Conditioning, packed columns

Water/waste water Extract with methylene chloride under alkaline and then acidic conditions Packed column GC/MS 1.6 pg/L 40-113 APHA 1992... 

The technology is based on the rapid equhibrium estabUshed between the reactants and products at high temperatures. The equhibrium shifts to the product side when potassium is removed continuously by distihation through a packed column. This process can produce high purity potassium metal. Appropriate adjustments of conditions give a wide range of potassium—sodium ahoys of specified compositions. 

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. 

Typical experimental values of HETP for a random packing such as 50-mm PaH rings, and a stmctured packing, such as Intalox 2T of Norton Co., under the same system conditions, are shown in Figure 25. Many designers of packed columns prefer the use of HETP instead of but the latter is more fundamental and discrirninates between Hquid- and vapor-phase resistances. It should be noted that terms such as H and N are based on... 

Packed Columns versus Plate Columns Packed columns are usually specified when plate devices would not be feasible because of undesirable fluid charac teristics or some special design requirement. Conditions favoring packed columns are ... 

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. 

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. 

Calculation of column diameter (for packed columns, this is usually based on flooding conditions, and, for plate columns, on the optimum gas velocity or the liquid-handling capacity of the plate)... 

The checkers purchased trifluoroacetic acid from Aldrich Chemical Company, Inc., and distilled it from phosphorous pentoxide. The submitters point out that some trifluoroacetic anhydride, whose effects have not been fully investigated, is obtained under these conditions. The submitters prefer to use trifluoroacetic acid which has been distilled through a glass packed column without the use of a drying agent. 

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. 

Katz et fl/.[l] searched the literature for data that could be used to identify the pertinent dispersion equation for a packed column in liquid chromatography. As a result of the search, no data was found that had been measured with the necessary accuracy and precision and under the sufficiently diverse solute/mobile phase conditions required to meet the second criteria given above. It became obvious that a... 

In the previous two chapters, equations were developed to provide the optimum column dimensions and operating conditions to achieve a particular separation in the minimum time for both packed columns and open tubular columns. In practice, the vast majority of LC separations are carried out on packed columns, whereas in GC, the greater part of all analyses are performed with open tubular columns. As a consequence, in this chapter the equations for packed LC columns will first be examined and the factors that have the major impact of each optimized parameter discussed. Subsequently open tubular GC columns will be considered in a similar manner. 

Table 1. Typical Chromatographic Operating Conditions for an LC Packed Column...

With soft gels, column packing has often been plagued with such problems as inferior reproducibility and excessive time requirements. These problems are alleviated with physically stable Toyopearl HW media. However, an improperly packed column can have significantly reduced efficiency. The two key variables for the successful packing of Toyopearl HW media, packing velocity and column size, have been evaluated to determine the optimal packing conditions. 

An on-line supercritical fluid chromatography-capillary gas chromatography (SFC-GC) technique has been demonstrated for the direct transfer of SFC fractions from a packed column SFC system to a GC system. This technique has been applied in the analysis of industrial samples such as aviation fuel (24). This type of coupled technique is sometimes more advantageous than the traditional LC-GC coupled technique since SFC is compatible with GC, because most supercritical fluids decompress into gases at GC conditions and are not detected by flame-ionization detection. The use of solvent evaporation techniques are not necessary. SFC, in the same way as LC, can be used to preseparate a sample into classes of compounds where the individual components can then be analyzed and quantified by GC. The supercritical fluid sample effluent is decompressed through a restrictor directly into a capillary GC injection port. In addition, this technique allows selective or multi-step heart-cutting of various sample peaks as they elute from the supercritical fluid... 

A weighed portion of the AOS sample is dissolved in water and ethanol containing a small amount of n-decane and the mixture is shaken with petroleum spirit. The organic phase is subjected to GC using a 2 m x 10 mm packed column of 5% carbowax 20M on Chromorb T applying the following conditions ... 

In a countercurrent packed column, n-butanol flows down at a rate of 0.25 kg/m2 s and is cooled from 330 to 295 K. Air at 290 K, initially free of n-butanol vapour, is passed up the column at the rate of 0.7 m /m2 s. Calculate the required height of tower and the condition of the exit air. 

Under these chromatographic conditions, the CS2 retention time is about 3 min on a fused-silica capillary column and about 2 min on a Teflon Chromosil 330 packed column. 

Instead of the packed column mentioned in Section 6.3, a megabore column may also be used for gas-chromatographic determination. The operating conditions are as follows ... 

Equation (I.IS) Is valid for open tubular columns under all normal conditions and for packed columns at low mobile phase velocities. The average carrier gas velocity is calculated from the outlet velocity by correcting the latter for the pressure drop across the column, and is simply given by u - ju, where j is the gas compressibility correction factor, defined In equation (1.2). 

Figure 1.17 Separation of large ring polycyclic aroaatic hydrocarbons extracted from carbon black on a 1.8 x 0.2 n I.D. fused silica capillary column packed with 3 micrometer spherical octadecylsllanized silica gel eluted with a stepwise solvent gradient at a flow rate of 1.1 mlcroliters/min with an inlet pressure of about 360 atmospheres. Under isocratic conditions this column yielded ca. 225,000 theoretical plates. (Reproduced with permission from ref. 238. Copyright Friedr. Vieweg t Sohn).

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