硫酸塩中の微量セレンの吸光光度定量

概要

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Selenium in sulfate reagents was determined by spectrophotometric method using 3, 3-diaminobenzidine. Twenty grams of sulfate reagent (G. R.) was dissolved in 80 ml of water, and spike selenium of less than 20 μg was added. The solution was treated with hydrazine hydrochloride solution in the presence of 10 ml of hydrochloric acid for reducing selenium. The selenium was filtered through a fritted glass filter of the finest pore, and was transfered into a beaker by dissolving with a few 1 ml portions of hydrochloric acid and washed several times with water. Color development was made by the 3, 3-diaminobenzidine method of K. L. Cheng, and the absorbance was measured at 420 mμ. A plot of a series of results on 5 to 20 μg of added selenium on the sample gave a selenium vs. absorbance curve which was parallel with the calibration curve of selenium. Gradient of the calibration curve was about 30% lower than the calibration curve without separation process before color development, probably because of a loss of selenium during reduction and filtration, but the reproducibility of the result was fairly good as seen in Table I. G. R. grade ammonium sulfate and sodium sulfate were found to contain 0.02 and 0.01 ppm of selenium, respectively.
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