A Triple Layer of Immiscible Solvents for NMR Sample Preparation: Enhanced Sensitivity and Reduced Deuterated Solvent

2019 ◽  
Vol 4 (44) ◽  
pp. 12928-12937
Author(s):  
Bikash Baishya ◽  
Atish Chandra
Keyword(s):  
Sample Preparation ◽  
Enhanced Sensitivity ◽  
Triple Layer ◽  
Nmr Sample Preparation

scholarly journals A Triple Layer of Immiscible Solvents for NMR Sample Preparation: Enhanced Sensitivity and Reduced Deuterated Solvent for Observation of Heteronuclei

2019 ◽  
Author(s):  
Bikash Baishya ◽  
Atish Chandra
Keyword(s):  
Sample Preparation ◽  
Signal To Noise Ratio ◽  
Bottom Part ◽  
Enhanced Sensitivity ◽  
Magnetic Field Homogeneity ◽  
Field Homogeneity ◽  
Nmr Sample Preparation ◽  
Set Up ◽  
The Magnetic Field ◽  
Sample Dilution

<p>Organic chemistry labs routinely perform NMR in a standard 5 mm NMR tube. NMR sample is prepared by filling the lowermost 4 cm length of a regular 5 mm 0.d. tube that holds approximately 0.55 ml of a deuterated solvent. This is actually a sample dilution procedure as the signal mainly comes from the central part, i.e. 1.8 cm length sample that fits the typical coil length of 1.8 cm in regular NMR spectrometers. The diluted top and bottom part of the sample is away from the coil and contributes less signal. This dilution procedure amplifies the requirement of expensive deuterated solvent and lowers sensitivity. The present study explores a new way of sample preparation which involves sandwiching a small amount of the deuterated solvent (D<sub>2</sub>O) of length 1.8 cm containing the analyte between two non-deuterated solvents (CCl<sub>4</sub> at bottom of length ≈ 1 cm and similarly C<sub>6</sub>H<sub>6</sub> at top), which are immiscible with the former using a regular 5 mm o.d. NMR tube in such a way that total length is still 4 cm as demanded by the magnetic field homogeneity considerations. The analyte now being closer to NMR coil dissolved in 1.8 cm solvent, improves sensitivity and reduces deuterated solvent hitherto required. <sup>13</sup>C and <sup>15</sup>N spectra from such a set-up display two to three-fold higher signal to noise ratio and hence four to eightfold savings in experimental time or faster data collection.</p><br>

scholarly journals A Triple Layer of Immiscible Solvents for NMR Sample Preparation: Enhanced Sensitivity and Reduced Deuterated Solvent for Observation of Heteronuclei

2019 ◽  
Author(s):  
Bikash Baishya ◽  
Atish Chandra
Keyword(s):  
Sample Preparation ◽  
Signal To Noise Ratio ◽  
Bottom Part ◽  
Enhanced Sensitivity ◽  
Magnetic Field Homogeneity ◽  
Field Homogeneity ◽  
Nmr Sample Preparation ◽  
Set Up ◽  
The Magnetic Field ◽  
Sample Dilution

<p>Organic chemistry labs routinely perform NMR in a standard 5 mm NMR tube. NMR sample is prepared by filling the lowermost 4 cm length of a regular 5 mm 0.d. tube that holds approximately 0.55 ml of a deuterated solvent. This is actually a sample dilution procedure as the signal mainly comes from the central part, i.e. 1.8 cm length sample that fits the typical coil length of 1.8 cm in regular NMR spectrometers. The diluted top and bottom part of the sample is away from the coil and contributes less signal. This dilution procedure amplifies the requirement of expensive deuterated solvent and lowers sensitivity. The present study explores a new way of sample preparation which involves sandwiching a small amount of the deuterated solvent (D<sub>2</sub>O) of length 1.8 cm containing the analyte between two non-deuterated solvents (CCl<sub>4</sub> at bottom of length ≈ 1 cm and similarly C<sub>6</sub>H<sub>6</sub> at top), which are immiscible with the former using a regular 5 mm o.d. NMR tube in such a way that total length is still 4 cm as demanded by the magnetic field homogeneity considerations. The analyte now being closer to NMR coil dissolved in 1.8 cm solvent, improves sensitivity and reduces deuterated solvent hitherto required. <sup>13</sup>C and <sup>15</sup>N spectra from such a set-up display two to three-fold higher signal to noise ratio and hence four to eightfold savings in experimental time or faster data collection.</p><br>

Submicro Scale NMR Sample Preparation for Volatile Chemicals

2004 ◽  
Vol 30 (11) ◽  
pp. 2153-2161 ◽  
Author(s):  
Satoshi Nojima ◽  
David J. Kiemle ◽  
Francis X. Webster ◽  
Wendell L. Roelofs
Keyword(s):  
Sample Preparation ◽  
Volatile Chemicals ◽  
Nmr Sample Preparation

A new solution 31 P NMR sample preparation scheme for marine sediments

2017 ◽  
Vol 15 (4) ◽  
pp. 381-393 ◽  
Author(s):  
Delphine Defforey ◽  
Barbara J. Cade-Menun ◽  
Adina Paytan
Keyword(s):  
Sample Preparation ◽  
Marine Sediments ◽  
Nmr Sample Preparation

Vacuum and Pressure System for NMR Sample Preparation

1963 ◽  
Vol 34 (8) ◽  
pp. 944-944 ◽  
Author(s):  
Robert A. Cacciarelli ◽  
Burch B. Stewart
Keyword(s):  
Sample Preparation ◽  
Pressure System ◽  
Nmr Sample Preparation
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