chemsample-NMR-methods


 * __ NMR Protocol in General Terms ~ __**

First we cleaned 8 id NMR tubes using acetone and chloroform - done under a hood. We made sure to keep this under a hood because the chloroform is a toxic carcinogen. Then we put 0.5 mL of chloroform into each of the NMR tubes. A drop of each solution was added to each NMR tube: Unknowns # 2, # 3, # 4, # 7, & # 11 as well as ethyl-4-methylbenzoate, acetophenone and ethyl acetate. Each tube was put in the NMR machine one by one.



When dealing with the NMR machine, we put each NMR tube in the narrow opening, making sure to press the button in the machine and releasing it slowly. The switch was then flipped to make sure that the tube would spin. The lid of the NMR machine was closed and then the computer was used to obtain a graph. When the NMR machine calibrated we typed in "shim", pressed enter, typed "2" when prompted, and pressed enter. When the machine was done we typed "zg", pressed enter, and saved the file on the desktop.

01) Open NUTs. 02) File > open file. 03) Process > FT 04) Process > Phase > Auto phase. 05) Enter twice. 06) Type "zo". Highlight spectra peaks and back click on highlighted region. 07) Enter twice. 08) Type ID and click two times on the left side of each peak and once on the right side. Do no do this for the TMS peak. 09) Enter twice. 10) Control I 11) Type "pp" and enter. 12) Print screen and paste this graph into paint and upload onto wiki.
 * The NUTs program was used to open the files and look at the graphs.** The following steps were used to successfully alter the graph so we could look at the peaks:


 * __ Sub-Group Protocols ~ __**

//Conducted by: Student A//
 * __NMR ~__**

Essentially, the protocol I followed while working on my NMR samples was the same as above ... I simply want to mention the minor differences, and the manner in which I conducted them (done so in a bullet sort of format below).

- Prepared two 5 mm (i.d.) NMR tubes (one for known, and one for unknown). The tubes were cleaned under a fume hood in the Orgo lab with (first) acetone, and (second) dichloromethane. The outside of the tube was then thoroughly cleaned with a kim wipe (or two).

- Returning to the spec lab, I prepared each sample ... - Sample 1, known ( 2-pentanone ): prepared by adding two drops of the liquid, followed by 0.5 mL chloroform (pipetted). The tube was then capped and labeled. - Sample 2, Unknown ( # 3 ): prepared in the same manner.

- After preparation was finished, I waited for about ... //Forever!// ... until the NMR machine was available. The procedure for running the samples, and obtaining a spectra are described above - refer for protocol on operation.

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