Preconcentration of lead in water samples using combined cloud point‐solid phase extraction based on TiO₂/Mn₃O₄/Fe₃O₄ nanocomposite

Abstract

In this work, the TiO₂/Mn₃O₄/Fe₃O₄ nanocomposite was successful developed for enrichment of lead ions by using combined cloud point‐solid phase extraction. Lead ions were then determined by GF‐AAS spectroscopy. The nanocomposite was characterized by SEM, EDX, and XRD techniques. The result showed that the nanocomposite is composed of relatively uniform granules with particle size distribution in the range of 40÷80nm. The combined cloud point‐solid phase extraction procedure was optimized for lead ions with the optimal parameters as the absorbent dosage of 10 mg, the extraction time of 40 min, 10 mL of 10 % Triton X‐100, 1 mL of 1M NaCl in neutral media at 80°C. The parameters for the elution of Pb²⁺ ions such as concentration, volume, and the time of elution were also studied. The results showed that the elution efficiency of Pb²⁺ ions reached 97.0 % using 5 mL of HNO₃ 1M with continuous shaking for 5 minutes. Under optimized conditions, the linear range was 0.5÷80.0 μg/L of Pb²⁺ ions (r² = 0.998) with a detection limit of 0.27 μg/L. The relative standard deviation was calculated to be 5.61 % and the recovery efficiency of the method was about 96.30 %. The studied method was applied for the determination of lead content in water samples.