What is NMR?

Nuclear Magnetic Resonance (NMR) spectroscopy is (probably)

the most powerful tool available for determining the structure
of organic compounds. This technique relies on the ability of
atomic nuclei to behave like a small magnet and align
themselves with an external magnetic field. This magnetic field
makes the possible spin-states of the nucleus differ in energy,
and using NMR techniques the spins can be made to create
observable transitions between the spin states. Common NMR
active nuclei are 1H, 13C, 31P, 15N, 29Si, and many more.
Nearly every element has at least one isotope that is NMR
active

What is it used for?

To identify and/or elucidate detailed structural information
about chemical compounds, For example:

Determining the purity of medicines before they leave the

factory.

Identifying contaminants in food, cosmetics, or medications

Helping research chemists discover whether a chemical

reaction has

occurred at the correct site on a molecule

Identifying drugs seized by police and customs agents

Checking the structure of plastics, to ensure they will have the

desired

properties

How does it work?

It works by placing a sample between the pole pieces of
magnet (electromagnet), surround by coil of wire. Radio
frequency (r.f.) is fed into wire at a swept set of frequencies,
when the combination of the field and frequency match the
resonant frequency of each nucleus r.f. is emitted and captured
by receiver coil. This emission is then plotted against frequency.
This will record it as signal or peak.

Magnetic safety?
A NMR contains a magnet for operation and the magnetic fields
within about one meter of this magnet are extremely strong. Do
not bring any iron containing material (tools, gas cylinder,
electric equipment and mechanical watches) near the magnet.
People with a pacemaker should not enter the NMR room. The
force exerted by the magnet increases dramatically within a
certain critical distance. You may not even notice an attractive
force until it is too late and the object is stuck to the magnet.
Magnetic media such as floppy disks, tapes and credit cards
can be erased if brought close to the magnet. Make sure you
keep these items outside the 5 gauss perimeter of the magnet
(gauss is the unit describing the strength of the magnetic field
3 meter distance).

How to prepare a perfect NMR sample for

analysis

1. It is general practice to use deuterated solvents for two

reasons.

a. The deuterium can be used for field frequency lock,

making spectral resolution easier to assure and
thereby saving you valuable time.

b. Solvents containing regular hydrogen yield large

signals that may swamp those of your sample: the
situation is made worse by saturation effects that
broaden large signals. We recommend the use of
deuterated solvents wherever possible.
2. The sample must be sufficiently soluble to yield an NMR
spectrum. For 1H NMR, it is recommended to dissolve
between 5 and 10 mg in between 0.4 and 0.6 mL of
solvent so that the sample depth is at least 4.0 cm in the
tube. For high molecular weight samples, more
concentrated solutions are sometimes recommended.
However, too concentrated a solution leads to lower
resolution due to saturation and/or increased viscosity. For
13
C NMR between 10 and 20 mg of sample is
recommended. If you do not have enough sample or
cannot achieve high enough solubility, it may still be
possible to obtain a spectrum although it is recommended
that you request 500 MHz service and the spectrum will
take longer to acquire. We have observed 1H signals with
less than 0.1 mg of sample and 13C signals with less than 1
mg of sample.
 APPENDIX 1
Basic NMR acquisition and processing

STEP 1: INSERT SAMPLE

Load your sample into the Auto sampler. Be careful to avoid
blocking the location

reserved for the sample currently in use.

STEP 2: CREATE A NEW STUDY

Fill in the information associated with your sample, such as sample
name,

Solvent, sample number and any other comments.

STEP 3: BULID EXPERIMENT QUEUE

Click on the button(s) in the experiment selector, such as proton,
carbon.

2D .etc that correspond to the experiments you wish to collect on

your

Sample and optimise the parameters of the experiment.

STEP 4: RUN EXPERIMENT QUEUE

Once the study Queue has been built with desired experiments,
select location

and clicks submit. Then click cancel to exit submit mode.

STEP 5: PROCESSING PROGRESS CAN BE MONITORED IN THE

STUDY QUEUE WINDOW
Select View Spectrometer. And from drop-down list select your run.
 Note that completed nodes are green, the active node is blue, and

Queue nodes are yellow.

STEP 6: PHASE CORRECTION

Click on the process tab and then click on Default panel to select

Auto phase. This will correct the base line.

STEP 7: CALIBRATION
Narrow the spectrum to the area where the calibration peak is

Put the red cursor at the centre of reference peak, and then click
at

panel by TMS. This will calibrate the spectrum.

7.26 for CDCl3

0.00 for TMS etc
4.76 for HOD

STEP 8: INTEGRATION
Click on integration button in the right toolbar

Perform integration as per notes

STEP 9: PEAK LABELLING

Click on peak Thresh hold and then click find peaks

Perform the labelling.

STEP 10: PLOT

Click on Plot, then Auto plot Preview. Once you satisfied with
spectrum, then

print the spectrum.