Reactions Between Solids: Reactions of Transition Metal Complexes with Onium and Alkali Metal Salts at High Pressures and/or Elevated Temperatures

摘要

Work included in the report varies from solid-solid, gas-solid reactions of coordination compounds to the automation of thermoanalytical techniques. Several phases of the research were involved with kinetics and thermochemical investigations of the deaquation of metal chelate hydrate systems. Perhaps the most significant phase of the research was the solid-solid trans preferred reactions of the bis(ethylenediamine)cobalt(III) complexes. The reactions are unique in that they always yield the trans-isomer. Another significant result of this research has been the automation of thermoanalytical techniques, namely, differential thermal analysis (DTA) and thermogravimetry (TG). The equipment, both DTA and TG, is completely automated in that the eight individual samples can be studied in a sequential manner, under various conditions of furnace atmosphere and heating rate. The samples are contained in a rotating sample tray and individually positioned into the instrument furnace. After pyrolysis to a preselected upper temperature limit, the sample is removed and a new sample introduced. Once the instrument has been activated, it requires no operator attention until the completion of the run. (Author)