Protocol: Mqmas3qzf2d  Sequence: mqmas3qzf2d.c  Apptype: solidseq1d

Description: 

3-quantum multiple quantum MAS with a third Z-filter pulse and a choice 
of SPINAL64 or TPPM decoupling. Used to obtain a 2D MQMAS spectrum for 
all spins 3/2 to 9/2. 

Additional Software: 

reset_mqmas - sets a 2D spectrum with par2d.  This macro is run from 
              the protocol. 
mqf1shear - macro that sets the parameter daslp that is used to shear 
              the data in F1. 
mqf1ref3q - references and scales F1 using the "split T1" dwell time.
mqf1ref3qs - references and scales F1 using the scaled method of 
              Amoureux and Pruski.    

Setup: 

Load a calibrated data set and select the protocol Mqmas3qzf2d.  For a 
new nucleus calibrate with Onepul and then select Mqmas3qzf2d.  

Select the desired decoupling method, TPPM or SPINAL. The manual file 
onepul describes calibration of decoupling. 

Step 1. With a solid quadrupolar sample determine the maximum of the 
hard-pulse nutation curve using Onepul. The nutation curve will be 
quite distorted and the maximum will be one-half to one-third the 
calibrated pwX90 of a solution. Record aX90 and pwX90 for the maximum. 

Step 2. Redo the nutation measurement with an amplitude 20 to 30 times 
smaller. It may be necessary to reset tpwr to obtain the smaller 
amplitude. This nutation curve will be a sinusoid. 

Select Mqmas3qzf2d. Set pw1Xmqmas = 3.0*pwX90 from (step 1). Set pw2Xmqmas 
= pwX90 from (step 1).  Set aXmqmas = aX90 from (step 1). 

Set pwXzfsel = pwX90 from (step 2). Set aXzfsel = aX90 from (step 2). 
Set dbXzfsel = tpwr from (step 2). 

Set tXzfsel = 10 ?s. Set ival to the spin of the observe nucleus, 1.5, 
2.5 etc. 

Set the F1 spectral width on the Acquisition page equal to the MAS 
Rate, ni = 64 and phase = 1,2. Press Setdaslp on the Sequence page to 
set daslp. 

With ni = 1 and nt = 24 or a multiple, fine adjust pw1Xmqmas and 
pw2Xmqmas with a double array. 

Reset ni and run the 2D experiment. When complete process with wft2da. 
Reference F1 based on F2 by pressing method 1 or method 2. 

Parameter Groups: 

mqmasX:  Module:  no 
Sequence:  mqmas3qzf2d.c      
Description:  Implements two-pulse MQMAS on obs with an F1 delay d2 in 
              between the pulses.
Parameters:  Sequence Page
       aXmqmas - the amplitude of the obs pulses. 
       pw1Xmqmas - the first pulse of MQMAS, typically a 20 to 40-
              degree flip angle, based on the solution-state 90-degree 
              pulse. 
       pw2Xmqmas - the second pulse of MQMAS, typically a 90-degree 
              flip angle based on the solution-state 90-degree pulse.  

3QshearX: (processing) Module:  no
Sequence:  mqmas3qzf2d.c     
Description:  Shows the parameters for MQMAS shearing for 3Q sequences.  
Parameters:  Sequence Page
       ival - the spin quantum number.
       daslp - first-order phase increment in F1.
       scalesw1 - scale factor for F1.
Macros: 
       mqf1shear - sets daslp. 
       mqf1ref3q - scales F1 to correspond to a "split-t1" dwell time. 
       mqf1ref3qs- scales F1 according to the procedure of Amoureux and 
              Pruski.  

zfselX:  Module:  no
Sequence:  mqmas3qzf2d.c  
Description:  Implements a selective, square 90-degree pulse with both 
              amplitude and attenuation control to provide a Z-filter 
              in MQMAS and STMAS experiments.  The amplitude change 
              takes 3.0 us during the t1Xzfsel delay. The attenuation must 
              be reset for further hard pulses.  
Parameters:  Sequence Page
       aXzfsel - amplitude of the selective obs Z-filter pulse. 
       dbXzfsel - attenuator setting for the selective obs Z-filter 
              pulse. 
       tXzfsel - delay before the refocusing pulse requires a minimum 
              value of 3.0 us for the attenuator change. 
       pwXzfsel - selective 90-degree flip on obs. 

Hseq:  Module:  yes 
Sequence:  tancpx.c      
Description: Chooses SPINAL or TPPM decoupling on the dec channel 
             during acquisition.
Parameters:  Sequence Page - the Hspinal and Htppm groups overlap.
       Hseq - chooses the decoupling sequence, TPPM or SPINAL. 
Implementation:  DSEQ dec = getdseq("H");  The router implements 
             getspinal() or gettppm(). 
Underscore functions: _dseqon(dec); runs _tppm(); or _spinal();_
             dseqoff(dec); runs decprgoff();  

Hspinal:  Module:  yes 
Sequence: tancpx.c  
Description:  Implements SPINAL decoupling on the dec channel during 
              acquisition.  
Parameters:  Sequence Page
       aHspinal - amplitude of the dec channel. 
       pwHspinal - approximate 180-degree flip angle on resonance. 
       phHspinal - +/- small angle phase. SPINAL64 is implemented 
              with phases = +/- 1.0, +/- 1.5 and +/-2.0 times 
              phHspinal. 
       chHspinal = 'dec' must be set (not shown).
Implementation: SPINAL dec = getspinal("H"); or DSEQ dec = 
              getdseq("H");  
Underscore functions: _spinal(dec); and decprgoff(); or 
             _dseqon(dec); and _dseqoff(dec);   

Htppm:  Module:  yes 
Sequence:  tancpx.c      
Description:  Implements TPPM decoupling on the dec channel during 
              acquisition.  
Parameters:  Sequence Page
       aHtppm - amplitude of the dec channel. 
       pwHtppm - approximate 180-degree flip angle on resonance. 
       phHtppm - +/- small angle phase. TPPM is implemented 
              with phases = +/- 1.0 times phHtppm for alternating 
              pulses.  
       chHtppm = 'dec' must be set (not shown).
Implementation: TPPM dec = gettppm("H"); or DSEQ dec = getdseq("H");   
Underscore functions: _tppmon(dec); and decprgoff(); or _dseqon(dec);
              and _dseqoff(dec);   
