Iron speciation by solid phase extraction and flame atomic absorption spectrometry using N,N′-bis-(2-hydroxy-5-bromobenzyl)-2-hydroxy-1,3-diiminopropane |
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Authors: | Emre Pehlivan Derya Kara |
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Institution: | (1) Department of Chemistry, Art and Science Faculty, Balikesir University, TR-10100 Balikesir, Turkey |
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Abstract: | A new Schiff base, N,N′-bis-(2-hydroxy-5-bromobenzyl)-2-hydroxy-1,3-diiminopropane, has been synthesized for the very sensitive
determination of iron(III) and iron(II) in natural water samples. It enabled a very selective and rapid method for iron determination
to be developed. The method has also been applied to total iron determination in sediment samples. In the preconcentration
system, the Schiff base reagent is mixed with the samples and chelates containing iron(III). The complexes are then adsorbed
on silica gel within a column system. Elution of the adsorbed chelate from the silica gel was performed with a small volume
of acetone containing 2.5% nitric acid. The iron is measured off-line by flame atomic absorption spectrometry. The method
can be applied to the preconcentration, separation and speciation of iron. The effects of parameters such as pH, sample flow
rate, eluent flow rate, foreign ions and ligand concentration have been investigated. The effect of humic acid that can produce
complexes with metal ions in natural systems has also been investigated. The results obtained indicate that the method is
not affected by the presence of up to 10 ppm humic acid, which would be a very high concentration to be present in natural
systems. The solid phase extraction method developed has been applied to the determination of iron in both natural water samples
and sediment samples. The LOD was found to be 0.17 mg L−1 when no preconcentration was used, although preconcentration factors of 100 could be achieved. The recovery values for spiked
samples were between 100 and 104%. The results were compared statistically with those from the standard 1,10 phenanthroline
method used for iron speciation in water systems. A Student’s t-test indicated no significant difference between the two methods. In addition, this method was applied to the analysis of
a certified sediment sample, LGC 6156. Generally, a 10-fold preconcentration factor was required for the analysis of natural
water samples. |
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Keywords: | : Solid phase extraction silica gel N N′ -bis-(2-hydroxy-5-bromobenzyl)-2-hydroxy-1 3-diiminopropane iron(III) iron(II) |
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