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出 处:《应用化学》2007年第1期71-75,共5页Chinese Journal of Applied Chemistry
基 金:黑龙江省自然科学基金(B01-07);黑龙江省教育厅科研基金(10541082)资助项目
摘 要:在pH=3.51的HAc-NaAc介质中,测得1-苯基-3-甲基4-(α-呋喃甲酰基)吡唑啉酮-5(HPMαFP)与2,2′-联吡啶(dipy)合铅三元配合物的灵敏极谱波(-0.73 V(vs.SCE))。铅浓度在0.002~9×10-6 g/mL范围内与峰电流分段呈良好的线性关系,检测下限为2.0×10-9 g/mL。采用多种电化学方法研究了极谱波的性质和电极反应机理。结果证明,-0.73 V处的极谱波为多元配合物吸附波,峰电流由中心离子Pb2+还原产生。根据直线法测得多元配合物组成为n(Pb2+):n(dipy):n(HPMαFP)=1:1:1,表观稳定常数为5.06×106。体系用于粗盐、蔗糖和化妆品中铅测定,标准回收率为99.3%~100.4%。In a medium of HAc-NaAc(pH =3.51), a triple complex is formed via Pb( Ⅱ ) reacting with 1-pheny1-3-methyl-4- ( a-furoyl ) pyrazolone-5 ( HPMotFP ) and 2,2'-dipyridine ( dipy ), and there appears a sensitive polarographic wave at - 0. 73 V ( vs. SCE ) for the triple complex. The peak current exhibits linear relation with the concentration of Pb( Ⅱ ) from 2 × 10^-9 g/mL to 9 × 10^ -6 g/mL. The detection limit is 2 × 10^-9 g/mL. By using different electrochemical methods, the properties of the polarographic wave and the mechanism of electrode reaction were studied. The results indicate that the polarographic wave at -0. 73 V is an adsorptive wave of the complex:. The peak current is produced by the reduction of the Pb ( Ⅱ) ion . The molar ratio of Pb ( Ⅱ ) with dipy to HPMctFP in the complex is 1:1:1 ; and the conditional formation constant of the complex is 5.06 × 10^6. The method was used to determine lead in thick salt, cane sugar and comestic samples. The recovery is 99. 3% - 100. 4% .
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