Fractionation methods adsorption column

Its principles include polar extraction with acetone-water (2 1, v/v), homogeneous partitioning of the target molecules into an organic solvent, GPC cleanup on Bio-Beads, fractionation by adsorption column chromatography on silica gel (Si02) deactivated with 1.5% water and finally GC with various selective detection methods (NPD, BCD, FPD). 

Few analytical methods are available for the determination of total petroleum hydrocarbons in biological samples, but analytical methods for several important hydrocarbon components of total petroleum hydrocarbons may be modified. Most involve solvent extraction and saponification of lipids, followed by separation into aliphatic and aromatic fractions on adsorption columns. Hydrocarbon groups or target compounds are determined by gas chromatography-flame ionization or... 

In this study the USBM-API separation procedure was modified slightly. Monoaromatic and diaromatic compound types were eluted with specific solvents from an adsorption column. A three- to four-ring aromatic fraction was also desorbed with a stronger eluant. These fractions were separated on the basis of the carbon number of alkyl substituents by GPC. The subfractions obtained from LC and GPC separations were analyzed by mass spectroscopy. This technique provides a method of determining the chemical structure of coal liquids, which is complementary to NMR techniques (9). 

From amongst the numerous applications of adsorption column chromatography, an interesting example is provided by the separation of a mixture of two enantiomers into its constituents whose separation cannot be carried out by the other usual physical methods like fractional crystallization or fractional distillation. A well-known illustration of the separation of enantiomers without their having to be converted into diastereoisomers by chemical reaction with optically active acids is the resolution of Troger s base, effected by V. Prelog and P. Wieland in 1944,... 

The method described by Teichman et al. [15] and discussed in section 9.1.1.2 for the determination of chlorinated insecticides and PCBs in soils has also been applied to sediments. The procedure involves adsorption chromatography on alumina and charcoal, elution with increasing fractional amounts of hexane on alumina columns, and with acetonediethyl ether and benzene on charcoal columns. The polychlorobiphenyl and pesticides are then determined by gas chromatography on the separate elutes without interference. 

The development of adsorption as a method of fractionation has been analogous to the development of distillation. In both cases the operation was originally carried out in a simple batch unit. After many years, rectification was added and close fractionation became possible. In the case of distillation this was done by adding a packed or bubble plate column to the still kettle. In the case of adsorption it involved the use of an adsorbent-packed column to obtain chromatographic separation, which gave a rectification effect. 

---