Abstract
This apparatus was developed to study the solid-state reactions and physico-chemical changes involving absorption or evolution of gases, and structurally consists of a modified gas effluent analysis equipment and a high-precision gas mixer. The new apparatus is more useful in the fields of inorganic chemistry, organic chemistry, metallurgy, etc. than a conventional EGA equipment.The sample is heated or cooled at the constant rate in a mixed flow of two or more different gases such as He-O2, He-CO2, Ar-H2, etc. The changes in the composition of the gas passing through the reactor due to the decomposition or the gas-solid reaction are detected with high sensitivity by a thermal conductivity detector. The sample weight required for the usual measurement is 5∼50 mg. It is applicable to the range from room temperature to 1600°C and the gas flow of any mixing ratio (200: 1∼1: 200). Although the limits of determination are affected by the operating conditions, an evolution or absoption of 0.01-0.0001 ml of oxygen by the sample in the He-O2 mixture can be detected.This paper describes the following reactions as the applications of this apparatus: reduction of vanadium pentaoxide by hydrogen, thermal decomposition of calcium oxalate monohydrate, oxidation and reduction of iron oxide, formation and decarbonation of calcite, and hydrogenation and formation of uranium hydride.
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