title: An improved matrix separation method for characterization of ultrapure germanium (8N).
abstract: An improved matrix separation method has been described to characterize ultrapure germanium of 8N (99.999999%) purity. In this method, temperature of the reaction vessel in which in-situ generated chlorine gas reacts with germanium solid material directly is optimized to quantitatively remove Ge matrix from all its impurities. Optimized reaction temperature has been found to be 230±5°C. Recovery studies on more than 60 elements have been carried out at the optimized temperature. Recoveries of all the analytes except As, Se, Sn, Hg, Tl are found to be quantitative. The method has been examined for various amounts of Ge material and found to be suitable even for 10g of Ge sample and provides low parts per billion and trillion levels of process blanks. Determination of concentrations of impurities has been done by inductively coupled plasma quadrupole mass spectrometer (ICP-QMS) and high resolution continuum source graphite furnace atomic absorption spectrometer (HR-CS-GFAAS). In the absence of certified reference materials for ultrapure germanium, accuracy of the proposed method is established by spike recovery tests. Precision of this method is found to vary from 7% to 50% for concentrations between 4 and 0.004ngg(-1). Limits of detection (LOD) for the target analytes are found to be between 6 and 0.011ngmL(-1) or 1.8-0.003ngg(-1) for the proposed procedure. The method has been successfully applied for that characterization of ultrapure germanium material of 8N purity.
authors.affiliation: National Centre for Compositional Characterization of Materials (NCCCM) Bhabha Atomic Research Centre, Hyderabad 500062, India.
authors.forename: M A
authors.initials: MA
authors.lastname: Reddy
authors.affiliation: National Centre for Compositional Characterization of Materials (NCCCM) Bhabha Atomic Research Centre, Hyderabad 500062, India. Electronic address: shekhar_raparthi@rediffmail.com.
authors.forename: R
authors.initials: R
authors.lastname: Shekhar
authors.affiliation: National Centre for Compositional Characterization of Materials (NCCCM) Bhabha Atomic Research Centre, Hyderabad 500062, India.
authors.forename: Sunil
authors.initials: S
authors.lastname: Jai Kumar
keywords: Chemical analysis; Detection limits; GFAAS; ICPMS; Matrix volatilization; Ultrapure germanium