Analysis of degradation products by thermal volatilization analysis at subambient temperatures

In the subambient thermal volatilization analysis (TVA) technique, degradation products initially at ?196°C are allowed to warm up to ambient temperature in a controlled manner under vacuum conditions, and volatilization from the sample tube to a trap at ?196°C is monitored by means of a Pirani gauge. The technique is discussed in relation to earlier TVA work in which volatilization from a heated polymer sample was followed. Design and operation of a subambient TVA system are described, and examples of the application of the technique to the study of the degradation products of seven polymers are considered.     

Behavior of 2-nitroso-4-nitropropiophenone under conditions of cyclization to haloanthranils

The cyclization of 2-nitroso-4-nitropropiophenone under the influence of hydrogen chloride proceeds in a more complex manner than in the cases previously described for other 4-substituted-2-nitrosopropiophenones: three, rather than two, haloanthranils are formed, and their formation is accompanied simultaneously by a number of redox transformations. This fact is explained by a decrease in the ability of the carbonyl group in the investigated ketone to undergo protonation.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1334–1337, October, 1976.     

Structure of ammonium salts of 2-oxy-1,4-butylene-and 2-oxy-1,5-amylenephosphoric acids

The structures of dioxaphosphepane (I) and dioxaphosphecane (II) salts prepared by hydrolysis of the corresponding bicyclophosphates have been compared. In both cases, hydrolysis occurs with breaking of the P–O bond of the fragment at the secondary carbon atom of bicyclophosphate. In phosphocycles I and II, the endocyclic bond angles O–P–O are 104.2 and 104.9°, and the exocyclic ones are 117.7 and 118.6°, respectively. Conformations of the anions in I and II differ substantially: for I it is a twist conformation^C1T_C4, and for II a distorted armchair. The data obtained are compared with those found earlier for similar molecules.Moscow State Pedagogical University. Translated fromZhurnal Strukturnoi Khimii, Vol. 34, No. 4, pp. 154–160, July–August, 1993.Translated by T. Yudanova     

Substoichiometric extraction of mercury with malonic anilide

Determination of mercury (II) by substoichiometric extraction with malonic anilide into a mixture of ether and MIBK is reported. The method has been applied in the estimation of the metal in industrial effluents.