Capillaries coating methods

A number of developments have increased the importance of capillary electrophoretic methods relative to pumped column methods in analysis. Interactions of analytes with the capillary wall are better understood, inspiring the development of means to minimize wall effects. Capillary electrophoresis (CE) has been standardized to the point of being useful as a routine technique. Incremental improvements in column coating techniques, buffer preparation, and injection techniques, combined with substantive advances in miniaturization and detection have potentiated rugged operation and high capacity massive parallelism in analysis. 

The efficacy of CE separation depends considerably on the type of capillary. Fused-silica capillaries without pretreatment are used most frequently. Its outside is coated with a polymer layer to make it flexible and to lessen the occurrence of breakage. The polymer coating has to be dissolved with acid or burned away at the detection point. Capillaries with an optically transparent outer coating have also found application in CE. The objectives of the development of chemically modified capillary walls were the elimination of electro-osmotic flow and the prevention of adsorption on the inner wall of the capillary. Another method to prevent the adsorption of cationic analyses and proteins is the use of mobile phase additives. The modification of the pH of the buffer, the addition of salts, amines and polymers have all been successfully employed for the improvement of separation. 

The further development of chemicals and capillaries, coatings and consumables, and ready-to-use generic methods... 

The buffer used was CEofix Anions 5 (Analis Suarlee, Belgium), consisting of a PDC acid at pH 5.6 and a poly cation for capillary coating. The method was based on the standatd... 

CZE-ELD, with a Au microelectrode at —0.6 V vs. SSCE and a Pt wire as auxiliary electrode, using sodium borate buffer and dodecyltrimethylanunonium bromide for dynamic coating of the capillary internal surface, can be applied for separation and determination of ultra-trace amounts of many oxidizing substances. Thus, the concentration of peroxodisulfate (S208 ) and peroxomonosulfate (S05 ) ions in pickling baths can be monitored by this method. The faster emergence of the heavier peroxodisulfate ion is attributed to different adsorption of the two analyte ions by the capillary coating . ... 

Several different analytical and ultra-micropreparative CEC approaches have been described for such peptide separations. For example, open tubular (OT-CEC) methods have been used 290-294 with etched fused silicas to increase the surface area with diols or octadecyl chains then bonded to the surface.1 With such OT-CEC systems, the peptide-ligand interactions of, for example, angiotensin I-III increased with increasing hydrophobicity of the bonded phase on the capillary wall. Porous layer open tubular (PLOT) capillaries coated with anionic polymers 295 or poly(aspartic acid) 296 have also been employed 297 to separate basic peptides on the inner wall of fused silica capillaries of 20 pm i.d. When the same eluent conditions were employed, superior performance was observed for these PLOT capillaries compared to the corresponding capillary zone electrophoresis (HP-CZE) separation. Peptide mixtures can be analyzed 298-300 with OT-CEC systems based on octyl-bonded fused silica capillaries that have been coated with (3-aminopropyl)trimethoxysilane (APS), as well as with pressurized CEC (pCEC) packed with particles of similar surface chemistry, to decrease the electrostatic interactions between the solute and the surface, coupled to a mass spectrometer (MS). In the pressurized flow version of electrochromatography, a pLC pump is also employed (Figure 26) to facilitate liquid flow, reduce bubble formation, and to fine-tune the selectivity of the separation of the peptide mixture. 

The desired IL monomers are mixed with a free-radical initiator (azobisiso-butyronitrile, AIBN) in dichloromethane and coated onto the wall of the capillary column using the static coating method. The capillary is then sealed at both ends and heated to initiate polymerization. Finally, the capillary is unsealed and placed in a gas chromatograph and subsequently conditioned to remove any excess AIBN that did not completely decompose or react. 

Coating of capillary column using static coating method... 

Analytical Methods. The samples of PAH were extracted with cyclohexane, and the extract was subjected to liquid-liquid extractions with N,N-dimethylformamide as reported elsewhere (26). Following a concentration step, the extract was analyzed by GCZ using a Carlo Erba Fractovap 2101 equipped with a flame ionization detector. The column was a 50 m x 0.32 mm i.d. persilanized glass capillary coated with 0V-73 according to the Grob method (27). 

The most convenient of these methods is viscosity measurement of a liquid in which particles coated with a polymer are dispersed, or measurement of the flow rate of a liquid through a capillary coated with a polymer. Measurement of diffusion coefficients by photon correlation spectroscopy as well as measurement of sedimentation velocity have also been used. Hydrodynamically estimated thicknesses are usually considered to represent the correct thicknesses of the adsorbed polymer layers, but it is worth noting that recent theoretical calculations52, have shown that the hydrodynamic thickness is much greater than the average thickness of loops. 

There are several ways to reduce or suppress the electroosmotic flow in capillaries. These methods involve either eliminating the zeta potential across the solution-solid interface or increasing the viscosity at this interface. One approach is to coat the capillary wall, physically, with a polymer such as methylcellulose or linear polyacrylamide. Because of the difficulty in deactivating the capillary surface reproducibly, however, alternative methods employing dynamic reduction of solute-capillary interactions have been developed. Dynamic reduction of these interactions include the addition of chemical reagents such as methylhydroxyethylcellulose, S-benzylthiouro-nium chloride, and Triton X-100. 

Jama, M.A. E)elmas, M.P.F., Ruthven, D.M., Diffusion of linear and branched C6 hydrocarbons in silicalite studied by the wall-coated capillary diromatographic Method. Zeolites 18 (1997) pp. 200-204. 

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