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Phase systems, chromatographic

It is clear that the separation ratio is simply the ratio of the distribution coefficients of the two solutes, which only depend on the operating temperature and the nature of the two phases. More importantly, they are independent of the mobile phase flow rate and the phase ratio of the column. This means, for example, that the same separation ratios will be obtained for two solutes chromatographed on either a packed column or a capillary column, providing the temperature is the same and the same phase system is employed. This does, however, assume that there are no exclusion effects from the support or stationary phase. If the support or stationary phase is porous, as, for example, silica gel or silica gel based materials, and a pair of solutes differ in size, then the stationary phase available to one solute may not be available to the other. In which case, unless both stationary phases have exactly the same pore distribution, if separated on another column, the separation ratios may not be the same, even if the same phase system and temperature are employed. This will become more evident when the measurement of dead volume is discussed and the importance of pore distribution is considered. [Pg.28]

Having established that a finite volume of sample causes peak dispersion and that it is highly desirable to limit that dispersion to a level that does not impair the performance of the column, the maximum sample volume that can be tolerated can be evaluated by employing the principle of the summation of variances. Let a volume (Vi) be injected onto a column. This sample volume (Vi) will be dispersed on the front of the column in the form of a rectangular distribution. The eluted peak will have an overall variance that consists of that produced by the column and other parts of the mobile phase conduit system plus that due to the dispersion from the finite sample volume. For convenience, the dispersion contributed by parts of the mobile phase system, other than the column (except for that from the finite sample volume), will be considered negligible. In most well-designed chromatographic systems, this will be true, particularly for well-packed GC and LC columns. However, for open tubular columns in GC, and possibly microbore columns in LC, where peak volumes can be extremely small, this may not necessarily be true, and other extra-column dispersion sources may need to be taken into account. It is now possible to apply the principle of the summation of variances to the effect of sample volume. [Pg.194]

A satisfactory chromatographic analysis demands, a priori, on an adequate separation of the constituents of the sample that will permit the accurate quantitative evaluation of each component of interest. To achieve this, an appropriate phase system must be chosen so that the individual components of the mixture will be moved apart from one another in the column. In addition, their dispersion must be constrained sufficiently to allow all the solutes of interest to be eluted discretely. At this stage it is necessary to introduce the concept of the Reduced Chromatogram. [Pg.361]

Whether the optimum phase system is arrived at by a computer system, or by trial and error experiments (which are often carried out, even after computer optimization), the basic chromatographic data needed in column design will be... [Pg.364]

It has been shown that, in LC, the size of the distribution coefficient of a solute between the two phases determines the extent of its retention. As a consequence, the difference between the distribution coefficients of two solutes establishes the extent of their separation. The distribution coefficients are controlled by the nature and strength of the molecular interactions that takes place between the solutes and the two phases. Thus it is the choice of the phase system that primarily determines the separation that is achieved by the chromatographic system. [Pg.93]

The purpose of this final chapter is to provide the analyst with a background of practical examples to aid in the selection of, firstly, the best chromatographic method and, secondly, the best phase system when faced with an hitherto unknown sample for analysis. The literature is rich with LC applications and frequently publications are available for the separation of closely similar mixtures to that of the sample. It is unlikely, however, that the chromatographic conditions for the actual separation required will be available and, even if they are, the conditions reported may well not be optimum. This is more likely to be true for those applications that are described in earlier publications. Nevertheless, conditions that have be successfully employed for related separations may certainly help to identify those conditions necessary for the sample supplied for assay. [Pg.281]

Chromatographic characterisation of hydrolysis products Hydrolysis products from sodium polypectate were analysed by thin-layer chromatography on silica gel G-60, using ethyl acetate / acetic acid / formic acid / water (9 3 1 4, by volume) as the mobile phase system. Sugars were detected with 0,2% orcinol in sulphuric add-methanol (10 90ml) [14]. [Pg.788]

Apart from the choice of an appropriate stationary and mobile phase, the essential problem for PLC is to attain equilibrium in a three-phase system — between the stationary, mobile, and gas phases. In a nonequilibrated system, the velocity of the mobile phase in a thicker layer (i.e., the effect of solvent evaporation) is less in a lower part of an adsorbent. Such a situation leads to the diffusion of bands and deterioration of the adjacent bands separation. This can be minimized or avoided by prerunning the plate with the mobile phase before spotting of the sample and the saturated chromatographic chambers. [Pg.259]

