Studies on the determination of trace elements in high-purity Sb using GFAAS and ICP-QMS |
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Authors: | M V Balarama Krishna D Karunasagar and J Arunachalam |
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Institution: | (1) National Centre for Compositional Characterisation of Materials, E.C.I.L. Post, Hyderabad-500 062, India, IN |
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Abstract: | Trace element impurities in high-purity antimony were determined employing three different methods for the removal of matrix;
on Dowex 50WX 8 by adsorption from 0.1 mol/L HF and elution with 4 mol/L HNO3; on Chelex-100 resin (in NH4
+ form) Bi, Cd, Co, Cu, and Pb were separated in the presence of tartaric acid at a pH of 9.0 ± 0.1 with subsequent elution
with 2 mol/L HCl; these determinations were carried out by GFAAS. The separation of trace impurities from Sb by volatilization
of the matrix from H2SO4 and HBr medium was also investigated. ICP-MS was used for the determination in these cases.
All the three procedures showed that the removal of the antimony matrix was nearly quantitative (> 99.99%). The recoveries
of trace elements were found to be > 95%. The relative standard deviations were in the range 2–7%. Standard addition calibrations
were used. The levels of process blanks indicate that with careful optimization, the volatilization procedure coupled with
ICP-QMS can be used for trace impurity characterization of 6N+ Sb.
Received: 25 May 1998 / Revised: 23 September 1998 / Accepted: 26 September 1998 |
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