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The determination of lead and cadmium by flame atomic absorption spectrometry after solid phase extraction on graphene oxide column with use of 4-acetamidothiophenol (ATP) as chelating reagent was described. PM6 semi-empirical and PBE density functional theory methods were used to investigation of adsorption mechanism of the complexes on GO sheet. The main factors influencing the preconcentration and determination of the analytes (pH, ATP amount, eluent type and concentration, flow rate and sample volume) were examined in detail. The effect of interfering ions on the separation-preconcentration of analytes was also investigated. For Pb(II) and Cd(II) solutions of 1.0 µg L-1, the preconcentration factor was as high as 250 (under the optimized conditions). The detection limits for Pb(II) and Cd(II) were 170 and 80 ng L-1, respectively. The validity of the proposed method was checked with standard reference materials and it has been successfully applied for the determination of trace Pb(II) and Cd(II) in water, herbal and fish samples with the recoveries of 99.4-103.5%.
We have recently reported an experiment in which GO and 3-(1-methyl-1H-pyrrol-2-yl)-1H-pyrazole-5-carboxylic acid (as adsorbent and chelating reagent, respectively) were applied to separation and preconcentration of Mn and Fe ions. This experiment led to apply the proposed procedure for simultaneous determination of mentioned ions at low concentrations in various aqueous samples, such as black and green tea, spinach, human hair, blood and urine. The adsorption mechanism of titled metals complexes on GO, was investigated by using a computational chemistry approach based on PM6 semi-empirical potential energy surface (PES).10 2-(tert-butoxy)-N-(3-carbamothioylphenyl) acetamide was used for Fe, Ni, Cu and Zn separation and preconcentration, in a same system.11 The aim of present study is to synthesize GO as a solid phase extractor and to investigate the feasibility of absorption of Pb(II) and Cd(II) on it, in the presence of the chelating agent. Synthesized material was first characterized by using transmission electron microscopy (TEM), Raman and Fourier transform infrared (FT-IR) spectroscopy. Chelates of lead and cadmium formed with 4-acetamidothiophenol (ATP) can be adsorbed on GO in column. The parameters including pH of the sample solution, amounts of ATP, sample volume, type of eluting agent and the effect of diverse ions were investigated. 153554b96e