BABA 2rotations: 1D/2D double quantum excitation, 2 rotor period, BABA pulse program for TopSpin2.1




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2D double-quantum excitation with BABA1 pulse sequence

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 P1 for selecting the 0Q -> -1Q coherence order jump.


*** Outline ***


Code for Avance III spectrometers with topSpin2.1 operating system

;baba2rot (TopSpin 2.0)

;2D SQ-DQ correlation experiment for 2 rotor periods recoupling using BABA 
;for weaker dipole dipole interactions, e.g. 19F 
;compensated for pulse imperfections
;M. Feike, D.E. Demco, R. Graf, J. Gottwald, S. Hafner, and H.W. Spiess JMR A 122, 214-221 (1996)
;written by JOS, 11/12/03

;parameters:
;d1 : recycle delay
;d0 : incremented delay (2D) [1 usec]
;pl1 : for 90 degree BABA pulses
;p1 : 90 degree pulse (in BABA sequence and in presaturation sequence)
;l1 : number of rotor cycles for recoupling, any integer
;l2 : l2*2=l1=(number rotorcycles)
;d20 :delay between saturation pulses
;l20 : # of pulses in saturation pulse train, 0 if undesired
;cnst31 : rotation rate in Hz
;ns : n*16
;FnMode: States-TPPI or STATES

;$COMMENT=SQ-DQ correlation experiment with BABA for 2 rotor periods
;$CLASS=Solids
;$DIM=1D
;$TYPE=direct excitation
;$SUBTYPE=homonuclear correlation
;$OWNER=Bruker

define delay tau
  "tau=0.5s/cnst31-p1*2"

  "d0=1u"
  "in0=1s/cnst31"
  "l1=l2*2"
  "l0=2*l1"

;cnst11 : to adjust t=0 for acquisition, if digmod = baseopt
"acqt0=1u*cnst11"

  ze
1 d1

#ifdef presat                    ;set with -Dpresat
pres, d20                        ;delay between saturation pulses
  (p1 pl1 ph1):f1                ;saturation loop if required
  lo to pres times l20
#endif /* presat */

2 d1
5 (p1 pl1 ph12):f1               ;DQ excitation block
  tau
  (p1 ph12)
  (p1 ph13)
  tau
  (p1 ph14)
  (p1 ph12)
  tau
  (p1 ph12)
  (p1 ph14)
  tau
  (p1 ph13)
  lo to 5 times l2

  d0                             ;evolution of DQ coherence if more than 1 rotor period DQ excitation

7 (p1 ph23 ipp23)                ;DQ reconversion if more than one rotor period
                                 ;increment phase ph23 pointer
  tau
  (p1 ph23 ipp23)                ;increment phase ph23 pointer
  lo to 7 times l0

  (p1 ph6):f1
  go=2 ph31
  d1 mc #0 to 1 F1PH(ip12 & ip13 & ip14, id0)
HaltAcqu, 1m
exit


ph1= 0                           ;for saturation pulse

ph12=(8) 0 2 4 6                 ; x  y -x -y
ph13=(8) 2 4 6 0                 ; y -x -y  x
ph14=(8) 6 0 2 4                 ;-y  x  y -x
ph23= 0 0 1 3 0 0 3 1            ; x  x  y -y  x  x -y  y
ph6 = 0 0 0 0 1 1 1 1 2 2 2 2 3 3 3 3
ph31= 0 2 0 2 1 3 1 3 2 0 2 0 3 1 3 1
  

Example: 31P in VPI-5 zeolite with AV500

31P 2D spectrum of VPI5 obtained with baba2rot DQ pulse program

31P BABA2rot DQ-SQ spectrum of VPI-5 zeolite; rotor spinning speed: 14 kHz.


