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Journal of the Korean Chemical Society (JKCS)

ISSN 1017-2548(Print)
ISSN 2234-8530(Online)
Volume 40, Number 12
JKCSEZ 40(12)
December 20, 1996 

Organic Precipitate Flotation of Trace Metallic Elements with Ammonium Pyrrolidinedithiocarbamate(Ⅰ). Determination of Bismuth, Cadmium, Cobalt and Lead in Water Samples by Coprecipitation-Flotation with Cu-pyrrolidinedithiocarbamate

Ammonium Pyrrolidinedithiocarbamate에 의한 극미량 금속원소의 유기침전 부선에 관한 연구(제 1보) Cu-pyrrolidinedithiocarbamate 공침부선에 의한 물시료중 비스무트,카드뮴,코발트 및 납의 정량
Yong-June Jung, Jong-Moon Choi, Hee-Seon Choi, Young-Sang Kim

물시료중 흔적량 비스무트, 카드뮴, 납, 코발트를 Cu(Ⅱ)-pyrrolidinedithiocarbamate 착물로 공침-부선시켜 분리 정량하는 방법에 관하여 연구하였다. 부선조건인 시료용액의 pH, 공침제로 이용되는 구리의 양, 착화제인 APDC의 양, 저어주는 시간, 계면활성제 등을 조사하여 최적화시켰다. 흔적량 분석원소가 포함된 시료용액 1.0L에 공침제 이온인 1,000 μg/mL Cu(Ⅱ) 표준용액을 3mL 가하고, 자석젓개로 저으면서 질산용액으로 pH 2.5로 조절하였다. 2.0% ammonium pyrrolidinedithiocarbamate(APDC) 용액을 첨가하여 Cu(Ⅱ)-PDC 착물을 침전시켜 분석원소를 공침시켰다. 여기에 계면활성제인 0.2% sodium lauryl sulfate 용액을 가하고, 다공성 유리판을 통해 질소를 불어서 침전을 띄웠다. 표면에 뜬 침전을 포집한 다음, 걸러서 진한 질산으로 녹여 탈염수로 25.0mL가 되게 하였고, 흑연로 원자흡수 분광광도법으로 농축된 분석원소를 정량하였다. 본 방법을 네 가지 물시료에 적용하여 흔적량 원소를 동시에 농축 정량하였고, 일정량의 분석원소를 동일 시료에 첨가하여 정량한 회수율은 90∼120%로서 여기서 제시한 분석법이 흔적량 분석에 정량적임을 알 수 있었다.

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 μg/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.

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