Separation of mixtures using

Barter, R.M. (1945) Separation of mixtures using zeolites as molecular sieves. I. Three classes of molecular-sieve zeolite./. Soc. Chem. Ind., 64, 130. 

R. DeBono, A. Grigoriev, R. Jackson, R. James, F. Kuja, A. Loveless, S. Nacson, A. Rudolph and Y. Sun, Separation of mixtures using gas chromatography coupled to ion mobility spectrometry, International Journal for Ion Mobihty Spectrometry 5(2) (2002) 194-201. 

As a rule of thumb, one can say that the efficiency of separation of mixtures and the simplicity of operating and maintaining apparatus are much greater for GC than for LC. Hence, other things being equal, GC is most often the technique of first choice and can be used with a very wide variety of compound types. However, for nonvolatile or thermally labile substances like peptides, proteins, nucleotides, sugars, carbohydrates, and many organometallics, GC may be ruled out completely... 

Prior separation of mixtures into individual components may not be needed. If the mass spectrometer is capable of MS/MS operation, one of the mass spectrometers is used to isolate individual ions according to m/z value (mass-to-charge ratio), and the other is used to examine their fragmentation products to obtain structural information. 

Chromatography A method of analysis using separation of mixtures based on selective adsorption. 

FIGURE 4.7 Separation of mixture of proteins and peptides on a TSK-GEL G2000SWxl column using Wyatt/Optilab DSP and miniDawn detectors. 

The separation of mixtures involving N-methyl-JLtetrahydropyridines into their pure components by means of gas-liquid chromatography was discussed in a report by Holik et al. (87). They found that, using tris(/3-cyanoethoxymethyl)-y-picoline as the stationary phase, the primary factors involved in the specific retention volumes of these enamines is the electronic effect of a methyl substituent and the nitrogen atom on the carbon-carbon double bond. It was observed that 1,3-dimethyl-Zl -tetrahydropyridine (141) has a smaller specific retention volume and, hence, is eluted before... 

Figure 15.4 Separation of mixtures of beta-blockers by using micellar HPLC, employing the following mobile phases (a) 0.12M SDS, 5% propanol, 0.5% tiiethylamine (b) 0.06 M SDS, 15% propanol (c) 0.1 IM SDS, 8% propanol. Adapted from Journal of Chromatographic Science, 37, S. Carda-Broch et al., Analysis of urine samples containing cardiovascular drugs by micellor liquid chromatography with fluorimetric detection , pp. 93-102, 1999, with permission from Preston Publications, a division of Preston Industries, Inc.

The use of heart-cuts to analyze a sample of 90% evaporated gasoline is illustrated in Figure 15.9. Each of the lettered chromatograms illustrates the further separation of mixture components which is not possible on a single column. The initial... 

Chromatography is a separation process employed for the separation of mixtures of substances. It is widely used for the identification of the components of mixtures, but as explained in Chapters 8 and 9, it is often possible to use the procedure to make quantitative determinations, particularly when using Gas Chromatography (GC) and High Performance Liquid Chromatography (HPLC). 

H- and 3//-Azepines are generally unstable in aqueous acid solution and the few examples of simple azepinium salts, namely perchlorates,77 bromides,105 picrates35201 and a solitary iodide,105 have been prepared under nonaqueous conditions. The fractional crystallization of oxalate salts has been used for the separation of mixtures of 4- and 6-substituted 3f/-azepines,66 and 3,6-di-tm-butyl- and 2,5-di-tert-butyl-3//-azepine, on treatment with tetrafluoroboric acid in acetonitrile, are converted quantitatively into their crystalline tetrafluoroboratc salts.70... 

Finally an example is included of the use of a Cl 8 reverse phase column. The packing is also a silica based but is contained in a short column 3.3 cm long, 4.6 mm in diameter and packed with particles 3 Jim in diameter. The example of its use is in the separation of mixture of growth regulators which is shown in figure 9. 

Ion chromatography can be used in unique ways and by appropriate modification can often be applied to the separation of mixtures where the components themselves do not ionize or do not normally produce interactive ions in aqueous solution. A good example of this type of separation is afforded by the analysis of saccharide mixtures using ion exchange interactions. An illustration of such a separation is given in figure 15. 

