Development of a new analytical method for Pb preconcentration and its further determination in water and foodstuffs using relatively low-sensitivity flame atomic absorption spectrometry

摘要

The present study describes chelation of Pb(II) with ascorbic acid and formation of a charge-transfer sensitive ion-pair in the presence of Rhodamine 6G at pH 5.5, and then its extraction to the micellar phase of non-ionic surfactant, PONPE 7.5 by an ultrasound-assisted cloud point extraction method before analysis by FAAS. The various variables affecting ion-pair formation and extraction efficiency were studied and optimised. Under the optimised conditions, the good linear relationships in the ranges of 0.4-150 mu g L-1 and 0.8-120 mu g L-1 for solvent-based calibration and matrix-matched calibration curves, respectively, were achieved with a pre-concentration factor of 71.4 from pre-concentration of 50-mL sample. Moreover, the limits of detection with good sensitivity enhancements of 124 and 114.5 were 0.13 and 0.24 mu g L-1, respectively, while the intra-day and inter-day precision (as RSD%, for five replicate measurements of 5 and 100 mu g L-1 in the same day and three succeed days) were in range of 2.8-5.4% and 3.7-6.3%, respectively. The matrix effect on triplicate determination of 50 mu g L-1 Pb(II) was also investigated. The accuracy of the method was statistically verified by the analysis of two certified reference materials (CRMs) after digestion with acid mixtures (HNO3-H2O2-HF and HNO3-H2O2) and dilution at suitable ratios. It has been observed that there is statistically not a significant difference between the certified- and found-values. The accuracy was also controlled using the pre-treated sample solutions spiked at different concentration levels, and the good spiked recoveries were obtained in range of 90-102.8%. The method was successfully applied to the determination of trace amounts of lead in water and food matrices with satisfactory results.