;cpcpmg.fau (TopSpin 2.1 pl3) ;cp 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 : proton 90 at power level pl12 ;p4 : 180 degree pulse at pl22 ;p15 : contact time at pl1 (f1) and sp0 (f2) ;pl1 : X power level during contact ;sp0 : proton power level during contact ; sp0 is the max power level during shape pulse ;pl2 : =120dB, not used ;pl12 : decoupling power level (if not pl13) ;pl13 : special decoupling power level ;pl22 : rf power level ;d1 : recycle delay ;d3 : time to allow pulse ringdown, 10 to 100 us ;d6 : duration of FID ;pcpd2 : pulse duration 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) ;spnam0 : use e.g. ramp.100 for variable amplitude CP ;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 ;cnst21 : on resonance, usually = 0 ;$COMMENT=cp experiment with CPMG detection ;$CLASS=Solids ;$DIM=1D ;$TYPE=cross polarisation ;$SUBTYPE=simple 1D ;$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 #include <p15_prot.incl> ;make sure p15 does not exceed 10 msec ;let supervisor change this pulseprogram if ;more is needed #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 (p3 ph1):f2 (1u pl12):f2 ;proton 90° pulse (p15 pl1 ph2):f1 (p15:sp0 ph10):f2 ;use square.100 or ramp.100 shape for sp0 ;in proton channel F2 1u cpds2:f2 ;select appropriate decoupling sequence, switch on ;cw or tppm15 decoupling executed at power level pl12 ;or LG-decoupling executed at power level pl13 1u pl22:f1 ;set 180° pulse power level STARTADC ;arm adc RESETPHASE ;reset reference phase for detection 0.1u 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 ;set decoupling off 0.1u DWL_CLK_OFF rcyc=2 ;loop NS times 1m do:f2 ;set decoupling off 100m wr #0 ;write signal HaltAcqu, 1m ;jump address for protection exit ph0= 0 ph1= 1 3 ph2= 0 0 2 2 1 1 3 3 ph3= 0 0 2 2 1 1 3 3 ph10=0 ph30=0 ph31=0 2 2 0 1 3 3 1
Graphic representation associated with the TopSpin2.1 cpcpmg.fau pulse program.
29Si echo train of TSP-d4 in 4-mm diameter rotor spinning at 10 kHz. A contact duration P15 = 8 ms increases the amplitude of the echo train by two.
Acquisition parameters:
General | |
PULPROG | cpcpmg.fau |
TD | 7644 |
NS | 1920 |
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 |
P15 [µs] | 4000.00 |
P4 [µs] | 12.40 |
PL1 [dB] | 6.00 |
PL1W [W] | 130.4819793 |
PL22 [dB] | 6.00 |
PL22W [W] | 130.4819793 |
SFO1 [MHz] | 99.3774009 |
Channel f2 | |
CNST21 | 0.00000000 |
CPDPRG2 | tppm15 |
NUC2 | 1H |
P3 [µs] | 11.00 |
PCPD2 [µs] | 20.70 |
PL2 [dB] | 120.00 |
PL2W [W] | 0.00000000 |
PL12 [dB] | 16.00 |
PL12W [W] | 8.05732536 |
SFO2 [MHz] | 500.2113720 |
SP0 [dB] | 10.00 |
SP0W [W] | 32.07678986 |
SPNAM0 | ramp.100 |
SPOAL0 | 0.500 |
SPOFFS0 [Hz] | 0.00 |
29Si echo train of TSP-d4 in 4-mm diameter rotor spinning at 10 kHz, NS = 8, and decoupling with PL12 = 16 dB
29Si echo train of TSP-d4 in 4-mm diameter rotor spinning at 10 kHz, NS = 8, and decoupling with PL12 = 10 dB