チタン酸バリウム中の微量アルミニウムの吸光光度定量 : エレクトロセラミックスおよびその材料の分析に関する研究(第2報)

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Aluminum in small amounts in barium titanate was determined spectrophotometrically. Barium(II) was precipitated as barium sulfate and aluminum was extracted into methyl iso-butyl ketone (MIBK) as the oxine complex. Titanium(IV) was masked as the hydrogen peroxide complex. The oxidized product of oxine was formed by interaction between oxine and hydrogen peroxide and extracted into MIBK. It had the absorption peak at about 370 nm in MIBK and interfered in the aluminum determination. The interference of the product could be overcome by smallest possible addition of hydrogen peroxide and adjusting pH of sample solutions at low temperature. The method is accurate, reliable, and applicable to 50 ppm of aluminum in barium titanate. Procedure: Weigh exactly about 400 mg of the finely ground samples and add 30 ml of hydrochloric acid (1+1). Heat to dissolve, cool to room temperature, and dilute to 100 ml exactly. Take 10 ml of this solution and add 5 ml of 10% sodium sulfate solution and 1 ml of 5% hydrogen peroxide solution. Cool the solution in an ice bath and add 3 ml of 1% oxine solution. Neutralize with ammonium hydroxide and add 10 ml of pH 10 buffer solution (NH3-NH4Cl). Transfer the solution to a separately funnel, dilute to about 50 ml, and add 10 ml of MIBK. Shake for a minute and allow to stand for 10 minutes. Discard the water layer and transfer the MIBK layer into a beaker. Add 1 g of unhydrous sodium sulfate. Measure the absorbance of the MIBK at 385 and 470 nm against the reagent blank. Calculate the corrected absorbance at 385 nm using the following equation and find the aluminum content from a calibration curve. Acorr 385 = A385-A470·A385 of 1 μgFe/A470 of 1 μgFe
社団法人日本分析化学会の論文

チタン酸バリウム中の微量アルミニウムの吸光光度定量 : エレクトロセラミックスおよびその材料の分析に関する研究(第2報)

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