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Briana Halbert Qualitative Application of NMR Spectroscopy: 1.

Determination of Mole Ratio of a Binary Mixture by 1H NMR April 09, 2013 Purpose/Background: To determine the mole ratio of a binary mixture by 1H NMR. 1H NMR spectrum of a pure compound is proportional to the area of a peak and the area of another peak that is proportional to the number of protons responsible for that peak. The ratio of the actual number of hydrogen atoms for each signal is also equal to the mole ratio of hydrogen atoms for each signal of the molecule. For non-equivalent protons in a compound, the ratios of integral values corresponding to one proton will be 1:1:1, because the different signals belong to the same compound. In the 1H NMR spectrum of a mixture of compounds however, the ratio of integral units for 1H or any equal number of hydrogen atoms for each component of the mixture will be equal to the mole ratio of the components in the mixture. Table of Reagent: Compound Ethyl Acetate Structure M.W. 88.11 B.P./M.P. M -83.6C B 77.1C Methyl Propanoate 88.12 M -88C B 67.9 C 0.898 density 0.897

Procedure: The student picked an unknown mixture of ethyl acetate and methyl propanoate which was vial A. Recorded the ID of sample in my laboratory note book. Placed one drop of sample into the NMR sample tube provided, using the disposable plastic pipette provided as well. Using the second clean disposable plastic pipette provided added 1.0 mL of CDCl3 to dissolve the sample. Covered the sample tube with its plastic cap and gave to the instructor to process, the 1H NMR of your sample. Using the processed 1H NMR spectra of the pure samples, labeled the signals of a, b, and c proton sets for each compound in the spectrum of unknown sample. Carried out calculations of the mole ratio of the unknown mixture, each time, using integrals for different sets of matched signals from each component of the mixture. From the two calculated ratios, determine an average ratio.


Calculations: Mole ratio: Singlet MP/Singlet EA 0.26/0.26=1 meaning 1:1 Quartet EA/Quartet MP 0.18/0.16=1.125 meaning 1:1 Triplet EA/Triplet MP

0.69/2=.345/3=.115 meaning 1:1 Discussion: So the overall mole ratio is 1:1. The unknown letter is Sample C. The researcher found this out by carrying out a set of calculations used to find the mole ratio of two compounds from proton NMR spectra. The calculations determined how accurate the mixture and spectra was. It also taught the researcher that there are other ways of determining the mole ratio of the product.