Polychlorobiphenyls, determination

Pedensen-Bjergaard et al. [364] compared three different methods (GC-ECD, GC-MS, GC-AED) for the determination of polychlorobiphenyls in highly contaminated marine sediments. 

Bush, B., R.W. Streeter, and R.J. Sloan. 1990. Polychlorobiphenyl (PCB) congeners in striped bass (Morone saxatilis) from marine and estuarine waters of New York state determined by capillary gas chromatography. Arch. Environ. Contam. Toxicol. 19 49-61. 

Spectrofluorimetric methods are applicable to the determination of aliphatic hydrocarbons, and humic and fulvic acids in soil, aliphatic hydrocarbons polyaromatic hydrocarbons, optical whiteners, and selenium in non-saline sediments, aliphatic aromatic and polyaromatic hydrocarbons and humic and fulvic acids in saline sediments. The only application found in luminescence spectroscopy is the determination of polychlorobiphenyl in soil. Generally speaking, concentrations down to the picogram (pg L 1), level can be determined by this technique with recovery efficiencies near f00%. 

This technique has been used for the determination of polychlorobiphenyls, polychlorodibenzo-p-dioxins, polychlorodibenzofurans, alkyl phosphates, chlorinated insecticides, organophosphorus insecticides, triazine herbicides. Dacthal insecticide, insecticide/herbicide mixtures, mixtures of organic compounds and organotin compounds in soils, and polyaromatic compounds, polychlorobiphenyls, chlorinated insecticides and organotin compounds in non-saline sediments and anionic surfactants in sludges. 

This technique has been applied to the determination of heteroaromatic compounds, anthropogenic hydrocarbons, polymers, haloaromatic compounds in soils, polyaromatic hydrocarbons, cationic surfactants and polychlorobiphenyls and mixtures of organic compounds in non-saline sediments and bacteria identification in sludges. 

This technique has been used to determine the following types of organic compounds in soil polychlorobiphenyls, chlorinated insecticides, triazine herbicides, paraquat and diquat. 

Electrophoretic and isotachoelectrophoretic techniques are gaining in popularity in soil analysis with applications to polyaromatic hydrocarbons, polychlorobiphenyls, tetrahydrothiophene and triazine herbicides, Paraquat and Diquat and growth regulators. Other lesser-used techniques include spectrophotometric methods (five determinants), spectrofluorimetric methods (two determinants), luminescence methods (one determinant), titration methods (one determinant), thin-layer chromatography (five applications), NHR spectroscopy (two applications) and enzymic immunoassays (one determinant). 

Von Bavel et al. [55] used a solid phase carbon trap in conjunction with supercritical fluid chromatography for the simultaneous determination of polychlorobiphenyls, pesticides, polychlorodibenzo-p-dioxins and polychlorodibenzofurans in soils. 

Supercritical fluid extraction with carbon dioxide has been applied to the determination of polychlorobiphenyls in soil [113]. 

Gas chromatography has been used extensively for the determination of polychlorobiphenyls in river sediments [30, 38, 59-67]. Both capillary [60— 63] and packed [38, 42, 64-67] columns have been used. 

Goerlitz and Law [59] determined chlorinated insecticides in sediment and bottom material samples, which also contained polychlorobiphenyls by extracting the sample with acetone and hexane. The combined extracts were passed down an alumina column. The first fraction (containing most of the insecticides and some polychlorinated biphenyls and polychlorinated naphthalenes) was eluted with hexane and treated with mercury to precipitate sulphur. If the polychlorinated hydrocarbons interfered with the subsequent gas chromatographic analysis, further purification on a silica gel column was necessary. 

Kerkhoff et al. [60] used capillary gas chromatography to determine polychlorobiphenyls in various Dutch river sediments. 

The electron capture gas chromatographic and ETISA procedures described in section 5.6.1.1 have been applied to the field determination of polychlorobiphenyls in sediments [46]. 

McMurtrey et al. [65] investigated the feasibility of determining polychlorinated biphenyls adsorbed on soils and sediments, by a procedure involving pyrolytic desorption at 1000°C, followed by gas chromatography and mass spectrometry. The procedure was capable of demonstrating the presence of polychlorobiphenyls on air-dried sediment at the lOppm level. 

Lee and Chau [66] have discussed the development and certification of a sediment reference material for total polychlorobiphenyls. Alford Stevens et al. [49] in an inter-laboratory study on the determination of polychlorobiphenyls in environmentally contaminated sediments showed the mean relative standard deviation of measured polychlorobiphenyl concentrations was 34%, despite efforts to eliminate procedural variations. Eganhouse and Gosset [67] have discussed the sources and magnitude of bias associated with the determination of polychlorobiphenyls in environmental sediments. Heilman [30] studied the adsorption and desorption of polychlorobiphenyl on sediments. 

