Adsorption studies of Cd(II) onto Al2O3/Nb2O5 mixed oxide dispersed on silica matrix and its on-line preconcentration and determination by flame atomic absorption spectrometry

The present study describes the adsorption characteristic of Cd(II) onto Nb2O5/Al2O3 mixed oxide dispersed on silica matrix. The characterization of the adsorbent has been carried out by infrared spectroscopy (IR), scanning electronic microscopy (SEM), energy dispersive spectroscopy (EDS), energy dispersive X-ray fluorescence analysis (EDXRF) and specific surface area (SBET). From batch experiments, adsorption kinetic of Cd(II) was described by a pseudo-second-order kinetic model. The Langmuir linear isotherm fitted to the experimental adsorption isotherm very well, and the maximum adsorption capacity was found to be 17.88mgg−1. Using the effective material, a method for Cd(II) preconcentration at trace level was developed. The method was based on on-line adsorption of Cd(II) onto SiO2/Al2O3/Nb2O5 at pH 8.64, in which the quantitative desorption occurs with 1.0molL−1 hydrochloric acid towards FAAS detector. The experimental parameters related to the system were studied by means of multivariate analysis, using 24 full factorial design and Doehlert matrix. The effect of SO42−, Cu2+, Zn2+ and Ni2+ foreign ions showed no interference at 1:100 analyte:interferent proportion. Under the most favorable experimental conditions, the preconcentration system provided a preconcentration factor of 18.4 times, consumption index of 1.08mL, sample throughput of 14h−1, concentration efficiency of 4.35min−1, linear range from 5.0 up to 35.0μgL−1 and limits of detection and quantification of 0.19 and 0.65μgL−1 respectively. The feasibility of the proposed method for Cd(II) determination was assessed by analysis of water samples, cigarette sample and certified reference materials TORT-2 (Lobster hepatopancreas) and DOLT-4 (Dogfish liver).