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Thallium(I)-Selective Electrodes Based on Calix[4]pyrroles
박경순,정성욱,이심성,김재상,Park, Gyeong Sun,Jeong, Seong Uk,Lee, Sim Seong,Kim, Jae Sang Korean Chemical Society 2000 Bulletin of the Korean Chemical Society Vol.21 No.9
Thallium(I) selective electrodes based on meso-alkyl substituted calix[4]pyrroles such as, meso-octamethyl-calix[4]pyrrole (L1), meso-octaethylcalix[4]pyrrole (L2) and meso-tetraspirocyclohexylcalix[4]pyrrole (L3) as sensor molecules have been pre pared and tested. The conditioned electrode (E4) incorporating L3gave best results with a wide working concentration range of 10-5.5 ~10-1 M near-Nernstian slope of 56.0 mV/decade of activity and detection limit of 10-6.0 M. This electrode exhibited a fast response time of 30 s and high selectivity over Na+ , K+ and other metal ions with only Ag+ interfering. The electrode works well in the pH range 2.0-11.0 and can be successfully employed for the determination of Tl+.This proposed electrode was also used as an indicator electrode in potentiometric titration of Tl+.
염석추출법에 의한 칼륨(Ⅰ)의 미분펄스폴라로그래프법적 정량
서무룡,이심성,박태명 慶尙大學校 기초과학연구소 1991 基礎科學硏究所報 Vol.7 No.-
비수용매인 아세토니트릴과 거대고리화합물인 dibenzo-18-crown-6(DB18C6)의 분석적 응용으로서 수용액에 있는 K(I) 이온을 염석추출법으로 정량하였다. 곧 borax 완충용액으로 수용액의 pH를 9.2로 조절하고, DB18C6를 포함하는 아세토니트릴용액을 넣어 K(I)-DB18C6 착물을 형성시킨 다음 염석추출법으로 추출분리하고 유기용매층의 K(I)-DB18C6 착물의 미분 펄스폴라로그램을 측정하였다. 이 때 -1.97volt vs. Ag/Ag^+ [0.1M AgNO_3(AN)]에서 피이크 전류를 측정하여 추출조건, 곧 적당한 염석제의 양, pH 범위, 적당한 킬레이트의 양을 구하고 K(I) 이온을 정량하는데 있어서의 정량성과 공존이온 효과를 조사하였다. 실험결과로부터 공존하는 이온의 영향을 별로 받지 않아 선택성이 좋았으며 본 실험방법에 의한 정량한계는 0.1ppm이었다. As one of the analytical application of dibenzo-18-crown-6 (DB18C6) and aprotic solvent, the extraction method with a salting-out technique was applied for the determination of potassium (I) in the aqueous solution. After potassium(I) was extracted into the acetonitrile (AN) layer as a K(I)-DB18C6 complex from the aqueous solution of borax buffer at pH 9.2 by the salting-out technique, the differential pulse polarograms for the K(I)-DB18C6 complex was recorded. In this case magnesium chloride was used as a salting-out reagent. The peak potential of the K(I)-DB18C6 complex in the organic phase was -1.97 volt vs. Ag/Ag^+[0.1M Ag/AgNO_3(in AN)]. The effect of concentration of the salting-out reagent and chelating reagent and pH of aqueous phase on the extractability were investigated. And the calibration curve for the determination of potassium (I) was obtained and diverse ion effect was discussed. By salting-out extraction technique, we can be determined until the concentration of potassium (I) of 0.1 ppm.