Separation techniques, organic

Phase Separation. Microporous polymer systems consisting of essentially spherical, intercoimected voids, with a narrow range of pore and ceU-size distribution have been produced from a variety of thermoplastic resins by the phase-separation technique (127). If a polyolefin or polystyrene is insoluble in a solvent at low temperature but soluble at high temperatures, the solvent can be used to prepare a microporous polymer. When the solutions, containing 10—70% polymer, are cooled to ambient temperatures, the polymer separates as a second phase. The remaining nonsolvent can then be extracted from the solid material with common organic solvents. These microporous polymers may be useful in microfiltrations or as controlled-release carriers for a variety of chemicals. 

It is the determination of volatile organic compounds produced from natural products that requires separation techniques that allow isolation of stereoisomers. The most commonly determined groups are the terpene and sesquiterpene species present in essential oils, which are used as key indicators of biological factors such as the growth season, geographic location, climate, etc. These species are also released directly into the atmosphere by very many plants and trees, and make a substantial contribution to global biogeochemical cycles. 

One example of normal-phase liquid chromatography coupled to gas chromatography is the determination of alkylated, oxygenated and nitrated polycyclic aromatic compounds (PACs) in urban air particulate extracts (97). Since such extracts are very complex, LC-GC is the best possible separation technique. A quartz microfibre filter retains the particulate material and supercritical fluid extraction (SPE) with CO2 and a toluene modifier extracts the organic components from the dust particles. The final extract is then dissolved in -hexane and analysed by NPLC. The transfer at 100 p.1 min of different fractions to the GC system by an on-column interface enabled many PACs to be detected by an ion-trap detector. A flame ionization detector (PID) and a 350 p.1 loop interface was used to quantify the identified compounds. The experimental conditions employed are shown in Table 13.2. 

Separation technique Time Organic phase vol source aqueous phase vol pH of source phase Transported metal ions Figure no. 

Separation techniques may have to be applied if the given sample contains substances which act as interferences (Section 21.10), or, as explained above, if the concentration of the element to be determined in the test solution is too low to give satisfactory absorbance readings. As already indicated (Section 21.10), the separation methods most commonly used in conjunction with flame spectrophotometric methods are solvent extraction (see Chapter 6) and ion exchange (Chapter 7). When a solvent extraction method is used, it may happen that the element to be determined is extracted into an organic solvent, and as discussed above it may be possible to use this solution directly for the flame photometric measurement. 

Flocculation or clarification processes are solids-liquid separation techniques used to remove suspended solids and colloidal particles such as clays and organic debris from water, leaving it clear and bright. Certain chemicals used (such as alums) also exhibit partial dealkaliz-ing properties, which can be important given that the principal alkaline impurity removed is calcium bicarbonate—the major contributory cause of boiler and heat exchanger scales (present in scales as carbonate), although closely followed by phosphate. 

A fourth separation technique employs charcoal. Charcoal has adsorption characteristics such that most organic molecules will adhere to its surface. However, charcoal is also very porous, thereby allowing smaller molecules to enter into its pores and become trapped in them. The charcoal is first coated with dextran or hemoglobin which covers its outer surface. 

The strategy of using two phases, one of which is an aqueous phase, has now been extended to fluorous . systems where perfluorinated solvents are used which are immiscible with many organic reactants nonaqueous ionic liquids have also been considered. Thus, toluene and fluorosolvents form two phases at room temperature but are soluble at 64 °C, and therefore,. solvent separation becomes easy (Klement et ai, 1997). For hydrogenation and oxo reactions, however, these systems are unlikely to compete with two-phase systems involving an aqueous pha.se. Recent work of Richier et al. (2000) refers to high rates of hydrogenation of alkenes with fluoro versions of Wilkinson s catalyst. De Wolf et al. (1999) have discussed the application and potential of fluorous phase separation techniques for soluble catalysts. 

Both IC and CE are separation techniques used to examine aqueous samples for anions, cations and trace levels of organic acids. CE produces separations by a different mechanism than IC, and produces sharper peaks. Therefore, CE can easily perform some separations that are difficult by IC. The determination of inorganic anions by IC and CE was compared [841],... 

Principles and Characteristics Mass-spectral analysis methods may be either indirect or direct. Indirect mass-spectral analysis usually requires some pretreatment (normally extraction and separation) of the material, to separate the organic additives from the polymers and inorganic fillers. The mass spectrometer is then used as a detector. Direct mass-spectrometric methods have to compete with separation techniques such as GC, LC and SFC that are more commonly used for quantitative analysis of polymer additives. The principal advantage of direct mass-spectrometric examination of compounded polymers (or their extracts) is speed of analysis. However, quite often more information can be... 

Tzschucke, C.C., Markert, C., Bannwarth, W., Roller, S., Hebei, A. and Haag, R. (2002) Modern separation techniques for the efficient workup in organic synthesis. Angewandte Chemie International Edition, 41 (21), 3964-4000. 

Purify the biotinylated protein or molecule using dialysis or gel filtration. For small molecule biotinylation where these separation methods may not be appropriate, other procedures may have to be developed, such as reverse-phase chromatography or organic precipitation techniques. 

---