Kinetic control of reagent dissolution for the flow injection determination of iron at trace levels

Abstract

A novel methodology for the determination of iron at the ppb level by spectrophotometric flow injection analysis is described. The method is based on the control of the flow dissolution of the colorimetric reagent 1,10-phenanthroline. This is achieved by means of the minimization of the area of contact between the carrier and the solid reagent, thus allowing the use of the fairly soluble organic compound without affecting the reactor lifetime. The reagent is melted inside an acrylic column (3.0 × 0.5 cm id) in such a way that a hollow space is left in the center after cooling. This new design improves some aspects of the performance of the classical solid-phase reactors as no problems related to the increase in the backpressure of the system are evidenced. Furthermore, the total reagent loading of the column is increased as no inert support is needed. A comparison between the performance of this novel methodology and that of the conventional packed reactor was performed and several advantages were observed: the use of higher flow rates, an increase in the reactor lifetime and a decrease in reagent consumption. A mathematical model to fit the concentration profiles of the dissolved reagent as a function of the residence time of the sample within the column is presented. The application of this strategy to the determination of Fe(II) improves the figures of merit in comparison to those obtained with a single-line homogeneous system: the limit of detection is 2 μg Fe L⁻¹ (3s) and the sensitivity is similar to that of the batch procedure. Results obtained for the determination of iron in natural waters are also presented.