Column static phase

The static phase, for a silica gel column, would consist almost entirely of that portion of the mobile phase that is trapped in the pores of the silica gel. Consequently, it would appear reasonable to assume that, in equation (1),... 

The internal volume of a column is occupied by three substances, the mobile phase, the stationary phase and the support. The term mobile phase is a misnomer as it impfies that all the mobile phase is moving, which is not so. The mobile phase within the pores is also stationary and thus constitutes part of the stationary phase. Nevertheless, it is such a well established term, it will still be used to denote the total mobile phase in the column, moving and sialic. The term moving phase will be used for liial fraction of the mobile phase that actually moves, whereas the term static phase will be used for that fraction of the mobile phase that is trapped in the pores, or in the interstices of the support particles, and does not move. 

Insertion/introduction of the needle into the GC port, depression of the plunger, and thermal desorption of the analytes. Alternatively, the analytes are washed out of the fiber by the HPLC mobile phase via a modified HPLC six-port injection valve and a desorption chamber that replaces the injection loop in the HPLC system. The SPME fiber is introduced into the desorption chamber, under ambient pressure, when the injection valve is in the load position. The SPME-HPLC interface enables mobile phase to contact the SPME fiber, remove the adsorbed analytes, and deliver them to the separation column. Analytes can be removed via a stream of mobile phase (dynamic desorption) or, when the analytes are more strongly adsorbed to the fiber, the fiber can be soaked in mobile phase or another stronger solvent for a specific period of time (e.g., 1 min) before the material is injected onto the column (static desorption) (Fig. 6). 

Here we will pay attention to the gas-liquid reactors. The reaction takes place usually in the liquid phase. Three main types of contact may be distinguished following the phase ratio (1) gas bubbles dispersed in liquid, (2) liquid drops dispersed in gas, and (3) gas and liquid in film contact. In the first category we may cite gas-liquid bubble columns, plate or packed absorption columns, agitated tanks, agitated columns, static mixer columns, pump-type reactors. As examples in the second class we may name spray columns or liquid injection systems. The third category can be used with very exothermic reactions or viscous liquids. 

In a detailed study of a 25 cm x 4.6 mm I.D. column packed with Zorbax C8 (5 p,m particles and a surface area 330 m /g) with methanol-water (1 4) as mobile phase it was shown that 33% of the column volume was occupied by the fixed stationary phase [690]. The pore volume (21 % of the column volume) consisted of 21% adsorbed solvent and 79% bulk solvent. The interparticle volume (46% of the column volume) consisted of 73% moving phase and 27% static phase. It is not easy, however, to determine the various column volume elements, and generally kinetic and thermodynamic parameters have been determined for inadequately defined phase ratios and may not be correct in the absolute sense. 

Glass Capillary Gas Chromatography. For the quantitative analysis of the PAH a Varian 3700 gas chromatograph equipped, with a flame-ionization detector and coupled with a data system of Spectra Physics was used. The glass capillary columns statically coated with different stationary phases (OV 101, "SE 30 , SE 52,... 

The headspace analysis procedure is simple the food is sealed in a container, then brought to the desired temperature and left for a while to establish an equilibrium between volatiles bound to the food matrix and those present in the vapor phase. A given volume of the headspace is withdrawn with a gas syringe and then injected into a gas chromatograph equipped with a suitable separation column (static headspace analysis). Since the water content and an excessively large volume of the sample substantially reduce the separation efficiency of gas chromatography, only the major volatile compounds are indicated by the detector. The static headspace analysis makes an important contribution when the positions of the aroma sub-... 

Static headspace GC/MS. The partitioning of volatile and semivolatile compounds between two phases in a sealed container. An aliquot of the headspace gas generated is injected onto a gas chromatographic column. This is followed by mass spectrometric analysis of compounds eluting from the gas chromatograph. 

This unit is usually used as the reboiler for the distillation column and, in this service, operates by the thermosiphon action of the difference in static head in the column and in the vapor-liquid phase leaving the reboiler. When tied into the bottom chamber, the liquid is usually recirculated many times, vaporizing only 10-25% of the reboiler feed per pass however, when used as a draw-off from the bottom tray seal pan, the feed to the reboiler is not recirculated flow. The basic operation is the same, however. 

In effect, the composition of the mobile phase, and thus the selectivity of the chromatographic system, has been changed. As mentioned in the text, dynamic FAB operates effectively with lower concentrations of matrix than static FAB and although its effect may be minimal it should always be considered. Post-column addition of matrix overcomes potential problems of this nature. 

Reactors with a packed bed of catalyst are identical to those for gas-liquid reactions filled with inert packing. Trickle-bed reactors are probably the most commonly used reactors with a fixed bed of catalyst. A draft-tube reactor (loop reactor) can contain a catalytic packing (see Fig. 5.4-9) inside the central tube. Stmctured catalysts similar to structural packings in distillation and absorption columns or in static mixers, which are characterized by a low pressure drop, can also be inserted into the draft tube. Recently, a monolithic reactor (Fig. 5.4-11) has been developed, which is an alternative to the trickle-bed reactor. The monolith catalyst has the shape of a block with straight narrow channels on the walls of which catalytic species are deposited. The already extremely low pressure drop by friction is compensated by gravity forces. Consequently, the pressure in the gas phase is constant over the whole height of the reactor. If needed, the gas can be recirculated internally without the necessity of using an external pump. 

There are basically three methods of liquid sampling in GC direct sampling, solid-phase extraction and liquid extraction. The traditional method of treating liquid samples prior to GC injection is liquid-liquid extraction (LLE), but several alternative methods, which reduce or eliminate the use of solvents, are preferred nowadays, such as static and dynamic headspace (DHS) for volatile compounds and supercritical fluid extraction (SFE) and solid-phase extraction (SPE) for semivolatiles. The method chosen depends on concentration and nature of the substances of interest that are present in the liquid. Direct sampling is used when the substances to be assayed are major components of the liquid. The other two extraction procedures are used when the pertinent solutes are present in very low concentration. Modem automated on-line SPE-GC-MS is configured either for at-column conditions or rapid large-volume injection (RLVI). 

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