ポルフィリン-パラジウム(II)錯体の生成反応に対するL-アスコルビン酸の促進効果とその微量パラジウムの吸光光度定量への応用

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The direct incorporation reaction of Pd(II) into α,β,γ,δ-tetraphenylporphine-trisulfonate (TPPS) was very slow and had no practical value. However, in the presence of 2×10^<-5> to 2×10^<-4> mol dm^<-3> of L-ascorbic acid, the reaction was accelerated extensively to form TPPS-Pd complex within 7 minutes under boiling condition at pH range of 2.8 to 7.0. The complex once formed was stable over pH2 to 11, and its absorbance was constant for 12h. The soret bands of TPPS and TPPS-Pd at pH 2.5 were located at wavelength of 434nm (ε=5.0×10^<-5>) and at 411.6nm (ε=2.76×10^5), respectively. Thus, the both or one of the bands can be applied for the spectrophotometric determination of 10ng levels of Pd(II): take 15cm^3 of sample solution containing (1〜6)μg of Pd(II) into 50cm^3 beaker and add 6cm^3 of 1×10^<-5>mol dm^<-3> TPPS solution. 1cm^3 of 1×10^<-3>mol dm^<-3> L-ascorbic acid solution and 1cm^3 of 1mol dm^<-3> acetic acid solution (pH 3.0). Heat the mixture for 8minutes and allow to cool. Add 1cm^3 of 1mol dm^<-3> monochloroacetic acid, dilute to 25cm^3 with water (pH 2.5) and measure the absorbance at 411.6nm and/or 434nm against reagent blank. 500μg of Ba^<2+>, Cd^<2+>, Ni^<2+>, Pb^<2+> and VO_3- , 50μg of Al^<3+>, Ca^<2+>, Co^<2+>, Cr^<3+>,Ga^<3+>, Mg^<2+>, Mn^<2+>, Mg^<6+>, VO^<2+>, W^<6+> and Zn^<2+> and 5μg of Ag^+, Fe^<2+>, Fe^<3+>, In^<3+>, Pt^<2+> and Sn^<2+> did not interfered with the determination. However, 5μg of Cu^<2+> and Hg^<2+> interfered. At 411.6nm, Beer's law was confirmed over 0〜250ng Pd^<2+> cm^<-3> and the sensitivity for A=0.001 was 0.494ng Pd^<2+>cm^<-2>.
社団法人日本分析化学会の論文
1978-01-05

ポルフィリン-パラジウム(II)錯体の生成反応に対するL-アスコルビン酸の促進効果とその微量パラジウムの吸光光度定量への応用

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