results indicate that recovery from the four
compounds was quantitative, with recoveries of 99.8, 99.6, 102.5 and 102.3% for
Aroclor 1260, p, p
-DDE, γ-HCH and Dieldrin, and displays little scatter, with relative
standard deviations of 1.6, 3.1, 2.9 and 3.1% respectively for the four determinations.
Garcia-Gutierrez et al [156, 166] have shown that a gas chromatographic method
is suitable for the determination of Endrin, Aldrin, other chlorinated insecticides
and polychlorobiphenyls in sewage sludges. Maskarinec and Harvey et al [157] have
described a method for the screening of solid wastes and sludges for organic compounds. The technique involves sequential extraction with acidic, basic and neutral
media and the extracts are all analysed directly by gas chromatography with fused
silica columns.
Jensen et al [174] discuss complications in analysis caused by the presence of
elemental sulphur and organosulphur compounds in the gas chromatographic determination of DDT and of polychlorobiphenyls in sewage sludge. The sulphur interfering
in the gas chromatographic determination is removed in a non-destructive treatment
of the extract with tetrabutyl ammonium sulphate which converts sulphur to the
thiosulphate in an organic phase.
Recoveries of added organochlorines was above 80% and the detection limit
between 1 and 10 ppb for a 10 g sample.
Muscau et al [173] determined polychlorobiphenyls, organochlorine pesticides and
chlorobenzenes in sludge and sediment samples collected in a wastewater treatment
plant by GC x-GC-µEcD. The results were compared to previous data from GC-ECD
analysis. While only p,p
and very low amount of total polychlorobiphenyl (43 ng g
−1 )
were found by conventional analysis, GC × GC-µECD confirmed the total polychlorobiphenyl concentration, did not find any p,p
DDE, but did find polychlorinated
alkanes (PCAs).
Comprehensive two dimensional gas chromatography coupled with a micro
electron capture detector allows the analysis of polychlorobiphenyls, organochlorine
insecticides and organobromine compounds in a single analytical run. No
fractionination of the extracts was required prior to instrumental analysis.
Gas chromatography-mass spectrometry
Various workers have applied this technique to the analysis of municipal sludges
[167, 171]. PCBs and related compounds were eluted with 50 mL hexane; pesticides
and other compounds were eluted with 50 mL toluene.
Acidic components of the samples were treated and diazomethane and dimethyl
sulphate [168–170]. Analysis of all samples for PCBs was accomplished using a
Finnigan 3300 quadruple gas chromatograph-mass spectrometer. The glass column,
packed with 2% OV-101 on Chromosorb W, was held at 120
◦ C for 3 min, programmed to 230
◦ C at 12
◦ C min
−1 and held isothermally until all peaks had been
eluted by helium. The ionisation voltage was nominally 70 eV and multiplier voltages
were between 1.8 and 2.2 kV. Full scan spectra were obtained from m/e 100–500.
Samples were analysed under the following temperature conditions: up to 150
◦ C for
3 min, programmed to 230
◦ C at 80 min
−1 isothermally until all peaks had eluted.,
PCB’s were quantitated by gas chromatograph-mass spectrometry-computer using the
insecticides emerged in the diethyl ether-hexane eluate. A standard solution containing
Aroclor 1260, p, p
-DDE, γ-HCH and Dieldrin was carried through this separation
procedure in order to assess recovery. The results indicate that recovery from the four
compounds was quantitative, with recoveries of 99.8, 99.6, 102.5 and 102.3% for
Aroclor 1260, p, p
-DDE, γ-HCH and Dieldrin, and displays little scatter, with relative
standard deviations of 1.6, 3.1, 2.9 and 3.1% respectively for the four determinations.
Garcia-Gutierrez et al [156, 166] have shown that a gas chromatographic method
is suitable for the determination of Endrin, Aldrin, other chlorinated insecticides
and polychlorobiphenyls in sewage sludges. Maskarinec and Harvey et al [157] have
described a method for the screening of solid wastes and sludges for organic compounds. The technique involves sequential extraction with acidic, basic and neutral
media and the extracts are all analysed directly by gas chromatography with fused
silica columns.
Jensen et al [174] discuss complications in analysis caused by the presence of
elemental sulphur and organosulphur compounds in the gas chromatographic determination of DDT and of polychlorobiphenyls in sewage sludge. The sulphur interfering
in the gas chromatographic determination is removed in a non-destructive treatment
of the extract with tetrabutyl ammonium sulphate which converts sulphur to the
thiosulphate in an organic phase.
Recoveries of added organochlorines was above 80% and the detection limit
between 1 and 10 ppb for a 10 g sample.
Muscau et al [173] determined polychlorobiphenyls, organochlorine pesticides and
chlorobenzenes in sludge and sediment samples collected in a wastewater treatment
plant by GC x-GC-µEcD. The results were compared to previous data from GC-ECD
analysis. While only p,p
and very low amount of total polychlorobiphenyl (43 ng g
−1 )
were found by conventional analysis, GC × GC-µECD confirmed the total polychlorobiphenyl concentration, did not find any p,p
DDE, but did find polychlorinated
alkanes (PCAs).
Comprehensive two dimensional gas chromatography coupled with a micro
electron capture detector allows the analysis of polychlorobiphenyls, organochlorine
insecticides and organobromine compounds in a single analytical run. No
fractionination of the extracts was required prior to instrumental analysis.
Gas chromatography-mass spectrometry
Various workers have applied this technique to the analysis of municipal sludges
[167, 171]. PCBs and related compounds were eluted with 50 mL hexane; pesticides
and other compounds were eluted with 50 mL toluene.
Acidic components of the samples were treated and diazomethane and dimethyl
sulphate [168–170]. Analysis of all samples for PCBs was accomplished using a
Finnigan 3300 quadruple gas chromatograph-mass spectrometer. The glass column,
packed with 2% OV-101 on Chromosorb W, was held at 120
◦ C for 3 min, programmed to 230
◦ C at 12
◦ C min
−1 and held isothermally until all peaks had been
eluted by helium. The ionisation voltage was nominally 70 eV and multiplier voltages
were between 1.8 and 2.2 kV. Full scan spectra were obtained from m/e 100–500.
Samples were analysed under the following temperature conditions: up to 150
◦ C for
3 min, programmed to 230
◦ C at 80 min
−1 isothermally until all peaks had eluted.,
PCB’s were quantitated by gas chromatograph-mass spectrometry-computer using the