Use of an internal reference in 13C chemical shift measurements
The use of the nominal value of the chemical shift of the solvent to calibrate the spectrometer in 13C NMR spectroscopy was found to introduce errors due to the effect which the solute has on the solvent. In addition, hexamethyldisiloxane (HM) is proposed as an internal standard; owing to its high b...
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todo:paper_07491581_v28_n1_p1_deKowalewski2023-10-03T15:39:19Z Use of an internal reference in 13C chemical shift measurements de Kowalewski, D.G. de Los Santos, C. Marceca, E. 13C chemical shift measurement Internal reference The use of the nominal value of the chemical shift of the solvent to calibrate the spectrometer in 13C NMR spectroscopy was found to introduce errors due to the effect which the solute has on the solvent. In addition, hexamethyldisiloxane (HM) is proposed as an internal standard; owing to its high boiling point it is easier to manipulate than tetramethylsilane (TMS) and it is therefore possible to prepare solutions of known concentrations. In order to convert the data obtained with this standard to the TMS scale, the chemical shift of HM was determined in 16 solvents using cyclohexane as external standard in a spherical cell (5% w/w concentration of HM) as a function of the solvent factor g2. Comparing these results with a similar plot obtained previously for TMS by other workers, it is possible to convert one type of data to the other by a simple linear expression. Copyright © 1990 John Wiley & Sons, Ltd. Fil:Marceca, E. Universidad de Buenos Aires. Facultad de Ciencias Exactas y Naturales; Argentina. JOUR info:eu-repo/semantics/openAccess http://creativecommons.org/licenses/by/2.5/ar http://hdl.handle.net/20.500.12110/paper_07491581_v28_n1_p1_deKowalewski |
institution |
Universidad de Buenos Aires |
institution_str |
I-28 |
repository_str |
R-134 |
collection |
Biblioteca Digital - Facultad de Ciencias Exactas y Naturales (UBA) |
topic |
13C chemical shift measurement Internal reference |
spellingShingle |
13C chemical shift measurement Internal reference de Kowalewski, D.G. de Los Santos, C. Marceca, E. Use of an internal reference in 13C chemical shift measurements |
topic_facet |
13C chemical shift measurement Internal reference |
description |
The use of the nominal value of the chemical shift of the solvent to calibrate the spectrometer in 13C NMR spectroscopy was found to introduce errors due to the effect which the solute has on the solvent. In addition, hexamethyldisiloxane (HM) is proposed as an internal standard; owing to its high boiling point it is easier to manipulate than tetramethylsilane (TMS) and it is therefore possible to prepare solutions of known concentrations. In order to convert the data obtained with this standard to the TMS scale, the chemical shift of HM was determined in 16 solvents using cyclohexane as external standard in a spherical cell (5% w/w concentration of HM) as a function of the solvent factor g2. Comparing these results with a similar plot obtained previously for TMS by other workers, it is possible to convert one type of data to the other by a simple linear expression. Copyright © 1990 John Wiley & Sons, Ltd. |
format |
JOUR |
author |
de Kowalewski, D.G. de Los Santos, C. Marceca, E. |
author_facet |
de Kowalewski, D.G. de Los Santos, C. Marceca, E. |
author_sort |
de Kowalewski, D.G. |
title |
Use of an internal reference in 13C chemical shift measurements |
title_short |
Use of an internal reference in 13C chemical shift measurements |
title_full |
Use of an internal reference in 13C chemical shift measurements |
title_fullStr |
Use of an internal reference in 13C chemical shift measurements |
title_full_unstemmed |
Use of an internal reference in 13C chemical shift measurements |
title_sort |
use of an internal reference in 13c chemical shift measurements |
url |
http://hdl.handle.net/20.500.12110/paper_07491581_v28_n1_p1_deKowalewski |
work_keys_str_mv |
AT dekowalewskidg useofaninternalreferencein13cchemicalshiftmeasurements AT delossantosc useofaninternalreferencein13cchemicalshiftmeasurements AT marcecae useofaninternalreferencein13cchemicalshiftmeasurements |
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1782027140588371968 |