Selected topics in fast atom bombardment (FAB) mass spectrometry a)specially designed probe tips and ion generation, b)structures of vitamin B6 schiff base complexes

This thesis can be broken down into two sections. Section one is a study . of the ionization mechanisms and the ion source optimization for Fast Atom Bombardment (FAB) ionization. For this study, several specially designed probe tips were created and tested under various experimental conditions. The aIm of this section is to understand the operating characteristics of a FAB IOn source better. The second section involves the study of several Vitamin B6 Schiff Base complexes using both positive and negative ion FAB MS. This section is an exploration of the usefulness of FAB MS as a structure probe for the metalcoordination complexes of Vitamin B6.

Solid state NMR chemical shifts as an alternative to diffraction data in the determination of SIC polytypic structures

Silicon carbide, which has many polytypic modifications of a very simple and very symmetric structure, is an excellent model system for exploring, the relationship between chemical shift, long-range dipolar shielding, and crystal structure in network solids. A simple McConnell equation treatment of bond anisotropy effects in a poly type predicts chemical shifts for silicon and carbon sites which agree well with the experiment, provided that contributions from bonds up to 100 A are included in the calculation. The calculated chemical shifts depend on three factors: the layer stacking sequence, electrical centre of gravity, and the spacings between silicon and carbon layers. The assignment of peaks to lattice sites is proved possible for three polytypes (6H, 15R, and 3C). The fact that the calculated chemical shifts are very sensitive to layer spacings provides us a potential way to detennine and refine a crystal structure. In this work, the layer spacings of 6H SiC have been calculated and are within X-ray standard deviations. Under this premise, the layer spacings of 15R have been detennined. 29Si and 13C single crystal nmr studies of 6H SiC polytype indicate that all silicons and carbons are magnetically anisotropic. The relationship between a magnetic shielding tensor component and layer spacings has been derived. The comparisons between experimental and semi-empirical chemical shielding tensor components indicate that the paramagnetic shielding of silicon should be included in the single crystal chemical shift calculation.

HG 186.15-186.25 Thin Section

Coarse grained sample with multiple fine grained domains. Clasts range from small to medium and sub-angular to sub-rounded. Mainly contains grain crushing (with grains crushed into one another) and short distance lineations. A few rotation structures are seen and fine grained sand domains can also be seen.

HG 186.9-187.0 D.E.

Coarse grained sediment with a few fine grained matrices. Brown sediment with small to medium sized clasts. Clasts range from sub-angular to sub-rounded. Organic material present. It contains rotation structures throughout as well as edge-to-edge grain crushing. Fine grained clay domains are present and lineations can also be seen. Minor amounts of grain stacking can also be seen.

HG 230.75-230.85 Thin Section

Coarse grained sediment with fine grained domains, clay material, rotation structures and lineations. Clasts range from sub-angular to sub-rounded. Mainly brown sediment with darker patches of brown throughout. Major amounts of grain crushing can be seen in the coarse grained material.

HG 244.40-244.55-B Thin Section

Coarse grained sample with sub-angular to sub-rounded clasts ranging from small-large in size. Rotation structures, grain crushing and lineations were seen throughout the sample.

HG 246.30-246.45 Thin Section

Generally coarse grained, with a few different fine grained domains. Clasts range from small to large, ranging from sub-angular to sub-rounded in shape. Domain boundaries are clear, and the sample also contains rotation structures and lineations.

HG 249.40-249.55 Thin Section

Coarse grained sample with clasts ranging from small to medium. Clast shape ranges from angular to sub-angular. Lineations and rotation structures seen. Clay material and fine grained domains (darker colour) also seen.

251.8-251.9 D.E #5

Sample contains well dispersed clasts ranging from small to medium in size. They are sub-angular to sub-rounded in shape. Organic rich domains can be seen throughout the sample with clear boundaries. It also contains water escape structures, seen mainly through clay. Lineations are also present.

HG 276.80-276.95 Thin Section

Coarse grained sample, with grains ranging from small to large in size. Shapes range from angular to rounded. This sample is abundant in lineations, and rotation structures can also be seen around larger aggregates. Many large grains are fractured and minor grain stacking can also be seen.

293.9-294.0 DE # 7

Brown sediment with well dispersed clasts. Clasts range from small to medium in size and angular to sub-rounded in shape. Some appear to have been weathered. Water escape structures can be seen, mainly in finer, clay rich sediment. Lineations can also be seen throughout the sample. Minor grain stacking and crushing are also present.

HG 305.15-305.30

Dark grey sediment with medium to small sized grains. The grains are sub-angular in shape. Rotation structures and grain crushing are the most common microstructures seen. Dark organic material and lineations can also be seen.

HG 312.30-312.40

Grey sediment with clasts ranging from small to medium in size. Edge-to-edge grain crushing is abundant, with some lineations. Minor amounts of rotation structures can also be seen.

HG 316.65-316.80

Fine grained, dark brown sediment. Minor amounts of lineations can be seen. Faint water escape structures are also abundant.

HG 370.55-370.70 b

Light brown sediment with clasts ranging from small to large. The clast shape ranges from sub-rounded to rounded. Rotation structures and grain crushing is abundant. Some lineations can also be seen.