チオシアン酸錯体生成による微量モリブデンの抽出-吸光光度定量法

概要

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In order to determine traces of molybdenum in natural materials, the method of its analysis has been researched bacically in this paper. The difference in conditions for formation of the complex of molybdenum with thiocyanate depends upon the concentration of hydrochloric acid, ascorbic acid, cuprous chloride and potassium thiocyanate aqueous solution. Therefore, the solution containing a known quantity of molybdenum was ajusted to 3.6M hydrochloric acid, 0.5%ascorbic acid, 27×10^<-6>M cuprous chloride and 0.36M potassium thiocyanate. The complex of molybdenum formed was extracted into 5%tri-n-octylamine-cyclohexane solvent by shaking. This complex is considered as [MoO(SCN)_5]^<2->. The complex shows maximal optical absorption at 470nm. It was found that (0.01〜0.50)×10^<-6>M molybdenum in synthesis sample solution can be determined spectrophotometrically by measuring the absorbance of the complex. Calibration curve for molybdenum determination is expressed as the following formula, D_<470>=1.84_3C D_<470> is the absorbance at 470 nm, and C is the concentration of molybdenum (×10^<-6>M). Beer's law is obeyed for (0.01〜0.50)×10^<-6>M Mo. Apparent molar absorptivity is 2.94×10^4l mol^<-1> cm^<-1>.
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