0 5 instrmtn nmr spctromtr
TRANSCRIPT
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Nuclear Magnetic Resonance
ANIMATED ILLUSTRATIONS
MS Powerpoint Presentation Files
Uses Animation Schemesas available in MS XP or MS 2003 versions
A class room educational material
File-5 NMR Spectrometer: Instrumentation
http://ugc-inno-nehu.com/links_from_web.html
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cosine Sine arbitrary phae sinuous
Z-direction
Z-di
rection
100 MHzElectro-magnet/Permanent magnet
Systems
Supercon
magnet systems
above 100MHzup to 900MHz as
known currently
Magnet
Currentsource
Superconduc
ting current
carrying coils
Pulse widths
could be
10-2 s
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CW RF Oscillatormw power
RFCrystal
Detector
Display/RecordPulsed RF Transmitter
Probe with
sample coiland sample
in Magnetic
Field
High gain RF
receiver/detector
Time domain signal
to computer for FFT
Display monitor/Plotter
Signal
generation
Signal
receiving
and
detection
CW Modeof
detection
Pulsed
Mode of
Detection
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Flowing Current and Induced
Magnetic Fields in a Solenoid
Electrons (Blue
Circles) Moveand the
Conventional
Current Flows
in the Opposite
direction.
The MOTION of the (red)isolated (?) northpoles indicate the induced field
distributions and in reality there are no lines existing for the LINES of FORCES (as
drawn in the previous slide. It is a virtual line and LOCUS of the point North pole.)
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-1.50
-1.00
-0.50
0.00
0.501.00
1.50
0.0 5.0 10.0 15.0 20.0 25.0
cosine Exponenetial product(cos*exp)=fid
PULSE WIDTHPEAK to PEAK PULSE Amplitude
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Free
Induction
Digitized
FID analog signal
FID digitized points
Received
Analog
Signal
Analog to
Digital
Converter
A D C
Digitized
Signal
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FID
FT Real
FT Imag.
Integration
All the signal shapes have been calculated in MS EXCEL
In practice FFT program calculates Frequency domain spectra from the time domain signal
Time Domain Signal
Frequency Domain Spectra after FT
Similar to the CW mode Spectra
Pulsed
detection
mode
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ADC
CW RF
Source Gate
Pulse
Programmer
DC Pulse
Power
Amplifier
Rectangular RF Pulse
Sample
coil in the
Probe
withsample
Low noise RFPreamplifier
FID
High Gain Signal
Amplifier
Phase Sensitive
DetectorReference Signal
computer
[FFT]
Spectrum to
display
monitor/Plotter
High Power
RF Pulses toProbe
HR NMR in
Liquids 100W
NMR of Solids
3KW PP
Matched 50
TimeDomain
signal
Transmitter
Receiver
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CW Mode
Sample
tube with
sample
RF Bridge
(HybridJunction)
RF Source(sweep
generator)
Scope
50
RF Signal
receiver-
detector
Basic Probe unit is a
Resonance Circuit
with tunable splitcapacitors
configuration for
matching.
CW Mode
High-Power pulse
transmitterReceiver
off time
Low noise
pre-amplifier
/high gain
receiver/PSD/
Digital
computer/Plo
tterPulsed RF mode
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Transmitter ON
time
Probe &
sampleCrossed Diodes
ReceiverReceiverOFF time
Receiver
Silent or dead
time
DATA
acquisition
starts at this
time
12345
After the RF pulse, the FID is the
impulse response from the sample
spin system. The pulsing and FID can
be repeated and added to acquire the
averaged signal for better signal to
noise ratio
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exp1.9 exp2.8 exp5.8 exp8 exp12
exp1.9 exp12
Long T2
Short T2
Achieving a Sharp signal
depends on the homogeneity
of the magnetic filed:Shimmimngthe magnetic
field using gradient
correction coils and sample
spinning are the provisions in
the spectrometer system for
improving the homogeneity
Signal
level
Noise
Level
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HR PMR ch3ch2oh
0
1
2
3
4
5
23487398123148173198223248273298323348
frequency from TMS
Intensity/Amplitude
HR PMR ch3ch2oh
Moderate Resolution
HR PMR Spectrum
CH3
CH2OH
= 1.13 ppm
TMS= 0 ppm
Acidic medium: spin coupling
for OH protons do not show up
This calculated and simulated [60 MHz] spectrum has the chemical shift
and frequency values as obtained from a real NMR spectrum of alcohol.
The above figure plotted using MS Excel application and line drawing
from MS WORD drawing tools.High Resolution spectrum as shown
above would be possible with good homogeneity of the magnetic field.
5.24 ppm
3.61 ppm1.13 ppm
0
OH-CH2-CH3
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Equal number of lines pass through fixed area
of cross section along the length
3 lines
inside
6 lines
inside
Linear Field Gradient
along z-axis.
Along the length samenmr frequency for the
sample
NMR
frequency
will vary
linearlyalong the
length.
In the Pulsed Field GradientPFGand Magnetic Resonance Imaging
MRItechniques calculated fieldgradient are externally superposed.The inherentunwanted and
incidental
inhomogeneities
are reduced by
Shimming and
sample spinning