Trimethyllead Determination in Artificial Rainwater

Each ampoule had to be made up to one litre of working solution with the purest water available in the laboratory. 

A 20 mL solution was used for the analysis. Ethylation was carried out with 4% NaBEt4 after addition of acetate buffer. The ethylated compound was cryogenically trapped in a U-tube filled with chromatographic material (0.5 m length, 3 mm internal diameter, OV-101 as stationary phase loaded with 10% silica 80/100 mesh He as carrier gas at 120 mL min H2 as make-up gas at 30 mL min column temperature at 75 °C). Detection was by QFAAS at 283.3 nm (detector temperature at 800 °C). Calibration was by standard additions, using the MesPbCl provided by SM T. 

A 100 mL intake was used for analysis. Extraction was performed with 50 mL NaOH and 2 mL sodium acetate/acetic acid (2 mol L ) in 10 mL hexane. 

75 mL solution was used for the analysis. Buffering was performed with ammonium citrate at pH 9, followed by addition of 0.5 mL of 0.25 mol L diethyldithiocarbamate. Extraction was carried out with 5 mL pentane. The extract was dried with Na2S04, evaporated to 0.5 mL and redissolved into hexane. Derivatization was by addition of 0.5 mL of 2 mol L BuMgCl in THF, followed by addition of H2SO4. Separation was by CGC (fused silica column of 60 m length, 0.25 mm internal diameter, DB-1 as stationary phase, 0.25 pm film thickness He was used as carrier gas at 110 mL min injector temperature at 250 °C column temperature ranging from 50 to 260 °C). Detection was by MS (detector temperature at 280 °C), monitoring the ions 

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