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Abstract In this work two novel nano composite materials (PUF/ZnFe 2 O 4 and PUF/Mn 0.4 Zn 0.6 Fe 2 O 4 ) have successfully been utilized as a new solid phase extraction (SPE) sorbents for the separation of cadmium and copper ions in various water samples. The magnetic nano particles were successfully synthesized by using modified citrate sol-gel method. Then, the magnetic nano powders (0.1g of ZnFe 2 O 4 or Zn 0.6 Mn 0.4 Fe 2 O 4 ) were added to the PUF during the preparation step to have 30 g of the nano composite materials (PUF/ZnFe 2 O 4 or PUF/Mn 0.4 Zn 0.6 Fe 2 O 4 ). The phase composition, morphology, particle size, and saturation magnetization of the prepared nanoparticles were studied using X-ray diffraction (XRD), high resolution-transition electron microscopy (HR-TEM) and vibrating sample magnetometer (VSM). The microstructure of the prepared PUF/nanoparticles was observed using scanning electron microscope (SEM). The effects of pH, sorbent dose and shaking time of the composite nano materials on the Cd 2+ and Cu 2+ ions removal from an aqueous solution and real water (tap water, Qaroun lake water and Bahr Youssef water from Fayoum city, Egypt) were investigated. The XRD patterns show that the high crystallinity of the spinel phase and the average crystallite size of all nanoparticles in the range 16-25 nm. The HR-TEM images observed that the particle size of the prepared nanoparticles in PUF ranged from 5.3 to 25 nm. VSM measurements showed that Ms of ZnFe 2 O 4 and Zn 0.6 Mn 0.4 Fe 2 O 4 samples were 4.179 emu/g and 6.885 emu/g, respectively. The microstructure of the prepared ABSTRACT xii ABSTRACT xii composites observed the spongy structure (spherical shaped) and higher porosity of the sample ZnFe 2 O 4 /PUF than sample Zn 0.6 Mn 0.4 Fe 2 O 4 /PUF. The batch procedure shows the maximum extraction percentage on the two composite nano materials (PUF /ZnFe 2 O 4 and PUF/Mn 0.4 Zn 0.6 Fe 2 O 4 ) are 96% - 94% and 97% - 96% for Cd 2+ and Cu 2+ ions, respectively, at the optimal conditions (pH " ~ " 5 - 6, 60 min shaking time and sorbent weight 0.1gm from nano composite). While, the maximum extraction percentage on the two nano powder (ZnFe 2 O 4 & Mn 0.4 Zn 0.6 Fe 2 O 4 ) are 95 % - 93 % and 93% -93% for Cu 2+ and Cd 2+ , respectively, at the optimal conditions (pH " ~ " 5 - 6, 60 min shaking time and sorbent weight 0.1gm nano powder). The work presented in this thesis is divided into four chapters; as follows:- Chapter 1: Introduction. This chapter includes hazards of heavy metal ions on human and animal’s life and the aim of the work. Chapter 2: Review of Literature. This chapter includes some reviews about hazards of heavy metal ions especially cadmium and copper ions to be studied during the course of this work. Some techniques used in preconcentration and/or separation of trace levels of heavy metal ions are mentioned. Furthermore, this chapter includes some information about solid phase extraction and types of many sorbents such as nano sorbent, and foam sorbent Chapter 3: Materials and Methods. This chapter involves information about instruments, chemicals and reagents used in this work, methods preparation of nano ABSTRACT xii sorbent (ZnFe 2 O 4 and Mn 0.4 Zn 0.6 Fe 2 O 4 ) and synthesis of nano composite (PUF/ZnFe 2 O 4 and PUF/Mn 0.4 Zn 0.6 Fe 2 O 4 ), the methodology employed in this work and the recommended procedures are explained in details in this chapter. Chapter 4: Results and Discussion. Here, the characteristics of nano composite are discussed. Then, the chemical parameters such as pH, shaking time, sorbent weight and capacity of the prepared solutions were studied. The batch procedures show that the quantitative extraction percentages by the two composite nano materials (PUF/ZnFe 2 O 4 and PUF/Mn 0.4 Zn 0.6 Fe 2 O 4 ) are more than 95%. The optimum experimental conditions are determined. Applications of the two composite nano materials (PUF/ZnFe 2 O 4 and PUF/Mn 0.4 Zn 0.6 Fe 2 O 4 ) are outlined by preconcentration of tested metal ions from various real samples (tap water, Qaroun lake water and Bahr Youssef water) collected from Fayoum City, Egypt. Finally, the thesis demonstrates the references utilized in this work and conclusions achieved from the whole work together with the recommendations that may be undertaken in future. |