HPLC has proved to be fast and sensitive for the analyses of phenolic plant constit-nents, and is especially useful for the analysis of anthocyanins. The first application of HPLC to anthocyanin analyses was in 1975 by Manley and Shubiak and it has now become the method of choice for the separation of mixtures of anthocyanins and anthocyanidins. HPLC is now used for anthocyanin qualitative, quantitative, and preparative work, offering improved resolution compared to chromatographic procedures previously employed. It also allows for simultaneous rapid monitoring of the eluting anthocyanins. ... 

The same principle is used for the preparative separation of mixtures of biological materials, the extraction of different individual components from these mixtures, and their purification. In this case one uses an electrophoretic method with continued introduction of individual portions of the mixture and withdrawal of portions of pure fractions. There have been reports that such processes were accomplished in spacecraft where, since gravitational forces are absent, the liquid solutions can be used without the danger of natural convection. 

One of the most important problems of planar chromatography is that of the optimization of solvent systems for the separation of mixtures of different samples. An analyst is interested in obtaining the expected result using a minimum number of experiments. Snyder has introduced a new system for solvent classification that permits a logical selection of solvents both in term of polarity indices (F ) and selectivity parameters (Xj), proving theoretically the validity of such universal solvent systems [18,38,41,42]. 

The window diagram method can also be used to optimize the separation of mixtures when the number and identity of the components are unknown [421-423]. Two liquid phases, A and S, of different selectivity are chosen. Trial chromatograms are run on... 

GC/MS separation of mixtures of the compounds are usually performed on capillary columns with low and mid polarity and a length in the range of 30 50 m, with a total separation time of20 40 min, and temperature ramping from 40 to 300 °C. Total ion current (TIC) profiles are often obtained using ion trap or quadrupole analysers. Quantification is performed by selected-ion monitoring (SIM) detection using calibration curves. 

Hurme (1996) has used GA to solve the synthesis problem of the separation of mixture of hydrocarbons. He also compared GA with a pure random version in which the crossover and mutation operations were replaced by a procedure of random generation of new solutions. There was no difference during the first generations but it became significant after some generations. In this case GA reached the solution after ten generations with about 1100 different possible solutions, while the random version required tens of generations. GA seems to be both fast compared to random optimization and not too computationally intensive. 

One-dimensional multiple development and two-dimensional development Multiple developments through one or two dimensions can be applied to separate certain components in sequence, with detection at each step. This gives a theoretical increase in the capacity of the spots, so it is ideal for the separation of mixtures with a large number of components. In addition, it is a useful tool to confirm the purity of a given component. Though hyphenated HPLC could serve as a multiple separation technique, TLC takes the lead in this area by its faster separation and choice of different mobile phases and detection methods through each run. 

The chromatographic technique is important especially in initial separations of mixtures and in the final purification of compounds. However, owing to the limited amounts of substances which can be produced using such techniques, it would be desirable that, at some later stage, serious efforts aimed at developing better preparative routes to these clusters should be made. 

Analytical methods are ripe for attack using Al methods. Capillary electrophoresis is a routine separation technique, but like other separation techniques, its effectiveness is correlated strongly with experimental conditions. Hence it is important to optimize experimental conditions to achieve the maximum degree of separation. Zhang and co-workers41 studied the separation of mixtures in reserpine tablets, in which vitamin B1 and dibazolum may be incompletely separated, as may promethazine hydrochloride and chloroquine... 

Aromatic amines that have been used include o-toluidine, p-aminosali-cylic acid, p-aminobenzoic acid, diphenylamine and p-aminophenol. Their ability to react preferentially with a particular carbohydrate or class of carbohydrate is often useful, e.g. p-aminophenol, which shows some specificity for ketoses compared with aldoses and is useful for measuring fructose. These reagents have proved particularly useful for the visualization and identification of carbohydrates after separation of mixtures by paper or thin-layer chromatography, when colour variations and the presence or absence of a reaction aid the interpretation of the chromatogram. 

The ninhydrin colour reaction has proved very useful in qualitative work and is widely used in the visualization of amino acid bands after electrophoretic or chromatographic separation of mixtures. The reagent used in such circumstances is usually prepared in ethanol and, if 2,4,6-collidine is added, the variations in colour produced by different amino acids will aid their identification (Table 10.6). 

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