Search results for "Elution"

Stability of nitroaromatic specialty explosives in reversed-phase liquid chromatographic systems

2008

Abstract In this study, the stability of 2,4-dinitroanisole, 2,2′,4,4′,6,6′-hexanitrodiphenylsulfide, 2,3,4,6-tetranitroaniline, 2,4,6-trinitroaniline, 2,4,6-trinitroanisole, and 2,4,6-trinitrochlorobenzene in liquid chromatographic systems was studied under different solvent/eluent conditions. Stock solutions of the explosives were prepared in acetonitrile and diluted with acetone/water, acetonitrile/water, or methanol/water mixtures. Within 48 h, these working solutions were repeatedly injected onto a silica column and eluted with acetonitrile/water or methanol/water mobile phases. Under all conditions, 2,4-dinitroanisole was stable, whereas 2,4,6-trinitroaniline was stable only in the me…

Specific detection of cyclobutane pyrimidine dimers in phytoplankton DNA by a non-radioactive assay based on T4-endonuclease V digestion.

2001

The effect of artificial and natural UV irradiation on DNA in marine phytoplankton Isochrysis galbana monoculture was investigated. The presence of cyclobutane pyrimidine dimers (CPDs) in unlabelled I. galbana DNA was detected by a non-radiometric alkaline filter elution assay after T4-endonuclease V digestion. The quantity of CPDs was estimated by alkaline agarose gel electrophoresis. Precise determination of the amount of DNA in the presence of I. galbana pigments was achieved by oxazole yellow homodimer (YOYO) dye. T4-endonuclease V-sensitive sites frequency (ESS/kb), measured after exposure to 2-40 kJ m(-2) of artificial UV light, increased in a dose-dependent manner. Twelve hours after…

Trennung von spaltprodukten durch Extraktionschromatographie

1970

The separation of fission products which form anionic species in mineral acids and of uranium and neptunium from samples of neutron-irradiated uranium is described. The method used is extraction chromatography with tri-n-butylphosphate (TBP) and di-(2-ethylhexyl)-orthophosphoric acid (HDEHP) as extractants and polytrifluoromonochloroethylene powder as the solid support. In the first column Zr, U and Np are extracted with TBP from 8N HNO3/NaClO3. In the second column, HDEHP is applied as extractant and 9N HCl/NaClO3 as the mobile phase for the isolation of Nb, Sb, and I, and in the third column (HDEHP), the rare earths and Mo are extracted from 0.1N HCl. Finally with the fourth column (TBP),…

Approaches to model the retention and peak profile in linear gradient reversed-phase liquid chromatography.

2012

Abstract The optimisation of the experimental conditions in gradient reversed-phase liquid chromatography requires reliable algorithms for the description of the retention and peak profile. As in isocratic elution, the linear relationship between the logarithm of the retention factor and the solvent contents is only acceptable in relatively small concentration ranges of modifier. However, more complex models may not allow an analytical integration of the general equation for gradient elution. Alternative approaches for modelling the retention in linear gradient elution are here proposed. Those based on the quadratic logarithmic model and a model proposed for normal liquid chromatography yie…

Sensitive determination of polycyclic aromatic hydrocarbons in water samples using monolithic capillary solid-phase extraction and on-line thermal de…

2011

A methacrylate-based monolithic capillary column has been evaluated for the preconcentration of polycyclic aromatic hydrocarbons (PAHs) from environmental water samples. For this purpose, the monolyte was in situ synthesized in a 6cm×0.32mm id fused-silica capillary. The microextraction unit was fitted to a micro-HPLC pump to pass 10mL of sample. The isolated pollutants were eluted by means of 10μL of methanol, the organic phase being directly collected in a specific interface that can be fitted to the injection port of the gas chromatograph without modification. The interface allows the on-line thermal desorption of the PAHs, avoiding the dilution and providing enough sensitivity to reach …

Evaluation of methods aimed at complete removal of template from molecularly imprinted polymers

2001

Polymers imprinted with clenbuterol were used to study the influence of various post-polymerization treatments [e.g., thermal annealing, microwave assisted extraction (MAE), Soxhlet extraction and supercritical fluid template desorption] on the bleeding of residual template. The aim of the study was to reduce the bleeding to levels that would allow the use of the materials as affinity phases for extraction of clenbuterol from bovine urine at concentrations below 1 ng ml−1. After treatment, the clenbuterol imprinted polymers were packed into solid-phase extraction columns and the bleeding was estimated by quantifying the amount of template released in 10 ml of methanol–acetic acid (9 + 1 v/v…

Über die bestimmung der strömungsdispersion zur ermittlung von molekulargewichtsverteilungen mit der gelchromatographie

1974

Die Kenntnis der axialen Dispersion ist eine notwendige Voraussetzung zur Ermittlung von Molekulargewichtsverteilungen aus der gelchromatographischen Elutionskurve. Die vorliegende Arbeit beschaftigt sich mit der Bestimmung der axialen Dispersion unter Verwendung monodisperser Polymerer. Abschliesend wird ein Verfahren vorgeschlagen, welches aus der gelchromatographischen Elutionskurve von Proben mit bekannter Molekulargewichtsverteilung die Dispersion naherungsweise zu ermitteln gestattet. The knowledge of the axial dispersion is necessary for the determination of molecular weight distributions from gel permeation chromatography elution diagrams. This work deal with the determination of th…

1967

Gel chromatography can be considered as a network-limited partition. This leads to the conclusion that it is impossible to find a generalizing relationship between the molecular weight and the elution volume using parameters depending only on the solute. The preparation of gels with different chemical structure is discussed and possible methods for the alteration of pore size are described. Investigations of the influence of the physical and chemical structure on separation and separation efficiency have shown that the elution volume depends to some extent on the chemical nature, but the separation efficiency is mainly a function of the physical structure. Die Gelchromatographie kann als ei…

The efficiency of gel permeation chromatography

2007

The resolution power of gel permeation chromatography (GPC) columns and their combinations is tested as a function of the pore sizes of the gels and as a function of the elution velocity. The efficiency of GPC is characterized by the ratio UG/UT, where UG is the experimental, and UT the theoretical, inhomogeneity. The latter quantity is obtained from absolute measurements of Mw, and Mn. The ratio passes through a minimum for a series of columns with increasing pore sizes. The minimum occurs at that column or column set which is best suited to resolving a given polymer. UG/UT for any column decreases with decreasing elution velocity. At a certain velocity UG/UT becomes 1. This velocity is us…

Solution properties of polyelectrolytes. I. Exclusion chromatography of sodium polystyrene sulphonate in salt-free water as eluent

1987

The effect of concentration of sodium polystyrene sulphonate on the elution volume in exclusion chromatography has been investigated using salt-free water as eluent. A non-linear increase in the elution volume has been observed with increasing injected sample concentration. Concentration-dependent calibrations have been obtained which approach the universal calibration for uncharged polymers (dextrans) as polyelectrolyte concentration increases. The separation mechanisms are interpreted in terms of electrostatic and hydrodynamic interactions. A semi-empirical model is proposed to predict concentration effects of linear polyions in exclusion chromatography and good agreement has been found b…