Sur la stabilité thermique des étalons analytiques. XIII

Résumé L'examen de 12 substances proposées comme étalons révèle que le chlorure et l'iodure de zinc doivent être manipulés à l'abri de l'humidité atmosphérique après séchage au-dessous de 60°; l'acétate et le sulfate de zinc issus d'un flacon neuf peuvent être pesés directement; le fluorure de sodium est parfaitement stable jusqu'à 850°; le carbonate de sodium et de potassium peut être utilisé tel quel mais il est préférable de le déshydrater entre 250 et 700°; l'hydrogénosulfate de potassium est hygroscopique et doit être séché avant pesée, sans dépasser 200°; l'hexaméthylènetétramine, le morpholine N-dithiocarbonate de morpholinium, le tétraphénylborure de sodium sont bien secs; il ne faut pas dépasser 150° pour obtenir la chloramine T anhydre. Les auteurs précisent la différence de comportement entre l'hydrogénosulfate et le pyrosulfate de potassium.

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Summary Study of 12 materials suggested as standards reveals that zinc chloride and iodide should be handled away from the atmospheric moisture after drying below 60°. Zinc acetate and sulfate freshly taken from a new bottle may be weighed immediately. Sodium fluoride is perfectly stable up to 850°. Sodium-potassium carbonate may be used just as they are but it is preferable to dry them between 250 and 700° before weighing. Potassium hydrogen sulfate is hygroscopic and should be dried prior to weighing but not above 200°. Hexamethylenetetramine, morpholinium morpholine-N-dithiocarbonate, sodium tetraphenyl boron are quite dry. Chloramine T can be obtained anhydrous without going higher than 150°. The difference in behavior between potassium hydrogen sulfate and pyrosulfate is stated precisely.

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Zusammenfassung Die Untersuchung 12 als Standard vorgeschlagener Substanzen ergab, daß Zinkchlorid und -jodid nach Trocknung unterhalb 60° zur Entfernung der Luftfeuchtigkeit verwendet werden können. Zinkacetat und -sulfat können nach Entnahme aus einer frischen Packung direkt eingewogen werden. Natriumfluorid ist bis 850° stabil. Natrium-Kaliumcarbonat kann wohl unmittelbar verwendet werden, doch ist es besser, es zwischen 250 und 700° zu entwässern. Kaliumhydrogensulfat ist hygroskopisch und muß vor dem Einwägen getrocknet werden, ohne die Temperatur über 200° zu steigern. Hexamethylentetramin, morpholin-N-dithiocarbonsaures Morpholinium und Natriumtetraphenylborat sind hinreichend trocken. Um wasserfreies Chloramin T zu erhalten, darf man nicht über 150° gehen. Der Unterschied im Verhalten von Kaliumhydrogensulfat und -pyrosulfat wird genau angegeben.

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Pour le 12ème mémoire de cette série, voir Mikrochim. Acta [Wien]1963, 348.

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En l'honneur du ProfesseurA. A. Benedetti-Pichler.     

Untersuchung von Kaffee und Kaffee-Ersatzstoffen

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Sur la thermogravimétrie des précipités analytiques : Dosage du sodium

This thermogravimetric study has enabled the authors to specify a large number of points of detail in connection with the correct determination of sodium. Their attention has been particularly directed to the triple acetates, which they recommend should be weighed only in the form of pyro-uranates. The method of ball, less classical than the others, would merit greater attention on the part of analysts.     

Analyse der Luft

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A study of frost growth and densification on flat surfaces

The present study advances a theoretical and experimental investigation of the frost growth and densification on flat surfaces. This study focuses on the most important factors affecting the frost formation process, i.e. the surrounding air temperature, humidity and velocity, and the surface temperature. The processes of frost growth and densification were investigated experimentally in order to provide a physical basis for the development of a theoretical model to predict the variation of the frost layer thickness and mass with time. The mathematical model was based on mass and energy balances within the frost layer, assuming the frost as a porous medium and accounting for the supersaturation of the moist air on the frost surface. The governing equations for mass and heat diffusion were integrated analytically, giving rise to a semi-algebraic formulation which requires numerical integration of only one time dependent ordinary differential equation. When compared with experimental data, the model predictions of the frost thickness as a function of time agreed to within ±10% error bands. The experimentally-validated model was then used to predict the frost layer growth and densification with respect to the operation conditions such as plate surface temperature, air stream temperature, humidity and velocity.     

Crystal structure and theoretical calculations of Julocrotine,a natural product with antileishmanial activity

Julocrotine, N‐(2,6‐dioxo‐1‐phenethyl‐piperidin‐3‐yl)‐2‐methyl‐butyramide, is a potent antiproliferative agent against the promastigote and amastigote forms of Leishmania amazonensis (L.). In this work, the crystal structure of Julocrotine was solved by X‐ray diffraction, and its geometrical parameters were compared with theoretical calculations at the B3LYP and HF level of theory. IR and NMR spectra also have been obtained and compared with theoretical calculations. IR absorptions calculated with the B3LYP level of theory employed together with the 6‐311G+(d,p) basis set, are close to those observed experimentally. Theoretical NMR calculations show little deviation from experimental results. The results show that the theory is in accordance with the experimental data. © 2007 Wiley Periodicals, Inc. Int J Quantum Chem, 2008     

Neues Verfahren zur volumetrischen Bestimmung des Eisens

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Indium

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