The reduction of chromium (III) was studied in
normalLiCl‐normalKCl
eutectic at 500°C by means of cyclic voltammetry. It has been shown to proceed via a two‐step process to the metal. The intermediate Cr(II) species reacts with the solvent anions to form an insoluble compound,
CrCl2
. The pseudo first‐order rate constant for the chemical step is
0.028±0.008 sec−1
, while the heterogeneous rate constant for the charge transfer is
3.4±0.5×10−2 normalcm sec−1
. The diffusion coefficient of Cr+3 was determined to be
0.5±0.1×10−5cm2/sec
at 500°C. No adsorption of any species present in solution was found to occur on the vitreous carbon working electrode.
Thallous nitrate was investigated using TG, DTA, and DSC in conjunction with gas chromatography and X-ray diffraction analysis. TG showed a weight loss beginning at --, 380 ~ with a 50 percent loss by 520 ~ This weight loss was demonstrated to be caused by boiling rather than thermal decomposition. The DTA extrapolated onset temperature for the boiling was 467 ~ . Two solid-solid transition points and the melting point were determined by DTA to be 77, 145, and 207 ~ respectively. Heat of transition values determined by DSC were 0.15 kcal/mole at 77% 0.87 kcal/ mole at 145 ~ and 2.18 kcal/mole for the melting at 207 ~ In the course of an investigation of the surface tension of thallous nitrate conducted in this laboratory by Nissen [1 ] it became apparent that numerous inconsistencies exist in the literature with regard to the thermal analysis of T1NO3. Of particular concern in this study was the question of weight loss, its cause and temperature. Wendlandt [2] reported decomposition and loss of oxides of nitrogen in the range 265 to 370 ~ . Thomas [3] noted slow decomposition at 300 ~ with a rapid reaction at 450 ~ to form 02, N2, nitrogen oxides and T120 3. Duval [4] reported no weight change up to 410 ~ with decomposition above that temperature. Decomposition at 487 ~ was observed by Protsenko and Protsenko [5]. A boiling point of 430 ~ is listed for T1NO 3 by both Mellor [6] and Weast [7]. Rossini et al. [8] It has been well established that T1NO3 undergoes two crystal transformations when heated to about 60 to 80 ~ The orthorhombic crystals (Sin) transform into
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