マイクロウエーブ放冒発光分光分析法によるアルミニウム地金中の ppb レベルのヒ素の定量

概要

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This method is based on the conversion of arsenic into arsine followed by microwave excitation in a quarz discharge tube. An aluminum sample {(O.5〜1.0)g} was placed in a reaction vessel, 50ml of 6M hydrochloric acid and O・2 ml of 10% tin(II) chloride solution were added, and the vessel was quickly connected to a liquid nitrogen trap (50xO.8cm o.d., U-shaped glass tubing) via a CaCl_2 tube. Arsine generated was swept by a nitrogen flow of 30ml/min into the trap. When the sample had been completely dissolved, 2.0g of granular zinc was added to the vessel and the nitrogen was passed for another 60 min. The trap was then disconnected from the vessel and connected to a discharge tube. Argon was introduced into the trap at a rate of 30ml/min, and to optimize the discharge conditions, an additional argon flow of 470ml/min was fed to the discharge through a bypass.
1975-07-10