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Optica Publishing Group
  • Applied Spectroscopy
  • Vol. 56,
  • Issue 1,
  • pp. 75-82
  • (2002)

Evaluation of Low-Field Nuclear Magnetic Resonance Spectrometry for At-Line Process Analysis

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Abstract

A low-field medium-resolution NMR spectrometer, with an operating frequency of 29 MHz for <sup>1</sup>H, has been developed for use in process analysis. The information that is attainable at this field strength has been investigated with the use of samples from a wide range of applications including the qualitative monitoring of a benzene production process, the estimation of the average ethoxy chain length in nonyl phenol ethoxylates, and the determination of strong acid concentrations. At low field, the spectra of multi-component samples often exhibit overlapping peaks, so multivariate calibration methods are necessary for quantitative analysis. Simulated data have been used to illustrate the effects of signal-to-noise ratio (SNR), resolution, and line shape on the predictive ability of partial least-squares (PLS) calibration routines, with SNR shown to have a greater impact than resolution on accuracy and precision. PLS calibration models were applied successfully in the analysis of samples from a methacrylamide process and a simulated esterification reaction. The accuracy (<5%) and precision (<3%) were generally good for components at concentrations >1-5% w/w.

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