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MASKING OF OVERLOADED ZN(II) AND TRANSIENT ISOTACHOPHORESIS OF TRACE METALS IN HIGHLY SALINE SAMPLES

등록일
2005년 8월 25일 09시 09분 16초
접수번호
1021
발표코드
23P153포 이곳을 클릭하시면 발표코드에 대한 설명을 보실 수 있습니다.
발표시간
토 <발표Ⅳ>
발표형식
포스터
발표분야
분석화학
저자 및
공동저자
Asif Riaz, 류립천, 정두수
서울대학교 화학부,
Online masking of the overloaded metal ion such as Zn2+ from highly saline samples in capillary electrophoresis was achieved selectively by using thioglycolic acid as a masking agent in the background electrolyte (BGE). However, the trace amounts of Fe2+ and Ni2+ in the same samples as their anionic complexes with 4-(2-pyridylazo) resorcinol (PAR) could be successfully stacked by transient isotachophoresis (TITP) and determined without interference from the excessive amount of Zn2+. TITP stacking of Fe-PAR and Ni-PAR was induced by the sample chloride acting as a leading electrolyte where free-PAR in the sample acted as a terminating electrolyte. For masking we propose a selective sweeping mechanism by which the masking agent sweeps a particular metal ion selectively from the sample. The optimized BGE was composed of 95 mM N-tris(hydroxymethyl)methyl-3-aminopropanesulfonic acid and 73 mM triethylamine, 0.1 mM PAR, 2 mM TGA and 0.02% FC-PN (a fluorocarbon neutral polymeric surfactant) at pH 9.0. Using our method several hundred-fold enhancements in the absorbance response of Fe-PAR and Ni-PAR peaks was achieved in highly saline samples compared to the normal CE mode of injection even in the several thousand-fold excess of Zn2+ in the sample. The limits of detection (S/N = 3) were in the sub-ppb range (Fe2+; Ni2+). The method was successfully applied to determine the trace amounts of Fe and Ni in standard reference urine and human urine samples containing excessive amount of Zn2+.

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