Packed columns elevated temperatures

A fourth factor is the flow rate of the eluent (mobile phase). A too high rate decreases resolution because there is no time for molecules to diffuse into the pores of the matrix. In contrast, a very slow migration of solvent decreases the resolution by remixing the components by diffusion. The effect of diffusion is minimized if the chromatography is done at low temperature. If short separation times are necessary, pre-packed columns, elevated pressure, or HPLC columns are indispensable. 

Adsorbers, distillation colunuis, and packed lowers are more complicated vessels and as a result, the potential exists for more serious hazards. These vessels are subject to tlie same potential haz. uds discussed previously in relation to leaks, corrosion, and stress. However, llicse separation columns contain a wide variety of internals or separation devices. Adsorbers or strippers usually contain packing, packing supports, liquid distributors, hold-down plates, and weirs. Depending on tlie physical and chemical properties of the fluids being passed tlirough tlie tower, potential liazards may result if incompatible materials are used for llie internals. Reactivity with llie metals used may cause undesirable reactions, which may lead to elevated temperatures and pressures and, ullinialely, to vessel rupture. Distillation columns may contain internals such as sieve trays, bubble caps, and valve plates, wliicli are also in conlacl with tlie... 

SFC-NMR is available from 200 to 800 MHz, and is suitable for all common NMR-detected nuclei. SFC/SFE-NMR requires dedicated probe-heads for high pressure (up to 350 bar) and elevated temperature (up to 100 °C). SFC-NMR is carried out with conventional packed columns, using modifier, pressure and temperature gradients. The resolution of 1H NMR spectra obtained in SFE-NMR and SFC-NMR coupling under continuous-flow conditions approaches that of conventionally recorded NMR spectra. However, due to the supercritical measuring conditions, the 111 spin-lattice relaxation times 7) are doubled. 

Another approach to increase HPLC speed is the use of higher temperatures. The viscosity of a typical mobile phase used in reversed-phase separation decreases as the column temperature is increased. This allows an HPLC system to operate at a higher flow rate without suffering too much from increased back pressure. Zirconia-based packing materials provide excellent physical and chemical stability. They have been used successfully for high-throughput bioanalysis at elevated temperatures.9... 

The stability of zirconia and zirconia-based packings also allows the use of these columns at an elevated temperature. The key advantage of this is the reduction in analysis time due to the reduction in the viscosity of the mobile phase. In addition, the much broader temperature range also permits a fine-tuning of the selectivity of a separation compared with silica-based packings. 

The first gas chromatographic enantiomer separation on a cyclodextrin-based stationary phase was that of the apolar, racemic hydrocarbons a- and /i-pinenc and cis- and trans-pinane on packed columns coated with native a-cyclodextrin dissolved in formamide157. Very soon, it was recognized that alkylated cyclodextrins can be employed in capillary columns for high-resolu-tion enantiomer analysis. Thus, molten permethylated /(-cyclodextrin, hcptakis(2,3,6-tri-0-methyl)-/ -cyclodextrin (Table 2), was used158- 160 at elevated temperatures. 

Do not try to open or repack polymeric columns. They are usually under some pressure and come out of the tube like toothpaste. The column is of no use. Polymeric columns are usually packed in one solvent, then switched to a second solvent, which causes the packing to swell and squeeze out voids. They are then designed to be run in the second solvent. Polymeric ion exchangers are usually run at elevated temperature. This serves two purposes it decreases mobile phase viscosity, thereby reducing operating pressures, and it speeds... 

On the other hand, the lack of internal pore structure with micropellicular sorbents is of distinct advantage in the analytical HPLC of biological macromolecules because undesirable steric effects can significantly reduce the efficiency of columns packed with porous sorbents and also result in poor recovery. Furthermore, the micropellicular stationary phases which have a solid, fluid-impervious core, are generally more stable at elevated temperature than conventional porous supports. At elevated column temperature the viscosity of the mobile phase decreases with concomitant increase in solute diffusivity and improvement of sorption kinetics. From these considerations, it follows that columns packed with micropellicular stationary phases offer the possibility of significant improvements in the speed and column efficiency in the analysis of proteins, peptides and other biopolymers over those obtained with conventional porous stationary phases. In this paper, we describe selected examples for the use of micropellicular reversed phase... 

In contrast to some other procedures, the UV photoinitiated polymerization does not require elevated temperature for the reaction to be completed. Therefore, the mobile phase used for packing remains in both the outlet frit and the packing during polymerization of the inlet frit. Consequently, the conditioning time for the column prior to its use is shortened significantly. No bubble formation was observed while using packed capillary columns with photopolymer frits. 

One of the greatest hurdles for the application of biocatalysis is the need to operate processes under conditions that can differ dramatically from those in which the enzymes evolved. Many techniques are used in order to preserve catalytic activity and minimize the costs associated with the biocatalyst. In cases where the cost of the biocatalyst is a concern, an enzyme might be immobilized and used in a packed column or a fluidized bed reactor so as to enable reuse. Here also the enzyme must be stable for extended periods and may even be used under nonaqueous conditions and elevated temperatures. Recombinant technology has revolutionized the applications of biocat-... 

One of the popular methods for evaluating effective diffusivities in heterogeneous catalysts is based on gas chromatography. A carrier gas, usually helium, which is not adsorbed, is passed continuously through a column packed with catalyst. A pulse of a diffusing component is injected into the inlet stream and the effluent pulse recorded. The main advantages of this transient method are its applicability to particles of arbitrary shapes, and that experiments can be carried out at elevated temperatures and pressures. Haynes [1] has given a comprehensive review of this method. 

A procedure was developed by Hiatt (1983) and Dreisch and Munson (1983) to identify and quantify 1,1-dichloroethane in fish tissue samples by GC/MS, employing a fused-silica capillary column (FSCC) and vacuum distillation (extraction). An advantage of the vacuum extraction is that the system does not require elevated temperatures or the addition of reagents, which could produce unwanted degradation products (Hiatt 1981). The FSCC provides a more attractive approach than packed column for chromatographic analysis of volatile organic compounds, because FSCC can be heated to a higher-temperature (350°C) than that recommended for packed column thereby... 

The packing, or solid support in a packed column, serves to hold the liquid stationary phase in place so that as large a surface area as possible is exposed to the mobile phase. The ideal support consists of small, uniform, spherical particles with good mechanical strength and a specific surface area of at least 1 mVg. In addition, the material should be inert at elevated temperatures and be uniformly wetted by the liquid phase. No substance that meets all these criteria perfectly is yet available. 

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