1-(2-ベンゾチアゾリルアゾ)-9-フェナントールと界面活性剤を用いるニッケルの吸光光度定量

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1-(2-Benzothiazolylazo)-9-phenanthol (TAP) reacts with a small amount of nickel in the presence of a surface-active agent, Triton X-100, to form a soluble complex. The optimum conditions for spectrophotometric determination of nickel using the complex and the preventation of interference with the diverse ions were studied. The TAP-nickel complex has two absorption maxima at 555 and 590 nm and the reagent blank has it at 480 nm. The maximum absorbances are constant in the pH range from 6.0 to 7.5. Beer's low is obeyed up to 18.0μg/25 ml of nickel and the apparent molar absorptivity of the complex is about 5.5 × 10^4 1 mol^<-1> cm^<-1>, based on the calibration curve. The combining ratio of nickel and TAP in the com-plex is shown to be I : 2 by the molar ratio method and the continuous variation method. The proposed procedure is as follows: To the sample solution containing 10μg of nickel in a 100ml beaker, add about 5 ml of sodium acetate and borate buffer (pH 6.8) and I ml of the Triton X-100 (0.2 g/ml) solution. Then, control the total volume from 15 to 20 ml with water, and adjust to pH 7.0±0.2 with 0.1 M sodium hydroxide or 0.1 M hydrochloric acid. Add 0.7ml of 10^<-3>M TAP-dioxane to the solution, and heat the solution on a boiling water bath for about 10min, and cool. Transfer the solution into a 25 ml volumetric flask and dilute it to the mark with water. Measure the absorbance at 590 nm against the reagent blank or water. The determination gives a positive error in the presence of cobalt (II), copper (II), zinc, palladium (II), silver, cadmium or mercury (II), and gives a negative error in the presence of each of many kinds of ions, which are precipitated at pH 7.0±0.2. In order to remove the interference of those ions, solvent extraction of nickel dimethylglyoximate in ammoniacal tartarate solutions, masking of the colored interfering ions with EDTA were studied, and good results were obtained. In addition, nickel in metallic copper was determined successfully by this method.
社団法人日本分析化学会の論文
1979-09-05

1-(2-ベンゾチアゾリルアゾ)-9-フェナントールと界面活性剤を用いるニッケルの吸光光度定量

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