α,β.γ,δ-テトラキス(4-カルボキシフェニル)ポルフィンを用いる微量銅(II),亜鉛(II),マンガン(II)及びコバルト(II)の逆相分配高速液体クロマトグラフィー

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Simultaneous determination of small amounts of Cu(II), Zn(II), Co(II) and Mn(II) with α,β,γ,δ-tetrakis(4-carboxyphenyl) porphine (TCPP) by HPLC was developed. The metal-TCPP complexes were quantitatively formed within 20 min at room temperature in the presence of Hg(II) and pyridine ([Hg^<2+>]_<Total>≧10^<-6> mol dm^<-3> and [Pyridine]_<Total>≧10^<-2> mol dm^<-3>) over the following pH ranges of 7.0〜11.2(Cu), 7.0〜10.9(Zn), 8.2〜10.2(Co) and 7.8〜10.7(Mn). Pyridine not only acted as an accelerator for complexation, but also as a selective modifier, as seen by the retention behavior of the Go complex in the chromatogram. Recommended procedure : Prepare a sample solution containing up to 1.6 μg of Cu(II), Zn(II), Mn(II) and Co(II) in a 25 cm^3 ambercolored-volumetric flask, to which add 2 cm^3 of 1×10^<-4> mol dm^<-3> TCPP, 0.25 cm^3 of 1 mol dm^<-3> pyridine solution, 0.5 cm^3 of 0.1 mol dm^<-3> sodium tetraborate pH buffer solution (pH 9.3), and 1 cm^3 of 1×10^<-4> mol dm^<-3> mercury(II) solution. Leave to stand at room temperature for 30 min and dilute to 25 cm^3 with water. Inject 0.1 cm^3 of the mixture into the HPLC system [mobile phase : 50 w/w% mixture of acetonitrile and aqueous acetic acid-sodium acetate solution (pH 3.5), flow rate 0.5 cm^3/min, column : Merck CGC glass cartridge LiChrosorb RP-18 (5 μm : 3.2 mm i. d.×150 mm)], and measure the absorbance at 420 nm. The molar absorptivities (ε/cm^<-1> mol^<-1> dm^3) of Cu-, Zn-, Mn- and Co-complexes at 420 nm were 2.35×10^5, 5.81x10^5, 5.25×10^4 and 6.46×10^<-4>, respectively. The peak height calibration curves of these metal ions were linear over the range of 4×10^<-8> to 1×10^<-6> mol dm^<-3>, and the relative standard deviation (5 determinations) at the center of the calibration range were 3.6%(Cu), 3.3%(Zn), 1.6%(Co) and 4.3%(Mn). Up to 100 μg of alkali metal ions (Na^+, K^+), alkali earth metal ions (Mg^<2+>, Ca^<2+>, Ba^<2+>, Sr^<2+>), and anions (Cl^-, Br^-, NO_3^-, SO_4^<2->, ClO_4^-. CH_3COO^-) did not interfere with the determination.
社団法人日本分析化学会の論文
1986-09-05

α,β.γ,δ-テトラキス(4-カルボキシフェニル)ポルフィンを用いる微量銅(II),亜鉛(II),マンガン(II)及びコバルト(II)の逆相分配高速液体クロマトグラフィー

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