Analytica Chimica Acta 2008-01-01

Selective extraction, separation and speciation of iron in different samples using 4-acetyl-5-methyl-1-phenyl-1H-pyrazole-3-carboxylic acid

Şerife Saçmacı, Şenol Kartal, Şerife Saçmacı, Şenol Kartal, Şerife Saçmacı, Şenol Kartal

Index: Anal. Chim. Acta 623(1) , 46-52, (2008)

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Abstract

A method for speciation, preconcentration and separation of Fe(II) and Fe(III) in different matrices was developed using solvent extraction and flame atomic absorption spectrometry. 4-Acetyl-5-methyl-1-phenyl-1 H-pyrazole-3-carboxylic acid (AMPC) was used as a new complexing reagent for Fe(III). The Fe(III)–AMPC complex was extracted into methyl isobutyl ketone (MIBK) phase in the pH range 1.0–2.5, and Fe(II) ion remained in aqueous phase at all pH. The chemical composition of the Fe(III)–AMPC complex was determined by the Job's method. The optimum conditions for quantitative recovery of Fe(III) were determined as pH 1.5, shaking time of 2 min, 1.64 × 10 −4 mol L −1 AMPC reagent and 10 mL of MIBK. Furthermore, the influences of diverse metal ions were investigated. The level of Fe(II) was calculated by difference of total iron and Fe(III) concentrations. The detection limit based on the 3 σ criterion was found to be 0.24 μg L −1 for Fe(III). The recoveries were higher than 95% and relative standard deviation was less than 2.1% ( N = 8). The validation of the procedure was performed by the analysis of two certified standard reference materials. The presented method was applied to the determination of Fe(II) and Fe(III) in tap water, lake water, river water, sea water, fruit juice, cola, and molasses samples with satisfactory results.