Use of 1-(2-pyridylazo)-2-naphthol as the post column reagent for ion exchange chromatography of heavy metals in environmental samples
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文摘
Ion exchange chromatography (IEC) using a bi-functional column (quaternary ammonium and sulfonate groups), followed by post-column reaction (PCR) with 1-(2-pyridylazo)-2-naphthol (PAN), was used to separate and quantitate Cu(II), Ni(II), Zn(II), Co(II), Cd(II), Mn(II) and Hg(II) at low concentration levels. IEC–PCR separation was achieved within 14 min using the mobile phase containing 3 mmol L&#x22121 2,6-pyridinedicarboxylic acid (PDCA) and 3 mmol L&#x22121 oxalate at pH 12.5. Effects of pH as well as PAN, detergent and chloride ion concentrations during post-column reaction on detector response were examined. Detection limits were less than 4.5 μg L&#x22121 for all metals except Hg(II) (19 μg L&#x22121) using spectrophotometric measurements at 550 nm. Analytical validations showed good linearity for detection up to 6.0 mg L&#x22121, with R2 higher than 0.99. Precisions based on retention time evaluation for intra-day and inter-day measurements with the relative standard deviation (RSD) were less than 2.9 % and 3.6 % , respectively. The method gave good accuracy with the recoveries ranged from 80.5 to 105 % for all metal ions studied. The proposed method was applied to the analysis of metal ions in environmental samples (leachate, soil and sediment) in Northeastern Thailand. The results were in good agreement with atomic spectroscopic measurements on the same samples.

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