Nuclear Magnetic Resonance (1.40 T) and Mid Infrared (FTIR-ATR) Associated with Chemometrics as Analytical Methods for the Analysis of Methyl Ester Yield Obtained by Esterification Reaction
In this work, we compared 1.40 T nuclear magnetic resonance (NMR) to 7.05 T (60 and 300 MHz for proton, respectively), and mid-infrared with attenuated total reflectance (FTIR-ATR), associated with chemometrics methods, for the quantification of the reaction yield during esterification of fatty acids with methanol. The results showed that the integrated intensities of the ester C=O stretching region, relative to the total C=O stretching region, is useful to quantify the fatty acid methyl ester (FAME) concentration. Comparing the results obtained by the different final models: NMR (1.40 T and 7.05 T), FTIR-ATR using multivariate partial last squares regression (PLS) with orthogonal signal correction (OSC), and univariate ordinary least squares (OLS), the NMR of 1.40 T (60 MHz for proton) showed more advantages when compared to a high field spectrometer, due to the non-use of cryogenic and solvents and less laborious work for obtaining results.
| Main Authors: | , , , |
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| Format: | Digital revista |
| Language: | English |
| Published: |
Sociedade Brasileira de Química
2017
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| Online Access: | http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532017001001917 |
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| Summary: | In this work, we compared 1.40 T nuclear magnetic resonance (NMR) to 7.05 T (60 and 300 MHz for proton, respectively), and mid-infrared with attenuated total reflectance (FTIR-ATR), associated with chemometrics methods, for the quantification of the reaction yield during esterification of fatty acids with methanol. The results showed that the integrated intensities of the ester C=O stretching region, relative to the total C=O stretching region, is useful to quantify the fatty acid methyl ester (FAME) concentration. Comparing the results obtained by the different final models: NMR (1.40 T and 7.05 T), FTIR-ATR using multivariate partial last squares regression (PLS) with orthogonal signal correction (OSC), and univariate ordinary least squares (OLS), the NMR of 1.40 T (60 MHz for proton) showed more advantages when compared to a high field spectrometer, due to the non-use of cryogenic and solvents and less laborious work for obtaining results. |
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