DUMBOspindiffDQD: spin diffusion pulse program

*** Outline ***

• Code for Avance III spectrometers with topSpin2.1 operating system
• Example: ¹H in Glycine with AV500
• References

Code for Avance III spectrometers with topSpin2.1 operating system

;DUMBOspindiffDQD.ppm
;modified after Leskes, Madhu and Vega, Chem. Phys. Lett. to remove center artefact
;using STATES-TPPI, digital mode acquisition
;This pulse program was written according to the corresponding DUMBO-sequence from
;the ENS-Lyon Pulse Program Library

;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,

;p1 : proton detection pulse
;p11: excitation and reconversion proton pulses
;p9 : 1.7-4.5 usec, depending on probe deadtime

;d1 : recycle delay
;d5 : z filter delay

;l0 : 0 as initial t1
;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

;pl12: 1H power for pulses
;sp1 : 1H power for w-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

;FnMode: undefined
;MC2   : STATES-TPPI
;ns    : = 4n

;$COMMENT=homonuclear decoupling with w-dumbo
;$CLASS=Solids
;$DIM=2D
;$TYPE=homonuclear decoupling
;$SUBTYPE=explicit acquisition
;$OWNER=hf

;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+.1u"
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

1 ze                           ;acquire into a cleared memory
2 d1                           ;recycle delay
  1m rpp10
  1m rpp20
  10u reset1:f1                ;synchronise pulse and detection RF
  (p11 pl12 ph22):f1           ;excitation pulse

5 d3
  d3
  (p20:sp2 ph10^):f1           ;dumber-22
  d3
  d3
  (p20:sp2 ph10^):f1           ;dumber-22
  lo to 5 times l0

  (p11 pl12 ph23):f1           ;reconversion pulse
  d5 pl12:f1                   ;z filter delay
  STARTADC                     ;prepare adc for sampling, set reference frequency, 
                               ;defined in Avancesolids.incl
  RESETPHASE                   ;reset reference phase

  (p1 ph1):f1                  ;proton detection pulse at pl12
  .1u DWL_CLK_ON
7 dead
  acqu
  d9 RG_ON
  .1u RG_OFF                   ;take l11 complex data points
  (p10:sp1  ph20^):f1          ;w-dumbo, use 24 usec at 600 MHz or higher
  dead
  acqu
  d9 RG_ON
  .1u RG_OFF
  (p10:sp1  ph20^):f1
  lo to 7 times count          ;make sure td points are sampled

  rest
  1u  DWL_CLK_OFF
  1m
  rcyc=2                       ;next scan
  100m wr #0 if #0 zd          ;save data

  1m ip22                      ;increments all phases of ph22 by 90°
  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 rp22                     ;reset all phases of ph22 to its original values, 
                               ;i.e. to the values it had before the first ip22
                               ;in case of STATES remove semicolon at beginning of the line

  lo to 2 times count1         ;count1 = td1/2
  exit                         ;finished

ph0= 0
ph1= 0 1 2 3                   ;detection pulse phase
ph10=0 2
ph20=0 2

ph22=0 2                       ;excitation pulse phase
ph23=0                         ;reconversion pulse phase

ph30=0                         ;needed for acquisition, involved in RESETPHASE
ph31=ph22 + ph1                ;involved in STARTADC
                               ;the same data as ph31 = -ph22 + ph1