An optimized method for the simultaneous determinationof Cr(III) and Cr(VI) in aqueous solutions using ionchromatography with chemiluminescence detection isdescribed. Excellent resolution of the two chromiumspecies was obtained using a single mixed-bed ion-exchange column with continuous elution. After postcolumn reduction of Cr(VI) to Cr(III), the light emitted duringthe Cr(III)-catalyzed oxidation of luminol with hydrogenperoxide was measured. Parameters affecting the postcolumn reactions such as reductant concentration, reductant mixing, point of luminol introduction, and luminolflow rate were optimized. The calibration curves in therange tested (0.01-50
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g L
-1) were linear, and detectionlimits of 0.002
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g L
-1 for both Cr(III) and Cr(VI) wereobtained. The results of the analyses of the water referencematerials LGC CRM6010 and NIST SRM1643d withcertified chromium values of 49 ± 4 and 18.53 ± 0.20
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g L
-1 and found to contain only Cr(III) were 49.2 ± 1.8and 19.0 ± 1.5
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g L
-1, respectively. Values of 10.6 ±0.5 and 10.1 ± 0.5
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g L
-1 were obtained when asimulated water sample containing 10
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g L
-1 Cr(III) andCr(VI) was analyzed.