Modified matrix volatilization setup for characterization of high purity germanium

Abstract

Modified matrix volatilization (MV) method has been described to characterize high purity germanium material of 7N (99.99999%) purity. Transport of both, the chlorine gas generated in-situ in this method and the argon gas (carrier) is fine controlled by means of a mass flow controller. This enabled both uniform reaction of chlorine gas with the germanium matrix and smooth removal of germanium matrix as its chloride. This resulted in improvement in the reproducibility of the analytical results. The use of quartz reaction vessel has lead to the reduction in the process blank levels. The combined effect of these modifications in the MV setup has resulted in very consistent and low process blanks and hence improved detection limits of this method. Applicability of the method has been expanded to rare earth elements and other elements after examining their recoveries. The quantification is done by using inductively coupled plasma quadrupole mass spectrometer (ICP-QMS) and continuum source graphite furnace atomic absorption spectrometry (CS-GFAAS). In the absence of certified reference materials for high pure germanium, the accuracy of the method is established by spike recovery tests. The precision of the method has been found to vary from 1 to 30% for concentrations between 1 and 30ngg−1. The limits of detection (LOD) for the target analytes are found to be between 18 and 0.033ngg−1.