炎光光度法による純鉄中の極微量マンガンの定量法

概要

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Flame photometric method has been successfully adopted to the determination of micro amounts of manganese (0.00020.01%, sample taken 0.1 g) in pure iron. This determination, scarcely interfered with the co-existing elements, was found to be more suitable than colorimetric determination. The sensitivity was much increased by spraying manganese into oxyhydrogen flame after a TTA extraction. The recommended procedure is as follows. One tenth g of sample is decomposed with the mixed acids (HCl, HNO3 and HClO4) and iron is removed with a MIBK extraction. Hydrochloric acid layer is evaporated to almost dryness after perchloric acid is added. Five ml of 1 M ammonium tartrate and 8 ml of the mixed buffer solution (pH 8.5) are added, and the solution is diluted to 25 ml. Manganese is extracted with 10 ml of 0.005M TTA-mixed ketone (50 v/v % of 2-octanone in MIBK) solution. The organic layer is sprayed into oxyhydrogen flame (O2 : 1.0 kg / cm2, H2: 0.13 kg /cm2) and manganese is determined from the intensity at 403.3 mμ. An analysis was carried out in about 70 min.within an absolute error of 0.0001%. Twenty μg of 21 elements commonly found in pure iron hardly interfered when 5 μg of manganese was determined.
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