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

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.