Stationary phases recommended

The stationary phases designated for the USP methods are listed in Table 2.8. Also listed are equivalent stationary phases recommended by other chromatographic suppliers. 

For the GPC separation mechanism to strictly apply, there must be no adsorption of the polymer onto the stationary phase. Such adsorption would delay elution of the polymer, thereby resulting in the calculation of too low a molecular weight for the polymer. The considerable variety of undesirable interactions between polymers and column stationary phases has been well reviewed for GPC by Barth (1) and this useful reference is recommended to the reader. Thus, the primary requirement for ideal GPC is that the solvent-polymer interaction be strongly thermodynamically favored over the polymerstationary phase interaction. 

Knox and Piper (13) assumed that the majority of the adsorption isotherms were, indeed, Langmuir in form and then postulated that all the peaks that were mass overloaded would be approximately triangular in shape. As a consequence, Knox and Piper proposed that mass overload could be treated in a similar manner to volume overload. Whether all solute/stationary phase isotherms are Langmuir in type is a moot point and the assumption should be taken with some caution. Knox and Piper then suggested that the best compromise was to utilize about half the maximum sample volume as defined by equation (15), which would then reduce the distance between the peaks by half. They then recommended that the concentration of the solute should be increased until dispersion due to mass overload just caused the two peaks to touch. 

The recommended mobile phase must assure a proper adsorption isotherm for a given stationary phase. Chapter 2 discusses the adsorption planar chromatography in the nonhnear region. 

Silica gel or alumina is usually used as the stationary phase. For these active phases a solvent of weak elution power is recommended for dissolution of the sample. A... 

Support( ) Stationary Phase(%w/w) Polarity Isothermal Recommended for Temperature the Separation Limit ( C) of ... 

Chemical surface modifications The first surface modification for the purpose of eliminating EOF and protein adsorption was recommended by Hjerten.28 The attachment of vinyl silanes allowed the polymerization of a variety of molecules to the surface. Most of the chemical modifications used for preparing capillaries for electrophoresis originated from the experience acquired over the years preparing GC and LC stationary phases. Chemical modification should conform to certain requirements, including the prevention of adsorption, the provision of stable and constant EOF over a wide pH range, chemical stability, ease of preparation, and reproduciblity of preparation. The effects of silanization of the inner surface of capillaries on electrophoretic separations have been extensively studied.26-29... 

Although cSFC shows relatively poor figures of merit (speed, sensitivity, detection dynamic range and sample capacity) as well as a limited application area, its applications tend to be unique. These include solutes that can be solvated with pure SCCO2 and quantified with FID. Linear density programs typical in cSFC are ideal for homologous series found in surfactants, many prepolymers, etc. Selectivity in cSFC, which can be achieved by mobile phase density and temperature programming, relies on selective interactions with the stationary phase. Quantitative analysis in cSFC may be rendered difficult by small injected volumes the use of internal standards is recommended. 

Certain specific problems arise with the use of alkylamine-substi-tuted stationary phases. Since amines are readily oxidized, degassing the mobile phase and avoiding solvents that may contain peroxides, e.g., diethyl ether and tetrahydrofuran, are recommended. Samples or impurities in the mobile phase containing ketone or aldehyde groups may... 

Burtiset al, 1987). Current gas chromatographs have the capability of very complex temperature programs that can minimize the time per run and maximize the resolution of the compounds of interest. The minimum and maximum temperatures are usually the only nonvariable parameters. The solvent usually determines the minimum temperature because it must be volatized for sample introduction. The maximum temperature is determined by the stationary phase, because it may break down at high temperatures, which can result in an elevated baseline of the chromatograph. Thus, the manufacturer recommends a maximum temperature to maximize column life and minimize breakdown. 

C is not recommended and high-temperature LC has not been rigorously explored. With the advent of thermally stable phases such as zir-conia-based stationary phases, temperatures in excess of 150°C can now be utilized. Many zirconia-based phases are available, so the stability of stationary phases is less of an issue. 

There is no recommendation of one of the introduced methods (MIP, BET, or ISEC) as the most accurate, reliable, and universally valid technique for the determination of the porous properties of a stationary phase. MIP, BET, and ISEC have rather to be regarded as three independent methodologies, those results complement one another to yield a precise estimation of the porosity of an investigated column packing. The most important characteristics, limitations, and methodological strengths of MIP, BET, and ISEC are intended to be discussed in this section. 

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