Summary
A method has been developed for the analysis of trace impurities in high purity gallium at nanogram level. The gallium is separated from the trace elements by partial dissolution and by solvent extraction as HGaCl4 complex from 7N HCl with di-isopropyl ether. The aqueous phase containing the impurities is evaporated almost to dryness after adding 1 ml of 0.1N H2SO4, made up to 1 ml with 0.1N HCl and then analysed by atomic absorption spectrometry using electrothermal atomization. The limits of detection for the impurities lie in the range of 0.5 ng/g to 10 ng/g and the coefficient of variation varies from 1 to 5% at 50 ng/g level. The percentage recoveries for all the impurities are in the range 95–100%.
Zusammenfassung
Ein Verfahren zur Bestimmung von ng-Mengen Verunreinigungen in Reinstgallium wurde entwickelt. Das Gallium wird von den Spurenelementen durch teilweise Auflösung und durch Extraktion als HGaCl4 aus 7N HCl mit Diisopropyläther getrennt. Die wäßrige Phase mit den Verunreinigungen wird nach Zusatz von 1 ml 0,1 N H2SO4 fast bis zur Trockne abgedampft, mit 0,1N HCl auf 1 ml ergänzt und dann mittels Atomabsorptions-Spektrometrie unter Verwendung elektrothermischer Atomisierung analysiert. Die Nachweisgrenzen liegen zwischen 0,5 und 10 ng/g, der Variationskoeffizient zwischen 1 und 5% bei 50 ng/g. Die prozentuale Ausbeute für alle Verunreinigungen beträgt 95–100%.
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On leave from Nuclear Fuel Complex, Department of Atomic Energy, Hyderabad, India.
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Ramamurty, C.K., Kaiser, G. & Tölg, G. Determination of Al, Bi, Cd, Cr, Cu, Mn, Ni, Pb and Zn, in the ng/g range in high purity gallium by electrothermal vaporization AAS after preconcentration. Mikrochim Acta 73, 79–87 (1980). https://doi.org/10.1007/BF01197234
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DOI: https://doi.org/10.1007/BF01197234