Determination of the ethylene oxide content of polyether polyols by low-field H-1 nuclear magnetic resonance spectrometry

A Nordon, C Meunier, R H Carr, P J Gemperline, D Littlejohn

Research output: Contribution to journalArticle

20 Citations (Scopus)

Abstract

Methods have been developed and compared for the analysis of a glycerol-based polyether polyol using a low-field, medium-resolution NMR spectrometer, with an operating frequency of 29 MHz for 1 H. Signal areas in the time and frequency domains were used to calculate the ethylene oxide (EO) content of individual samples. The time domain signals (free induction decay) were analysed using a new version of the direct exponential curve resolution algorithm (FID-DECRA). Direct analysis of the H-1 NMR FF spectra gave percentage EO concentrations of reasonable accuracy (average percentage error of 1.3%) and precision (average RSD of 1.8%) when compared with results derived from high-field C-13 NMR spectrometry. The direct FID-DECRA method showed a negative bias (-0.8+/-0.12% w/w) in the estimation of percentage EO concentration, but the precision (average RSD of 0.9%) was twice as good as that of direct spectral analysis. When the 13C NMR analysis was used as a reference method for univariate calibration of the 1 H NMR procedures, the best accuracy (average percentage error of 0.5%) and precision (average RSD of 0.6%) were obtained using FID-DECRA, for EO concentrations in the range 14.8-15.5% w/w. An additional advantage of FID-DECRA is that the analytical procedure could be automated, which is particularly desirable for process analysis. (C) 2002 Elsevier Science B.V. All rights reserved.

LanguageEnglish
Pages133-140
Number of pages8
JournalAnalytica Chimica Acta
Volume472
Issue number1-2
DOIs
Publication statusPublished - 20 Nov 2002

Fingerprint

Ethylene Oxide
Polyethers
Spectrometry
ethylene
spectrometry
nuclear magnetic resonance
Spectrum Analysis
Magnetic Resonance Spectroscopy
Nuclear magnetic resonance
oxide
Glycerol
Spectrum analysis
spectral analysis
Calibration
Spectrometers
spectrometer
polyol
calibration
method
analysis

Keywords

  • low-field NMR spectrometry
  • process analysis
  • polyether polyols
  • ethylene oxide
  • direct exponential curve resolution algorithm

Cite this

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title = "Determination of the ethylene oxide content of polyether polyols by low-field H-1 nuclear magnetic resonance spectrometry",
abstract = "Methods have been developed and compared for the analysis of a glycerol-based polyether polyol using a low-field, medium-resolution NMR spectrometer, with an operating frequency of 29 MHz for 1 H. Signal areas in the time and frequency domains were used to calculate the ethylene oxide (EO) content of individual samples. The time domain signals (free induction decay) were analysed using a new version of the direct exponential curve resolution algorithm (FID-DECRA). Direct analysis of the H-1 NMR FF spectra gave percentage EO concentrations of reasonable accuracy (average percentage error of 1.3{\%}) and precision (average RSD of 1.8{\%}) when compared with results derived from high-field C-13 NMR spectrometry. The direct FID-DECRA method showed a negative bias (-0.8+/-0.12{\%} w/w) in the estimation of percentage EO concentration, but the precision (average RSD of 0.9{\%}) was twice as good as that of direct spectral analysis. When the 13C NMR analysis was used as a reference method for univariate calibration of the 1 H NMR procedures, the best accuracy (average percentage error of 0.5{\%}) and precision (average RSD of 0.6{\%}) were obtained using FID-DECRA, for EO concentrations in the range 14.8-15.5{\%} w/w. An additional advantage of FID-DECRA is that the analytical procedure could be automated, which is particularly desirable for process analysis. (C) 2002 Elsevier Science B.V. All rights reserved.",
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Determination of the ethylene oxide content of polyether polyols by low-field H-1 nuclear magnetic resonance spectrometry. / Nordon, A ; Meunier, C ; Carr, R H ; Gemperline, P J ; Littlejohn, D .

In: Analytica Chimica Acta, Vol. 472, No. 1-2, 20.11.2002, p. 133-140.

Research output: Contribution to journalArticle

TY - JOUR

T1 - Determination of the ethylene oxide content of polyether polyols by low-field H-1 nuclear magnetic resonance spectrometry

AU - Nordon, A

AU - Meunier, C

AU - Carr, R H

AU - Gemperline, P J

AU - Littlejohn, D

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N2 - Methods have been developed and compared for the analysis of a glycerol-based polyether polyol using a low-field, medium-resolution NMR spectrometer, with an operating frequency of 29 MHz for 1 H. Signal areas in the time and frequency domains were used to calculate the ethylene oxide (EO) content of individual samples. The time domain signals (free induction decay) were analysed using a new version of the direct exponential curve resolution algorithm (FID-DECRA). Direct analysis of the H-1 NMR FF spectra gave percentage EO concentrations of reasonable accuracy (average percentage error of 1.3%) and precision (average RSD of 1.8%) when compared with results derived from high-field C-13 NMR spectrometry. The direct FID-DECRA method showed a negative bias (-0.8+/-0.12% w/w) in the estimation of percentage EO concentration, but the precision (average RSD of 0.9%) was twice as good as that of direct spectral analysis. When the 13C NMR analysis was used as a reference method for univariate calibration of the 1 H NMR procedures, the best accuracy (average percentage error of 0.5%) and precision (average RSD of 0.6%) were obtained using FID-DECRA, for EO concentrations in the range 14.8-15.5% w/w. An additional advantage of FID-DECRA is that the analytical procedure could be automated, which is particularly desirable for process analysis. (C) 2002 Elsevier Science B.V. All rights reserved.

AB - Methods have been developed and compared for the analysis of a glycerol-based polyether polyol using a low-field, medium-resolution NMR spectrometer, with an operating frequency of 29 MHz for 1 H. Signal areas in the time and frequency domains were used to calculate the ethylene oxide (EO) content of individual samples. The time domain signals (free induction decay) were analysed using a new version of the direct exponential curve resolution algorithm (FID-DECRA). Direct analysis of the H-1 NMR FF spectra gave percentage EO concentrations of reasonable accuracy (average percentage error of 1.3%) and precision (average RSD of 1.8%) when compared with results derived from high-field C-13 NMR spectrometry. The direct FID-DECRA method showed a negative bias (-0.8+/-0.12% w/w) in the estimation of percentage EO concentration, but the precision (average RSD of 0.9%) was twice as good as that of direct spectral analysis. When the 13C NMR analysis was used as a reference method for univariate calibration of the 1 H NMR procedures, the best accuracy (average percentage error of 0.5%) and precision (average RSD of 0.6%) were obtained using FID-DECRA, for EO concentrations in the range 14.8-15.5% w/w. An additional advantage of FID-DECRA is that the analytical procedure could be automated, which is particularly desirable for process analysis. (C) 2002 Elsevier Science B.V. All rights reserved.

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