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Much of the fundamental work on complexation of cycloolefins by platinum metals has been laid down by several workers and ranges from complexes of butadiene those of cyclododecatriene. The work here was chiefly a continuation of research on cycloolefin complexes which appear in papers by Kuljian and Frye (30,31,44). Most of this work on the complexes of cyclic seven, eight, and twelve carbon ligands was repeated here to insure a more complete laboratory background and for verification of previously reported literature data on these compounds. These compounds were used a s basis for comparison to original compounds developed in the research. More precisely, the major cycloolefins involved in the current research are 1,3- and 1,5-cyclooctadiene, although complexes with cyclooctatetriene ligands have been attempted. As has been shown by several workers (5,31,51,52), the 1,3-cyclooctadiene, when complexed with a platinum metal ion, rearranges to the 1,5-cyclooctadiene moiety. With the idea of this rearrangement in mind, this research was continued with complexes using as a ligand, a substituted alkyl or phenyl group attached to the cyclooctadiene ring. The initial step in such a synthesis was the preparation of a substituted cyclooctadiene.This was accomplished by means of the Grignard reaction using a bromocyclooctadiene and alkyl- or phenyl-Grignard reagent. With the knowledge that rearrangement to the 1,5- position occurs with normally complexed cyclooctadiene, it was of interest to determine whether or not a substituted group on the ring would have (1) any inductive effect or (2) any steric effect on the speed of reaction or in double bond rearrangement.

D-Galactosamine has been known as one of the rarer amino sugars, occurring widely distributed in small concentrations in living organisms. The biological importance of D-galactosamine and its derivatives was thought to justify a study of the chemical properties of this group of compounds. As a result of this study the reactions of D-galactosamine have been found to differ more than previously thought from those of D-glucosamine, the more common amino sugar For this investigation D-galactosamine hydrochloride was isolated from chondroitin sulfate, a polysaccharide obtained from the cartilaginous tissues of animals. This was changed by appropriate reactions to the 1,3,4,6-tetra-0-benzoyl-N-carbobenzoxy-α-β-D-galactosamine (III). This sirup, when reacted with hydrogen bromide in glacial acetic acid, produced 3,4,6-tri-o-benzoyl-l-bromo-α-D-galactosamine bydrobromide (IV), which was used as the starting material for the subsequent reactions.

A personal computer based Fourier transform ion cyclotron resonance mass spectrometer has been designed and constructed. An IBM PC AT compatible computer is used to host the interface of the instrument. The advantages of using a personal computer to host the FT-ICR instrument include: (1) very low cost of the computer; (2) extensive graphic and mathematic capabilities; (3) easy performance alteration or expansion; (4) an abundance of application software; and (5) support for a wide range of output devices. A dedicated digital hardware interface, which provides high speed data transfer and accurate timing control, was assembled on the computer's extension board. The extension board is used to replace the frequency synthesizers and waveform recorders normally used for arbitrary waveform generation and data acquisition at a speed of several mega Hertz. The unique features of the digital hardware design include: (1) common memory for both excitation and data acquisition; (2) control logic for critical timing steps; (3) system memory mapping for fast data transfer. This design has not only led to great reduction in construction cost but has increased the flexibility of the instrument to perform complex experiments as well. A general phase modulation algorithm for the stored waveform inverse Fourier transform (SWIFT) excitation has been developed. The method can be used to generate arbitrary excitation waveforms with optimal dynamic range reduction. The maximum entropy spectral analysis (MEM) has been investigated. When the broad-band MEM method was demonstrated in the host computer, resolution and signal-to-noise ratio improvement was observed. New preamplifier, electron beam circuits, and the sample inlet system of the instrument were designed and constructed with computer control. This provides the instrument with reliability, stability, and functionality. A theoretical model for two dimensional Fourier transform ion cyclotron resonance mass spectrometry has been proposed. The model interprets the physical significance of the modulation of the ion signals in the additional dimension. According to the model, the additional time dimension (which is introduced as the duration between the pair of 2D excitation pulses) determines the speed of the primary ions just before the reaction period. The speed modulation may result in primary ion population modulation. In general, the speed modulation will transfer into ion signal modulation through a variety of channels, such as reactions and ion loss. The model also predicts that the ion modulation in the additional dimension is not sinusoidal (therefore, harmonics exist) and the ion signal modulation has definite phase relationships. The implementation of the 2D technique is developed and demonstrated.

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