Organic compounds in non-saline sediments 143
Trehy et al [110] and others determined linear alkyl benzene sulphonates in
sediments in amounts down to 0.5 mg kg
−1 using this technique.
6.3 HALOGEN CONTAINING COMPOUNDS
6.3.1 Volatile aliphatic chlorohydrocarbons
Gas chromatography
Murray and Riley et al [23, 24] and Novak et al [111] described gas chromatographic
methods for the determination of trichloroethylene, tetrachloroethylene, chloroform
and carbon tetrachloride in sediments. These sediments were separated and determined
on a glass column (4 m × 4 mm) packed with 3% of SE-52 on Chromosorb W (AW
DMCS) (80–100 mesh) and operated at 35
◦ C, with argon (30 ml min
−1 ) as carrier
gas. An electron capture detector was used, with argon-methane (9:1) as quench gas.
Chlorinated hydrocarbons were stripped from water samples by passage of nitrogen
and removed from solid samples be heating in a stream of nitrogen. In each case, the
compounds were transferred from the nitrogen to the carrier gas by trapping on a copper column (30 cm×6 mm) packed with Chromosorb W (AW DMCS) (80–100 mesh)
coated with 3% of SE-52 and cooled at −78
◦ C, and subsequently sweeping on to the
gas chromatographic column with the stream of argon. A limitation of this procedure
was that compounds which boil above 100
◦ C could not be determined.
Amin and Narang et al [26] closed loop stripped volatile haloparaffins from
sediments and adsorbed the volatiles on Poropack N. The compounds were eluted
with methanol and the elute analysed for organic compounds by gas chromatography
with electron capture and photoionisation detection. A detection limit of 7 µg
−1 for
each photoionisation active and 1 ng g
−1 for each electron capturing compound was
achieved. Samples could be stored in methanol for up to 90 days without significant
loss of the volatile compounds. Recoveries ranged from 71% (bromoform) to 111%
fluorobenzene
The following compounds were determines by this procedure: chloroform;
bromoform; 1,1,1-tricholoroethane; 1,1,2,2-tetrachloroethane; trichloroethylene;
benzene; carbon tetechloride; toluene; bromodichloromethane, chlorobenzenes;
1,1,2-trichloroethane; o, p-xylene; tetrachlorethylene; o, p-chlorotoluene, 1,2dibromoethane and fluorobenzene (used as in internal standard).
Zitko et al [112] has described a confirmatory method in which the chloroparaffins in sediments are reduced to normal hydrocarbons which are then analysed by gas
chromatography. This method lacks sufficient sensitivity for trace (sub-ppm) analysis and the confirmatory method may be difficult to apply. Friedman and Lombardo
et al [113] have described a gas chromatographic method applicable to chloroparaffins that are slightly volatile; the method is based on microcoulmometric detection
and photochemical elimination of chlorinated aromatic compounds that otherwise
interfere.
The application of gas chromatography to the determination of chlorinated hydrocarbons in water and sediments, with particular reference to the types of these
compounds used in industry, has been reviewed by Hassler and Rippa et al [114]. Glaze
et al [115] used flame ionisation electron capture and Coulson electrolytic detectors
Trehy et al [110] and others determined linear alkyl benzene sulphonates in
sediments in amounts down to 0.5 mg kg
−1 using this technique.
6.3 HALOGEN CONTAINING COMPOUNDS
6.3.1 Volatile aliphatic chlorohydrocarbons
Gas chromatography
Murray and Riley et al [23, 24] and Novak et al [111] described gas chromatographic
methods for the determination of trichloroethylene, tetrachloroethylene, chloroform
and carbon tetrachloride in sediments. These sediments were separated and determined
on a glass column (4 m × 4 mm) packed with 3% of SE-52 on Chromosorb W (AW
DMCS) (80–100 mesh) and operated at 35
◦ C, with argon (30 ml min
−1 ) as carrier
gas. An electron capture detector was used, with argon-methane (9:1) as quench gas.
Chlorinated hydrocarbons were stripped from water samples by passage of nitrogen
and removed from solid samples be heating in a stream of nitrogen. In each case, the
compounds were transferred from the nitrogen to the carrier gas by trapping on a copper column (30 cm×6 mm) packed with Chromosorb W (AW DMCS) (80–100 mesh)
coated with 3% of SE-52 and cooled at −78
◦ C, and subsequently sweeping on to the
gas chromatographic column with the stream of argon. A limitation of this procedure
was that compounds which boil above 100
◦ C could not be determined.
Amin and Narang et al [26] closed loop stripped volatile haloparaffins from
sediments and adsorbed the volatiles on Poropack N. The compounds were eluted
with methanol and the elute analysed for organic compounds by gas chromatography
with electron capture and photoionisation detection. A detection limit of 7 µg
−1 for
each photoionisation active and 1 ng g
−1 for each electron capturing compound was
achieved. Samples could be stored in methanol for up to 90 days without significant
loss of the volatile compounds. Recoveries ranged from 71% (bromoform) to 111%
fluorobenzene
The following compounds were determines by this procedure: chloroform;
bromoform; 1,1,1-tricholoroethane; 1,1,2,2-tetrachloroethane; trichloroethylene;
benzene; carbon tetechloride; toluene; bromodichloromethane, chlorobenzenes;
1,1,2-trichloroethane; o, p-xylene; tetrachlorethylene; o, p-chlorotoluene, 1,2dibromoethane and fluorobenzene (used as in internal standard).
Zitko et al [112] has described a confirmatory method in which the chloroparaffins in sediments are reduced to normal hydrocarbons which are then analysed by gas
chromatography. This method lacks sufficient sensitivity for trace (sub-ppm) analysis and the confirmatory method may be difficult to apply. Friedman and Lombardo
et al [113] have described a gas chromatographic method applicable to chloroparaffins that are slightly volatile; the method is based on microcoulmometric detection
and photochemical elimination of chlorinated aromatic compounds that otherwise
interfere.
The application of gas chromatography to the determination of chlorinated hydrocarbons in water and sediments, with particular reference to the types of these
compounds used in industry, has been reviewed by Hassler and Rippa et al [114]. Glaze
et al [115] used flame ionisation electron capture and Coulson electrolytic detectors