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Pellegrino Conte
pellegrino.conte@unina.it
Dipartimento di Scienze del Suolo, della Pianta e dellAmbiente Universit di Napoli Federico II Via Universit 100, 80055 Portici (Na), ITALY
1. Analyses of the organic and inorganic soil components 2. Quantification of the different chemicals belonging to natural organic matter (humic substances) 3. Evaluation of the transformation of soil organic matter as affected by soil management, soil formation, soil transformation and so on
Classical CPMAS
13C
NMR sequence
0 0
-1
2.96 s
The 1H 90 pulse is that obtained by halving the 180 pulse measured by inversion recovery
O
176 ppm 43 ppm
Glycine
OH
176
NH2
43
300
200
-100
Due to the circuit impedance, the inversion recovery experiment on glycine provided 1H 90 pulse that was too long. In fact, the P360 experiment revealed a residual NMR signal of both carbons of glycine.
O
176 ppm 43 ppm
Glycine
OH
176
NH2
43
Classical CPMAS 13C spectrum with 1H 90 pulse of 2.96 s P360 CPMAS 13C spectrum. 1H 360 pulse: 4 x 2.96 s= 11.84 s 4x90 CPMAS 13C spectrum. 1H 90 pulse: 2.80 s
300
200
-100
O O
H2 O C
79 ppm
33 ppm
S O
C H2
H2 C 24 ppm CH3
14 ppm
SDS
33
n=9
24 14
79
Classical CPMAS 13C spectrum with 1H 90 pulse of 2.96 s P360 CPMAS 13C spectrum. 1H 360 pulse: 4 x 2.96 s= 11.84 s 4x90 CPMAS 13C spectrum. 1H 90 pulse: 2.80 s
300
200
-100
OH
CMC
*
6
O
O H2C
74 C2-C6
4 5
HO
2 3
O
O O
n
104 ppm
104 178
62
A. CP spectrum of CMC obtained with a proton pulse of 2.80 s B. CMC spectrum acquired with the 4 x 90 pulse sequence and a 2.80 s proton pulse C. as in B. but with a proton pulse of 2.78 s;
300 200 100 Chemical Shift (ppm) 0 -100
HMB
A. CP spectrum of HMB with 1H pulse of 2.80 s B. 4 x 90 HMB spectrum with 1H pulse of 2.80 s C. 4 x 90 HMB spectrum with 1H pulse of 2.83 s.
Car
132
17
-CH3-
300
200
-100
pepsine
71 74 92 172 107 61 54 40 33 25
A. CP spectrum of pepsine obtained with a proton pulse of 2.80 s B. pepsine spectrum acquired with the 4 x 90 pulse sequence and a 2.80 s proton pulse;
128
300
200
-100
HA
33
52 72
A. CP spectrum of HA with 1H pulse of 2.80 s B. 4 x 90 HA spectrum with 1H pulse of 2.80 s C. 4 x 90 HA spectrum with 1H pulse of 2.78 s.
300
200
-100
CONCLUSIONS 1. The standard calibration by inversion recovery provided a too long 1H 90 pulse 2. Only few attempts were needed to find the correct 1H 90 pulse by 4x90 pulse sequence 3. The 4x90 pulse sequence was successfully and rapidly applied on very complex organic systems such as a protein (pepsine) and a humic acid 4. The 4x90 pulse sequence can efficaciously replace the standard calibration with the inversion recovery routine