High power decoupling CPMG pulse program for topSpin2.1 operating system

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High power decoupling Carr-Purcell-Meiboom-Gill echo train for topspin2.1

*** Outline ***

Code for Avance III spectrometers with topSpin2.1 operating system

;hpdeccpmg.fau (TopSpin 2.1 pl3)

;HPDEC experiment with CPMG detection
;written by FAU 08.01.2009
;use rotor-synchronized CPMG train of refocusing pulses to create the echoes

;Avance III version
;parameters: 
;p3 : 90 degree pulse at pl21
;p4 : 180 degree pulse at pl21
;pl2 : =120dB, not used
;pl12 : decoupling power level (if not pl13)
;pl13 : special decoupliong power level
;pl21 : cpmg rf power level
;pl22 : =pl21 usually, =120 dB if 180° are not desired
;d1 : recycle delay
;d3 : time to allow pulse ringdown, 10 to 100 us
;d6 : enter duration of FID
;pcpd2 : pulse length in decoupling sequence (for tppm15, ~(170/90)*90°pulse duration)
;cpdprg2 : cw, tppm (at pl12), or 
;          lgs, cwlg, cwlgs (LG-decoupling here pl13 is used instead of pl12)
;zgoptns : -Dfslg, -Dlacq, or blank
;p25 : dummy pulse, not used for acq.
;l22 : # of echos to be acquired
;cnst1 : set td to number of acquired complex data points, td=cnst1

;$COMMENT=hpdec experiment with CPMG detection
;$CLASS=Solids
;$DIM=1D
;$TYPE=high power decoupling
;$SUBTYPE=simple 1D
;$OWNER=Bruker

prosol relations=<solids_cp>

#include <Avancesolids.incl>             ;commands necessary for acquisition

#ifdef fslg
#include <lgcalc.incl>
;cnst20 : RF field achieved at pl13
;cnst21 : on resonance, usually = 0
;cnst22 : positive LG offset
;cnst23 : negative LG offset
;cnst24 : additional LG-offset
#endif /* fslg */

"cnst1=((d6*2+d3*2+p4)*l22+d6+d3)/dw"
define delay rest
"rest=aq-(cnst1*dw)"
"p25=1/cnst1"
;cnst11 : to adjust t=0 for acquisition, if digmod = baseopt
"acqt0=1u*cnst11"

1 ze

2 d1                           do:f2        ;recycle delay, decoupling off
#ifndef lacq
            ;disable protection file for long acquisition change decoupling power!!!
            ;or you risk probe damage
            ;if you set the label lacq (ZGOPTNS -Dlacq), the protection is disabled

#include <aq_prot.incl>
            ;allows max. 50 msec acquisition time, supervisor
            ;may change to max. 1s at less than 5% duty cycle
            ;and reduced decoupling field
#endif /* lacq */

    1u                  fq=cnst21:f2        ;used in tppm15 for example
                                            ;if cnst21=0, make sure cp is done with proton freq
                                            ;set by O2
    (1u pl21):f1        (1u pl12):f2        ;set 90° pulse power level on F1
                                            ;set 1H decoupling power level on F2
  STARTADC                                  ;arm adc
  RESETPHASE                                ;reset reference phase for detection
  (p3 pl21 ph1):f1                          ;pulse on F1 with power level pl21
  d3                        cpds2:f2        ;cpds2=composite pulse decoupling sequence 2 which 
                                            ;uses a text file whose name is given by the 
                                            ;acquisition parameter cpdprg2 (cw or tppm15) at pl12
  (p4 ph2):f1
  d3 DWL_CLK_ON
3 d6 RG_ON
    0.1u RG_OFF
  d3
  (p4 pl22 ph3):f1
  d3
  d6 RG_ON
  lo to 3 times l22
  d6
  d3
    rest RG_OFF                do:f2          ;1H decoupling off
    0.1u DWL_CLK_OFF
  rcyc=2                                      ;loop NS times
  1m                           do:f2          ;1H decoupling off
  100m wr #0                                  ;save data in current data set
HaltAcqu, 1m                                  ;jump address for protection
exit

ph0= 0
ph1= 0 2
ph2= 1 1 3 3
ph3= 1 1 1 1 3 3 3 3
ph30=0
ph31=2 0
  
High power decoupling Carr-Purcell-Meiboom-Gill echo train for topspin2.1

Graphic representation associated with the TopSpin2.1 hpdeccpmg.fau pulse program.


Example1: 29Si in TSP-d4 with AV500

Silicon-29 echo train in tsp-d4 acquired with hpdeccpmg pulse program

29Si echo train of TSP-d4 in 4 mm diameter rotor spinning at 10 kHz.