The enzyme immunoassay procedure [57] discussed in section 5.6.1.5 for the determination of polychlorobiphenyls in soils has also been applied to sediments. 

Three different detection methods (gas chromatography with electron capture, mass spectrometric and atomic emission detectors) have been compared for the determination of polychlorobiphenyls in highly contaminated marine sediments [74], Only atomic emission detection in the chlorine-selective mode provided excellent polychlorobiphenyl profiles without interferences. However, the lower sensitivity of the atomic emission detector, compared to the other two detectors required a 10 to 20g sample size for most analyses. 

Polychlorobiphenyl cogeners 77, 126 and 169 have been determined in sewage sludge at detection limits as low as 100kg by gas chromatography negative ion mass spectrometry [115]. 

Representative multiple ion mass chromatograms of soil samples are presented in Fig. 5.4. These gas chromatography-mass spectrometric determinations of polychlorodibenzo-p-dioxin and polychlorodibenzofurans, and non-ortho polychlorobiphenyls in differing types of samples serve to exemplify the versatility of the procedure for such analyses. The gas chromatography-mass spectrometric data were usually uncluttered by extraneous components, and interpretation of the data was routinely straightforward. 

Von Bavel et al. [55] have developed a solid phase carbon trap (PX-21 active carbon) for the simultaneous determination of polychlorodibenzo-p-dioxins and polychlorodibenzofurans also polychlorobiphenyls and chlorinated insecticides in soils using superfluid extraction liquid chromatography for the final determination. Supercritical fluid extraction with carbon dioxide has been applied to the determination of dioxins in soil [114],... 

The method described by Teichman et al. [15] and discussed in section 9.1.1.2 for the determination of chlorinated insecticides and PCBs in soils has also been applied to sediments. The procedure involves adsorption chromatography on alumina and charcoal, elution with increasing fractional amounts of hexane on alumina columns, and with acetonediethyl ether and benzene on charcoal columns. The polychlorobiphenyl and pesticides are then determined by gas chromatography on the separate elutes without interference. 

Wegmann and Hofstee [43] have developed a capillary gas chromatographic method for the determination of organochlorine insecticides in river sediments. Bottom soils from rivers, collected in slow current areas may contain high concentrations of organochlorine insecticides and polychlorobiphenyls. When the current moves more rapidly or benthic animals become more active, these compounds are stirred into the water along with suspended particles and become accessible to organisms that live in the bottom layer. 

Jensen et al. [45, 46] also discuss complications in analysis due to the presence of elementary sulphur and organosulphur compounds in the gas chromatographic determination of DDT and polychlorobiphenyls in sediments and sewage sludges. 

Various workers [50-62] have reported methods for the determination of polychlorobiphenyls and organochlorine insecticides in sewage and sewage sludges. 

Mattson and Nygren [57] have described the chromatographic procedure for the determination of polychlorobiphenyls and some chlorinated insecticides in sewage sludge. The capillary column is coated with silicone oil SF 96. 

Jensen et al. [45] applied the method described in section 9.1.2.1 for the determination of DDT and polychlorobiphenyls in sulphur containing sediments to the analysis of sludges. The results in Fig. 9.7 show the beneficial effects of pretreatment of the sewage with tetrabutyl ammonium sulphate-sodium sulphite reagent on the recovery of DDT and polychlorobiphenyls from a digested sewage sludge sample. 

McIntyre et al. [58, 59] described a method for the analysis of polychlorobiphenyls and chlorinated insecticides in sewage sludges in which homogenized samples are extracted with hexane, concentrated and cleaned up on an alumina/alumina plus silver nitrate column and eluted with hexane. After concentration of the eluent, polychlorobiphenyl and organochlorine compounds were determined by a silica gel chromatographic procedure and gas chromatography. 

Namiesnik et al. [33] have reviewed the analysis of soils and sediments for organic contaminants. They discuss methods of sample preparation and isolation-preconcentration prior to instrumental determination. Compound classes discussed include volatile organic compounds, polychlorobiphenyls, polyaromatic compounds, pesticides and polychlorodibenzo-p-dioxins and polychlorodibenzofurans. 

Jensen et al. [53] have described a method applicable to marine sediments for the determination of polychlorobiphenyls and organochlorine... 

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