Untersuchungen an oxidischen Katalysatoren. XXIX. Spektroskopische und katalytische Untersuchungen an Ni2+-, Co2+-, Cr3+- und Cu2+-ausgetauschten Mordeniten

Studies on Oxide Catalysts. XXIX. Spectroscopic and Catalytic Investigations on Ni²⁺-, Co²⁺-, Cr³⁺-, and Cu²⁺-exchanged Mordenites NiNaM, CoNaM, CrNaM und CuNaM (M = Mordenite) have been characterized by UV-VIS, EPR and i.r. spectroscopy and the results were compared with the catalytic activity and the activity-time-dependence in the cracking of n-octane and with the shape selectivity in the cracking of a n-octane and isooctane mixture. Water molecules acting as ligands of the exchanged cations are able to dissociate yielding Brönsted acidity. Brönsted sites may be regarded as catalytic active centers in the cracking reaction. Unreduced transition metal cations facilitate the “coking” of the mordenite. The unreduced chromium and cobalt cations for which a position within the main channel is expected, affect the diffusion of the branched paraffin molecule thus increasing shape selectivity.     

The composition of the evolved gases from the thermal decomposition of certain metal sulfates

By the use of TG—MS, the thermal dissociation of anhydrous CuSO₄ and Al₂(S0₄)₃ was found to proceed according to the reactions:

followed by the reactions:

No SO₃ was indicated in the dissociation of alunite. The sulfate ion appears to dissociate by at least two different mechanisms although the parameter which controls the mechanisms has not been elucidated.     

Reactions of Silver (I) salts in potassium halide matrices: A differential scanning calorimetry study

Reactions of AgCl, AgSO₄, and Ag₂CO₃ in and with pressed KCl, KBr, and KI disks as well as those of unpressed mixtures were followed by TG and DSC. Except for Ag₂CO₃ and Ag₂SO₄ in KI, the curves obtained were readily interpreted in terms of eutectic melting, decomposition, and complex formation.     

Reactions of barium chloride dihydrate in potassium halide matrices: A differential scanning calorimetry study

The deaquation of BaCl₂·2H₂O in pressed KCl, KBr, and KI disks was followed by TG and DSC at pressures ranging from one to 34 atmospheres. Resolution of the DSC peaks of the first deaquation reaction and subsequent water vaporation was not improved by use of the matrix; for the second deaquation reaction, resolution was greater in the matrix. Evidence of a ternary eutectic involving BaCl₂, KI, and H₂O, which melted at 219°C, was obtained.     

The use of differential scanning calorimetry to identify methaqualone samples: forensic applications.

The d.s.c. curves of commercial samples of methaqualone—Qu$\text{aa}$lude (U.S.A.), Qu$\text{aa}$lude (Mexico), Sopar, Mandrax and Parest — are presented. Similar d.s.c. curves were found for Qu$\text{aa}$lude (U.S.A.), Qu$\text{aa}$lude (Mexico), and Mandrax, while Sopar and Parest exhibited different types of curves. New and old formulations of the Qu$\text{aa}$lude (U.S.A.) brand could be differentiated by differences in the tablet filler and binder. Unfortunately, d.s.c. could not be used to determine the country of origin of the drug, although it was useful to characterize it. The technique can be used to identify samples of 0.15 mg or less.     

The thermal dissociation of some metal cupferrate chelates

The thermal dissociation of the cupferron complexes with Cu(II), Ni, Co(II), Zn, Cd, Mn(II), Hg(II), Mg, Ca, Ba, Sr, Al, Fe(III). Ce(III), La, and Nd was studied by differential thermal analysis (DTA) and by pyrolysis into a mass spectrometer. The DTA curves consisted mainly of endothermic peaks although some contained exothermic peaks as well. The mass spectrometer showed that cupferron decomposes slightly above room temperature, giving off N₂, NO, N₂O, NH₃ and H₂O. A mechanism for the thermal dissociation of the coppcr(II) cupferrate is proposed.     

The thermal decomposition of the 2-methyl-8-quinolinol (8-hydroxyquinaldine) chelates of scandium,thorium, uranium (VI) and the rare earth elements

The thermal decomposition of the 2-methyl-8-quinolinol (8-hydroxyquinaldine) chelates of scandium, thorium, uranium(VI), yttrium and the rare earth elements was studied on the thermobalance. It was found that the scandium and uraniurn(VI) chelates can lose the extra molecule of solvation by thermal decomposition. The thorium chelate was found to be the most stable of all the chelates studied. The temperature limits for the chelates and the minimum oxide level temperatures are given.     

A convenient AC electrical conductivity (EC) apparatus

A convenient AC electrical conductivity apparatus is described. The sample, which is in the form of a pressed disk, is placed between two platinum plates located in a small cylindrical furnace. A 1–10V, 100 Hz potential is applied to the sample and the resulting current, in μA, is recorded on an X-Y recorder as a function of temperature. An EC curve of the dehydration of BaCl₂ - 2H₂O to BaCl₂ - H₂O is presented to illustrate the operation of the apparatus.