フェロインの抽出比色による水中の超微量鉄の定量

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Extractive spectrophotometric determination of trace amounts of iron in water for high pressure boilers, brewing industry etc. has been investigated. To extract ferroin, the complex of 1, 10-phenanthroline and iron (II), from water to chloroform, sodium dioctylsulfosuccinate was selected by a preliminary experiment from a number of anionic surface active agents. Ferroin becomes soluble in chloroform when its cationic charge is discountered with dioctylsulfosuccinate ion. The analytical procedure is as follows. Four ml of purified 7M hydrochloric acid is added to 200 ml of sample solution, which is heated in a water bath of above 80°C for 30 min. After it is cooled to the room temperature, 4 ml of 10% hydroxylamine hydrochloride solution and 10 ml of 0.12% 1, 10-phenanthroline solution are added into it. After the solution is neutralized with purified 7M ammonium hydroxide to pH 5.25.8, 10 ml of buffer solution containing sodium acetate and hydrochloric acid is added to adjust the pH to 4.6. The solution is allowed to stand for 30 min. and its pH is lowered to 2.4 with purified 1M hydrochloric acid. The solution is transferred into a separatory funnel, to which are added 3 ml of 1% aqueous sodium dioctylsulfosuccinate solution and 10 ml of chloroform. Then the solution is shaken for 2 min. and the extraction is repeated with two 7 ml portions of choloroform. The extract is collected into a 25 ml volumetric flask containing 3 ml ethanol and diluted to the mark with pure chloroform. The absorbance is measured at 515 mμ in a 50 mm cell, using a reagent blank as a reference. Three ppb of iron can be determined, whereby 90% confidence interval extends from 2.23 ppb to 3.67 ppb. The regression line is given by x=164.112 y +0.219, where y is the absorbance for the iron concentration x.
社団法人日本分析化学会の論文

フェロインの抽出比色による水中の超微量鉄の定量

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