• Journal of the Korean Chemical Society
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• v.40 no.12
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• pp.724-732
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• 1996

The organic precipitate flotation using Cu(II)-pyrrolidinedithiocarbamate complex as a coprecipitant was studied for the preconcentration and determination of trace Cd, Pb, Bi and Co in several water samples. Experimental conditions such as pH of solution, amounts of Cu(II) and ammonium pyrrolidinedithiocarbamate(APDC), stirring time, the type and amount of surfactant, etc. were optimized for the effective flotation of analytes. After 3.0 mL of 1,000 ${\mu}g/mL$ Cu(II) solution was added to 1.00 L water sample, the pH of the solution was adjusted to 2.5 with HNO3 solution. Trace amounts of analytes were coprecipitated by adding 2.0% APDC solution. And the precipitates were flotated onto the surface of solution with the aid of nitrogen gas and sodium lauryl sulfate. The floats were collected from mother liquor, and filtered through the micropore glass filter by suction. The precipitates were dissolved with 4 mL conc. HNO3, and then diluted to 25.00 mL with deionized water. The analytes were determined by graphite furnace atomic absorption spectrophotometry. This flotation technique was applied to the analysis of some water samples, and the 90 to 120% of recoveries were obtained from the spiked samples, this procedure could be concluded to be simple and applicable for the trace element analysis in various kinds of water.

• Analytical Science and Technology
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• v.9 no.4
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• pp.336-344
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• 1996

The extraction of trace cobalt, copper, nickel, cadmium, lead and zinc in urine samples of organic and alkali metal matrix into chloroform by the complex with a dithizone was studied for graphite furnace AAS determination. Various experimental conditions such as the pretreatment of urine, the pH of sample solution, and dithizone concentration in a solvent were optimized for the effective extraction, and some essential conditions were also studied for the back-extraction and digestion as well. All organic materials in 100 mL urine were destructed by the digestion with conc. $HNO_3$ 30 mL and 30% $H_2O_2$ 50 mL. Here, $H_2O_2$ was added dropwise with each 5.0 mL, serially. Analytes were extracted into 15.0 mL chloroform of 0.1% dithizone from the digested urine at pH 8.0 by shaking for 90 minutes. The pH was adjusted with a commercial buffer solution. Among analytes, cadmium, lead and zinc were back-extracted to 10.00 mL of 0.2 M $HNO_3$ from the solvent for the determination, and after the organic solvent was evaporated, others were dissolved with $HNO_3-H_2O_2$ and diluted to 10.00 mL with a deionized water. Synthetic digested urines were used to obtain optimum conditions and to plot calibration-eurves. Average recoveries of 77 to 109% for each element were obtained in sample solutions in which given amounts of analytes were added, and detection limits were Cd 0.09, Pb 0.59, Zn 0.18, Co 0.24, Cu 1.3 and Ni 1.7 ng/mL, respectively. It was concluded that this method could be applied for the determination of heavy elements in urine samples without any interferences of organic materials and major alkaline elements.