A novel method for the filterless preconcentration of iron

Abstract

A novel method of analysis of iron by filterless preconcentration is presented. This is the first example of efficient preconcentration of a refractory transition metal where coprecipitation and columns were omitted. The method applies a manifold of flow injection analysis (FIA) to iron species that are preconcentrated on the inner walls of a tubular reactor. It was found that the adsorption of iron species to the walls was particularly pronounced in reactors of nylon material and enrichment factors of 30–35 could be attained, as dependent on the length of the reactor and on the time of preconcentration. In the preconcentration step of the FIA accessory, the optimum efficacy was obtained when the acidity of the samples was adjusted by HCl to pH = 2.5 whereas the ammonia preconcentration buffer should be kept alkaline at pH = 9.8. After being preconcentrated on the tubular reactor, the iron species were eluted by hydrochloric acid and analysed by flame atomic absorption spectrometry (FAAS). An unprecedented low limit of detection (LOD, 3σ) of 1.8 µg L⁻¹ was thus obtained for the analysis of iron by FAAS, and the calibration line was linear up to 100 µg L⁻¹. A high sampling frequency of 40 per hour was obtained and the protocol allowed analysis of small amounts of iron in drinking water, in digested samples and in saline water. The major influence of interferences originated from ligands that are known to complex strongly to iron species. The method thus developed was uncomplicated in operation and it exhibited an excellent long-term stability and a high selectivity. Further, it was environmentally safe owing to production of non-toxic waste disposals. Equally high enrichment factors (EF) were obtained for Fe(II) and Fe(III), which is explained by the very low solubility product of both species.