NMR A
CQUISITION
:
THE
BASICS
S
OLID
S
AMPLE
:
Weigh 30 mg of sample into a clean and DRY test tube. If you do not have 30 mg, you may use less, but let your instructor know how much you weighed out. Obtain a disposable Pasteur Pipette and bulb and then use a “sharpie” to draw a line on the pipette at the 0.6 mL mark.
Add 0.6 mL of CDCl3 or other deuterated solvent to the test tube containing your solid.
Swirl to dissolve, then transfer the contents to a clean, dry NMR tube.
NEVER “DOUBLE DIP” INTO solvent bottle.
L IQUID S AMPLE :
Weigh 3 drops of your sample into a clean and DRY test tube.
Add 0.6 mL of CDCl3 or other deuterated solvent to the test tube containing your solid.
Swirl to dissolve, then transfer the contents to a clean, dry NMR tube.
NEVER “DOUBLE DIP” INTO solvent bottle.
P
OSITION THE SAMPLE IN THE
S
PINNER
:
Handling the Spinner with a Kimwipe, insert the capped NMR tube into the spinner such that the bottom of the tube protrudes from the spinner. Use the depth gauge at the front of the NMR magnet casing to position the NMR tube at the correct level before inserting it into the probe.
P LACE SAMPLE INTO P ROBE :
For EM-360 (furthest from door):
Holding the top of the NMR tube, place the tube/spinner in the probe with the AIR ON
(the air is ON when the arrow-shaped valve is directed forward toward the user. The air should be audible)
Turn the arrow-shaped valve counter-clockwise 90° to lower the air so that the sample is allowed to drop into position.
Turn the arrow-shaped valve another 90° counter-clockwise to increase the air pressure slightly so that the sample spins.
For EM-360A (closest to door):
Follow directions in attached document

A
CQUIRE THE SPECTRUM
:
The commands described below represent just a few of the commands that may be necessary during acquisition and processing of a 1H NMR spectrum. Take careful notes in your notebook so that you can later acquire an NMR spectrum on your own.
Sitting at the Console, use the mouse to select “
(aii)
” from the tabs at the bottom of the screen.
Enter the following commands at the H1> prompt at the bottom of the blue acquisition window. (If H1> prompt is missing, contact your instructor)

Prompt Command (TYPE bold characters)
H1>
H1>
H1>
Menu
Enter bold characters
Shim <enter>
2 <enter> ns 4
zg <enter>
<enter>
Action
This command is only necessary if you are the first person to acquire a spectrum on this instrument.
This is an automated subroutine to optimize the signal and requires approximately 2 minutes to complete
Number of scans =
4
(set to 8 or more if sample is very dilute)
Zero memory Go acquire
Store signal under
“pnmrfid” filename
Once acquisition is complete (white box in corner has disappeared), and the signal looks good, you may save the FID as follows:
Select “FILE” from menu then
Homegroup  NMRUSER  Documents  Armstrong
Give the FID a filename “yourname_experiment”
SAVE (or <enter>)
This stores the signal so that it may be processed at either one of the two work stations
Move over to workstation, open NMR (“NUTS”)
software application and only then open your file
Select “NMR” from tabs at bottom of screen to enter white processing window
<enter> a5
Note: in this application, commands do not require a carriage return. Don’t type <enter> unless you are
Macro that takes time domain signal and applies

at command line
>
>
>
> trying to exit a subroutine (or unless the directions explicitly call for it)
Fourier transformation into frequency domain. Also performs some signal processing to reduce noise and correct baseline. ap Auto phasing of signal;
If signal still looks out-of-phase after this command, contact your
instructor
HOLD DOWN LEFT MOUSE BUTTON SO CURSOR IS
ON TMS signal. Type letter
O (for offset) then number 0 (zero for 0.0 ppm)
<enter>
Sets TMS signal to zero
This is LETTER O for Offset
This is NUMBER zero for zero ppm
If you want to zoom in on a particular region of the spectrum, use “zoom” subroutine as follows: zo click left mouse button and drag through area of interest;
CTRL-E will zoom in on highlighted (Expanded) region
CTRL-F will zoom out to Full Spectrum
The Zoom subroutine can be accessed at any time. Note that if you want to integrate from within the Zoom subroutine, you must use “I”as the integrate command rather than “ID” as described below.
A carriage return will exit the zoom subroutine fb deselect areas that are NOT baseline by clicking mouse button to remove them
(pink color will disappear)
Fix Baseline

> l
<enter>
LETTER “l” to apply Least squares or
LETTER “c” for polynomial
Correction
You will see numbers flash on screen but no other visible change id c
Using left mouse button, double click at baseline to the left of each signal then move mouse to right of most signal (again at baseline) and click just once.
Repeat the double then single clicks at left and right, respectively, of each signal in the spectrum except the TMS signal until all integration regions have been selected.
If you make a mistake, you may clear by typing c or delete one integral by left clicking on the bad integral and type d
Holding mouse at smallest signal suspected to be part of spectrum, type
V
1
<enter> p
<enter>
<enter>
Integrate Data
Clear old stops
Selects a region to integrate. Integral should be displayed above
“step” for each integration region.
Sets integral values relative to a given number
VALUE of “1” implies 1 relative
H for that signal.
All other signals will be measured relative to this value.
Prints spectrum.

Type “p” twice for two copies.
Exits integration subroutine