Closed-vessel microwave assisted volatilization of Ge, Se, Si and quartz as their volatile compounds , for the determination of trace impurities in high purity Ge, Se, Si and quartz is reported. The volatilization of Ge is 98.7% using vapors of aqua regia whereas vapors generated from 72:1 ratio of HCl:HNO3 is required to volatilize 99.2% of Se. Using vapor of 10:5 ratio of HF:HNO3 , the volatilization of Si is 98.6%, and the volatilization of quartz is 99.0% with 15:3 ratio of the mixed acids. The recoveries of Mg, Cr, Mn,, Ni, Co, Cu, Zn, Cd, Ba and Pb are in the range 83-116%. Determinations are carried out using inductively coupled plasma mass spectrometer with Dynamic Reaction CellTM (DRC ICP-MS). Isobaric interferences, due to the formation of 40Ar12C+, 35Cl16OH+, 40Ar16O+ and 40Ar74Ge+ on the determination of 52Cr+, 56Fe+ and 114Cd+, have been alleviated using ammonia cell gas in DRC. Matrix volatilization using in situ generated acid vapors in closed containers resulted in sub ng mL-1 experimental blanks. Method detection limits are in the low ng g-1 level. The methods developed have been applied to determine trace impurities in high purity Ge, Se, Si and quartz samples.