This paper reports the utilization of 4-(2-pyridylazo) resorcinol (PAR) as a chelating reagent for in-column derivatization and the determination of trace Co, Fe, and Ni ions by reversed-phase high-performance liquid chromatography with photodiode array detector. A good separation of Co, Fe, and Ni chelates were achieved by using an Inertsil ODS-3 column and a mobile phase, consisted of methanol-THF-water mixture (50:5:45) containing ammonium acetate buffer (pH 5.0) and PAR. After full optimization, good repeatability of retention times (relative standard deviation (RSD) < 0.05%) and peak areas (RSD < 1.7%) was achieved as well as a good linearity (r (2) > 0.9991). The detection limits (S/N = 3), expressed as micrograms per liter, were 0.50 (Co), 9.07 (Fe), and 2.00 (Ni). The applicability and the accuracy of the developed method were estimated by the analysis of spiked water samples and certified reference material BCR 715 wastewater-SRM.
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