Analytical Sciences

Abstract − Analytical Sciences, 25(3), 379 (2009).

Simultaneous Spectrophotometric Determination of Orthophosphate and Silicate Ions in River Water Using Ion-Exclusion Chromatography with an Ascorbate Solution as Both Eluent and Reducing Agent, Followed by Postcolumn Derivatization with Molybdate
Nobutake NAKATANI,* Wakako MASUDA,* Daisuke KOZAKI,* Ryozo GOTO,* Nobukazu NAKAGOSHI,* Masanobu MORI,** Kiyoshi HASEBE,*** and Kazuhiko TANAKA*
*Graduate School for International Development and Cooperation, Hiroshima University, 1-5-1 Kagamiyama, Higashi-Hiroshima, Hiroshima 739-8529, Japan
**Graduate School of Engineering, Gunma University, 1-5-1 Tenjin-cho, Kiryu, Gunma 376-8515, Japan
***Faculty of Human Life Sciences, Fuji Women's University, Hanakawa, Ishikari, Hokkaido 061-3204, Japan
Ion-exclusion chromatography was examined for the simultaneous spectrophotometric determinations of orthophosphate and silicate ions in river water using an ascorbate solution as both an eluent and a reducing agent, followed by postcolumn derivatization using molybdate. The detector responses for both ions increased with increased ascorbic acid concentration in the eluent, but peak tailing was observed for the orthophosphate ion. This suggests that the amounts of undissociated orthophosphate ions increased with decreased eluent pH, resulting in the penetration of the phosphate to the Donnan's membrane formed on the resin surface. Using a neutral sodium ascorbate solution as an eluent, the peak shape was improved. With optimized separation and derivatization conditions (eluent, 20 mM sodium ascorbate; color-forming reagent, 10 mM sodium molybdate-60 mM sulfuric acid; flow rates of eluent and color-forming reagent, 0.4 and 0.2 mL min-1; coil length, 6 m), the detection limits of orthophosphate and silicate ions were 0.9 and 1.0 µg L-1, respectively. This method was successfully applied to the determination of orthophosphate and silicate ions in Kurose River water and the quantitative evaluations of the effects of water intake to a reservoir and discharge from a biological sewage treatment plant on the fluxes of these ions in the river.