Pulseprogram parameters for baba2rot.ppm:

General  
PULPROG baba2rot.ppm
TD 2048
NS 128
DS 0
SWH [Hz] 12500.00
AQ [s] 0.0819700
RG 4
DW [µs] 40.000
DE [µs] 6.50
CNST11 0.0000000
CNST31 14000.0000000
d0 [s] 0.00000100
D1 [s] 10.00000000
D20 [s] 0.10000000
in0 [s] 0.00007143
l0 28
l1 14
L2 7
L20 20
ST1CNT 85
ZGOPTNS -Dpresat
tau [µs] 0.00003171
Channel f1  
NUC1 31P
P1 [µs] 2.00
PL1 [dB] 5.00
PLW1 [W] 110.88822174
SFO1 [MHz] 202.4830869

Acquisition parameters:

  F2 F1
Experiment    
PULPROG baba2rot.ppm  
AQ_mod DQD  
FnMODE   States-TPPI
TD 2048 170
NS 128  
DS 0  
TD0 1  
Width    
SW [ppm] 61.7336 69.1402
SWH [Hz] 12500.000 13999.720
IN_F [µs]   71.43
AQ [s] 0.0819700 0.0060715
Nucleus1    
NUC1 31P 31P
O1 [Hz] -1584.14 -1584.14
O1P [ppm] -7.824 -7.824
SFO1 [MHz] 202.4830869 202.4830869
BF1 [MHz] 202.4846710 202.4846710


References

  1. N. Chandrakumar
    1D double quantum filter NMR studies,
    in Annual Reports on NMR Spectroscopy, Graham A. Webb (Ed.), Elsevier, Amsterdam, vol. 67, pages 265-329 (2009).
    Abstract
     
  2. Mahdy M. Elmahdy, Mihail Mondeshki, Xi Dou, Hans-Jürgen Butt, Hans W. Spiess, Klaus Müllen, and George Floudas
    Slow kinetics of phase transformation in a dipole-functionalized discotic liquid crystal,
    J. Chem. Phys. 131, 114704/1-114704/9 (2009).
    Abstract
     
  3. Ingo Schnell
    Dipolar recoupling in fast-MAS solid-state NMR spectroscopy,
    Prog. Nucl. Magn. Reson. Spectrosc. 45, 145-207 (2004).
    Abstract
     
  4. V. M. Litvinov, M. Bertmer, L. Gasper, D. E. Demco, and B. Blümich
    Phase composition of block copoly(ether ester) thermoplastic elastomers studied by solid-state NMR techniques,
    Macromolecules 36, 7598-7606 (2003).
    Abstract
     
  5. Juraj Pivarč
    Application of the Multiple Quantum NMR Spectroscopy for Investigation of the Dipole-Dipole Couplings in Amorphous Polymers,
    Halle, 4 July 2000.
    Dissertation
     
  6. Stephan Dusold and Angelika Sebald
    Dipolar recoupling under magic-angle spinning conditions,
    in Annual Reports on NMR Spectroscopy, Graham A. Webb (Ed.), Elsevier, Amsterdam, vol. 41, pages 185-264 (2000).
    Abstract
     
  7. Ingo Schnell, Adonis Lupulescu, Siegfried Hafner, Dan E. Demco, and Hans W. Spiess
    Resolution enhancement in multiple-quantum MAS NMR spectroscopy,
    J. Magn. Reson. 133, 61-69 (1998).
    Abstract
     
  8. M. Feike, D. E. Demco, R. Graf, J. Gottwald, S. Hafner, and H. W. Spies
    Broadband multiple-quantum NMR spectroscopy,
    J. Magn. Reson. A 122, 214-221 (1996).
    Abstract
     
  9. Helen Geen, Jeremy J. Titman, Johannes Gottwald, and Hans W. Spiess
    Solid-state proton multiple-quantum NMR spectroscopy with fast magic angle spinning, (DRAMA, adamantane, polycarbonate)
    Chem. Phys. Lett. 227, 79-86 (1994).
    Abstract
     

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