A brief survey of typical problems in the analysis of aluminum powder in aluminized solid propellants and in analysis of condensed combustion products of these propellants was carried out. Recommendations for applying the versions developed by the authors of the known methods are given. The permanganatometric variant of the titrimetric method was found suitable for most tasks concerning the measuring of the metallic/unburned aluminum. The determination of aluminum nitride in combustion products using the combination of chemical and X‐ray diffraction methods was described and illustrated by results obtained from condensed combustion products of propellant formulations containing highly active ultrafine aluminum powder. Even for this formulation the content of aluminum nitride in the final condensed combustion products was found to be negligibly small independently of the nature of the gas (argon or nitrogen) used for bomb pressurization.
The thermal stability and non-isothermal kinetics of the decomposition of alkali metal bifluorides were studied using a derivatograph. The removal of hydrogen fluoride from LiF. HF and NaF 9 HF takes place before melting and their decomposition occurs in a single stage; however, potassium, rubidium and cesium bifluorides at first undergo polymorphous transformation and melting on heating, and their decomposition proceeds stepwise. The thermal stability of alkali metal bifluorides has been found to increase with increasing ionic radius of the cation, reflecting its correlation with the hydrogen bond strength in these compounds.Of the presently known hydrofluorides the alkali metal bifluorides MF 9 HF (MHF~) are the most stable thermally. The thermal stability of these compounds is important from the point of view of their practical application. However, the literature data on this point are sometimes contradictory. The variety of methods used by the authors of the works mentioned above makes the comparison of the results difficult as they often differ greatly. The insufficient purity of the studied substances, especially in the early works, also gave rise to inaccuracies. The kinetics of the decomposition of bifluorides has not been studied at all. In the present work the thermal stability and non-isothermal kinetics of the decomposition of alkali metal bifluorides were studied by thermogravimetry.Lithium bifluoride was obtained by crystallization from a saturated solution of lithium fluoride (analytical grade) in hydrofuoric acid of special purity [3]. The crystals obtained were washed several times with anhydrous hydrogen fluoride to remove water, and then excess HF was exhausted in a vacuum desiccator 1" 3., Thermal AnaL 2, 1970
The review deals with the available information on metal hydrogen fluorides. The methods of synthesis of hydrogen fluorides and their physical and chemical properties are examined and studies on the hydrogen bonds in hydrogen fluorides and their structures are discussed. The principal trends in the research in this field have been outlined on the basis of these data. The bibliography includes 190 references. CONTENTS
The reactions of alkali and ammonium bifluorides with aluminium and silicon were studied by DTA. Reaction temperatures were determined and reaction products identified. The reaction mechanism of the fluorinating reaction was established. Hydrofluorides appear very promising fluorinating agents.The fluorinating actions of elemental fluorine, halogen fluorides and hydrogen fluoride are well known and these compounds are widely applied for synthetizing inorganic fluorides [1 ]. Lately, however, interest in solid fluorinating agents has continually grown, since they possess many advantages. By way of example, silver difluoride [2], cobalt and manganese trifluorides [3][4][5], xenon fluoride [6] and alkali fluorohalogenates [7] can be mentioned.Much attention has been paid to ammonium bifluoride as a potential fluorinating agent, because the melting and evaporation temperatures of this compound are relatively low. The reactivity of NH4F " HF is close to that of anhydrous hydrofluoric acid and the compound can be successfully applied as a fluorinating agent in many reactions [1,[8][9][10]. It is obvious that other bifluorides are also suited for such purposes.In the present paper we wish to report studies on the reaction of alkali and ammonium bifluoiides with aluminium and silicon. The method used was differential thermal analysis and the reaction products were identified by X-ray phase analysis and thermal analysis. In reactions of metals with bifluorides, the thermal properties of the latter are very important. The thermal stabilities and decomposition kinetics of hydrofluorides were earlier studied by thermogravimetry [I 1, 12]. It was found that lithium and sodium bifluorides are decomposed before melting, whereas potassium, rubidium and caesium bifluorides first undergo polymorphous transformation on heating, and subsequently melt without perceptible decomposition. On further heating, hydrogen fluoride is evolved from the melt [12]. Ammonium bifluoride too melts without perceptible decomposition, and on further heating decomposes, hydrogen fluoride being split off. ExperimentalAlkali and ammonium bifluorides were synthetized according to data on the HF-MF-H20 systems, and identified by methods of chemical, X-ray phase , L Thermal Anal. 5, 1973
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