Abstract
Molybdenum was separated and preconcentrated as molybdate on microcolumns of octadecyl silica sorbents and silica-based strongly basic anion exchanger prior to its determination by ICP-AES. With octadecyl silica Separon™ SGX C18 and Separon™ SGX RPS, the retention of 0.01–0.4 µg·mL−1 Mo from 50–1000 mL sample solutions was quantitative in the presence of the cationic surfactants carbethoxypentadecyltrimethylammonium bromide (Septonex®), dodecylbenzyldimethylammonium bromide (Ajatin®) or tetradecylbenzyldimethylammonium chloride (Zephyramine®) at pH 6–8. 96% ethanol was the most suitable eluent of the molybdate/surfactant associate. For the strongly basic anion exchanger Separon™ SGX AX, the optimal conditions for sorption of 5–20 µg Mo from 50–250 mL sample solutions were at pH 2 in the presence of 0.05 M ascorbic acid and ammonium citrate. 3 M HNO3 was a satisfactory eluent in this case. Organic solvents and excess of acids were removed by evaporation prior to the determination of Mo by ICP-AES in eluates. Both procedures can be used for the determination of ion-level molybdenum in waters.
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