Efficiency parameter, column

The height equivalent to a theoretical plate, H, is that length of column that represents one theoretical plate, or one equilibration step. Obviously, the smaller the value of this parameter, the more efficient the column. The more theoretical plates packed into a length of column, the better the resolution. It is calculated by dividing the column length by N ... 

Figure 3.2. Column efficiency parameters used in Equa tion 1. See text for details.

Hence, resolution, a key criterion for HPLC column users, is maximized for a given mobile phase/stationary phase system by maximizing N. Therefore, even if researchers are inclined to measure h as their column efficiency parameter, manufacturers... 

The practical goal of most separations is not to achieve the greatest resolution possible, but rather to obtain sufficient resolution to separate all components in the shortest amount of time. To optimize for speed, the starting condition is that there is a minimum resolution requirement for the separation. Resolution is a function of three parameters column efficiency, or theoretical plates (N), selectivity (a), and the retention factor (k) ... 

In the classification scheme in Sec. 1.4.1, the first three entries under liquid-solid separation methods, i.e., ion-exchange, adsoiption, and sorbent extraction, all belong to column separation techniques. While in the batch approach, separations based on these principles may be performed either by static equilibration or by a column technique, online columns are invariably used in FI separations, both for convenience and efficiency. FI column separation systems based on different sorptive mechanisms do not differ strongly in the principles of system design and optimization of operational parameters. Therefore, the principles discussed in the following sections are generally applicable to the different approaches. 

Wen, E., Asiaie, R., and Horvdth, C., Dynamics of capillary electrochromatography n. Comparison of column efficiency parameters in microscale high-performance liquid chromatography and capillary electrochromatography, J. Chromatogr. A, 855, 349,1999. 

This parameter is used to compare the relative column efficiencies for columns having packing materials with different particle size. 

Equations 12.21 and 12.22 contain terms corresponding to column efficiency, column selectivity, and capacity factor. These terms can be varied, more or less independently, to obtain the desired resolution and analysis time for a pair of solutes. The first term, which is a function of the number of theoretical plates or the height of a theoretical plate, accounts for the effect of column efficiency. The second term is a function of a and accounts for the influence of column selectivity. Finally, the third term in both equations is a function of b, and accounts for the effect of solute B s capacity factor. Manipulating these parameters to improve resolution is the subject of the remainder of this section. 

The required number of actual plates, A/p, is larger than the number of theoretical plates, because it would take an infinite contacting time at each stage to estabhsh equihbrium. The ratio is called the overall column efficiency. This parameter is difficult to predict from theoretical... 

Nonisothermal Gas Absorption. The computation of nonisothermal gas absorption processes is difficult because of all the interactions involved as described for packed columns. A computer is normally required for the enormous number of plate calculations necessary to estabUsh the correct concentration and temperature profiles through the tower. Suitable algorithms have been developed (46,105) and nonisothermal gas absorption in plate columns has been studied experimentally and the measured profiles compared to the calculated results (47,106). Figure 27 shows a typical Hquid temperature profile observed in an adiabatic bubble plate absorber (107). The close agreement between the calculated and observed profiles was obtained without adjusting parameters. The plate efficiencies required for the calculations were measured independendy on a single exact copy of the bubble cap plates installed in the five-tray absorber. 

The above approach will usually result in a conservative design, since the stage efficiency is usually much higher in the production column than in the pilot column. A comparison of the controlling parameters which exist in the pilot and production scales are depicted in Fig. 15-43. 

Column design involves the application of a number of specific equations (most of which have been previously derived and/or discussed) to determine the column parameters and operating conditions that will provide the analytical specifications necessary to achieve a specific separation. The characteristics of the separation will be defined by the reduced chromatogram of the particular sample of interest. First, it is necessary to calculate the efficiency required to separate the critical pair of the reduced chromatogram of the sample. This requires a knowledge of the capacity ratio of the first eluted peak of the critical pair and their separation ratio. Employing the Purnell equation (chapter 6, equation (16)). 

The smallest size difference that can be resolved is related to the pore volume, the solute shape, and the efficiency of the column (see Fig. 2.6). However, this is at very low loadings. At higher loadings the sample volume will contribute to zone broadening and may, in some cases, be the dominating factor for resolution. Thus, for fractionation, an optimum exists with respect to column efficiency (represented by the flow rate as operational parameter) and sample volume for processing a particular volume of feed per unit time. As a rule of thumb this optimum can be found at a relative sample volume of 2-5% of the column volume (Hagel et al., 1989). 

In order to achieve the best efficiency the SEC column should be operated at optimized operating parameters. The most important ones are flow rate [cf. van Deemter equation for band-broadening effects (21)], sample viscosity (depends on molar mass and concentration of the sample), and injection volume (7). 

One of the most important properties of a chromatographic column is the separation efficiency. A measure of this parameter could be the difference of the retention volume for two different compounds. The result of a GPC analysis is usually, however, only one large peak, and a separation into consecutive molar mass species is not possible. Additionally there is no standard for higher molar masses consisting only of a species that is truly monodisperse. Therefore, the application of the equation to the chromatographic resolution of low... 

Most size exclusion chromatography (SEC) practitioners select their columns primarily to cover the molar mass area of interest and to ensure compatibility with the mobile phase(s) applied. A further parameter to judge is the column efficiency expressed, e.g., by the theoretical plate count or related values, which are measured by appropriate low molar mass probes. It follows the apparent linearity of the calibration dependence and the attainable selectivity of separation the latter parameter is in turn connected with the width of the molar mass range covered by the column and depends on both the pore size distribution and the pore volume of the packing material. Other important column parameters are the column production repeatability, availability, and price. Unfortunately, the interactive properties of SEC columns are often overlooked. 

Traditionally, column efficiency or plate counts in column chromatography were used to quantify how well a column was performing. This does not tell the entire story for GPC, however, because the ability of a column set to separate peaks is dependent on the molecular weight of the molecules one is trying to separate. We, therefore, chose both column efficiency and a parameter that we simply refer to as D a, where Di is the slope of the relationship between the log of the molecular weight of the narrow molecular weight polystyrene standards and the elution volume, and tris simply the band-broadening parameter (4), i.e., the square root of the peak variance. 

Figures 9-63A and -63B illustrate for a specific packing the hydraulic flood and mass-transfer efficiency limitations. The differences in crimp height can influence the results. Figure 9-63B shows the effect of a higher flow parameter taken using larger columns the system apparendy was approaching its critical, but the cause of the performance is not yet known.

The column must be efficient enough to separate completely the condensation water from the volatile reactants which could be distilled off at the same time. If these conditions are observed the various experimental parameters can be kept constant from the beginning to the end of the reaction. 

Increasing the speed of analysis has always been an important goal for GC separations. All other parameters being equal, the time of GC separations can be decreased in a number of ways (1) shorten the column (2) increase the carrier gas flow rate (3) reduce the column film thickness (4) reduce the carrier gas viscosity (5) increase the column diameter and/or (6) heat the column more quickly. The trade-off for increased speed, however, is reduced sample capacity, higher detection limits, and/or worse separation efficiency. 

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