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31.
C. Lange 《Journal of mass spectrometry : JMS》1993,28(11):1285-1296
Oxirane chemical ionization (CI) gives numerous ions, including C2H3O+ and C2H5O+. These ions react with organic molecules through various specific ion–molecule reactions such as hydride abstraction, protonation, additions or cycloadditions. Oxirane CI allows discrimination between unsaturated compounds with [M + 43]+ and [M + 57]+ adduct ions and heteroatom functions with [M + 45]+ adduct ion. All are diagnostic ions. Oxirane CI permits selectivity during the ionization process of a mixture and discrimination of isomers. 相似文献
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33.
The determination of carbonyl compounds in gaseous samples is usually accomplished by enrichment methods, in which 2,4-dinitrophenyl-hydrazine (DNPH) as a derivatization reagent has become established to a large extent. However, the conventional methods of DNPH-impingers and of DNPH-cartridges are applicable to emission measurements in a limited way only, depending on the NO2-concentration in the exhaust gas. It could be proved that DNPH-derivatives, as well as DNPH, are also decomposed by NO2 at a different speed, in which the hydrazones of unsaturated carbonyl compounds are probably more sensitive than those of the saturated carbonyl compounds. In view of this fact, the collecting methods had to be modified to avoid losses with the enrichment. The analysis of the compounds is carried out by HPLC with an effective gradient-system which is able to separate and detect the carbonyl compounds in exhaust gas within 16 min. Furthermore, a simple working-up procedure is presented which facilitates a parallel analysis by GC. 相似文献
34.
SGTx1 is a new neurotoxin from the venom of Scodra griseipes. Because of the small quantity of this natural peptide available, mass spectrometry was used to obtain information on its higher-order structure. The kinetics of reduction by 1,4-dithiothreitol (DTT) was monitored by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS), and showed that one of the three disulfide bridges was appreciably more accessible to the DTT. Studies based on the charge state distribution (CSD) and H/D exchange of the non-reduced peptide, under neutral and acidic conditions, were performed using electrospray mass spectrometry (ES-MS). In neutral solution, SGTx1 showed a maximum charge state of four compared with seven potentially protonated basic residues, and all labile hydrogens were exchanged. However, under acidic conditions, a maximum charge state of only five was observed, and four of the labile hydrogens could not be deuterated. These observations are interpreted in terms of a rigid structure maintained by the disulfide bridges, which can be temporarily relaxed by disulfide bridge scrambling only at higher pH values. 相似文献
35.
R. S. A. de Lange K. -N. P. Kumar J. H. A. Hekkink G. M. H. van de Velde K. Keizer A. J. Burggraaf W. H. Dokter H. F. van Garderen T. P. M. Beelen 《Journal of Sol-Gel Science and Technology》1994,2(1-3):489-495
Microporous SiO2 and SiO2/MO2 (M=Ti, Zr, Al; 10 mol% MOx) materials for gas separation membrane applications have been prepared from polymeric sols. Characterization of these sols with SAXS showed that the mean fractal dimension of the SiO2 sols is 1.3–1.4 with a radius of gyration of approximately 2.5 nm. The dried and calcined films are microporous and the pore size distribution was bimodal with maxima at diameters of 0.5 nm and 0.75 nm. For the SiO2/TiO2, SiO2/ZrO2 and SiO2/Al2O3 systems, much milder reaction conditions proved to be necessary to obtain sols with comparable fractal dimensions due to the high reactivity of the Ti/Zr/Al-alkoxides. Microporous supported membranes with molecular sieve-like gas transport properties can be prepared from a relatively wide range of sol structures: from polymers too small to characterize with SAXS to structures with fractal dimensions: 1<d
f<2.04. 相似文献
36.
Brigitte Sarry und Arno Lange 《Fresenius' Journal of Analytical Chemistry》1968,241(3):186-196
Zusammenfassung Die optimalen Bedingungen für die photometrische Bestimmung von Tantal mit Pyrogallol in schwefelsaurer Lösung bei 405 nm wurden ausgearbeitet. Das Verfahren wurde statistisch überprüft.
Für die Durchführung der Untersuchungen standen Mittel aus dem ERP-Sondervermögen und dem Fonds der Chemischen Industrie zur Verfügung, für die wir auch an dieser Stelle bestens danken.
Herrn Professor Dr. E. Asmus zum 60. Geburtstag gewidmet. 相似文献
Investigations on the photometric determination of tantalum with pyrogallol
The optimum conditions for the photometric determination of tantalum with pyrogallol in sulphuric acid solution at 405 nm have been elaborated. The method has been checked statistically.
Für die Durchführung der Untersuchungen standen Mittel aus dem ERP-Sondervermögen und dem Fonds der Chemischen Industrie zur Verfügung, für die wir auch an dieser Stelle bestens danken.
Herrn Professor Dr. E. Asmus zum 60. Geburtstag gewidmet. 相似文献
37.
Boesten WH Seerden JP de Lange B Dielemans HJ Elsenberg HL Kaptein B Moody HM Kellogg RM Broxterman QB 《Organic letters》2001,3(8):1121-1124
[reaction: see text]. Diastereoselective Strecker reactions based on (R)-phenylglycine amide as chiral auxiliary are reported. The Strecker reaction is accompanied by an in situ crystallization-induced asymmetric transformation, whereby one diastereomer selectively precipitates and can be isolated in 76-93% yield and dr > 99/1. The diastereomerically pure alpha-amino nitrile obtained from pivaldehyde (R1 = t-Bu, R2 = H) was converted in three steps to (S)-tert-leucine in 73% yield and >98% ee. 相似文献
38.
39.
Auf der Grundlage des Zirkulations-Diffusions-Prinzips wurden zwei Trennrohre für die Hochanreicherung von Gasen enytwickelt. Als Modellgasmischungen dienten H2-N2 Kr-CH4 und Luft. Neben Wasserdampf wurden Methanol- und Äthaanoldämpfe als Treibmittel benutzt. Gute Trennungen wurden in einem nur 20 cm langen Rohr erzielt, dessen Trennspalt horizontal durch Lamellen in kleine Sektionen und durch ein Drahtdiaphragma vertikal in zwei Ringkammern geteilt wird. Drei Rohre dieses Typs wurden in einer rechteckigen Kaskadenanordnung getestet. Die Theorie des Transportes im Trennrohr sowie die Behandlung des hydrodynamischen Problems werden angegeben. Eine Anwendung des beschriebenen Trennrohres zur Isotopentrennung und zur Gashochanreicherung erscheint aussichtsreich. 相似文献