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Optica Publishing Group
  • Applied Spectroscopy
  • Vol. 58,
  • Issue 10,
  • pp. 1187-1194
  • (2004)

Studies of Liquid-Phase Complexes in Acetonitrile/Water Solutions by Attenuated Total Reflection Infrared Spectroscopy with Acetaldehyde as a Model Solute

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Abstract

Chemometric methods combined with infrared (IR) spectroscopy, using attenuated total reflectance (ATR) sampling, are employed here to characterize the stoichiometry of complexes of solvent molecules in the liquid phase. The spectral information provides insight into the liquid microstructure present in liquid chromatographic mobile phases. This information should make it easier to understand and predict the effects of changes in mobile phase composition on the results of chromatographic separations. In this paper, mobile phases consisting of 0 mol % to 100 mol % acetonitrile in water were studied, with the addition of acetaldehyde as a model solute at concentrations ranging from 3 to 8 mol %. Using three-way multivariate curve resolution by the alternating least squares method (MCR-ALS) it was possible to resolve eight unique spectra: four mobile phase components, and four unique spectra of acetaldehyde solvated in different environments. The directions of the shifts of the important acetaldehyde infrared bands show good correlation with those predicted by gas-phase<i> ab initio</i> calculations of small solvated clusters.

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