Instant Notes: Analytical Chemistry

(Tina Meador) #1
spectrum mathematically in less than a second by a computer using a fast
Fourier transform(FFT) algorithm. Multiple interferograms can be rapidly
accumulated and averaged to increase sensitivity by as much as three orders of
magnitude.
A block diagram of a typical NMR spectrometer is shown in Figure 9 and
comprises five main components:

● a superconducting solenoid or electromagnet providing a powerful magnetic
field of up to about 17 Tesla;
● a highly stable RF generator and transmitter coil operating at up to about
750 MHz;
● a receiver coil with amplifying and recording circuitry to detect and record
sample resonances;
● a sample probe positioned between the poles of the magnet;
● a dedicated microcomputer for instrument control, data processing (FFT of
interferograms) and data storage.

The homogeneity and stability of the magnetic field should be at least 1 in 10^9
to ensure narrow absorption bands and good resolution. Sample tubes are made
to spin in the sample probe at about 50 Hz by an air turbine so as to increase the
apparent field homogeneity further. The direction of the magnetic field and the
orientations of the transmitter and receiver coils must be mutually perpendic-
ular to detect sample resonances and eliminate spurious signals in the detector
cicuit as shown in Figure 9.

E12 – Nuclear magnetic resonance spectrometry: principles and instrumentation 259


Transmitter
coil

Receiver coil

Sample tube

Magnet

Sweep coils

z, B 0

RF amplifier

AF amplifier Detector RF amplifier
Recorder

ADC

Switch

Pulse
generator

RF generator
x

y

AF AF RF

Computer RECEIVER

TRANSMITTER

Fig. 9. Diagrammatic representation of an NMR spectrometer. Reproduced from R. Kellner et al., Analytical
Chemistry, 1998, with permission from Wiley-VCH, and from Nuclear Magnetic Resonanceby P.J. Hore (1995) by
permission of Oxford University Press © P.J. Hore, 1995.

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