Packed columns loading

Ethane-Deuteroethanes. Chromatographic separation of ethane and perdeuteroethane was first reported by Van Hook and Kelly (32) using packed columns loaded with methylcyclopentane at subambient temperatures. These authors also reported the partial resolution of protio-ethane from mono and di-deuteroethanes. The chromatographic properties of the perdeutero-ordinary system were further investigated on a variety of liquid substrates using packed column GLC techniques by Van Hook and Phillips (34) and on an open tubular etched glass column with a wetted wall (subsequently called wet glass in this paper) by Bruner, Cartoni, and Liberti (8). 

To minimize the multiple path and mass transfer contributions to plate height (equations 12.23 and 12.26), the packing material should be of as small a diameter as is practical and loaded with a thin film of stationary phase (equation 12.25). Compared with capillary columns, which are discussed in the next section, packed columns can handle larger amounts of sample. Samples of 0.1-10 )J,L are routinely analyzed with a packed column. Column efficiencies are typically several hundred to 2000 plates/m, providing columns with 3000-10,000 theoretical plates. Assuming Wiax/Wiin is approximately 50, a packed column with 10,000 theoretical plates has a peak capacity (equation 12.18) of... 

For total-reflux distillations carried out in packed columns, regions of loading and flooding are identified by their effects on mass-transfer efficiency, as shown in Fig. 14-47. Gas and liquid rate increase... 

Flooding and Loading Since flooding or phase inversion normally represents the maximum capacity condition for a packed column, it is desirable to predict its value for new designs. The first generalized correlation of packed-column flood points was developed by Sherwood, Shipley, and Holloway [Ind. Eng. Chem., 30, 768 (1938)] on the basis of laboratory measurements primarily on the air-water system. 

Strigle [94] proposed this term to better describe the performance of a packed column at or near the previously described loading point. Kister [93] evaluated the limited published data and proposed using the MOC at 95% of the flood point. The flood point can be estimated by Equation 9-20 or from the plots in References 90 and 93. The data are reported to be within 15-20% of the prediction [93]. See Figure 9-22 for the identification of MOC on the HETP vs. Cg chart For more accurate information... 

Differential pressure control is often used on packed columns to ensure that the packing operates at the correct loading see Figure 5.22d (see p. 234). 

Production of hypochlorite takes place in a two-step absorption unit in which 23% caustic solution is fed counter-currently to the chlorine feed-stream. In the first step -the liquid jet-loop reactor - about 90% of the chlorine is converted to hypochlorite. In step two - a packed column - a very efficient absorption [1-3] is carried out in which the chlorine concentration in the off-gas is reduced to <1 ppm. The operating window of this apparatus with respect to chlorine load is quite large and varies from 100 to 6000 kg h-1 of chlorine. This high capacity is necessary for the consumption of peak loads from the electrolysis plant during short time periods. During start-up or shutdown of one electrolyser the total chlorine peak load can vary from 100 to 300 kg in just a few minutes. 

There are several ways of calculating the pressure drop across a packed column when gas and liquid are flowing simultaneously and the column is operating below the loading point. 

In many industrial applications of packed columns, it is desirable to know the volumetric hold-up of the liquid phase in the column. This information might be needed, for example, if the liquid were involved in a chemical reaction or if a control system for the column were being designed. For gas-liquid systems the hold-up of liquid Hw for conditions below the loading point has been found(48) to vary approximately as the 0.6 power of the liquid rate, and for rings and saddles this is given approximately by ... 

Chiral SFC can be performed in open tubular [41,42], and packed column [43,44] modes. Packed column SFC can be further categorized into analytical, semipreparative, and preparative SFC [7, 8], Packed column SFC is more suitable for fast separations than open tubular column SFC, since a packed column generally provides low mass transfer resistance and high selectivity [45, 46], Packed column SFC also provides high sample loading capacity [27,47], which can increase sensitivity. Only packed column SFC is suitable for preparative-scale enantioseparation. This chapter will focus on chiral separation using packed column SFC in the analytical scale. 

Inlet Pressure Maximum Column Load Multipath Packing Factor Longitudinal Diffusion Packing Factor Column Mobile Phase Fraction... 

The most popular method used is a dynamic method, the saturation method. In this technique, the non-volatile, heavy solid solute is loaded into a saturator, or a battery of two or more saturators connected in series, and remains there as a stationary phase during the experiment. In most cases the saturator is in the form of a packed column. At constant pressure, a steady stream of supercritical fluid (solvent) passes through a preheater, where it reaches the desired system temperature. Then this fluid is continuously fed to the bottom of the saturator, and the solute is stripped from the stationary heavy phase in the column. The supercritical fluid saturated with the solute leaves the saturator at the top. 

---