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Extra-column Band Broadening in Ultra High Performance Liquid Chromatography

Topper, Sarah L. (2011) Extra-column Band Broadening in Ultra High Performance Liquid Chromatography. Master's Thesis, University of Pittsburgh.

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    Abstract

    Advances in column technologies for high performance liquid chromatography (HPLC) have led to the use of small, highly efficient packing materials. The use of these materials requires short, small diameter columns as well as instruments capable of withstanding high pressures (up to 1000bar) and sometimes temperature (in excess of 100°C), a technique dubbed ultra-high performance liquid chromatography or UPLC. The advantage is a greater than ten-fold reduction in analysis time without a loss of peak capacity or resolution. Due to the small volumes inherent in the new columns, the extra-column volumes of the instrument can become a significant source of dispersion leading to extra-column broadening of chromatographic peaks. Uncontrolled or accounted for, this variance severely limits the separation potential of improved column packings and reduces the accuracy of evaluations of instruments and columns. An investigation is made of the source and nature of the band broadening in instrumental components with an eye towards reduction of variance without loss of performance. Different methods for calculating the degree of extra-column band broadening are discussed. Applications of the calculated data for evaluation of the kinetic parameters of UPLC are reviewed.


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    Item Type: University of Pittsburgh ETD
    ETD Committee:
    ETD Committee TypeCommittee MemberEmail
    Committee ChairWeber, Stephen Gsweber@pitt.edu
    Committee MemberMichael, Adrian Camichael@pitt.edu
    Committee MemberTrakselis, Michael Amtraksel@pitt.edu
    Title: Extra-column Band Broadening in Ultra High Performance Liquid Chromatography
    Status: Unpublished
    Abstract: Advances in column technologies for high performance liquid chromatography (HPLC) have led to the use of small, highly efficient packing materials. The use of these materials requires short, small diameter columns as well as instruments capable of withstanding high pressures (up to 1000bar) and sometimes temperature (in excess of 100°C), a technique dubbed ultra-high performance liquid chromatography or UPLC. The advantage is a greater than ten-fold reduction in analysis time without a loss of peak capacity or resolution. Due to the small volumes inherent in the new columns, the extra-column volumes of the instrument can become a significant source of dispersion leading to extra-column broadening of chromatographic peaks. Uncontrolled or accounted for, this variance severely limits the separation potential of improved column packings and reduces the accuracy of evaluations of instruments and columns. An investigation is made of the source and nature of the band broadening in instrumental components with an eye towards reduction of variance without loss of performance. Different methods for calculating the degree of extra-column band broadening are discussed. Applications of the calculated data for evaluation of the kinetic parameters of UPLC are reviewed.
    Date: 06 June 2011
    Date Type: Completion
    Defense Date: 19 April 2011
    Approval Date: 06 June 2011
    Submission Date: 19 April 2011
    Access Restriction: No restriction; The work is available for access worldwide immediately.
    Patent pending: No
    Institution: University of Pittsburgh
    Thesis Type: Master's Thesis
    Refereed: Yes
    Degree: MS - Master of Science
    URN: etd-04192011-120702
    Uncontrolled Keywords: capillary; Gaussian; injector; variance
    Schools and Programs: Dietrich School of Arts and Sciences > Chemistry
    Date Deposited: 10 Nov 2011 14:39
    Last Modified: 23 May 2012 13:28
    Other ID: http://etd.library.pitt.edu/ETD/available/etd-04192011-120702/, etd-04192011-120702

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