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941.
Capillary electrophoresis (CE) with head-column field-amplified sample stacking (FASS) in presence of a water plug inserted at the capillary tip is a robust approach providing a more than 1000-fold sensitivity enhancement when applied to low-conductivity samples that are analyzed in an integrated instrument. Employing modular systems comprising a small hydrodynamic buffer flow (siphoning) towards the capillary end and featuring UV absorption or electrospray ionization mass spectrometric (MS) detection, insertion of a water plug is demonstrated to deteriorate the performance of head-column FASS or making it unfunctional. Electroinjection in the absence of the water plug can be employed instead and is shown to provide a ng/ml sensitivity when applied to low conductivity samples. With some suction of sample into the capillary during electroinjection, contamination of the sample vial with buffer is thereby largely avoided. Electroinjection applied to the CE-ion trap MS-MS and MS-MS-MS analysis of twofold diluted urines, urinary solid-phase extracts and urinary liquid-liquid extracts is shown to provide much improved sensitivity compared to hydrodynamic injection of these samples. With electroinjection from diluted urine and urinary solid-phase extracts, the presence of free opioids and their glucuronic acid conjugates can be unambiguously confirmed in urines that were collected after single-dose administration of small amounts of opioids (tested with about 7 mg codeine and 25 mg dihydrocodeine, respectively). Thus, CE-multiple MS with direct electroinjection of opioids from untreated urines could prove to become a rapid and simple approach for unambiguous urinary testing of drug abuse. Procedures leading to the reduction of siphoning in modular CE setups are briefly discussed as well. 相似文献
942.
A high performance liquid chromatographic (HPLC) method is described for the determination of the four major aflatoxins, B1, B2, G1 and G2, in peanut products. The aflatoxins are extracted by adapting a procedure developed by Pons (1) at the SRRC, USDA, and quantitated utilizing a new 5 mum reverse-phase column with NaCl/acetontrile/methanol mobile phase (3 + 1 + 1). The 5 mum column achieved baseline resolution of each of the four aflatoxins. Retention times and peak heights were reproducible. The procedure was successfully applied to several types of peanut products and was applicable to both roasted and unroasted peanuts, which is a decided advantage over the current CB and BF extraction methods. Additionally, it can be used for sweetened peanut matrixes with no interferences in the chromatography. The total time required for sample preparation and aflatoxin determination is less than 1.5 hours. 相似文献
943.
The intramolecular cyclization reactions of tri-1-hex-5-enyl Group III derivatives and of 1-hex-5-enyllithium have been investigated and it is proposed that the reactions may be depicted as internal addition across the terminal double bonds of the alkenyl species. The cyclization reaction proceeds more readily for the 1-hex-5-enyl derivatives than for any other chain length and is dependent on temperature, concentration and solvent. 1H NMR data and cryoscopic molecular weight data are presented for several diisobutyialkenyl- and diisobutylalkyl-aluminum derivatives. These data have been interpreted in terms of a direct intramolecular interaction between the metal center and the π-electron system of the olefinic site. The intramolecular cyclization reactions for the 1-hept-6-enyl, 1-oct-7-enyl- and 1-undec-10-enylaluminum derivatives also were investigated and it was found that cyclization occurred only for the 1-hept-6-enyl derivative. 相似文献
944.
Zusammenfassung Die komplexe Koazervation im SystemG-A-H2O kann als zweistufiger Prozeß aufgefaßt werden. Das erste Stadium ist die Bildung des elektrisch neutralen Komplexes zwischen G und A unter Einfluß der elektrostatischen Anziehungskräfte. Die Stöchiometrie der gewonnenen Verbindung wird durch die Äquivalenz der Makroionen bestimmt.Nur elektrisch neutrale Komplexe können die neue Phase, d. h. das komplexe Koazervat bilden. Deshalb muß die Zusammensetzung der koazervaten Phase von pH abhängen und bei Veränderung des Verhältnisses der Polymere im Gemisch unveränderlich bleiben.Bei einem Verhältnis der Polymere, kleiner als das stöchiometrische, ist die Bildung geladener Komplexe möglich.Den Prozeß der komplexen Koazervation kann man mittels der Methode der Trübungsmessung bei Cs<6·10–3 g/100 g untersuchen. Hierbei ist die optische Dichte proportional der Menge des komplexen Koazervats oder des elektrisch neutralen Komplexes im System. 相似文献
945.
19F nuclear magnetic resonance studies on imidosulphuroxide difluorides Non equivalent fluorine atoms bounded to hexavalent sulphur of the NSOF2 group in thionyl compounds give extreme AB-spectra. 相似文献
946.
C. F. Parrish G. L. Kochanny H. W. Rinn 《Journal of polymer science. Part A, Polymer chemistry》1969,7(9):2531-2535
The phase diagram of the acrylic acid–acrylamide system as determined by DTA and the supporting x-ray diffraction data are presented. This diagram shows that the system forms a 1 : 1 addition compound which decomposes above 0°C. There is also one eutectic point at a 67 mole-% acrylic acid composition. 相似文献
947.
[formula: see text] A new chiral azetidinone-carboxylate ligand for dirhodium(II) catalysis enhances reactivity toward diazo decomposition and selectivity toward cyclopropanation enabling diazomalonates, vinyldiazoacetates, and aryldiazoacetates to be effectively used with a dirhodium(II) carboxamidate catalyst. 相似文献
948.
W. Sterzel 《无机化学与普通化学杂志》1970,374(3):271-285
Fundamental vibrations of ions which are IR-inactive due to molecular and site symmetry may appear in the IR spectra of crystals with lattice imperfections. In the case of several carbonates with calcite structure this effect is observed. By means of plastic deformation or special preparation as well as heating various degrees of imperfection are produced in carbonate samples. A quantitative relation between the imperfections (measured by x-ray methods and surface determination) and the intensities of the activated symmetric stretching band v1 of the carbonate ion is established. 相似文献
949.
The alkaline-earth group was isolated, after removal of silica, by precipitation as sulfates from an alcoholic solution. Those sulfates were reduced and dissolved by treatment with hydriodic acid. The alkaline earths were separated from each other by ion-exchange chromatography. The results are in good agreement with the values reported by the National Bureau of Standards. 相似文献
950.
P. A. Beeley J. M. Brushwood M. G. Henesy M. W. Collins C. A. Haywood 《Journal of Radioanalytical and Nuclear Chemistry》1997,215(1):135-139
The measurement of16N and18F activity in the primary coolant of the JASON Argonaut reactor has been used to monitor in-core reactor power. The16N is produced by the16O(n, p)16N reaction and the 6.1 MeV photopeak was measured on-line using a BGO detector adjacent to the primary coolant circuit. These data provided a relative measure of power stability during steady state operation and a measure of linearity at different power levels. The18F is produced in the primary coolant by the18O(p, n)18F reaction and aliquots of primary coolant were sampled from the reactor dump tank for off-line radiochemical analysis. The18F was separated as trimethylfluorosilane and the activity was determined by measurement of the 0.511 MeV annihilation photopeak using a NaI(TI) detector. The measured18F activity was used to determine actual in-core reactor power using both ab-initio calculations and by comparison of results with a calibrated power reactor. The18F data also provided a method of nomalising the16N data for direct monitoring of in-core reactor power in JASON. 相似文献