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A procedure was developed for the fast simultaneous speciation analysis of Fe(II)-EDTA and Fe(III)-EDTA in the absorbing liquid of a denitrification system with LC-ICP-OES based on ultrasound-assisted replacement reaction. Under ultrasonication, Fe was replaced from Fe(II)-EDTA by Cu at pH = 1, subsequently Fe and Fe(III)-EDTA were separated by LC before introduction into the ICP-OES for measurement. The effects of several key factors, such as pH, concentration of Cu, and ultrasonication time on the efficiency of the replacement reaction were investigated. Under the optimized conditions, the limits of detection of 1.2 × 10 mol L for Fe(III)-EDTA and 1.6 × 10 mol L for Fe(II)-EDTA were obtained, with a relative standard deviation (n=11, at 1.79 × 10 mol L for both) of 4.7% for Fe(II)EDTA and 2.1% for Fe(III)-EDTA. These results successfully fulfill the requirement of speciation analysis of Fe(II)-EDTA and Fe(III)EDTA (typical concentration: 0.025 ~ 0.1 mol L) in the absorbing liquid of the denitrification system. Common interferences from Na, K, SO3 2− , SO4 2− , Ca, Mg were also investigated. Routine spike recovery tests with randomly selected samples showed the satisfactory results of 84.0% ~ 93.0% and 92.0 ~ 101.3% for Fe(II)-EDTA and Fe(III)-EDTA, respectively. The proposed method is simple yet sensitive for screening of Fe(II)-EDTA and Fe(III)-EDTA in the absorbing liquid samples of a denitrification system, it is also a potential analytical method for other sample matrices.

atomic spectroscopy

Ultrasound-assisted Replacement Reaction for the Simultaneous Speciation Analysis of Fe(II)-EDTA and Fe(III)-EDTA in Absorbing Liquid of Denitrification System with LC-ICP-OES