STUDIES ON THE PRECIPITATION OF SOME PHOSPHATES AND CONFORMATIONS OF CYCLIC COMPOUNDS FROM X-RAY DIFFRACTION DATA

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Date
1997
Authors
AJIBOLA , VICTOR OLATUNJI
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Abstract
In part I of the thesis, studies were carried out on the precipitation of hydroxyapatite. A preliminary experiment involving the preparation of calcium hydroxyapatite (HAP) using three different sets of starting materials was done. The crystallinity and stoichiometry of the HAP were dependent on the starting materials. The precipitation of amorphous calcium phosphate (ACP), and its transformation to HA? in the presence of various compounds and ions have also been studied using x-ray diffractometry. The nucleotides, AMP, ADP and ATP (usually regarded as type II inhibitors) caused a slight but discernible decrease in the mean size of the apatitic crystals. However, citrate another type II inhibitor did not appear to alter the mean cryst size in agreement with literature. It would appear that the effect an inhibitor has on the resultant apatitic crystal is dependent on the mechanism of inhibition and not necessarily on whether it is a type I or type II inhibitor. Results obtained for casein and L-glutamate shows that they may be regarded as type II inhibitors. Tetracycline, a broad spectrum antibiotic which may also be classified as type II inhibitor, caused a slight decrease in the mean size of the apatitic crystals Inhibition by this compound seems to be more as a result of steric hinderance rather than attachment to the active site of the HAP nuclei. Preparation of tin hydroxyapatite was attempted using hydrateci cin (II) oxide as the starting material. To the best of our knowledge, a new tin (II) phosphate was obtained which has strong similarit; 3 with calcium hydroxyapatite (HAP) . This new tin (II) phosphate gave a molybdenum blue colouration due to the reduction f molybdophosphoric acid during phosphate determination, indicating that tin existed in the +2 oxidation state. X-ray diffraction patterns of the products obtained in the attempted preparation of tin calcium hydroxyapatite by aqueous and solid state reactions were obtained. Precipitation from aqueous system containing 3 atom % tin in solution gave product which is essentially featureless and characteristic of amorpnous compounds, in agreement with literature. At tin concentration significantly greater than 20 atom %, the products of solid state reaction at both 500° and 700°C were amorphous. In part II of the thesis, the conformations adopted by some ring compounds in the solid state are describe, and parameterized. The effects of the molecular environment on the geometry and conformation of the rings, have been elucidated based on x-ray diffraction structural data. For cycloheptane ring derivatives, the boat
Description
A Thesis Submitted to the postgraduate School, Ahmadu Bello University, Zaria. In Partial Fulfilment of the Requirements for the Degree of Doctor of Philosophy in Chemistry. Department of Chemistry Faculty of Science Ahmadu Bello University Zaria, Nigeria.
Keywords
STUDIES,, PRECIPITATION,, PHOSPHATES,, CONFORMATIONS,, CYCLIC COMPOUNDS,, X-RAY DIFFRACTION DATA,
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