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.     

电子探针定量分析的标准样品——几种多元氧化物单晶

在很高的温度和适宜的生长条件下,分别采用熔盐籽晶法和高温引上法生长了高质量的YAP、NAB、KTP、LN、BBO、SBN等多元氧化物单晶,它们具有优良的物理化学性能,严格的化学比,固定的组成与结构以及较好的化学均匀性和电子束轰击下的稳定性。广泛地用于激光和非线性光学领域。我们选用这些晶体为原材料研制电子探针定量分析的标准样品。经过测量和标定,这些单晶标样符合中华人民共和国国家标准GB 4930-85(电子探针显微分析标准样品通用技术条件)的规定。含有稀土元素的标样如NAB和YAP能发出绿色荧光,是电子显微术中理想的阴极发光材料。     

Synthesis of 1,7-bis(4′-aminophenylamido)-m-carborane and 1,7-bis(4′-aminophenylcarboxy)-m-carborane

Conclusion 1,7-Bis(4-aminophenylamido)- and l,7-bis(4-aminophenylcarboxy)-m-carboranes were prepared and characterized.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 12, pp. 2786–2787, December, 1986.     

Lactam and acid amide acetals. 71. New synthesis of 3-nitro-6-hydroxyindole derivatives

Previously unknown 3-nitro-6-hydroxyindole derivatives were synthesized by condensation of p-benzoquinone with secondary -nitro enamines.See [1] for Communication 70.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 1, pp. 40–45, January, 1992.     

Photoreduction de la benzophenone par des phtalimidines et des dihydro isoquinolones: Etude chimique par RMN PNIC

Benzophenone is photoreduced by pthalimidines and dihydro isoquinolones. The hydrogen atom α to the nitrogen atom is abstracted and radical coupling leads to adducts. CIDNP studies of these adducts show inversion of polarisation for the adduct on the N-alkyl chain when the nitrogen is bound to a benzylic methylene. This inversion is explained by considering that the radical on the N-alkyl chain derives from the radical on the ring.     

Catalytic hydroamination of furfuryl and tetrahydrofurfuryl alcohols with nitriles

Reaction of furfuryl and tetrahydrofurfuryl alcohols with nitriles over copper oxide catalysts under a hydrogen pressure of 15 atm at a temperature of 230C gives N-alkylfurfuryl- (yield 46–50%) and N-alkyl-tetrahydrofurfurylamines (49–53%), and N-alkylpiperidines (28–41%). A reaction mechanism is proposed.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 1, pp. 23–26, January, 1988.     

Thermochemical reactions in polycomplexes

Polycomplex formation between poly(methacrylic acid) and polyacrylamide in aqueous solutions has been studied by means of viscometry, potentionetry and elemental analysis. Stoichiometry of the polycomplex was found to be 1:1 with respect to unit-moles. I.R.-spectroscopic data give evidence of the co-existence of ladder-like regions and loops in the polycomplexes formed by poly(methacrylic acid) with polyacrylamide and poly(ethylene glycol). The reactivities of the same functional groups in ladder-like regions and loops are different. This difference has been shown taking as an example thermochemical reactions in the above polycomplexes. Dehydrocyclization in the poly(methacrylic acid) chain was found to occur in the loops of both polycomplexes. This intramolecular reaction in the polycomplex of poly(methacrylic acid) with polyacrylamide is followed by intermolecular formation of imide bonds in ladder-like regions.