α,β,γ,δ-テトラキス(4-カルボキシフェニル)ポルフィンをプレカラム誘導体化試薬とする逆相分配高速液体クロマトグラフィーによる鉄鋼中の微量亜鉛の定量

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A novel method for the determination of trace amounts of zinc in iron and steel has been demonstrated by a reversed-phase HPLC using α,β,γ,δ-tetrakis(4-carboxyphenyl)porphine as a derivatizing reagent. Certified reference materials of iron and steel were used to prepare digestive samples by decomposition followed by 4-methyl-2-pentanone extraction and sulfuric acid fuming. The digested sample solutions were derivatized with Cd(II)-α,β,γ,δ-tetrakis(4-carboxyphenyl)porphine solution in ammonium buffer (pH 9.0) solution, using 5-sulfosalicylate as a masking reagent. Aqueous-acetonitrile (45 : 55 w/w) containing 7.0×10^<-2>molkg^<-1> of lactate buffer (pH 4.15) was used as an eluent and was monitored at 422 nm. A linear calibration was observed in the concentration range from 1×10^<-8>moldm^<-3> to 1×10^<-6> moldm^<-3>. The detection limit (3σ) of zn(II) was 1.3×10^<-9>moldm^<-3>, which corresponded to 0.32ppm in iron and steel samples. The recoveries of zinc added to the digested solution of iron and steel were with in 97 to 107%. The good recovery and high sensitivity indicate that the proposed system is of great promise for the determination of zinc present in iron and steel.
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