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  • 1
    Electronic Resource
    Electronic Resource
    Fabrication of Stable Packed Capillary Reversed-Phase Columns for Protein Structural Analysis (1997)
    Springer
    The protein journal 16 (1997), S. 425-431 
    Details
    ISSN: 1573-4943
    Keywords: Reversed-phase microcolumn liquid chromatography ; protein concentration ; column end-frit fabrication ; phenylthiohydantoin amino acid analysis ; capillary chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Capillary column (≤320-μm ID) liquid chromatography is an essential tool for the separation and concentration of low-picomole amounts of proteins and peptides for mass-spectrometric based structural analysis. We describe a detailed procedure for the fabrication of stable and efficient 50- to 180-μm ID polyimide fused-silica columns. Columns were packed by conventional slurry packing with reversed-phase silica-based supports followed by column bed consolidation with acetonitrile and sonication. PVDF membrane or internal fused-silica particles were employed for column end-frit construction. The ability of these columns to withstand high back pressures (300–400 bar) enabled their use for rapid chromatography (〉3400 cm/hr; i.e., ∼40 μl/min for 200-μm ID columns) and the loading of large sample volumes (up to 500 μl). The accurate low flow rates (0.4–4.0 μl/min) and precise gradient formation necessary to operate these columns were achieved by a simple modification of conventional HPLC systems [Moritz et al. (1992), J. Chromatogr. 599, 119–130]. Column performance was evaluated for ability to resolve low-fmol amounts of all components of a mixture of PTH-amino acids and to separate peptides for on-line LC/MS analysis of peptide mixtures derived from in situ digestion of 2-DE resolved protein spots.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1026345023941
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    Paper (German National Licenses)
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  • 2
    Electronic Resource
    Electronic Resource
    A new type of two-dimensional packed+capillary column GC system. III. Instrumentation (1987)
    Springer
    Chromatographia 23 (1987), S. 499-501 
    Details
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Packed+capillary GC switching system ; Precolumn construction, oven and connector
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The constractional details of precolumns, its oven and connector have been given with two types of multiflow control modules. Two types of phases made in China, a silanized pellicular beads and a non silanized pellicular silica beads, with an optimum particle size of 20μm to 30μm were packed in the precolumn 20mm in length with the column efficiency of 4620 plates/meter at column temperature of 49°C. A 25m×0.22mm i.d. capillary column coated with bonded methylsilicone phase from Chrompack connected with the precolumn (250°C) has an efficiency of 5376 plates/meter for n-octane. But it decreased to 3149 plates/meter by decreasing the precolumn temperature to 130°C.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF02309418
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    Paper (German National Licenses)
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  • 3
    Electronic Resource
    Electronic Resource
    Unified gas and supercritical fluid chromatography on 50 μm i.d. Columns (1992)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 15 (1992), S. 505-509 
    Details
    ISSN: 0935-6304
    Keywords: Unified chromatography ; Gas chromatography ; Supercritical fluid chromatography ; Open tubular column ; Injection technique ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A unified approach to sequential gas and supercritical fluid Chromatography using 50 μm i.d. open tubular columns is described. Sample introduction is performed by means of a rotary injection valve. In order that linear velocities can be optimized independently, a second rotary valve in the chromatographic oven is used to direct the flow of column eluate to the flame ionization detector through either fused silica tubing in GC, or a frit restrictor in SFC.Applications of sequential GC-SFC on a 50 μm i.d. open tubular column are demonstrated, and comparisons made between sequential GC-SFC on 50 and 100 μm i.d. columns.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240150804
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  • 4
    Electronic Resource
    Electronic Resource
    Band broadening during mobile phase change in unified chromatography (GC-SFC) (1993)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 5 (1993), S. 237-243 
    Details
    ISSN: 1040-7685
    Keywords: unified chromatography ; gas chromatography ; supercritical fluid chromatography ; open tubular columns ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Band broadening brought about by changing the mobile phase from the GC mode to the SFC mode in unified chromatography is discussed. Its origin is shown to result from several factors: the replaceable volume of the tubing and valves in front of and following the column; the volume, internal diameter, and film thickness of the open tubular column; the initial pressure of the supercritical mobile phase; and the column temperature. Improvements to restrict band broadening were achieved by optimizing the system and its operating conditions.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mcs.1220050308
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  • 5
    Electronic Resource
    Electronic Resource
    Theoretical studies of the preparation of packed capillary columns for chromatography (1995)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 7 (1995), S. 265-278 
    Details
    ISSN: 1040-7685
    Keywords: packing method ; packed capillary column ; column technology ; packed capillary liquid chromatography ; supercritical fluid ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The theoretical aspects of the preparation of packed capillary columns for chromatography have been studied. The variation of the mean bulk density of the columns prepared with carbon dioxide fluids in different physical states and under different supercritical fluid conditions has been investigated. A new concept of the packing formation during the preparation of packed capillary columns with supercritical CO2 as packing fluid is described. A mathematical model for column preparation is derived that indicates the importance of the sonication effect in packing process. This studies indicate that the column performances (density and efficiency) can be controlled by varying the packing conditions. The wall effect in packed capillary columns (the effect of the packing densities on the column efficiencies) and the explanation for the production of very long columns are also discussed. © 1995 John Wiley & Sons, Inc.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mcs.1220070311
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    Paper (German National Licenses)
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  • 6
    Electronic Resource
    Electronic Resource
    Unified open tubular column chromatography: Sequential gas chromatography, at normal pressures, and supercritical fluid chromatography on the same column (1991)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 3 (1991), S. 403-409 
    Details
    ISSN: 1040-7685
    Keywords: unified chromatography ; supercritical fluid chromatography ; gas chromatography ; open tubular column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A unified chromatograph was constructed in which open tubular column gas chromatography, at normal helium carrier gas pressures, followed by supercritical fluid chromatography with carbon dioxide mobile phase was carried out in a single run using a 100-μm i. d. column. Sample introduction was accomplished by means of a pneumatically-actuated rotary injection valve. A second rotary valve was used post-column to direct the flow of column effluent to the flame ionization detector through an uncoated fused silica restrictor during the GC separation mode or to the FID through a frit restrictor during the SFC separation mode. This novel valve switching arrangement allowed system operating parameters of temperature and pressure programs and linear velocities to be optimized independently of each separation mode. The unified GC/SFC system was demonstrated for practical applications in various fields of process and product quality control.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mcs.1220030504
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  • 7
    Electronic Resource
    Electronic Resource
    Preparation and evaluation of supercritical carbon dioxide-packed capillary columns for HPLC and SFC (1994)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 6 (1994), S. 249-255 
    Details
    ISSN: 1040-7685
    Keywords: packed capillary column ; column technology ; liquid chromatography ; supercritical fluid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Preparation of packed capillary columns with supercritical carbon dioxide as the packing carrier is demonstrated; column performance was evaluated by both HPLC and SFC. It is shown that this procedure yields excellent column performance. The density of the packed bed can be controlled by varying the restrictor dimensions and the packing pressure. Column preparation using a supercritical fluid is more rapid than with liquid slurry packing and yields good column stability. Because supercritical fluids have a wider range of viscosities and velocities, in comparison with gases and liquids, a wide choice of packing conditions is available. Several applications of columns packed by this method are presented.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mcs.1220060309
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