Chapter 11
Organometallic compounds in sludges
11.1 ORGANOLEAD COMPOUNDS
Spectrophotometric methods
Imura et al [1] have described a spectrophotometric procedure employing 1-hydroxy4-(4-nitrophenylazo)-2-naphthoate as a chromogenic reagent for the determination
of triethyllead ions in sediments and sludges. The coloured adduct is extracted with
chloroform. The absorption maximum is at 440 nm and the optimum pH for the
extraction from 1% aqueous sodium chloride is 8.1–8.3. Dimethyl and diethyllead
ions and Pb
2+ masked with 0.01 M ethylenediamine NN’-bis (2-hydrocyphenylacetic
acid) (disodium salt) and copper and ferrous iron are masked with 0.01 M 1,2diaminocyclohexane-NNN’N’-tetracetate. The limit of determination is 0.2 mg L
−1
of triethyllead.
Atomic absorption spectrometry
Aneva et al [2] used graphic furnace atomic absorption spectrometry to determine
4–100 µ g L
−1 of tetraalkyllead compounds in sludge. Compounds were extracted with
hexane, converted into water soluble iodides by reaction with iodine in the extract and
re-extracted into dilute nitric acid. The mean recovery was 95% and no interference
was experienced from other metallic or non-metallic ions.
11.2 ORGANOTIN COMPOUNDS
Gas chromatography
Muller et al [7] has described a comprehensive method for determining trace analysis of mono-, di-, tri- and some tetrasubstituted organotin compounds in sewage
sludge. The ionic compounds are extracted from diluted aqueous solutions as chlorides by using a Tropolon-C 18 silica cartridge and from sewage sludge or sediments
by using an ethereal Tropolon solution. The extracted organotin compounds were
ethylated by a Grignard reagent and analysed by using high-resolution gas chromatography with flame photometric detection. Gas chromatography-mass spectrometry
was used for confirmation. The extraction behaviour, gas chromatographic retention,
and photometric response of a series of organotin compounds are described, and the
identification via electron impact (EI) and chemical ionisation (CI) mass spectrometry
Organometallic compounds in sludges
11.1 ORGANOLEAD COMPOUNDS
Spectrophotometric methods
Imura et al [1] have described a spectrophotometric procedure employing 1-hydroxy4-(4-nitrophenylazo)-2-naphthoate as a chromogenic reagent for the determination
of triethyllead ions in sediments and sludges. The coloured adduct is extracted with
chloroform. The absorption maximum is at 440 nm and the optimum pH for the
extraction from 1% aqueous sodium chloride is 8.1–8.3. Dimethyl and diethyllead
ions and Pb
2+ masked with 0.01 M ethylenediamine NN’-bis (2-hydrocyphenylacetic
acid) (disodium salt) and copper and ferrous iron are masked with 0.01 M 1,2diaminocyclohexane-NNN’N’-tetracetate. The limit of determination is 0.2 mg L
−1
of triethyllead.
Atomic absorption spectrometry
Aneva et al [2] used graphic furnace atomic absorption spectrometry to determine
4–100 µ g L
−1 of tetraalkyllead compounds in sludge. Compounds were extracted with
hexane, converted into water soluble iodides by reaction with iodine in the extract and
re-extracted into dilute nitric acid. The mean recovery was 95% and no interference
was experienced from other metallic or non-metallic ions.
11.2 ORGANOTIN COMPOUNDS
Gas chromatography
Muller et al [7] has described a comprehensive method for determining trace analysis of mono-, di-, tri- and some tetrasubstituted organotin compounds in sewage
sludge. The ionic compounds are extracted from diluted aqueous solutions as chlorides by using a Tropolon-C 18 silica cartridge and from sewage sludge or sediments
by using an ethereal Tropolon solution. The extracted organotin compounds were
ethylated by a Grignard reagent and analysed by using high-resolution gas chromatography with flame photometric detection. Gas chromatography-mass spectrometry
was used for confirmation. The extraction behaviour, gas chromatographic retention,
and photometric response of a series of organotin compounds are described, and the
identification via electron impact (EI) and chemical ionisation (CI) mass spectrometry