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91.
V. G. Berezkin E. G. Sumina S. N. Shtykov V. Z. Atayan D. A. Zagniboroda G. A. Nekhoroshev 《Chromatographia》2006,64(1-2):105-108
A new variant of thin-layer chromatography (TLC), based on a gradual change of mobile phase acidity during elution, is proposed.
The pH change occurs in the mobile phase moving along the TLC plate as a result of its contact with an acidic or a basic gas
phase that replaces the initial mobile phase vapor in the TLC chamber. The potential of this approach has been demonstrated
by using carbon dioxide and ammonia gases to improve the resolution of benzoic acids and aromatic amines on polyamide TLC
plates. 相似文献
92.
Paul-Henri Ducrot Albert Kollmann Adil E. Bala Amel Majira Lucien Kerhoas Robert Delorme Jacques Einhorn 《Tetrahedron letters》1998,39(52):7282-9658
Two new antifungal resveratrol dimers, cyphostemmins A-B (1–2), have isolated from the roots of Cyphostemma crotalarioides planch (Vitaceae) together with resveratrol 3 and previously known reseveratrol dimers (4–7). Structures of these new compounds have been established on the basis of their MS and 1H and 13C NMR spectroscopic data. 相似文献
93.
A. Szafranek J. Szafranek 《Journal of inclusion phenomena and macrocyclic chemistry》1993,15(4):351-358
This paper reports TG analyses of inclusion complexes of-cyclodextrin with benzene, acetylsalicylic acid and methyl salicylate. The data were used for calculation of the compositions of the three body complexes and the apparent kinetic parameters of the thermal decompositions. Water exclusion proceeds as a reaction with ordern=1 and an activation energy about 20 kJ/mol. The expulsion of aromatic guest molecules follows ann=1 order process with the activation energy above 155 kJ/mol, except that for the methyl salicylate complex, which was found to be ca. 64 kJ/mol. 相似文献
94.
H. G. Struppe F. Franke J. Hofmann B. Ondruschka 《Journal of chromatography. A》1996,750(1-2):239-244
In contrast to usability of Curie-point pyrolysis at 700°C directly attached to gas chromatography-mass spectrometry (GC-MS) for determination of organic wood preservatives in waste wood samples the investigation method reported here consists of thermal desorption at temperatures about 260°C in connection with GC-MS for peak identification or GC with flame ionization detection for quantitative analyses. So-called “modified closeable sampling columns” are used as batch-reactor in thermal desorption experiments. Desorbed vapours can be introduced on capillary columns without sample discrimination and without a disturbing lost of resolution. In this manner a lot of individual polycyclic aromatic hydrocarbons were determinated in waste wood samples, especially in railway sleepers. 相似文献
95.
N-Methylmorpholinium 4-aryl-5-cyano-2-oxo-2-oxo-1,2,3,4-tetrahydropyridine-6-thiolates were obtained by the condensation of
aromatic aldehydes, cyanothioacetamide, and Meldrum's acid in the presence ofN-methylmorpholine. They were then used in the syntheses of substituted 6-alkylthio-3,4-dihydropyridin-2(1H)-ones and 4,5-dihydrothieno[2,3-b]pyridin-6(7H)-ones.
Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 10, pp. 1852–1856, October, 1997. 相似文献
96.
Molecular routes to metal oxides has become an area of intensescientific interest due to the technological relevance of thesematerials. Molecular routes are proving important as a result ofthe possibility to control the physical and chemical propertiesof the final materials.We have chosen to study non-hydrolytic methods, namely esterelimination reactions between two prototypical molecularprecursors metal alkoxides, M(OR)n, and metal carboxylates, M(O2CR)n, to synthesize metal oxides:
This method allows for the synthesis of pure metal oxides bycomplete elimination of the organic supporting ligands withconcomitant formation of M-O-M bridges.Furthermore, incomplete esterelimination can lead to isolation of molecular clusters asintermediates which can also be used as building blocks for theformation of metal oxides with controlled microstructure.Here we report a series of reactions between Sn and Si alkoxidesand carboxylates designed to gain further insight into thefactors governing ester elimination reactions. By choosingcompounds with varying coordination environments and stericaccessibility we have devised a set of criteria which shouldallow for successful ester elimination between metal alkoxide andcarboxylate compounds. Furthermore we have also shown theability of ester elimination derived molecular clusters withspecific microstructure to be used in the synthesis of bulkmaterials retaining the structural attributes of the precursor cluster. 相似文献
97.
Summary A computer interactive identification system is proposed which is based on the relationship between retention and molecular
properties such as the size and shape of polycyclic aromatic hydrocarbons (PAHs). This system offers an automatic analytical
process for liquid chromatography, providing a reliable identification of the separated components. The identification can
be further enhanced by the use of multiple detectors such as a multichannel UV detector. The system can be used for optimization
procedures, resulting in a highly automatic complex analytical system. 相似文献
98.
99.
Chromatography has been an important tool in marine laboratories. Since the 1960s, marine laboratories have been involved in the analysis of polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs), polycyclic aromatic hydrocarbons (PAHs), and brominated flame retardants (BFRs). Column chromatography and liquid chromatography (LC) techniques have been used, mainly in the clean-up phase, while gas chromatography (GC) has been used extensively in the final determination of these contaminants. Developments have been observed from the use of packed GC columns, via capillary columns to the use of heart-cut multi-dimensional GC and comprehensive multi-dimensional GC. The progress made in interlaboratory studies and the availability of certified reference materials are discussed. 相似文献
100.
Ilya I. Moiseev Tatiana A. Stromnova Irina N. Busygina Natalya Yu. Tihonova Natalya Yu. Kozitsyna Arkady M. Ellern Mikhail Yu. Antipin Yury T. Struchkov 《Journal of Cluster Science》1992,3(4):411-421
Thermolysis of tetranuclear palladium clusters Pd4(-Q)4 Pd4(-Q)4(-O2CR)4 (Q=CPh2 or CO;R=Me, CMe3, Ph, CH2Cl or CF3) has been found to involve innersphere oxidation of carbene or carbonyl ligands during which an oxygen atom transfer occurs from the carboxylate group to the carbene or carbonyl ligand. The thermolysis of the carbonyl clusters gives rise to the products of CO2 insertion into the C–H bond of benzene or toluene used as solvents forming benzoic acid from benzene and a mixture of phenylacetic and toluic acids from toluene. The reaction of [Pd(OAc)2(PPh3)]2 with HCO2H includes the transfer of an O atom from formate ligand to the P atom and cleavage of the P-Ph bond accompanied by transfer of the Ph group from PPh3 ligand to the palladium atom. The structure of the complex formed, [Pd(-O2PPh2)(C6H5)(PPh3)]2, has been resolved by X-ray analysis. 相似文献