Theoretical plate types

NTU (Number of Transfer Units) The NTU required for a given separation is closely related to the number of theoretical stages or plates required to cariy out the same separation in a stagewise or plate-type apparatus. For equimolal counterdiffusion, such as in a binary distillatiou, the number of overall gas-phase transfer units Nqg required for changing the composition of the vapor stream from yi to yo is... 

The plate to plate type calculation is a fundamental procedure wherein the tower is assumed to be composed of theoretical equilibrium plates. The actual plates required are determined from the number of theoretical plates using a predicted overall tower efficiency. The starting point for a tower calculation is usually a specified feed composition, feed temperature, and tower operating pressure. The procedure involves defining the compositions and temperamres on each plate in the tower and subsequently the resultant compositions and temperatures of the product streams. The actual computations, which involve trial... 

Column type Bed volume (ml) Column dimension (i.d. X L) (cm x cm) Column material" (tube/frit) Column fittings (inlet/outlet) Theoretical plates (N/m) Maximum operating pressure/flow rate (kPa)/(ml/min)... 

Column type Column size (mm) Theoretical plate number Particle size (/im) Pore size (A) Maximum flow rate (ml/min) Maximum pressure (kgffcm ) Maximum temperature (°C) Exclusion limit ... 

Column type Column size (mm) Theoretical plate number Range Flow rate (ml/min) Max Analytical column... 

Additional factors influencing column performance are the type and quality of the packing process, which mainly determines the theoretical plate count (N) of the column. In contrast to HPLC columns the efficiency of the separation itself is determined predominantly by the quality of the sorbent alone (pore... 

The selection of the column type is mainly determined by the composition of the sample. In general open-tubular (capillary) columns are preferred for low-density (gas-like) SFC, whereas packed columns are most useful for high-density (liquid-like) SFC. Open-tubular columns can provide a much larger number of theoretical plates than packed columns for the same pressure drop. Volumetric flow-rates are much higher in packed column SFC (pSFC) than in open-tubular column SFC (cSFC), which makes injection and flow control less problematic. 

A particular column can be used for different types of LC by changing the eluent components. For example, a column packed with RP-18 bonded silica gel can be used for SEC with THF, NPLC with n-hexane, and RPLC with aqueous acetonitrile. When separation cannot be achieved by improving the theoretical plate number of a column, it may be achieved by selection of an appropriate stationary phase material and/or eluent. 

As with distillation, the correlation for overall tray efficiency for absorbers, given in Equation 10.7, should only be used to derive a first estimate of the actual number of trays. More elaborate and reliable methods are available, but these require much more information on tray type and geometry and physical properties. If the column is to be packed, then the height of the packing is determined from Equation 9.64. As with distillation, the height equivalent of a theoretical plate (HETP) can vary... 

Correlation was found between domain size and attainable column efficiency. Column efficiency increases with the decrease in domain size, just like the efficiency of a particle-packed column is determined by particle size. Chromolith columns having ca. 2 pm through-pores and ca. 1pm skeletons show H= 10 (N= 10,000 for 10 cm column) at around optimum linear velocity of 1 mm/s, whereas a 15-cm column packed with 5 pm particles commonly shows 10,GOO-15,000 theoretical plates (7 = 10—15) (Ikegami et al., 2004). The pressure drop of a Chromolith column is typically half of the column packed with 5 pm particles. The performance of a Chromolith column was described to be similar to 7-15 pm particles in terms of pressure drop and to 3.5 1 pm particles in terms of column efficiency (Leinweber and Tallarek, 2003 Miyabe et al., 2003). Figure 7.4 shows the pressure drop and column efficiency of monolithic silica columns. A short column produces 500 (1cm column) to 2500 plates (5 cm) at high linear velocity of 10 mm/s. Small columns, especially capillary type, are sensitive to extra-column band... 

The fractionating column was of the Whitmore-Lux type 1 2 and had about 14 theoretical plates. The packed section was 37 by 1.1 cm. (o.d.) and was packed with %2-in- single-turn glass helices. The distilling flask was a 200-ml. round-bottomed flask. A metal bath or the oil bath described in Note 4 may be used for heating. 

Unfortunately, the fractionating column you usually get is not a bubble-plate type. You have an open tube that you fill with column packing (see Class 3 Fractional Distillation ) and noplates. The distillations up this type of column are not discreet, and the question of where one plate begins and another ends is meaningless. Yet, if you use this type of column, you do get a better separation than if you used no column at all. It s as if you had a column with some bubble-plates. And if your distilling column separates a mixture as well as a bubble-plate column with two real plates, you must have a column with two theoretical plates. 

Packed columns are still used extensively, especially in routine analysis. They are essential when sample components have high partition coefficients and/or high concentrations. Capillary columns provide a high number of theoretical plates, hence a very high resolution, but they cannot be used in all applications because there are not many types of chemically bonded capillary columns. Combined use of packed columns of different polarities often provides better separation than with a capillary column. It sometimes happens that a capillary column is used as a supplement in the packed-column gas chromatography. It is best, therefore, to house the capillary and packed columns in the same column oven and use them selectively. In the screening of some types of samples, the packed column is used routinely and the capillary column is used when more detailed information is required. 

HPTLC is conducted on TLC plates which are coated with purified silica gel with a particle range of 2-10 fjm as opposed to 2-25 jum for standard commercial TLC plates. The narrower particle size range means that a greater number of theoretical plates are available for separation and thus the spots on the TLC plate remain tighter. These type of plates may be run in a standard type of TLC tank but optimal performance is obtained from horizontal development of the plates using apparatus of the type shown in Figure 13.10. 

The NTU required for a given separation is closely related to the number of theoretical stages or plates required to carry out the same separation in a stage-wise or plate-type apparatus. 

Otherwise expressed, the number of theoretical plates required for a given separation increases when the reflux ratio is decreased, i.e. when the amount of condensed vapour returned to the column is decreased and the amount distilled off becomes greater. The variation in the reflux ratio is achieved by the use of a suitable take-off head (or still-head), usually of the total condensation variable take-off type. In use, all the vapour is condensed and the bulk of the condensate is returned to the fractionating column, small fractions of the condensate being allowed to collect in a suitable receiver. The design may be appreciated from the line diagram shown in Fig. 2.107 in which the controlled collection of distillate is by the socket-cone screw-operated valve sited just below the condenser drip end. 

Apart from the above-discussed parameters for HPLC optimization of chiral resolution on antibiotic CSPs, some other HPLC conditions may be controlled to improve chiral resolution on these CSPs. The effect of the concentrations of antibiotics (on stationary phase) on enantioresolution varied depending on the type of racemates. The effect of the concentrations of teicoplanin has been studied on the retention (k), enantioselectivity (a), resolution (Rs), and theoretical plate number (N) for five racemates [21]. An increase in the concentration of teicoplanin resulted in an increase of a and Rs values. The most surprising fact is that the theoretical plate number (N) increases with the increase in the concentration of teicoplanin. It may be the result of the resistance of mass transfer resulting from analyte interaction with free silanol and/or the linkage chains (antibiotics linked with silica gel). This would tend to trap an analyte between the silica surface and the bulky chiral selector adhered to it. This is somewhat... 

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