The choice of the chromatographic system depends on the chemical character of the extracts being separated. The mobile phase should accomplish all requirements for PLC determined by volatility and low viscosity, because nonvolatile components (e.g., ion association reagents and most buffers) should be avoided. It means that, for PLC of plant extracts, normal phase chromatography is much more preferable than reversed-phase systems. In the latter situation, mixtures such as methanol-ace-tonitrile-water are mostly used. If buffers and acids have to be added to either the... [Pg.259]

De Jong, G. J. Optimization and characterization of silica-based reversed-phase liquid chromatographic systems for the analysis of basic pharmaceuticals./. Chromatogr. A 2000, 897,1-22. [Pg.351]

Gilpin, R. K., Jaroniec, M., and Lin, S., Dependence of the methylene selectivity on the composition of hydro-organic eluents for reversed-phase liquid chromatographic systems with alkyl bonded phases, Chromatographia, 30,393, 1990. [Pg.192]

Jandera, P., Holcapek, M., Theodoridis, G. (1998). Investigation of chromatographic behavior of alcohol ethoxylate surfactants in normal-phase and reversed-phase systems using high-performance liquid chromatography-mass spectrometry. J. Chromatogr. A 813(2), 299-311. [Pg.444]

Wei JQ, Wei JL, Zhou XT. 1990. Optimization of an isocratic reversed phase liquid chromatographic system for the separation of fourteen steroids using factorial... [Pg.192]

Uf course, the enhancement of chromatographic selectivity by secondary chemical equilibria is neither new nor confined to reversed-phase systems. Most widespread probably has been the exploitation of protonic equilibria by appropriately ati usting the pH of the eluent so that the degree of ionization of the eluite is altered. Generally the ionized and neutral forms of an eluite are retained differently (2( 7. 208). Formation of metal complexes of certain eluites has also been utilized for modulating retention behavior for higher selectivity. [Pg.118]

It is seen that the separation ratio is independent of all column parameters and depends only on the nature of the two phases and the temperature. Thus providing th sam phase system is used on two columns, and the solutes are chromatographed at the same temperature, then the two solutes will have the same separation ratio on both columns, The separation ratio will be independents the phase ratios of the two columns and the flow-rates. It follows, that the separation ratio of a solute can be used reliably as a means of solute identification. ... [Pg.26]

It can be clearly seen from equation (9) that the expression for the retention volume of a solute, although generally correct, is grossly over simplified if accurate measurements of retention volumes are required Some of the stationary phase may not be chromatographically available and not all the pore contents have the same composition as the mobile phase and, therefore, being static, can act as a second stationary phase. This situation is akin to the original reverse phase system of Martin and Synge where a dispersive solvent was absorbed Into the pores of support to provide a liquid/liquid system. As a consequence a more accurate form of the retention equation would be,... [Pg.30]

Whether the optimum phase system is arrived at by a computer system, or by trial and error experiments (which are often carried out, even after computer optimization), the basic chromatographic data needed in column design will be identified. The phase system will define the separation ratio of the critical pair, the capacity ratio of the first eluted peak of the critical pair and the capacity ratio of the last eluted peak. It will also define the viscosity of the mobile phase and the diffusivity of the solute in the mobile phase. [Pg.181]


See other pages where Phase systems, chromatographic is mentioned: [Pg.4]    [Pg.7]    [Pg.259]    [Pg.136]    [Pg.284]    [Pg.196]    [Pg.282]    [Pg.8]    [Pg.218]    [Pg.222]    [Pg.334]    [Pg.410]    [Pg.420]    [Pg.221]    [Pg.264]    [Pg.234]    [Pg.344]    [Pg.157]    [Pg.568]    [Pg.717]    [Pg.313]    [Pg.377]    [Pg.203]    [Pg.12]    [Pg.29]    [Pg.130]    [Pg.150]    [Pg.538]    [Pg.5]    [Pg.329]    [Pg.601]    [Pg.21]   
See also in sourсe #XX -- [ Pg.176 , Pg.183 ]




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