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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 49 (1999), S. 333-337 
    ISSN: 1612-1112
    Keywords: Supercritical fluid chromatography ; Gas chromatography ; Solvating gas chromatography ; Peak capacity
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In this paper, a general peak capacity expression was evaluated using columns containing various packing materials under solvating gas chromatography (SGC) conditions. Differing from column efficiency, peak capacity can describe both separation capability and speed when introducing the dead time into the peak capacity expression. Various factors that influence peak capacity in SGC are described, including particle pore size, chemical surface modification, particle size, column length, temperature, and pressure.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Capillary electrophoresis ; Column technology ; Deactivation ; Polyethyleneoxides ; Ribonucleotides
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In this study, a variety of fused silica capillaries with different combinations and sequences of treatments with HMDS and polyethylene oxide were prepared in order to develop an optimized column modification method for analysis of ribonucleotides. The 12 most common ribonucleotides (UTP, CTP, ATP, GTP, UDP, CDP, ADP, GDP, UMP, CMP, AMP, and GMP) in human cells were used as test solutes. Column performance measurements, including electroosmotic flow (EOF), solute migration speed and retention, column efficiency, peak shape, and resolution were investigated. By analyzing solute migration speed and retention of various hydrophilic/hydrophobic solutes, the column wall effects (EOF and adsorption) can be distinguished. This analysis method can give guidance in optimizing polymer coating properties (hydrophilicity/hydrophobicity) for CE columns. By studying the performance of these columns after various surface treatments, we were able to improve the separation of ribonucleotides from real samples to within 16 minutes with high efficiency and stability (over 300 analyses) using columns first deactivated with hexamethyldisilazane, and then coated with polyethylene oxide.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 1612-1112
    Keywords: Supercritical fluid chromatography ; Surface modification ; Deactivation ; Silica particles ; Stationary phases ; Packing materials ; Packed capillary columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Spherical porous silica particles (10 μm diameter, 300 Å and 80 Å pores), spherical nonporous silica particles (10 μm diameter), and irregular porous silica particles (≈10 μm diameter, 80 Å pores) were deactivated with polymethylhydrosiloxane (PS). The surface activities of the deactivated silica particles were investigated using various polar compounds under supercritical fluid chromatography (SFC) conditions (neat CO2), and compared with a commercial C18-bonded phase. The small pore (80 Å) silica particles could be more completely deactivated than larger pore (300 Å) and nonporous silica particles. The success of the PS deactivation method is ascribed to the excellent match between the reactive groups on the polymer backbone and the silica surface, and the formation of a highly crosslinked polymeric layer over the surface. Physical processes, such as adsorption and desorption of the deactivation reagent on the surface and diffusion from the surface, were found to have important effects on the deactivation. Using capillary columns packed with PS deactivated silica particles, typical polar organic compounds, including hydroxyl-containing compounds, carbonyl-containing compounds, free amines, and free carboxylic acids, were separated by SFC and compared with results from a commercial C18-bonded phase. While the results clearly show that the PS deactivated particles were more inert than the C18-bonded phase, better deactivation methods are still needed for separation of free acids and alkylamines.
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  • 4
    ISSN: 1612-1112
    Keywords: Solvating gas chromatography ; Supercritical fluid chromatography ; Packed capillary columns ; Solvating power
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The efficiency (plate number per unit time) and elution power (range ofn-alkanes) of packed capillary SFC and SGC using CO2 as the mobile phase were compared. A higher plate number per unit time was obtained in SGC than in SFC using the same column under the same applied conditions. SGC is more suitable for fast separations than SFC. The solvating ability of the mobile phase, at the column exit end, decreased remarkably after the restrictor was removed. However, the elution molecular weight range in SGC can be greatly extended by increasing the column temperature.n-Alkanes with carbon numbers as high as 80 were separated under SGC conditions using a 35 cm ×250 μm i.d. column packed with 10 μm polymer-encapsulated silica particles at 200 atm, with a temperature program of 100–380°C at 10°C min−1.
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  • 5
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Supercritical fluid chromatography ; Solvating gas chromatography ; Polybutadiene coated zirconia ; CO2 mobile phase
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary In this paper, practical considerations of column efficiency, separation speed, thermal stability, and column polarity of capillary columns packed with polybutadiene-coated zirconia were investigated under solvating gas chromatography (SGC) conditions using carbon dioxide as mobile phase. When compared with results obtained from conventional porous octadecyl obtained from conventional porous octadecyl bonded silica (ODS) particles, PBD-zirconia particles produced greater change in mobile phase linear velocity with pressure than conventional ODS particles under the same conditions. The maximum plate number per second (Nt) obtained with a 30 cm PBD-zirconia column was approximately 1.5 times higher than that obtained with an ODS column at 100 °C. Therefore, the PBD-zirconia phase is more suitable for fast separations than conventional ODS particles in SGC. Maximum plate numbers per meter of 76,900 and 63,300 were obtained using a 57 cm×250 μm i.d. fused silica capillary column packed with 3 μm PBD-zirconia at 50 °C and 100 °C, respectively. The PBD-zirconia phase was stable at temperatures up to 320 °C under SGC conditions using carbon dioxide as mobile phase. Polarizable aromatic compounds and low molecular weight ketones and aldehydes were eluted with symmetrical peaks from a 10 cm column packed with 3 μm PBD-zirconia. Zirconia phases with greater inertness are required for the analysis of more polar compounds by SGC.
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