title: Volatilization of in situ generated antimony trichloride using aqua regia vapors for the determination of ultra trace impurities in high-purity antimony using inductively coupled plasma-mass spectrometry.
abstract: Volatilization of Sb has been carried out using vapors generated from aqua regia for the determination of non-volatile impurities present in antimony. The antimony trichloride (SbCl3) thus generated was volatilized >99.9% at 250 degrees C in 90 min. Recoveries of spiked impurities Al, Mn, Co, Ni, Cu, Sr, Ag, Cd, Ba, Pb were found to be >90% (47% for Pb) after volatilization of the matrix element. The only reagent used (aqua regia vapors) was generated in situ in a closed environment minimizing the external contamination. The procedure offers experimental blanks and method detection limits at lower ng g(-1) using ICP-MS. The method has been applied for the determination of impurities in two Sb samples of 99.5 and 99.999% (5N) purity. The developed method was validated using bromide volatilization procedure. The results obtained by the present method were also compared with those of Sector Field ICP-MS (SF-ICP-MS).
authors.affiliation: National Centre for Compositional Characterisation of Materials, Hyderabad, India.
authors.forename: A C
authors.initials: AC
authors.lastname: Sahayam
authors.forename: Shiuh-Jen
authors.initials: SJ
authors.lastname: Jiang
authors.forename: Chia-Ching
authors.initials: CC
authors.lastname: Wan