Packed columns, flow

A restriction to the operation of GC-MS can be caused by solvent peaks. If the solvent injected onto a packed column flows via a separator into the ion source of the mass spectrometer, it results in an unacceptable increase in pressure which causes the built-in pressure protection devices to shut the mass spectrometer down. It also much reduces the lifetime of source components such as filaments and heaters. Therefore a valve is fitted at the end of the column, which allows effluent to be vented to a pump or to tile atmosphere until the solvent has passed. The flow rates associated with the use of capillary coliunns are such that the pressure generated by the solvent is not as great as with a packed column. The total effluent may therefore be passed directly into... 

Instrument Packing Column Flow rate Solvent... 

The column is swept continuously by a carrier gas such as helium, hydrogen, nitrogen or argon. The sample is injected into the head of the column where it is vaporized and picked up by the carrier gas. In packed columns, the injected volume is on the order of a microliter, whereas in a capillary column a flow divider (split) is installed at the head of the column and only a tiny fraction of the volume injected, about one per cent, is carried into the column. The different components migrate through the length of the column by a continuous succession of equilibria between the stationary and mobile phases. The components are held up by their attraction for the stationary phase and their vaporization temperatures. 

The most common mobile phases for GC are He, Ar, and N2, which have the advantage of being chemically inert toward both the sample and the stationary phase. The choice of which carrier gas to use is often determined by the instrument s detector. With packed columns the mobile-phase velocity is usually within the range of 25-150 mF/min, whereas flow rates for capillary columns are 1-25 mF/min. Actual flow rates are determined with a flow meter placed at the column outlet. 

Pig. 22. Schematic representation of typical pressure drop as a function of superficial gas velocity, expressed in terms of G = /9q tiQ, in packed columns. O, Dry packing , low Hquid flow rate I, higher Hquid flow rate. The points do not correspond to actual experimental data, but represent examples. 

Selection of Equipment Packed columns usually are chosen for very corrosive materials, for liquids that foam badly, for either small-or large-diameter towers involving veiy low allowable pressure drops, and for small-scale operations requiring diameters of less than 0.6 m (2 ft). The type of packing is selected on the basis of resistance to corrosion, mechanical strength, capacity for handling the required flows, mass-transfer efficiency, and cost. Economic factors are discussed later in this sec tion. 

Example 13 Packed Column Pressure Drop Air and water are flowing coiinterciirrently through a bed of 2-inch metal Pali rings. The air mass velocity is 2.03 kg/s-m (1500 Ihs/hr-fd), and the liquid mass velocity is 12.20 kg/s-m (9000 Ihs/hr-fr). Calculate the pressure drop hy the generalized pres-... 

As indicated above, packed column internals include hqiiid distributors, packing support plates, redistributors (as needed), and holddown plates (to prevent movement of packing under flow conditions). Costs of these internals for columns with random packing are given in Fig. 14-80, based on early 1976 prices, and a Marshall and Swift cost index of 460. 

G = Fractionator vapor rate, Ib/hr or packed column gas rate, Ibs/ft sec or pump flow, gpm GPM = Pump flow, gpm... 

It is clear that the separation ratio is simply the ratio of the distribution coefficients of the two solutes, which only depend on the operating temperature and the nature of the two phases. More importantly, they are independent of the mobile phase flow rate and the phase ratio of the column. This means, for example, that the same separation ratios will be obtained for two solutes chromatographed on either a packed column or a capillary column, providing the temperature is the same and the same phase system is employed. This does, however, assume that there are no exclusion effects from the support or stationary phase. If the support or stationary phase is porous, as, for example, silica gel or silica gel based materials, and a pair of solutes differ in size, then the stationary phase available to one solute may not be available to the other. In which case, unless both stationary phases have exactly the same pore distribution, if separated on another column, the separation ratios may not be the same, even if the same phase system and temperature are employed. This will become more evident when the measurement of dead volume is discussed and the importance of pore distribution is considered. 

The column may be packed or it may be an open tube but in this example, a packed column will be specifically considered. The column is considered to have a length (L) and inlet and outlet pressures and inlet and outlet velocities of (Pi), (Po) (ui) and (uo), respectively. The pressure and velocity at a distance (x) from the front of the column is (Px) and (ux), respectively. According to D Arcy s equation for fluid flow through a packed bed, at any point in the column. 

Equation (11) accurately describes longitudinal diffusion in a capillary column where there is no impediment to the flow from particles of packing. In a packed column, however, the mobile phase swirls around the particles. This tends to increase the effective diffusivity of the solute. Van Deemter introduced a constant (y) to account... 

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