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NMR-1-theory and Instr
NMR-1-theory and Instr
Detects
E1
ΔE = h (Planck 1900)
Magnetic Nuclei
u
e.g. 4
He, 126C, 168O ….etc
2
I = 1/2 e.g. 1
1
H, 13
6
C, 19
9
F, 31
P…… etc
15
I = 1 e.g. 2
1
D, 14
N……etc
7
ω = Bo ……… (1)
- gyromagnetic ratio
ω = Bo ……… (1)
= /p (2)
p = Ih/2 (3)
(3) in (2)
= 2h (4)
=2 (5)
(1) & (5)
2= o (6)
(4) in (6)
(7) in
2I + 1
-1
- 1/2
E = o
E = o 0
E = o
+ 1/2
+1
- 3/2
- 1/2 E = h
E = o
= Bo
+ 1/2
+ 3/2
Bo = Applied field
Frequency and Field Strength
-1/2
+1/2
Frequency (MHz) and Field Strength (T)
1
H 60 100 200 300
13
C 15.1 25.1 50.3 75.5
19
F 56.5 94.1 188.2 288.2
31
P 24.3 40.5 81.0 121.3
e 3.9x104
Magnetic Properties of Some Nuclei
Isotope Spin Natural Sensitivity ν (MHz)
Abundance Rela Absb at T = 2.3
%
1
H 1/2 99.98 1 1 100.00
2
D 1 1.5 x 10-2 9.65 x 10-3 1.45 x 10-6 15.35
13
C 1/2 1.108 1.59 x 10-2 1.76 x 10-4 25.14
14
N 1 99.63 1.01 x 10-3 1.01 x 10-3 7.22
15
N 1/2 0.37 1.04 x 10-3 3.85 x 10-6 10.13
19
F 1/2 100 0.83 0.83 94.08
31
P 1/2 100 6.63 x 10-2 6.63 x 10-2 40.48
a
At constant field for equal number of nuclei, b
product of rel sensitivity & NA
The Boltzmann Distribution
- E/kT
E = e
At thermal equilibrium
N < N Δ E << kT
At 1.4 T, state is only 0.001% more populated
than state
Even at 11.7 T, (500 MHz) Δ E ~ 10-4 kJ
-x
= 1- E/kT e = 1-x + x2/ 2! -x3/ 3!
Relaxation Processes
Saturation of signal N = N
Spin-Lattice relaxation T1
Spin-Spin relaxation T2
Line width Δ
Varian Associates, CA
Introduced NMR (1955)
Improved version A-60 (1961)
• Richard Earnst (Varian), Nobel Prize 1991
Electromagnet
Superconducting Magnet
Nb alloy solenoid, dipped in liquid He (-259oC)
Special dewars: He inner chamber, N2 outer chamber
The Probe
Dedicated: 1H or 1H-13C Multinuclear (broad band)
Superconducting gradient
coils-factory set Y
Deuterium Lock
Constant ratio between the magnetic field and
RF maintained by making adjustments to the
field such that D always absorbs at the same
frequency
Resonance
o
= 2 E
= o/2
I
N
T
E
N
S FID
I
T
Y
T time
Delay Delay
FID – Free Induction Decay
A range of frequencies
Abs T1 & T2
PULSE
-1/t +1/t
Simultaneous excitation of all
the nuclei in the region by an
F
RF pulse (0-4000 Hz)
Signal to Noise Ratio (S/N)