Determination of Trace Amounts of Si and P in Iron and Steel Using Gel Chromatographic Separation Followed by ICP-MS
✍ Scribed by Hanada, K. ;Fujimoto, K. ;Shimura, M. ;Yoshioka, K.
- Publisher
- John Wiley and Sons
- Year
- 1998
- Tongue
- English
- Weight
- 134 KB
- Volume
- 167
- Category
- Article
- ISSN
- 0031-8965
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✦ Synopsis
Analytical methods were investigated to improve the sensitivity of detecting trace amounts of Si and P in high-purity iron and steels. Silicon and P in the solutions were converted to SiMo 12 O 40 4À and P 2 Mo 18 O 62 6À , respectively, and adsorbed on a dextran gel column (Sephadex 1 G25 medium). For the analysis of Si, the column was washed with 10 w/v% oxalic acid + 10 v/v% nitric acid solution to remove the molybdophosphate, and the molybdosilicate was eluted with aqueous ammonia. The Mo in the eluate was determined by ICP-MS, which resulted in the determination of Si. For the analysis of P, the adsorbed molybdophosphate, which was in the form of ªmolybdophosphate yellowº, was reduced to ªmolybdophosphate blueº by Sn(II). This conversion prevented the molybdophosphate from being eluted in the column washing process. After washing the column with 5 v/v% hydrochloric acid, the molybdophosphate was eluted with aqueous ammonia, and P was determined in the same fashion as the determination of Si. The determination of Si and P by the present method was not interfered by the presence of Al, As, Co, Cr, Cu, Mn, Ni, and Ti. The limits of determination were 0.05 ppm for Si, and 0.4 ppm for P.