Since non-phase cycling is applied to the BABA reconversion pulse, four-phase cycling is applied to the BABA excitation pulse for filtering DQ coherences and four-phase cycling is applied to the detection pulse P12 for selecting the 0Q -> -1Q coherence order jump.
;DUMBOdqBABA1sq (Avance II+ version) ;2D DQ-SQ proton-proton correlation, with BABA1 DQ excitation/reconversion ;with homonuclear DUMBO decoupling DQ evolution without prepulses during t1 ;and windowed DUMBO acquisition ;S. P. Brown, A. Lesage, B. Elena and L. Emsley, J. Am. Chem. Soc. 126, 13230-13231 (2004). ;M. Feike, D.E. Demco, R. Graf, J. Gottwald, S. Hafner, and H.W. Spiess JMR A 122, 214-221 (1996) ;modified after Leskes, Madhu and Vega, Chem. Phys. Lett. to remove center artefact ;p9 2.4-4.5 usec, depending on probe deadtime, usually: ;for 200 and 300 MHz, CRAMPS probe required or use 4.5 usec, ;acqu or p9 must be as short as possible, avoiding dipolar coupling effects between DUMBO sequences, ;l11 or d9 must be as large as possible to improve S/N ratio, but keeping acqu positive and small, ;parameters: ;p1 : 90 degree pulse in BABA and presaturation sequences ;p12 : 90 degree 1H detection pulse ;p9 : acquisition window, 1.7-4.5 usec, depending on probe deadtime ;p10 : windowed dumbo pulse for t2 ;p20 : dumber-22 pulse for t1 ;d1 : recycle delay ;d5 : z filter delay ;d20: delay between saturation pulses ;l0 : 0 as initial t1 ;l1 : number BABA1 cycles, for protons 2-4 in real solids ;l3 : t1-increment multiplier, usually 2-4, to reduce required number of rows ;l11: number of oversampled data points to be averaged into one dwell point ;l20: # of pulses in saturation pulse train, 0 if undesired ;pl1 : 1H BABA1 and presaturation power ;pl12: 1H power for pulses P1 ;pl13: dumbo power ;sp1 : 1H power for windowed dumbo-1 (t2) ;sp2 : 1H power for dumber-22 (t1) (usually somewhat less power than sp1 since ; there is no window), set to pl13 as in setup experiments ;cnst31 : rotation rate in Hz ;ns : n*16 ;FnMode : undefined ;MC2 : STATES-TPPI ;zgoptns:-Dpresat or blank ;$COMMENT=SQ-DQ experiment with BABA for 1 rotor period ;$DIM=2D ;$TYPE=direct excitation ;$SUBTYPE=homonuclear correlation ;$OWNER=Bruker ;$CLASS=Solids ;cnst11 : to adjust t=0 for acquisition, if digmod = baseopt "acqt0=1u*cnst11" dwellmode auto #include <Avancesolids.incl> #include <Delayssolids.incl> "d3=p9" ;p9 sets the window to make sure it is in microseconds "d9=0.1u*(l11)" ;set the sampling window, defined in Avancesolids.incl "blktr2 = 0.6u" ;this opens the transmitter gate 0.6 usec before the ;pulse, so the transmitter noise is not sampled "l0=0" ;reset F1 dwell counter "inf1=(l3*(2*d3+p20))*2" ;t1 increment "sp1=pl13" "sp2=pl13" define delay dead "dead=1.2u" define delay acqu ;small window, defined by d3, 2.5-4.5 usec depending "acqu=2*p9-1.2u-d9-.1u" ;on probe deadtime ;acqu or p9 must be as short as possible, avoiding dipolar coupling effects ;l11 or d9 must be as large as possible but keeping acqu positive define delay cycle "cycle=4*p9+2*p10+.2u" define loopcounter count "count=aq/cycle" ;make sure td datapoints are sampled define delay rest ;make sure sampling proceeds throughout the sequence "rest=aq-(count*cycle)" define loopcounter count1 ;for STATES-TPPI procedure "count1=td1/2" ;and STATES cos/sin procedure define delay tau "tau=0.5s/cnst31-p1*2" "d31=1s/cnst31" 1 ze ;acquire into a cleared memory 2 d31 #ifdef presat ;set with -Dpresat pres, d20 ;delay between saturation pulses (p1 pl1 ph4):f1 ;saturation loop if required lo to pres times l20 #endif /* presat */ d1 ;recycle delay 10u reset1:f1 ;synchronise pulse and detection RF 1m rpp15 ;reset phase list pointer in w-dumbo 1m rpp25 ;reset phase list pointer in dumber-22 3 (p1 pl1 ph1):f1 ;BABA1 DQ excitation: tau (p1 ph10):f1 (p1 ph11):f1 tau (p1 ph12):f1 lo to 3 times l1 5 d3 ;DQ evolution: d3 (p20:sp2 ph25^):f1 ;dumber-22 d3 d3 (p20:sp2 ph25^):f1 ;dumber-22 lo to 5 times l0 6 (p1 pl1 ph2):f1 ;BABA1 DQ reconversion: tau (p1 ph20):f1 (p1 ph21):f1 tau (p1 ph22):f1 lo to 6 times l1 d5 pl12:f1 ;z filter delay STARTADC ;prepare adc for sampling, set reference frequency, ;defined in Avancesolids.incl RESETPHASE ;reset reference phase (p12 ph3):f1 ;90° detection pulse at pl12 .1u DWL_CLK_ON 7 dead acqu d9 RG_ON .1u RG_OFF ;take l11 complex data points (p10:sp1 ph15^):f1 ;w-dumbo, use 24 usec at 600 MHz or higher dead acqu d9 RG_ON .1u RG_OFF (p10:sp1 ph15^):f1 lo to 7 times count ;make sure td points are sampled rest 1u DWL_CLK_OFF rcyc=2 ;next scan 100m wr #0 if #0 zd ;save data 1m ip1 ;increments all phases of ph1, ph10, ph11, 1m ip10 ;and ph12 by 45°, but 90° phase for DQ coherence 1m ip11 1m ip12 lo to 2 times 2 ;t1 quadrature detection 8 1m iu0 ;increment counter l0 by 1 lo to 8 times l3 ;for multiple t1 increment ;1m rp1 ;reset all phases of ph1, ph10, ph11, and ph12 ;1m rp10 ;to their original values, i.e. to the values they ;1m rp11 ;had before the first ip1, ip10, ip11, and ip12 ;1m rp12 ;in case of STATES remove semicolon at beginning of the 4 lines lo to 2 times count1 ;count1 = td1/2 exit ;finished ph4=0 ;for presaturation pulse ph1= (8) 0 2 4 6 ; x y -x -y ph10=(8) 4 6 0 2 ;-x -y x y ph11=(8) 2 4 6 0 ; y -x -y x ph12=(8) 6 0 2 4 ;-y x y -x ph2= 0 ; x ph20=2 ;-x ph21=1 ; y ph22=3 ;-y ph25=0 2 ;dumber-22 phase during t1 ph15=0 2 ;windowed dumbo phase during t2 ph3= 0 0 0 0 1 1 1 1 2 2 2 2 3 3 3 3 ;detection pulse ph30=0 ;needed for acquisition, involved in RESETPHASE ph31=0 2 0 2 1 3 1 3 2 0 2 0 3 1 3 1
RN-DQ/SQ-DUMBO excitation pulse sequence.
BABA-DQ/SQ-SAM excitation pulse sequence.
DQ-DUMBO excitation pulse sequence.