Quantitative analysis using external standards with a benchtop NMR spectrometer

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dc.contributor.authorLee Y
dc.contributor.authorMatviychuk, Yevgen
dc.contributor.authorHolland, Daniel
dc.date.accessioned2025-02-13T21:36:07Z
dc.date.available2025-02-13T21:36:07Z
dc.date.issued2020
dc.description.abstractThis paper investigates the use of benchtop NMR spectrometers for quantitative analysis with external standards. Specifically, it focuses on the measurement of aqueous samples with analyte concentrations ranging from 30 mM to 1.7 M and electrical conductivity of up to 84mScm-1 using a 43 MHz instrument. It is demonstrated that measurements using the PULCON method cannot achieve an average error in quantification of <4% with the benchtop NMR tested here unless the standard and analyte are very similar. Our analysis indicates that this comparatively large error arises from the fixed tuning and matching of the benchtop spectrometer. We confirm that for moderately dilute samples (less than 0.2 M), the integral area of the solvent peak is suitable for use as an internal standard to mitigate this error. Furthermore, a round robin study demonstrates that the second major source of uncertainty in these measurements arises from the manual processing of the spectra by different analysts. Here we propose heuristics for manual baseline and phase correction to reduce this analyst-dependent error to about 3 %. We also demonstrate that semi-automated quantification using qGSD is able to achieve similar accuracy of integration, but with reduced sensitivity to the processing of the operator.
dc.identifier.citationLee Y, Matviychuk Y, Holland DJ (2020). Quantitative analysis using external standards with a benchtop NMR spectrometer. Journal of Magnetic Resonance. 320. 106826-.
dc.identifier.doihttp://doi.org/10.1016/j.jmr.2020.106826
dc.identifier.issn1090-7807
dc.identifier.issn1096-0856
dc.identifier.urihttps://hdl.handle.net/10092/107261
dc.languageeng
dc.publisherElsevier BV
dc.rightsAll rights reserved unless otherwise stated
dc.rights.urihttp://hdl.handle.net/10092/17651
dc.subjectBenchtop instruments
dc.subjectExternal standard
dc.subjectMedium-field NMR
dc.subjectMixture analysis
dc.subjectQuantitative NMR spectroscopy
dc.subject.anzsrc34 - Chemical sciences::3401 - Analytical chemistry::340101 - Analytical spectrometry
dc.subject.anzsrc34 - Chemical sciences::3401 - Analytical chemistry::340107 - Quality assurance, chemometrics, traceability and metrological chemistry
dc.subject.anzsrc51 - Physical sciences::5102 - Atomic, molecular and optical physics::510203 - Nonlinear optics and spectroscopy
dc.titleQuantitative analysis using external standards with a benchtop NMR spectrometer
dc.typeJournal Article
uc.collegeFaculty of Engineering
uc.departmentChemical and Process Engineering
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