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Total peak shape analysis: detection and quantitation of concurrent fronting, tailing, and their effect on asymmetry measurements.

Authors
  • Wahab, M Farooq1
  • Patel, Darshan C1
  • Armstrong, Daniel W2
  • 1 Department of Chemistry and Biochemistry, University of Texas at Arlington, Arlington, TX, 76019, United States. , (United States)
  • 2 Department of Chemistry and Biochemistry, University of Texas at Arlington, Arlington, TX, 76019, United States. Electronic address: [email protected] , (United States)
Type
Published Article
Journal
Journal of chromatography. A
Publication Date
Aug 04, 2017
Volume
1509
Pages
163–170
Identifiers
DOI: 10.1016/j.chroma.2017.06.031
PMID: 28647145
Source
Medline
Keywords
Language
English
License
Unknown

Abstract

Most peak shapes obtained in separation science depart from linearity for various reasons such as thermodynamic, kinetic, or flow based effects. An indication of the nature of asymmetry often helps in problem solving e.g. in column overloading, slurry packing, buffer mismatch, and extra-column band broadening. However, existing tests for symmetry/asymmetry only indicate the skewness in excess (tail or front) and not the presence of both. Two simple graphical approaches are presented to analyze peak shapes typically observed in gas, liquid, and supercritical fluid chromatography as well as capillary electrophoresis. The derivative test relies on the symmetry of the inflection points and the maximum and minimum values of the derivative. The Gaussian test is a constrained curve fitting approach and determines the residuals. The residual pattern graphically allows the user to assess the problematic regions in a given peak, e.g., concurrent tailing or fronting, something which cannot be easily done with other current methods. The template provided in MS Excel automates this process. The total peak shape analysis extracts the peak parameters from the upper sections (>80% height) of the peak rather than the half height as is done conventionally. A number of situations are presented and the utility of this approach in solving practical problems is demonstrated. Copyright © 2017 Elsevier B.V. All rights reserved.

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