Page 154 - Illustrated Pocket Dictionary of Chromatography
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154     PREPARATIVE (HPLC)














        An HPLC precolumn is used as a sacrificial column when harsh/reactive mobile
        phases are used. The packing material should match the identity of the analytical
        column but can be made from much less expensive large-particle material (30–
        40mm). The column is dry packed and flushed with mobile phase to remove air
        before attaching to the system.

        from particularly aggressive solvents (e.g, high and low pH, etc). The
        premise of the precolumn is that it acts as a “sacrificial” column. The
        aggressive solvent dissolves the material in the precolumn, thereby
        becoming saturated with the bonded phase, hence the reason for the
        bonded phase needing to match the analytical column phase. It should
        be noted that the particle size is often much larger for the precolumn
        because system efficiency is unaffected (it is placed before the injec-
        tor). The 40- to 60-mm particles found in many solid-phase extraction
        columns are acceptable. Precolumns are typically dry-packed and
        then equilibrated with mobile phase off-line.

        preparative (HPLC) Columns that have an ID >2cm and lengths
        >25cm are used to process large samples masses and are termed
        preparative columns. For preparative columns the packing is usually
        ≥40mm, flow rates are >10mL/min, and injection volumes are >0.1mL.

        preparative thin-layer chromatography (TLC) To increase
        the sample load capacity over a normal TLC plate, a preparative TLC
        plate has a a thicker sorbent layer (500–2000mm vs. ~250mm). Larger
        plates, height and width, may also be used. In preparative TLC the
        bands are identified and the sorbent containing the band is scraped
        from the plate. The analyte is then desorbed from the sorbent by
        placing the sorbent is a very strong solvent. The solvent is removed
        or exchanged for a long-term storage solvent.

        pressure Pressure in chromatographic systems is reflective of the
        resistance that the system (in particular the column) has to forced
        mobile-phase flow through it. An operational diagnostic for the proper
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