A rapid and sensitive method for the sequential determination of Cr(III) and Cr(VI) in water samples based on flow injection on-line preconcentration and separation with two-microcolumn system-flame atomic absorption spectrometry has been developed. The Cr(III) and Cr(VI) in water samples were respectively retained in a microcolum with cation exchange resin and in a microcolumn with anion exchange resin and were eluted directly by 15% HNO3 and 8% NH4NO3, respectively. The characteristic concentrations (pre-concentration time of 1 min) for Cr(III) and Cr(VI) were 1.50 micrograms.L-1 and 1.39 micrograms.L-1, respectively, The relative standard deviations at 10 micrograms.L-1 level were 3.41% and 1.80%, and the corresponding detection limits (3 sigma) were 1.03 micrograms.L-1 and 0.54 microgram.L-1, respectively. The satisfactory recovery of 93.48%-107.5% could be obtained from water samples.

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