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Thesis submitted 23-03-2012.pdf - University of Limpopo ...

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and spherical in shape with an average size <strong>of</strong> 34 – 58 nm with the mean<br />

particle diameter <strong>of</strong> 42.41 nm ± 12.<strong>03</strong> nm and standard deviation <strong>of</strong> (σ)<br />

0.27 nm indicating broad size distribution for the superparamagnetic iron<br />

oxide nanoparticles (SPION), the particle diameters for the gold coated<br />

SPION are in the range 34-54 nm while the average particle size as<br />

determined from the TEM image for the selected fraction is 44.26 nm <br />

6.93 nm. The relative standard deviation <strong>of</strong> the sizes <strong>of</strong> the nanoparticles<br />

is 0.16 nm and the TEM for the functionalized gold coated SPION shows<br />

monodispersed particles which appear in spherical, cubic, irregular<br />

hexagon and oblong shapes with an average diameter <strong>of</strong> 44.65 nm. The<br />

HRTEM image, shows the existence <strong>of</strong> lattice planes which confirms the<br />

crystallinity <strong>of</strong> the material. The spacing between adjacent lattice planes is<br />

about 0.<strong>23</strong> nm which corresponds to the (311) interplanar distance <strong>of</strong><br />

Fe3O4 nanocrystals. Atomic force microscopy (ATM) was used to confirm<br />

the transmission electron microscopy (TEM) and HRTEM findings.<br />

The UV-Visible absorption spectra <strong>of</strong> the deionised water used in the<br />

procedure <strong>of</strong> preparation <strong>of</strong> the as-synthesized nanoparticles showed no<br />

absorption peak in a wavelength range <strong>of</strong> 350-750 nm, but after<br />

introducing the suspension <strong>of</strong> the Au-coated magnetic nanoparticles, an<br />

absorption peak located at 526 nm appeared which is ascribed to the<br />

surface plasmon <strong>of</strong> nanosized Fe3O4@Au nanoparticles.<br />

The kinetic studies using UV-visible spectrometer and the HRTEM images<br />

confirmed the adsorption <strong>of</strong> the porphyrin macromolecules as a coat on the<br />

magnetites particles. At a 5000 revolution per second (rps), aliquot sample<br />

<strong>of</strong> the aqueous phase <strong>of</strong> the suspension <strong>of</strong> 0.002 mM Fe3O4@Au in<br />

contact with the organic phase solution <strong>of</strong> the porphyrin taken for<br />

absorbance measurement at every 600 s showed a decrease in the<br />

concentration <strong>of</strong> the suspension while a noticeable and appreciable<br />

increase was also noted in the concentration <strong>of</strong> the porphyrin<br />

macromolecules measured at a λ max <strong>of</strong> 420 nm representing the<br />

iii

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