Mass packed column

The accuracy of temperature controllers and sensors is typically about 0.1°. Because of their high-thermal mass, packed columns are more often operated isothermally, while due to their low-thermal mass, capillary columns are most often temperature programed. Important parameters related to basic column dimensions are shown in Table 14.4. 

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... 

Time, Cost, and Equipment Analysis time can vary from several minutes for samples containing only a few constituents to more than an hour for more complex samples. Preliminary sample preparation may substantially increase the analysis time. Instrumentation for gas chromatography ranges in price from inexpensive (a few thousand dollars) to expensive (more than 50,000). The more expensive models are equipped for capillary columns and include a variety of injection options and more sophisticated detectors, such as a mass spectrometer. Packed columns typically cost 50- 200, and the cost of a capillary column is typically 200- 1000. 

Kovat s retention index (p. 575) liquid-solid adsorption chromatography (p. 590) longitudinal diffusion (p. 560) loop injector (p. 584) mass spectrum (p. 571) mass transfer (p. 561) micellar electrokinetic capillary chromatography (p. 606) micelle (p. 606) mobile phase (p. 546) normal-phase chromatography (p. 580) on-column injection (p. 568) open tubular column (p. 564) packed column (p. 564) peak capacity (p. 554)... 

To use all of these equations, the heights of the transfer units or the mass transfer coefficients and must be known. Transfer data for packed columns are often measured and reported direcdy in terms of and and correlated in this form against and... 

Experimental Mass Transfer Coefficients. Hundreds of papers have been pubHshed reporting mass transfer coefficients in packed columns. For some simple systems which have been studied quite extensively, mass transfer data may be obtained directiy from the Hterature (6). The situation with respect to the prediction of mass transfer coefficients for new systems is stiU poor. Despite the wealth of experimental and theoretical studies, no comprehensive theory has been developed, and most generalizations are based on empirical or semiempitical equations. 

Other correlations based partially on theoretical considerations but made to fit existing data also exist (71—75). A number of researchers have also attempted to separate from a by measuring the latter, sometimes in terms of the wetted area (76—78). Finally, a number of correlations for the mass transfer coefficient itself exist. These ate based on a mote fundamental theory of mass transfer in packed columns (79—82). Although certain predictions were verified by experimental evidence, these models often cannot serve as design basis because the equations contain the interfacial area as an independent variable. 

Pulsed Columns. The efficiency of sieve-plate or packed columns is increased by the appHcation of sinusoidal pulsation to the contents of the column. The weU-distributed turbulence promotes dispersion and mass transfer while tending to reduce axial dispersion in comparison with the unpulsed column. This leads to a substantial reduction in HETS or HTU values. 

Gas Handling. The reactants are often gaseous under ambient conditions. To maximize the rate of the catalytic reaction, it is often necessary to minimize the resistance to gas—Uquid mass transfer, and the gases are therefore introduced as swarms of bubbles into a weU-stirred Hquid or into devices such as packed columns that faciHtate gas—Hquid mixing and gas absorption. 

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. 

In 1966, in a paper that now is considered a classic, Danckwerts and Gillham [Tmns. Inst. Chem. Eng., 44, T42 (1966)] showed that data taken in a small stirred-ceU laboratoiy apparatus could be used in the design of a packed-tower absorber when chemical reactions are involved. They showed that if the packed-tower mass-transfer coefficient in the absence of reaction (/cf) can be reproduced in the laboratory unit, then the rate of absorption in the l oratoiy apparatus will respond to chemical reactions in the same way as in the packed column even though the means of agitating the hquid in the two systems might be quite different. 

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... 

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-... 

Mass-Transfer Contact Section Where there is a strong possi-bihty that not all of the incoming vapors will be condensed in the pool, a direct-contact mass-transfer section is superimposed on the quench tank. This can be a baffle-tray section (as shown in Fig. 26-21) or a packed column sec tiou. 

The dispersion of a solute band in a packed column was originally treated comprehensively by Van Deemter et al. [4] who postulated that there were four first-order effect, spreading processes that were responsible for peak dispersion. These the authors designated as multi-path dispersion, longitudinal diffusion, resistance to mass transfer in the mobile phase and resistance to mass transfer in the stationary phase. Van Deemter derived an expression for the variance contribution of each dispersion process to the overall variance per unit length of the column. Consequently, as the individual dispersion processes can be assumed to be random and non-interacting, the total variance per unit length of the column was obtained from a sum of the individual variance contributions. 

It is seen that, for GC packed columns operated under the conditions assumed, the two factors contributing to dispersion by resistance to mass transfer are of the same order of magnitude. Consequently, equations (20) and (21) cannot be simplified and must be used in their existing form for all optimization procedures using packed GC columns. If the conditions differ significantly from those assumed, then by using the same procedure the possibility of modifying expressions (20) and (21) can be reexamined. 

Now, it is of interest to determine if either the resistance to mass transfer term for the mobile phase or, the resistance to mass transfer term in the stationary phase dominate in the equation for the variance per unit length of a GC packed column. Consequently, taking the ratio of the two resistance to mass transfer terms (G)... 

The second type of mass-exchange units is the differential (or continuous) contactor. In this category, the two phases flow through the exchanger in continuous contact throughout without intermediate phase separation and recontacting. Examples of differential contactors include packed columns (Fig. 2.6), spray towers (Fig. 2.7), and mechanically agitated units (Fig. 2.8). 

The mass-exchange columns are assumed to be packed and have a depreciation period of three years. One-meter diameter columns are used. The following cost may be used ... 

For measuring the inert species, some of which are present in the majority of gases, the thermal-conductivity detector (TCD) is often the detector of choice for gas analyses. Since the TCD is a concentration detector and its sensitivity is lower than that of mass-flow detectors such as the flame-ionization detector (FID), relatively high concentrations of compounds in the carrier gas are needed. This means that packed columns, with their high loadability, are still quite popular for such analyses. 

It is concluded that gas bubble-columns exhibit mass-transfer rates of the same order of magnitude as packed columns at low liquid flow rates, and much higher mass-transfer rates at high liquid flow rates. The pressure drop across a bubble-column is much greater than that across packed columns of the same height. 

The mass-transfer rates obtainable across the gas-liquid interface are of nearly the same magnitude in the different operations. Bubble-column slurries exhibit rather higher transfer rates than conventional packed columns... 

Danckwerts et al. (D6, R4, R5) recently used the absorption of COz in carbonate-bicarbonate buffer solutions containing arsenate as a catalyst in the study of absorption in packed column. The C02 undergoes a pseudo first-order reaction and the reaction rate constant is well defined. Consequently this reaction could prove to be a useful method for determining mass-transfer rates and evaluating the reliability of analytical approaches proposed for the prediction of mass transfer with simultaneous chemical reaction in gas-liquid dispersions. 

A number of analytical techniques such as FTIR spectroscopy,65-66 13C NMR,67,68 solid-state 13 C NMR,69 GPC or size exclusion chromatography (SEC),67-72 HPLC,73 mass spectrometric analysis,74 differential scanning calorimetry (DSC),67 75 76 and dynamic mechanical analysis (DMA)77 78 have been utilized to characterize resole syntheses and crosslinking reactions. Packed-column supercritical fluid chromatography with a negative-ion atmospheric pressure chemical ionization mass spectrometric detector has also been used to separate and characterize resoles resins.79 This section provides some examples of how these techniques are used in practical applications. 

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