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41.
Summary A packed flow cell was used for fluorometric detection in micro high-performance liquid chromatography. The flow cell consisted of fused-silica tubing packed with the same material as the separation column. A focusing effect of the stationary phase on the signal intensity was observed, leading to an improvement of the mass detection limit, as achieved by on-column detection. 相似文献
42.
Stationary phase crosslinking conditions for fused silica capillary columns were optimized with the use of a factorial design experiment. This experimental strategy was chosen because it provided for the determination of two-factor interactions. A predictive model was developed for the desired chromatographic performance parameters as a function of the variables of the crosslinking reaction. Confirmatory experiments proved the usefulness of the mathematical model which resulted in the production of capillary columns of superior performance with significant improvements in reproducibility. 相似文献
43.
The introduction of selected fractions from a liquid chromatograph into a gas chromatograph has been described; however, analyses were performed by off-line experiments requiring collection and reinjection of the separate fractions or by on-line procedures where disadvantageously, only a fraction of the separated peak or a well resolved component in a mixture could be introduced into a gas chromatograph. This disadvantage is overcome by the apparatus and method described in this paper, which utilizes a multidimensional chromatography system employing a high efficiency, packed capillary LC column coupled on-line to a capillary gas chromatograph. The liquid chromatograph (so designed) can act as a highly efficient clean-up or chemical class fractionation step prior to introduction into the gas chromatograph, significantly reducing sample preparation times in many applications. Thus minor components in a complex matrix can be determined without prior sample clean-up, an example of which is the determination of polychlorinated biphenyls in a complex hydrocarbon matrix. 相似文献
44.
A comparison is made between dichlorosilanes and cyclic siloxanes as starting materials in the synthesis of stationary phases for capillary gas chromatography (CGC) and supercritical fluid chromatography (SFC). Siloxanes containing one or more of the side groups methyl, vinyl, phenyl, and cyanoethyl in various ratios were synthesized and compared. These phases were characterized by chromatographic (gel permeation, GPC), spectroscopic (IR, 1H NMR, 29Si NMR), and thermal (DSC) methods. Coated fused silica columns were evaluated with respect to polarity, crosslinkability with several free-radical initiators, and thermal stability. A new liquid phase, 7% cyanoethyl, 7% phenyl, 1% vinyl methyl polysiloxane is shown to be more polar than OV-1701, more temperature stable, easily crosslinked and suitable for use in supercritical fluid chromatography. 相似文献
45.
Fused silica capillaries deactivated with D4 and coated with OV-1 were subjected to cobalt-60 gamma radiation in order to elucidate the effect of incident radiation on column performance. The chromatographic performance of these open tubular columns in which OV-1 was polymerized in situ was found to be dependent on the dosage of radiation and was evaluated before and after the irradiated columns were rinsed with solvent. Of the radiation dosages employed, 3 MRad produced superior chromatographic performance coupled with very favorable residual surface activity. 相似文献
46.
Summary Al2O3-PLOT columns are used with great advantage for the analysis of volatiles, because of the increased capacity ratio and selectivity compared to WCOT-columns. Their applicability is limited to relatively non-polar components with relatively low boiling points i. e. eluting before n-decane.In the analysis of the halocarbons in stratospheric air, the decomposition of certain compounds was observed. In this study the stability of a number of volatile organic compounds was determined in function dependence of the column temperature using a two-dimensional GC-system.A possible reaction mechanism for the decomposition is proposed and confirmed for several chlorinated ethanes. 相似文献
47.
I. M. Mutton 《Chromatographia》1998,47(5-6):291-298
Summary Rapid analyses were performed using reversed-phase liquid chromatography with short (20–100 mm) columns swept by fast yet
shallow gradients, and the results compared with those obtained with 150 mm columns and slow gradients. The resolution losses
incurred with shorter columns were minimised by employing elevated flow rates, to ensure that comparable mean retention factors
were experienced by individual analytes during gradients run on different columns. This conserves gradient steepness. High
quality performance was obtained with turn-around times of 5–10 minutes. An overall 5-fold enhancement in the rate of information
generation was obtained. The relevance of instrumental parameters and of column and packing dimensions, upon the potential
for improved performance is discussed. Some implications for the rapidly developing technique of capillary electrochromatography
are briefly indicated. 相似文献
48.
M. Baru A. Danilov I. Vagenina E. Gorbunova S. Moshnikov L. Mustaeva V. Cherskii 《Chromatographia》1997,45(1):351-354
Summary The design of new dynamic, axial-compression columns with a system for continous packed bed adjustment and monitoring of the
floating adapter position is described. The columns are meant for liquid chromatography at low pressures (up to 8 bar) in
aqueous and organic media with stationary phases of all types. The columns have adapter position pickups for continuous automatic
monitoring of the bed height (original “swellographic” monitoring). The column described with gas pressurisation was tested
with soft Sephadex G-10 and G-25. In spite of the reduction in external porosity there was no dramatic increase in back-pressure.
The column proved to provide long-term stability of the packed bed and improvement in resolution.
Presented at the 21st ISC held in Stuttgart, Germany, 15th–20th September, 1996 相似文献
49.
Xiong Wen Ye Yu Ping Zhang Ling Bo Qu Li Qun Fan Bo Li 《中国化学快报》2007,18(11):1399-1402
Microwave irradiation was firstly attempted for the preparation of organic-based monoliths of poly(styrene-divinylbenzene- methacrylic acid), which single step in situ polymerization was carried out during 15 min. The colunm permeability, electrophoretic and chromatographac behaviors were comparatively evaluated using pressure-assisted CEC, GEC and low pressure-driven separation modes. The largest theoretical plates for the preparing column could be close to 18,0000 plates/m for thiourea in the mode of p-CEC. It provided a viable alternative to traditional initiation means for the perparation of monolithic capillary columns. 相似文献
50.
The Saccharomyces strains uvarum, montuliensis, bayanus, capensis and florentinus were grown in liquid media prepared from a 1% aqueous glucose solution to which 0.05% of ammonium sulfate or urea were added as the only nitrogen supply. The amino acids exuded during incubation were isolated by cation exchange and derivatized as the corresponding N,O-heptafluorobutyryl isopropyl esters. Separation was achieved on a highly deactivated glass capillary column coated with OV-101. A characteristic amino acid profile was obtained for each of the species studied, allowing the construction of a chemotaxonomic tree, on the basis of present or absent acids. 相似文献