水溶性ポルフィリン-銀錯体を用いる硫化物イオンの吸光光度定量

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Silver complex of α, β, γ, δ-tetrakis (4-sulfophenyl) porphine (Ag_2-TPPS) was quantitatively formed within 1 min at room temperature in the pH range of 11.0 to 12.5. The complex easily relases the porphyrin in the presence of "soft base" anions such as S^<2->, CN^-, I^-, glutathione and L-cysteine within 5 min at room temperature in the above pH range. Based on this reaction, spectrophotometric determination of 10^<-7> mol dm^<-3> levels of sulfide ion was developed. The Soret band of TPPS and the Ag_2-TPPS complex at pH 12.0 and I=0.5 were located at wavelength of 414 nm (ε=41.4×10^4) and at 443 nm(ε=7.9×10^4), respectively. A recommended procedure : 1.0 cm^3 of 10^<-4> mol dm^<-3> TPPS solution, 10 cm^3 of 2.5 mol dm^<-3> sodium nitrate solution, 2.0 cm^3 of 10^<-4> mol dm^<-3> Ag (I) solution, and 5 cm^3 of 1 mol dm^<-3> sodium hydroxide solution are taken into a 50 cm^3 of amber-volumetric flask. After standing for 5 min, 30 cm^3 of sample solution containing less than 2.0 μg of sulfide is added and is diluted to 50 cm^3 with water. After 10 min, the absorbance at 414 nm against water is measured. The calibration curve was found to be linear in the range of 0〜2.0×10^<-6> mol dm^<-3>. The relative standard deviation was 3.75% for [S^<2->]_T=5×10^<-7> mol dm^<-3> (8 determinations). The detection limits was 7×10^<-8> mol dm^<-3> (S/N=3). The tolerance limits of diverse ions for determination of [S^<2->]_T=5×10^<-7> mol dm^<-3> were 5×10^<-4> mol dm^<-3> for NO_3^-, CI^-, SO_4^<2->, K^+ and Na^+, and 5×10^<-5> mol dm^<-3> for Ba^<2+>, Ca^<2+> and Fe^<3+>. However, 5×10^<-7> mol dm^<-3> of I^-, CN^-, Cd^<2+>, glutathione and L-cysteine were interfered. As Ag_2-TPPS complex reacts rapidly with various kinds of soft bases, it is expected as a highly sensitive and selective chromogenic reagent of postcolumn detection system in the LC for these ions.
社団法人日本分析化学会の論文
1988-06-05

水溶性ポルフィリン-銀錯体を用いる硫化物イオンの吸光光度定量

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