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991.
A new program for DSC purity analysis 总被引:1,自引:0,他引:1
DSC purity determinations have become very popular today [3]. The latest edition of the Mettler software package for thermal analysis, TA72.S GraphWare, now comprises a powerful purity evaluation program. It is based on the simultaneous calculation of the mole ratio of the sum of the eutectic impurities, the melting point of the pure component, the melting point of the substance present and the linearization term. The portion of the melting curve investigated is selected appropriately.Experience has shown, that the applied heating rate is a very important parameter which influences the duration of the measurement and also the possible exposure to elevated temperature where decomposition can become a problem and last but not least the accuracy of the calculated impurity value.
Zusammenfassung Die DSC-Reinheitsbestimmung ist heute eine weit verbreitete Methode, die mit einer einzigen Messung und unter Verwendung geeigneter Auswerteprogramme eine Bestimmung der absoluten eutektischen Reinheit einer Probe zulÄsst. Gleichzeitig können weitere thermodynamische Daten bestimmt werden, wie Schmelzpunkt der Probensubstanz und der reinen Hauptkomponente und die Schmelzenthalpie der Probe.Durch experimentelle Befunde konnte gezeigt werden, dass die Wahl der Aufheizrate kritisch ist in bezug auf die Genauigkeit und die Signifikanz der ermittelten Daten.相似文献
992.
V. A. Makarov A. L. Sedov O. S. Anisimova V. G. Granik 《Chemistry of Heterocyclic Compounds》1996,32(6):699-707
Highly polarized enediamines of the a, -diamino--cyano--nitroethylene type have been obtained by the hydrolysis of 4-chloro-5-nitropyrimidines. Several chemical conversions of the enamines obtained have been studied, particularly leading to derivatives of 2-(cyanonitromethylene)imidazoline and -hexahydropyrimidine, and also to derivatives of N, N-bisvinylpiperazine and 7 methylene-1, 4-diazabicyclo(2.2. 1 ]heptane.Center for Drug Chemistry, All-Russian Chemical and Pharmaceutical Research Institute, Moscow 119815. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 6, pp. 811–820, June, 1996. Original article submitted February 6, 1996.For Part 1, see [1]. 相似文献
993.
Malzert-Fréon A Abillon O Proust JE Gref R Benoît JP Boury F 《Colloids and surfaces. B, Biointerfaces》2005,42(2):97-106
In this paper, we compared the efficiency of polymer films, made of a poly(ethylene glycol) (PEG2,000)/poly(d,l-lactide) (PLA50) mixture, or a PEG2,000-PLA50 copolymer, to prevent adsorption of a model protein, the hen egg-white lysozyme (HEWL), at the air-water interface. This was achieved by analyzing the surface pressure/surface area curves, and the X-ray reflectivity data of the polymer films spread on a Langmuir trough, obtained in absence or in presence of the protein. For both the mixture and the copolymer, the amount of protein adsorbed at the air-water interface decreases when the density of the polymer surface coverage increases. It was shown that even in a condensed state, the polymer film made by the mixture can not totally prevent HEWL molecules to adsorb and penetrate the polymer mixed film, but however, protein molecules would not be directly exposed to the more hydrophobic phase, i.e. the air phase. It was also shown that the configuration adopted by the copolymer at the interface in its condensed state would prevent adsorption of HEWL molecules for several hours; this would be due in particular to the presence of PEG segments in the interfacial film. 相似文献
994.
Ibragimov A. G. Khafizova L. O. Zagrebel"naya I. V. Parfenova L. V. Sultanov R. M. Khalilov L. M. Dzhemilev U. M. 《Russian Chemical Bulletin》2001,50(2):292-296
A new method for the synthesis of dialkyl(ethyl)alanes by the reaction of EtAlCl2 with -olefins in the presence of Mg and a catalytic amount of Cp2TiCl2 (Ti(OPri)4, Ti(OBun)4) in THF was developed. 相似文献
995.
996.
Krasnov P. O. Kuzubov A. A. Romanova T. A. Avramov P. V. 《Russian Journal of Coordination Chemistry》2004,30(9):634-638
The geometry and the electronic structure of iron porphyrinate complexes with various heterocyclic molecules in the fifth coordination position and a CO molecule in the sixth position were studied by density functional theory calculations. In the series of complexes with furan, imidazole, and pyrimidine, the bond between the Fe atom and CO is weakened due to the decrease in the overlap of the corresponding AOs. 相似文献
997.
When boiled in aromatic hydrocarbons, solutions of α-nitro-α-azinylcyanoacetic esters of the pyrimidine, pyrazine, ands-triazine series gave the corresponding α-hydroxy derivatives of α-azinylcyanoacetic esters in high yields.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 7, pp. 1407–1409, July, 1997. 相似文献
998.
V. R. Khabibulin A. V. Kulik I. V. Oshanina L. G. Bruk O. N. Temkin V. M. Nosova Yu. A. Ustynyuk V. K. Bel’skii A. I. Stash K. A. Lysenko M. Yu. Antipin 《Kinetics and Catalysis》2007,48(2):228-244
The formation mechanism of the active catalyst in the oxidative carbonylation of terminal alkynes at the ≡C-H bond has been investigated for the catalytic system Pd(OAc)2-PPh3-p-benzoquinone (Q)-MeOH. It has been demonstrated by NMR spectroscopy, X-ray crystallography, and kinetic measurements that the catalytically active palladium is in the oxidation state 0 and is bound into complexes stabilized by p-benzoquinone (PdL2Q, where L = PPh3). A mechanism is suggested for the catalytic process, which includes the formation of the complex PdL2Q, the oxidative addition of the alkyne to this complex at the ≡C-H bond, the insertion of CO into the Pd-C bond, and steps in which hydride hydrogen is intramolecularly transferred to the p-quinone. 相似文献
999.
E. M. Suleimenov F. M. Smagulova O. V. Morozova V. A. Raldugin I. Yu. Bagryanskaya Yu. V. Gatilov V. I. Yamovoi S. M. Adekenov 《Chemistry of Natural Compounds》2005,41(6):689-691
The five known lactones matricarin, austricin, canin, and achillin guaianolides and argolide germacranolide and the two flavonoids
eupatilin and its 7-O-methyl ester were isolated for the first time from the aerial part of Artemisia albida Willd. The structure of eupatilin was confirmed by an x-ray structure analysis.
__________
Translated from Khimiya Prirodnykh Soedinenii, No. 6, pp. 568–570, November–December, 2005. 相似文献
1000.
Yu. V. Fedorov O. A. Fedorova N. E. Shepel’ S. P. Gromov M. V. Alfimov L. G. Kuz’mina J. A. K. Howard J. Saltiel 《Russian Chemical Bulletin》2005,54(9):2119-2128
Benzobisthiazole-based bis(crown ether) was synthesized and its complexation with alkali and alkaline earth cations was studied.
Photochemical transformations of the free ligand and its complexes with alkaline earth cations involve E,Z-photoisomerization and [2+2] photocycloaddition.
Dedicated to Academician N. S. Zefirov on the occasion of his 70th birthday.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 2056–2065, September, 2005. 相似文献