In-line monitoring of esterification using a miniaturised mid-infrared spectrometer

McGill, Colin A.; Ferguson, Rachel H.; Donoghue, Kathryn; Nordon, Alison; Littlejohn, David

Abstract

A miniaturised mid-infrared (MIR) spectrometer attached directly to an in-line immersion probe with an attenuated total reflectance crystal has been used to monitor the progression of the batch reaction of crotonic acid and 2-butanol in toluene. Univariate calibration, using the signal at 1188 cm−1 in the 2nd derivative spectrum, gave accurate (average error, 1.6%) and precise (average relative standard deviation, 5.2%) estimation of 2-butyl crotonate concentrations in the range 0.08–0.49 mol dm−3. Calibration by partial least squares was of no additional benefit in this application. The performance of in-line MIR spectrometry was comparable to that of an off-line reference gas chromatography method and superior to that of other in-line process analysis techniques (near-infrared, Raman or UV-visible spectrometries).

Citation

McGill, C. A., Ferguson, R. H., Donoghue, K., Nordon, A., & Littlejohn, D. (2003). In-line monitoring of esterification using a miniaturised mid-infrared spectrometer. Analyst, 128(12), 1467-1470. https://doi.org/10.1039/b311187n

• Journal Article Type: Article
• Acceptance Date: Oct 30, 2003
• Online Publication Date: Nov 18, 2003
• Publication Date: 2003
• Deposit Date: Jul 9, 2021
• Journal: The Analyst
• Print ISSN: 0003-2654
• Electronic ISSN: 1364-5528
• Publisher: Royal Society of Chemistry
• Peer Reviewed: Peer Reviewed
• Volume: 128
• Issue: 12
• Pages: 1467-1470
• DOI: https://doi.org/10.1039/b311187n
• Public URL: http://researchrepository.napier.ac.uk/Output/2782150