Separations columns

Most often, the GPC separation process takes place in the gel bed packed into a straight column that is formed by a tube provided with column end fittings. Coiled columns show generally lower performances. 

The typical inner diameter of analytical gel chromatographic columns ranges from 2 to 8 mm. Recently, attempts were reported to apply packed capillary columns to gel chromatography. Preparative separations are performed in columns with diameters up to several decimeters. 

The length of the gel chromatographic column covers the range from 100 to about 2000 mm, usually from 500 to 1250 mm in conventional GPC, and from 250 to 350 mm in HP GPC. Very often, several columns packed with different gels are combined forming the column system so that appropriate calibration curve is obtained (Fig. 4.6.1). 

The most simple improvisation of the end part of a column of the first generation is shown in Fig. 4.6.7. In the modem column constructions, the gel is supported by special end fittings that can be divided into fixed (Fig. 4.6.8) and movable (piston- 

The dispersing medium for soft gels is the eluent, and both semirigid and rigid gels are packed from dispersing media chosen so that their density equals the density 

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Due to possible environmental problems with acetone, new technologies are being developed for the production of deoiled lecithins involving treatment of Hpid mixtures with supercritical gases or supercritical gas mixtures (10—12). In this process highly viscous cmde lecithin is fed into a separation column at several levels. The supercritical extraction solvent flows through the column upward at a pressure of 8 MPa (80 bar) and temperature between 40 and 55°C. The soy oil dissolves together with a small amount of lecithin. 

Only trace amounts of side-chain chlorinated products are formed with suitably active catalysts. It is usually desirable to remove reactive chlorides prior to fractionation in order to niinimi2e the risk of equipment corrosion. The separation of o- and -chlorotoluenes by fractionation requires a high efficiency, isomer-separation column. The small amount of y -chlorotoluene formed in the chlorination cannot be separated by fractionation and remains in the -isomer fraction. The toluene feed should be essentially free of paraffinic impurities that may produce high boiling residues that foul heat-transfer surfaces. Trace water contamination has no effect on product composition. Steel can be used as constmction material for catalyst systems containing iron. However, glass-lined equipment is usually preferred and must be used with other catalyst systems. 

Multiple Products. If each component of a multicomponent distillation is to be essentially pure when recovered, the number of columns required for the distillation system is N — 1, where AJ is the number of components. Thus, ia a five-component system, recovery of all five components as essentially pure products requires four separate columns. However, those four columns can be arranged ia 14 different ways (43). 

Figures 6.6 and 6.7 show the effect of a solvent separation column. In the case of Fig. 6.7, the upper part of the figure shows the chromatogram of polyvinyl chrolide, which contains dioctyl phthalate (DOP), using KF-806L. In this case, DOP is not separated from a solvent peak. However, DOP can be separated from the solvent peak using KF-800D in conjunetion with KF-806L (Table 6.6).

For production-scale separations, column diameters up to 30 cm are recommended. Usually the length of the column is in the range of 600-1200 mm for smaller column diameters (less than 50 mm). Columns with larger diameters can be packed up to 900 mm. 

Adsorbers, distillation colunuis, and packed lowers are more complicated vessels and as a result, the potential exists for more serious hazards. These vessels are subject to tlie same potential haz. uds discussed previously in relation to leaks, corrosion, and stress. However, llicse separation columns contain a wide variety of internals or separation devices. Adsorbers or strippers usually contain packing, packing supports, liquid distributors, hold-down plates, and weirs. Depending on tlie physical and chemical properties of the fluids being passed tlirough tlie tower, potential liazards may result if incompatible materials are used for llie internals. Reactivity with llie metals used may cause undesirable reactions, which may lead to elevated temperatures and pressures and, ullinialely, to vessel rupture. Distillation columns may contain internals such as sieve trays, bubble caps, and valve plates, wliicli are also in conlacl with tlie... 

Figure 2.6 Gas cluotnatograni of a 10 ml test sample containing C I4 C26 alkanes in -hexane (about 1 ppb each) the earner gas (H2) inlet pressure was 2.5 bar for a 22 m X 0.32 mm id separation column coupled with a 2 m X 0.32 mm id uncoated precolumn (no vapour exit). Reprinted from Journal of High Resolution Chromatography, 9, K. Grob et al., Concunent solvent evaporation for on-line coupled HPLC-HRGC , pp. 95-101, 1986, with peimission from Wiley-VCH.

MODES OF THE LMCS USING COUPLED SEPARATION COLUMNS... 

H.-G. Schmarx, A. Mosandl and K. Grob, Stereoisomeric flavour compounds. XXXVIII dkect chir ospecific analysis of y-lactones using on-line coupled EC-GC with a chkal separation column , Chromatographia 29 125-130 (1990). 

Figure 13.3 Schematic diagram of the parallel cryogenic trap MDGC-IR-MS system A, splitless injection port B, RC-5 non-polar first-stage separation column C, HP 5970B MSD D, HP 5965B IRD E, four-poit two-way valve (300 °C maximum temperature) F, external auxiliary earner gas G, six-poit selection valve (300 °C maximum temperature) H, stainless-steel cryogenic caps I, tliree-poit two- way valve (300 °C maximum temperature) ...

Figure 13.5 Schematic presentation of the procedure involved in coupled-column RPLC AS, autosampler C-1 and C-2, first and second separation columns, respectively M-1 and M-2, mobile phases S-1 and S2, interferences A, target analytes HV, high-pressure valve D, detector. Reprinted from Journal of Chromatography, A 703, E. A. Hogendoom and R van Zoonen, Coupled-column reversed-phase liquid cliromatography in environmental analysis , pp. 149-166, copyright 1995, with permission from Elsevier Science.

Abtreib(e) apparat, m. distilling apparatus, still, -herd, m. refining hearth. pelle, /. refining cupel, -kolonne, /. separating column, distilling column, -mittel, n. expulsive agent abortifacient,... 

Figure 8-4. A flow diagram for the hydration of propylene to isopropanol (1) propylene recovery column, (2) reactor, (3) residual gas separation column, (4) aqueous - isopropanol azeotropic distillation column, (5) drying column, (6) isopropyl ether separator, (7) isopropyl ether extraction.

In IC this problem of electrolyte background is overcome by means of eluant suppression. Thus in the above example of sodium and potassium analysis, if the effluent from the separating column is passed through a strong base anion exchange resin in the hydroxide form (suppressor column) the following two processes occur ... 

The low-concentration eluants used to separate the sample ions on the separator column allow a substantial number of samples (typically about 50) to be analysed before the suppressor column is completely exhausted. Clearly an important practical consideration is the need to minimise the frequency of regeneration of the suppressor column and, for this reason, the specific capacity of the column is made as large as possible by using resins of moderate to high cross-linking. Some instruments contain two suppressor columns in parallel,... 

The detector. The function of the detector, which is situated at the exit of the separation column, is to sense and measure the small amounts of the separated components present in the carrier gas stream leaving the column. The output from the detector is fed to a recorder which produces a pen-trace called a chromatogram (Fig. 9.1fr). The choice of detector will depend on factors such as the concentration level to be measured and the nature of the separated components. The detectors most widely used in gas chromatography are the thermal conductivity, flame-ionisation and electron-capture detectors, and a brief description of these will be given. For more detailed descriptions of these and other detectors more specialised texts should be consulted.67 69... 

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