Organometallic compounds in sludges 253
reagent is used to generate bromine in the sample, is that the bromine quantitatively
cleaves both alkyl and aryl mercury compounds to inorganic mercury bromide.
Recoveries of inorganic mercury from distilled water spiked with phenylmercury (II) chloride thiomeral, ethylmercury (II) chloride, methylmercury (II) chloride,
phenylmercury (II) acetate and p-tolymercury (II) chloride obtained by this method
were compared with results obtained by a method based on digestion with acid permercuryonate [5]. These were very similar and the acid permanganate method has
an additional advantage in that it can easily be carried out while sampling on-site.
The sample is collected in glass bottles containing hydrochloric acid and the bromatebromide from the collection of the sample to the analysis in the laboratory and this
is far in excess of that necessary to decompose the organic mercury. In addition, as
aqueous mercury (II) solutions are stabilised by strong oxidising agents, the oxidising
conditions so created will help to preserve inorganic mercury formed.
Osland et al [8] has discussed the determination of inorganic mercury in sludges
by cold-vapour absorption spectrometry.
Thin-layer chromatography
Takeshita et al [11] have used thin-layer chromatography to detect alkylmercury compounds and inorganic mercury in sewage. The dithizonates were prepared by mixing
a benzene solution of the alkylmercury compounds and a 0.4% solution of dithizone.
When a green coloration was obtained the solution was shaken with N-sulphuric
acid followed by aqueous ammonia and washed with water. The benzene solution
was evaporated under reduced pressure, and the dithizonates, dissolved in benzene,
were separated by reversed-phase chromatography on layers of corn starch and Avicel
SF containing various proportions of liquid paraffin. Solutions of ethanol and of
2-methoxyethanol were used as developing solvents. The spots were observed in daylight. The detection limit was from 5 to 57 ng (Calculated as organomercury chloride)
per spot.
REFERENCES
[1] Imura, S., Kukutako, K., Aoki, H. & Sakai, T. (1971) Japan Analyst, 20, 704.
[2] Aneva, Z. (1985) Fresenius Zeitschrift Für Analytical Chemistry, 321, 680.
[3] HMSO (1992) Determination of Organic, Inorganic and Total Tin Compounds in Water
Sediments and Biota.
[4] Van Etekoven, K.G. (1980) H 2 O, 13, 326.
[5] Determination of Organomercury Compounds in the Water and Effluents, DOE and
NWC, UK HMSO, London 1972, 23p. PF22 Abenv 1978.
[6] Farey, B.J., Nelson, L.A. & Ralph, M.J. (1978) Analyst, 103, 656.
[7] Muller, M.D. (1987) Analytical Chemistry, 59, 617.
[8] Osland, R. (1970) Pye Unicam Spectrovision, No. 24, 11.
[9] Omang, S.H. (1972) Analytica Chimica Acta, 52, 415.
[10] Uthe, J.E., Armstrong, F.A. & Fisheries, M.P.J. (1970) Research Board, Canada, 27, 805.
[11] Takeshite, R., Agaki, H., Fujite, M. & Sakegamz, O. (1970) Journal of Chromatography,
51, 283.
reagent is used to generate bromine in the sample, is that the bromine quantitatively
cleaves both alkyl and aryl mercury compounds to inorganic mercury bromide.
Recoveries of inorganic mercury from distilled water spiked with phenylmercury (II) chloride thiomeral, ethylmercury (II) chloride, methylmercury (II) chloride,
phenylmercury (II) acetate and p-tolymercury (II) chloride obtained by this method
were compared with results obtained by a method based on digestion with acid permercuryonate [5]. These were very similar and the acid permanganate method has
an additional advantage in that it can easily be carried out while sampling on-site.
The sample is collected in glass bottles containing hydrochloric acid and the bromatebromide from the collection of the sample to the analysis in the laboratory and this
is far in excess of that necessary to decompose the organic mercury. In addition, as
aqueous mercury (II) solutions are stabilised by strong oxidising agents, the oxidising
conditions so created will help to preserve inorganic mercury formed.
Osland et al [8] has discussed the determination of inorganic mercury in sludges
by cold-vapour absorption spectrometry.
Thin-layer chromatography
Takeshita et al [11] have used thin-layer chromatography to detect alkylmercury compounds and inorganic mercury in sewage. The dithizonates were prepared by mixing
a benzene solution of the alkylmercury compounds and a 0.4% solution of dithizone.
When a green coloration was obtained the solution was shaken with N-sulphuric
acid followed by aqueous ammonia and washed with water. The benzene solution
was evaporated under reduced pressure, and the dithizonates, dissolved in benzene,
were separated by reversed-phase chromatography on layers of corn starch and Avicel
SF containing various proportions of liquid paraffin. Solutions of ethanol and of
2-methoxyethanol were used as developing solvents. The spots were observed in daylight. The detection limit was from 5 to 57 ng (Calculated as organomercury chloride)
per spot.
REFERENCES
[1] Imura, S., Kukutako, K., Aoki, H. & Sakai, T. (1971) Japan Analyst, 20, 704.
[2] Aneva, Z. (1985) Fresenius Zeitschrift Für Analytical Chemistry, 321, 680.
[3] HMSO (1992) Determination of Organic, Inorganic and Total Tin Compounds in Water
Sediments and Biota.
[4] Van Etekoven, K.G. (1980) H 2 O, 13, 326.
[5] Determination of Organomercury Compounds in the Water and Effluents, DOE and
NWC, UK HMSO, London 1972, 23p. PF22 Abenv 1978.
[6] Farey, B.J., Nelson, L.A. & Ralph, M.J. (1978) Analyst, 103, 656.
[7] Muller, M.D. (1987) Analytical Chemistry, 59, 617.
[8] Osland, R. (1970) Pye Unicam Spectrovision, No. 24, 11.
[9] Omang, S.H. (1972) Analytica Chimica Acta, 52, 415.
[10] Uthe, J.E., Armstrong, F.A. & Fisheries, M.P.J. (1970) Research Board, Canada, 27, 805.
[11] Takeshite, R., Agaki, H., Fujite, M. & Sakegamz, O. (1970) Journal of Chromatography,
51, 283.