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

ABSTRACT

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 μg L⁻¹ and 0.8–120 μg 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 μg L⁻¹, respectively, while the intra-day and inter-day precision (as RSD%, for five replicate measurements of 5 and 100 μg 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 µg 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.

KEYWORDS:

• Lead
• flame atomic absorption spectrometry
• Rhodamine 6G
• ascorbic acid
• ultrasound-assisted cloud point extraction
• water/foodstuffs

Acknowledgments

A partial financial support from Cumhuriyet University, Scientific Research Projects Commission (CUBAP) through F-536 is gratefully acknowledged. The author wishes to thank his colleague at the Analytical Research Labs., Assoc. Prof. Nail Altunay for the flame AAS analyses included in this study.

Disclosure statement

No potential conflict of interest was reported by the author.

Additional information

Funding

This work was supported by the Cumhuriyet University, Scientific Research Projects Commission [F-536];