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151.
Summary Further to Gilpin's observations in liquid chromatography of the irreversible transformation of alkyl grafts, following the replacement of an organic mobile phase by an aqueous one, we describe some gas chromatographic experiments which lead to similar (log Vs, I/T) plots, as a consequence of the same solvent release process.We use paraffin films on siliceous supports or hydroxylated liquid substrates or C22-alkyl bonded silica. These experiments demonstrate that this irreversible transition and the melting-like reversible transition are completely different phenomena. They confirm the existence of at least three kinds of monomeric alkyl films. 相似文献
152.
Band broadening in capillary columns is satisfactorily described by the Golay-equation extended to situations of appreciable pressure drop by Giddings. In practice, however, several simplifications are often made. The effect of these simplifications on the calculated values of the minimum plate height and optimum carrier gas velocity are treated systematically. 相似文献
153.
Dimitrakakis E Haberhauer-Troyer C Abe Y Ochsenkühn-Petropoulou M Rosenberg E 《Analytical and bioanalytical chemistry》2004,379(5-6):842-848
The use of solid-phase microextraction (SPME) with gas chromatography coupled to microwave-induced plasma atomic-emission detection (GC–MIP-AED) is described for selenite [Se(IV)] speciation. Aqueous standards were derivatised with sodium tetraethyl- or tetrapropylborate and extracted by SPME. Headspace extraction of the ethyl and propyl derivatives was studied. Relevant experimental conditions were optimised, including conditions for derivatisation and extraction and those of gas chromatographic analysis. The limits of detection achieved for headspace sampling of derivatised Se(IV) were in the low ng mL–1 range for both ethylation and propylation. When the method was applied to analysis of selenite in selenised yeast reference material results were in good agreement with the indicated values. 相似文献
154.
B. Gawdzik 《Chromatographia》1991,31(1-2):21-26
Summary Using inverse exclusion chromatography the porous structure of the copolymers of di(methacryloyloxymethyl)naphthalenes and divinylbenzene was investigated.In order to determine the pore size distributions of the copolymers, toluene, alkylphenones, phthalates and polystyrene standards were used as the probes.The measurements proved that the existence of micropores depend on the method of copolymerization. The copolymers obtained by suspension and emulsion methods are more or less microporous, but the copolymer prepared by thermal polymerization in mass does not include micropores in its internal structure. 相似文献
155.
156.
T. A. Gough 《Chromatographia》1979,12(4):195-196
Summary Several detectors which have a selective response toward nitrogen containing compounds are discussed. Data on sensitivities,
detection limits and reproducibility of response are given. The application of chemiluminescence to provide a nitrogen selective
GC detector is proposed. 相似文献
157.
158.
159.
Reported here is an analytical method enabling the stereochemical resolution of a new antianginal compound possessing two stereogenic centers, leading to four stereoisomers. Only one of these isomers is currently under development as a novel antianginal agent and consequently, the other three isomers are considered as unwanted chiral impurities. Therefore, an enantioselective method is required in order to check its enantiomeric purity. This paper presents a method exploiting the high efficiency of capillary electrophoresis and the complexing properties of cyclodextrins to achieve the separation of the four stereoisomers of this weakly basic compound (pKa = 7.4). For this purpose, the combination of a neutral cyclodextrin, hydroxypropyl-gamma-cyclodextrin (HP-gamma-CD), and an anionic cyclodextrin, carboxymethyl-beta-cyclodextrin (CM-beta-CD), was added to the separation buffer running in an uncoated silica capillary. After selection of the suitable cyclodextrin system, satisfactorily separation conditions were as follows: 30 mM phosphate buffer (pH 6.4) containing 10 mM of HP-gamma-CD and 10 mM of CM-beta-CD, running voltage +30 kV. The resulting run time and resolutions were respectively about 17 min and between 1.95 and 2.84. Linearity curves (0.993 < r2 < 0.998) are also shown. 相似文献
160.
H. Wätzig 《Chromatographia》1992,33(5-6):218-224
Summary It is still difficult to determine peaks and peak boundaries properly, though peak recognition is very important for the precision of quantitative data. A new computer program overcomes these problems using a method which is adapted from human judgements. The algorithm was developed for HPLC but can also be used in other fields of analytical chemistry. 相似文献