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Single particle transfer for quantitative analysis with total-reflection X-ray fluorescence spectrometry

全反射蛍光X線分析法を用いた個々の粒子中元素の定量分析法

江坂 文孝  ; 江坂 木の実; 間柄 正明  ; 桜井 聡 ; 臼田 重和; 渡部 和男

Esaka, Fumitaka; Esaka, Konomi; Magara, Masaaki; Sakurai, Satoshi; Usuda, Shigekazu; Watanabe, Kazuo

個々の粒子を電子顕微鏡に付設したマニピュレータにより測定用試料台上に移動し、全反射蛍光X線分析法により定量分析を行う方法について検討を行った。その結果、試料台上にあらかじめ内標準物質を添加しておくことにより、直径3.04-8.84マイクロメートルの銅粒子に対して計算値からの偏差10%以内で定量を行うことができた。一方、直径10.17マイクロメートル以上の銅粒子に対しては偏差が33%以上であり、正確な定量が不可能であった。しかし、このような大きな直径の粒子に対しても、粒子を測定に先立って溶解することにより偏差9%以内で定量が可能であった。本法は真ちゅう粒子の定量にも応用され、その有効性が確認された。今後、環境試料中の微粒子に含まれる核物質量の測定についても検討を行っていく。

Individual Cu particles were transferred, with a manipulator attached to a scanning electron microscope, onto individual Si carriers for subsequent quantitative analysis by means of total-reflection X-ray fluorescence spectrometry. By applying an internal standard to the carriers prior to the particle transfer, the amounts of Cu were successfully determined for the particles with diameters between 3.04 and 8.84 micrometer. The deviations of the measured values from the calculated ones were within 10%. However, the deviations were more than 33% if particle diameters were greater than 10.17 micrometer. This suggests that in such a case the fluorescent X-ray is not emitted from all parts of the particle. Even if particle diameters were greater than 10.17 micrometer, the amounts of Cu could be determined with the deviations within 9% when the particles were dissolved with HNO$$_{3}$$ solution. This technique was also successfully applied to the measurement of individual brass particles.

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パーセンタイル:21.1

分野:Instruments & Instrumentation

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