著者
高島 教一郎 河口 広司 中島 篤之助
出版者
社団法人 日本分光学会
雑誌
分光研究 (ISSN:00387002)
巻号頁・発行日
vol.11, no.1, pp.14-19, 1962

The evaporation method developed by Mandel' shtam and Zaidel is applied for the determination of impurity elements in uranium oxide.For the evaporation of impurity elements, most favorable sam-ple temperature, duration of heating, sample weight, and gap length between a collector electrode and a crucible are chosen.Calibration curves for the determination of Fe, Cr, Mn, Ni, Cu, B, Si, P and Cd are prepared.In the analyses of B and Cd, AgCl is added to uranium oxide (1%) as a carrier before evaporation and a d.c.arc excitation (10A) is used in the spectrographic procedure.Though the repeatability of analytical results is 10% or so for each element, the values determined for Fe and Ni are considerably deviated from the values obtained by the carrier-distillation method and chemical analysis.The evaporation rate is measured as a function of evaporation temperature for Sb, Fe and Cd by the use of radioactive tracers <SUP>124</SUP>Sb, <SUP>59</SUP>Fe and <SUP>115m</SUP>Cd respectively.
著者
加藤 金治 高島 教一郎 中島 篤之助
出版者
社団法人 日本分光学会
雑誌
分光研究 (ISSN:00387002)
巻号頁・発行日
vol.25, no.6, pp.293-298, 1976

In the atomic absorption spectrophotometry using an air-acetylene flame, both titanium and niobium existing as peroxo-complex compounds (presumably peroxo-) in nickel-base alloy sample solution seriously interfere with the determination of copper, manganese, and cobalt. Obtained absorbance readings for these elements show random values.<BR>The following two dissolution treatments have been examined: 0.5 g portions of the sample are dissolved in (1) HNO<SUB>3</SUB> (5 m<I>l</I>) +HCl (5 m<SUB>l</SUB>) +HF (1 m<SUB>l</SUB>), (2) 3N-H<SUB>2</SUB>SO<SUB>4</SUB> (25 m<I>l</I>) +HCl (10 m<I>l</I>) +H<SUB>2</SUB>O<SUB>2</SUB> (10 m<I>l</I>), and the solutions are diluted exactly to 100 m<I>l</I> with water. In the former, no interference effect is observed. In the latter, irregular absorbance readings are obtained for copper, manganese, and cobalt. No interference effect is observed, however, when a nitrous oxide-acetylene flame is used.<BR>The mechanism of the interference effects has been investigated by using an especially prepared twin-nebulizer. From the result, it is concluded that the origin of the interference effects can be attributed to the vaporization behavior of wet aerosols. Probably, these aerosols make refractory compounds in the air-acetylene flame and the compounds occlude copper, manganese, and cobalt and the incomplete dissociation of these compounds traversing the flame zone causes the irregular absorbance readings.
著者
高島 教一郎 中島 篤之助 河口 広司 大内 義彦
出版者
社団法人 日本分光学会
雑誌
分光研究 (ISSN:00387002)
巻号頁・発行日
vol.18, no.5, pp.262-267, 1969
被引用文献数
5

A direct, quantitative analytical technique for the analysis of gadolinium, dysprosium, europium and samarium in aluminum oxide using the X-ray-excited optical fluorescence spectra is described.<BR>Rare earth elements were coprecipitated with host aluminum from acid solution as aluminum hydroxide. Precipitated hydroxide was dried after centrifugal separation and then heated in a muffle furnace at 1000&deg;C for 2 hours. These oxides were then heated at 1450&deg;C in an electric resistance furnace for 60 seconds.<BR>Such an impulsive heating followed by quenching, described above, prominently enhances the luminescent intensities of rare earth elements. It was shown by the X-ray diffraction method that the crystal of Al<SUB>2</SUB>O<SUB>3</SUB> were transformed from &gamma;r-type oxide to the stable &alpha;-type oxide during the above heat treatment.<BR>Concentrations of gadolinium, dysprosium, samarium, europium have been determined by this method with detection limits ranging from 0.05 to 1.0ppm. Reproducibility was found to be 5-10%.The enhancement and suppression effect due to iron, silicon and copper were investigated and discussed.