Determination of germanium by hydride generation with reducing tube followed by graphite furnace atomic absorption spectrometry using CH4/Ar as sweeper gas

T. Inui, S. Terada, H. Tamura and N. Ichinose

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Abstract

A sensitive method for the hydride generation and graphite tube furnace atomic absorption spectrometric measurements with a reducing tube using mixed gas (CH4 10% + Ar 90%) as sweeper gas has been developed for the determination of germanium. Germanium hydrides were generated in a horizontal glass tube, in which a pellet of NaBH4 was placed. 0.61/min of sweeper gas flow rate, 2,700° C of atomization temperature and 2.5–3 M of acidity range were the best experimental conditions. The strong supression of the germanium signal by Ni and Co was effectively eliminated with 1,10-phenanthroline and thiosemicarbazide was comparatively effective for Au. The reducing tube used in this technique is extremely simple and can be connected to all the types of graphite furnaces. A detection limit of 2 ng was obtained with a precision of 3–4%
Bei dem beschriebenen Verfahren werden die Hydride in einem horizontalen Glasrohr erzeugt, das eine NaBH4-Perle enthält. Als optimale experimentelle Bedingungen ergaben sich: Spülgas (0,61/min) aus 10% CH4 und 90% Ar, Atomisierungstemperatur 2700° C, 2,5–3 M Säure. Die starke Beeinflussung des Ge-Signals durch Ni und Co wurde mit Hilfe von 1,10-Phenanthrolin eliminiert, die Störung durch Au mit Hilfe von Thiosemicarbazid. Das verwendete Reduktionsrohr ist sehr einfach und kann für alle Arten von Graphitöfen benutzt werden. Die Nachweisgrenze beträgt 2 ng, die Reproduzierbarkeit 3–4%.

Paper read at the Meeting of the Japan Society for Analytical Chemistry, June 1982

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