A comparison of non-uniform sampling and model-based analysis of NMR spectra for reaction monitoring

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dc.contributor.authorSteimers E
dc.contributor.authorMatviychuk, Yevgen
dc.contributor.authorFriebel A
dc.contributor.authorMünnemann K
dc.contributor.authorvon Harbou E
dc.contributor.authorHolland, Daniel
dc.date.accessioned2025-02-12T22:13:15Z
dc.date.available2025-02-12T22:13:15Z
dc.date.issued2021
dc.description.abstractNuclear magnetic resonance (NMR) spectroscopy is widely used for applications in the field of reaction and process monitoring. When complex reaction mixtures are studied, NMR spectra often suffer from low resolution and overlapping peaks, which places high demands on the method used to acquire or to analyse the NMR spectra. This work presents two NMR methods that help overcome these challenges: 2D non-uniform sampling (NUS) and a recently proposed model-based fitting approach for the analysis of 1D NMR spectra. We use the reaction of glycerol with acetic acid as it produces five reaction products that are all chemically similar and, hence, challenging to distinguish. The reaction was measured on a high-field 400 MHz NMR spectrometer with a 2D NUS-heteronuclear single quantum coherence (HSQC) and a conventional 1D 1H NMR sequence. We show that comparable results can be obtained using both 2D and 1D methods, if the 2D volume integrals of the 2D NUS-HSQC NMR spectra are calibrated. Further, we monitor the same reaction on a low-field 43 MHz benchtop NMR spectrometer and analyse the acquired 1D 1H NMR spectra with the model-based approach and with partial least-squares regression (PLS-R), both trained using a single, calibrated data set. Both methods achieve results that are in good quantitative agreement with the high-field data. However, the model-based method was found to be less sensitive to the training data set used than PLS-R and, hence, was more robust when the reaction conditions differed from that of the training data.
dc.identifier.citationSteimers E, Matviychuk Y, Friebel A, Münnemann K, von Harbou E, Holland DJ (2021). A comparison of non-uniform sampling and model-based analysis of NMR spectra for reaction monitoring. Magnetic Resonance in Chemistry. 59(3). 221-236.
dc.identifier.doihttp://doi.org/10.1002/mrc.5095
dc.identifier.issn0749-1581
dc.identifier.issn1097-458X
dc.identifier.urihttps://hdl.handle.net/10092/107272
dc.languageeng
dc.publisherWiley
dc.rightsAll rights reserved unless otherwise stated
dc.rights.urihttp://hdl.handle.net/10092/17651
dc.subjectBayesian analysis
dc.subjectbenchtop NMR
dc.subjectmodel-based quantification
dc.subjectnon-uniform sampling
dc.subjectquantitative NMR spectroscopy
dc.subjectreaction monitoring
dc.subject.anzsrc40 - Engineering::4004 - Chemical engineering::400408 - Reaction engineering (excl. nuclear reactions)
dc.subject.anzsrc40 - Engineering::4004 - Chemical engineering::400407 - Process control and simulation
dc.subject.anzsrc34 - Chemical sciences::3406 - Physical chemistry::340605 - Molecular imaging (incl. electron microscopy and neutron diffraction)
dc.titleA comparison of non-uniform sampling and model-based analysis of NMR spectra for reaction monitoring
dc.typeJournal Article
uc.collegeFaculty of Engineering
uc.departmentChemical and Process Engineering
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