キレート交換樹脂による前濃縮とα-ベンゾインオキシムを用いる溶媒抽出を併用するチオシアン酸吸光光度法による自然水中の微量モリブデンの定量

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A simple preconcentration method with chelating exchange resin followed by solvent extraction is described for the determination of molybdenum in natural waters by absorption spectrometry with thiocyanate. The results of experiments using chelatng resin, Dowex A-1, are shown as follows: 1. Chelating resin (Dowex A-1) was digested with 2M nitric acid for about five hours on a water bath at 60℃, and after filled with in 1cm diameter ion exchange columns to a depth of 6cm, the resin was washed with redistilled water until the pH of elution reached 4.5. 2. The optimum pH of 5.0 was determined by examining effects of pH on the amount of molybdenum in synthetic sample retained in the chelating resign (Dowex A-1). The amount of molybdenum added was 0.20μmol. 3. Synthetic sample solutions of various volumes containing 0.2μmole Mo were prepared to obtain the required pH of 5.0±0.2 for the experiment, and effects of the volume on recovery were investigated. Moreover, the complex of molybdenum-α-bensoineoxime formed in the system of water-ethanol was extracted with chloroform solvent, and extracted back with conc, hydrochloric acid. After this back extract was diluted with redistilled water, the complex of molybdenum-thiocyanate formed with thiocyanate was extracted with TNOA-cyclo-hexane, and its optical absorption at 470 nm was measured. Apparent molor absorptivity is 2.94×10^4 1 mol^<-1>cm^<-1>. The limit of determination was 0.99 nmol/ml. The method was applied to the determination of traces of molybdenum in river water and sea water with satisfactory results.
仙台大学の論文

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熊坂繁太郎
仙台大学

キレート交換樹脂による前濃縮とα-ベンゾインオキシムを用いる溶媒抽出を併用するチオシアン酸吸光光度法による自然水中の微量モリブデンの定量

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