Reversed-phase liquid chromatographic separation and determination of Ni(II), Cu(II), Pd(II), and Ag(I) using 2-pyrrolecarboxaldehyde-4- phenylsemicarbazone as a complexing reagent

Abstract

This paper reports the utilization of 2-pyrrolecarboxaldehyde-4- phenylsemicarbazone (PPS) as a complexing reagent for the simultaneous determination and separation of Ni(II), Cu(II), Pd(II), and Ag(I) by reversed-phase high-performance liquid chromatography with UV detector. A good separation was achieved using Microsorb C18 column (150 × 4.6 mm i.d.) with a mobile phase consisted of methanol: acetonitrile: water: sodium acetate (1 mM) (68: 6.5: 25: 0.5 v/v/v/v) at a flow rate of 1 mL/min. The detection was performed at 280 nm. The linear calibration range was 2-10 μg/mL for all metal ions. The detection limits (S/N = 3) were 80 pg/mL for Ni(II), 0.8 ng/mL for Cu(II), 0.16 ng/mL for Pd(II), and 0.8 ng/mL for Ag(I). The applicability and the accuracy of the developed method were estimated by the analysis of Ni(II) in hydrogenated oil (ghee) samples and Pd(II) in palladium charcoal. © 2013 Arfana Mallah et al.