Acquisition parameters:

General  
PULPROG hpdeccpmg.fau
TD 7644
NS 480
DS 0
SWH [Hz] 20000.00
AQ [s] 0.1911500
RG 114
DW [µs] 25.000
DE [µs] 6.50
const1 7642.463867
CONST11 0.0000000
D1 [s] 30.00000000
D3 [s] 0.00005000
D6 [s] 0.01000000
L22 9
P25 [µs] 0.00
ZGOPTNS -Dlacq
rest [s] 0.00008840
Channel f1  
NUC1 29Si
P3 [µs] 6.20
P4 [µs] 12.40
PL1 [dB] 6.00
PL1W [W] 130.4819793
PL21 [dB] 6.00
PL21W [W] 130.4819793
PL22 [dB] 6.00
PL22W [W] 130.4819793
SFO1 [MHz] 99.3774009
Channel f2  
CNST21 1.0000000
CPDPRG2 tppm15
NUC2 1H
PCPD2 [µs] 20.70
PL2 [dB] 120.00
PL2W [W] 0.00000000
PL12 [dB] 16.00
PL12W [W] 8.05732536
SFO2 [MHz] 500.2113720

Silicon-29 echo train in tsp-d4 rotating at 20 kHz acquired with hpdeccpmg pulse program

29Si echo train of TSP-d4 in 2.5 mm diameter rotor spinning at 20 kHz and low power decoupling.

Acquisition parameters:

General  
PULPROG hpdeccpmg.fau
TD 9252
NS 153
DS 0
SWH [Hz] 20000.00
AQ [s] 0.2313500
RG 512
DW [µs] 25.000
DE [µs] 6.50
const1 9250.399414
CONST11 0.0000000
D1 [s] 180.0000000
D3 [s] 0.00005000
D6 [s] 0.01000000
L22 11
P25 [µs] 0.00
ZGOPTNS -Dlacq
rest [s] 0.00009002
Channel f1  
NUC1 29Si
P3 [µs] 5.00
P4 [µs] 10.00
PL1 [dB] 120.0
PL1W [W] 0.00000000
PL21 [dB] 8.00
PL21W [W] 82.32855988
PL22 [dB] 8.00
PL22W [W] 82.32855988
SFO1 [MHz] 99.3782330
Channel f2  
CNST21 0.0000000
CPDPRG2 tppm15
NUC2 1H
PCPD2 [µs] 21.70
PL2 [dB] 120.00
PL2W [W] 0.00000000
PL12 [dB] 20.00
PL12W [W] 3.20767903
SFO2 [MHz] 500.2109330

Silicon-29 echo train in tsp-d4 rotating at 20 kHz acquired with hpdeccpmg pulse program

29Si echo train of TSP-d4 in 2.5 mm diameter rotor spinning at 20 kHz and high power decoupling.

Acquisition parameters:

General  
PULPROG hpdeccpmg.fau
TD 9252
NS 160
DS 0
SWH [Hz] 20000.00
AQ [s] 0.2313500
RG 512
DW [µs] 25.000
DE [µs] 6.50
const1 9250.399414
CONST11 0.0000000
D1 [s] 180.0000000
D3 [s] 0.00005000
D6 [s] 0.01000000
L22 11
P25 [µs] 0.00
ZGOPTNS -Dlacq
rest [s] 0.00009002
Channel f1  
NUC1 29Si
P3 [µs] 5.00
P4 [µs] 10.00
PL1 [dB] 120.0
PL1W [W] 0.00000000
PL21 [dB] 8.00
PL21W [W] 82.32855988
PL22 [dB] 8.00
PL22W [W] 82.32855988
SFO1 [MHz] 99.3782330
Channel f2  
CNST21 0.0000000
CPDPRG2 tppm15
NUC2 1H
PCPD2 [µs] 6.80
PL2 [dB] 120.00
PL2W [W] 0.00000000
PL12 [dB] 10.00
PL12W [W] 32.07678986
SFO2 [MHz] 500.2109330

Solid-state NMR bibliography for:

Aluminum-27
Antimony-121/123
Arsenic-75
Barium-135/137
Beryllium-9
Bismuth-209
Boron-11
Bromine-79/81
Calcium-43
Cesium-133
Chlorine-35/37
Chromium-53
Cobalt-59
Copper-63/65
Deuterium-2
Gallium-69/71
Germanium-73
Gold-197
Hafnium-177/179
Indium-113/115
Iodine-127
Iridium-191/193
Krypton-83
Lanthanum-139
Lithium-7
Magnesium-25
Manganese-55
Mercury-201
Molybdenum-95/97
Neon-21
Nickel-61
Niobium-93
Nitrogen-14
Osmium-189
Oxygen-17
Palladium-105
Potassium-39/41
Rhenium-185/187
Rubidium-85/87
Ruthenium-99/101
Scandium-45
Sodium-23
Strontium-87
Sulfur-33
Tantalum-181
Titanium-47/49
Vanadium-51
Xenon-131
Zinc-67
Zirconium-91
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