Double resonance experiments

(not involving protons)

19F/13C observe with 31P decoupling

13C/31P observe with 19F decoupling

31P/19F observe with 13C decoupling

 

Double resonance experiments that do involve protons, such as 13C observe with 1H decoupling, or 31P observe with 1H decoupling, 1H observe with 31P decoupling have been standard and straight forward to set up. In fact they have been so simple that, at least for the first two cases, you can just recall the standard parameters and "ga".

This is not the case for other double resonance experiments, which do not involve 1H. In fact there are quite some hardware changes necessary. We recommend that you talk to us, before you attempt these experiments. (Please keep in mind that if the spectrometer is set up wrong, in the best case you don’t get any signal or no effect to your spectrum. In the worst case, you can damage the spectrometer and probe).

19F observe with 31P decoupling

 

Software setup:

  1. Recall standard 19F parameters.
  2. then type dn=’P31’ dof=(your value from the 31P spectrum)
  3. rf(1,3,2)

Hardware setup:

  1. Terminate the cable labeled "Console Output #2" with the big black terminator.
  2. Connect the cable labeled "Console Output #3" to the input at magnet console interface box (MCIB) "B Band Amp" (from where you took off the cable labeled "Console Output #2").

 

When you are done, you have to set the instrument back to standard conditions!

Here is how to:

  1. Terminate the cable labeled "Console Output #3" with the big black terminator.
  2. Connect the cable labeled "Console Output #2" to the input at magnet stand "B Band Amp" (from where you took off the cable labeled "Console Output #2").

The software changes will be undone automatically, when you set up a new experiment.

13C observe with 31P decoupling,(and 1H decoupling)

 

Software setup:

  1. Recall standard 13C parameters.
  2. then type dn2=’P31’ dpwr2=45 dm2=’nny’ dmm2=’w’ homo2=’n’
  3. determine and enter dof2=(your value) from the phosphorous spectrum
  4. (only if proton decoupling is NOT wanted, type dm=’n’)

Hardware setup:

  1. Remove the terminator from the cable labeled "Console Output #3".
  2. Connect the cable to the filter "Bandpass 131-171 MHz".
  3. Connect the band pass filter to one input of the power combiner box ("2-Way combiner").
  4. Connect the filter "Bandpass 98-120 MHz" to the other input of the power combiner box.
  5. Detach the cable between the probe (X-nucleus) and the "Magnet Console Interface Box" (MCIB) from the MCIB. Attach this end to the output of the power combiner box (third connector, opposite side).
  6. Connect a new cable to the bandpass filter "98-120 MHz" and to the input at the magnet stand, from where you have just taken off the probe cable.

 

When you are done, you have to set the instrument back to standard conditions!

Here is how to:

  1. Terminate the cable labeled "Console Output #3" with the big black terminator.
  2. Connect the cable from the probe (X-nucleus) directly to the "Magnet Console Interface Box".
  3. Deposit all extra electronics back onto the spectrometer console.

The software changes will be undone automatically, when you set up a new experiment.

13C observe with 19F decoupling, (no 1H decoupling possible)

Software setup:

  1. Recall standard 13C parameters.
  2. then type dn=’F19’ dof=(your value determined from you 19F spectrum)
  3. rf(3,1,2)

Hardware setup:

  1. Place the big black 50 Ohm terminator from the cable labeled "Console Output #3" on to the cable labeled "Console Output #2", currently at the Magnet Console Interface Box (MCIB).
  2. Connect the cable labeled "Console Output #3" to the input at the MCIB "B Band Amp" (from where you took the cable labeled "Console Output #2").
  3. Open the right door of the console. In the upper right corner you find three boards labeled XMTR. Move the lowest cable (J2X5) from the middle XMTR board to the equivalent BNC connector at the left board.

 

When you are done, you have to set the instrument back to standard conditions!

Here is how to:

  1. Terminate the cable labeled "Console Output #3" with the big black terminator.
  2. Reconnect the cable labeled "Console Output #2" to the input at MCIG "B Band Amp" (from where you took off the cable labeled "Console Output #3").
  3. Change the cabling in the console back from the left to the middle XMTR board

The software changes will be undone automatically, when you set up a new experiment.

31P observe with 19F decoupling, (no 1H decoupling possible)

Software setup:

  1. Recall standard 31P parameters.
  2. then type dn=’F19’ dof=(your value determined from you 19F spectrum)
  3. rf(3,1,2)

Hardware setup:

  1. Place the big black 50 Ohm terminator from the cable labeled "Console Output #3" on to the cable labeled "Console Output #2", currently at the Magnet Console Interface Box (MCIB).
  2. Connect the cable labeled "Console Output #3" to the input at the MCIB "B Band Amp" (from where you took the cable labeled "Console Output #2").
  3. Open the right door of the console. In the upper right corner you find three boards labeled XMTR. Move the lowest cable (J2X5) from the middle XMTR board to the equivalent BNC connector at the left board.

 

When you are done, you have to set the instrument back to standard conditions!

Here is how to:

  1. Terminate the cable labeled "Console Output #3" with the big black terminator.
  2. Reconnect the cable labeled "Console Output #2" to the input at MCIG "B Band Amp" (from where you took off the cable labeled "Console Output #3").
  3. Change the cabling in the console back from the left to the middle XMTR board

The software changes will be undone automatically, when you set up a new experiment.

31P observe, 13C decoupling, (and 1H decoupling)

(you probably only want to do this with 13C enriched samples or to remove the small 13C satellites)

Software setup:

  1. Recall standard 13C parameters.
  2. then type dn2=’C13’ dpwr2=45 dm2=’nny’ dmm2=’w’ homo2=’n’
  3. determine and enter dof2=(your value) from the carbon spectrum
  4. (only if proton decoupling is NOT wanted, type dm=’n’)

Hardware setup:

  1. Remove the terminator from the cable labeled "Console Output #3".
  2. Connect the cable to the filter "Bandpass 98-120 MHz".
  3. Connect the band pass filter to one input of the power combiner box ("2-Way combiner").
  4. Connect the filter "Bandpass 131-171 MHz" to the other input of the power combiner box.
  5. Detach the cable between the probe (X-nucleus) and the "Magnet Console Interface Box" (MCIB) from the MCIB. Attach this end to the output of the power combiner box (third connector, opposite side).
  6. Connect a new cable to the bandpass filter "131-171 MHz" and to the input at the magnet stand, from where you have just taken off the probe cable.

 

When you are done, you have to set the instrument back to standard conditions!

Here is how to:

  1. Terminate the cable labeled "Console Output #3" with the big black terminator.
  2. Connect the cable from the probe (X-nucleus) directly to the "Magnet Console Interface Box".
  3. Deposit all extra electronics back onto the spectrometer console.

The software changes will be undone automatically, when you set up a new experiment.

19F observe with 13C decoupling, (no 1H decoupling possible)

(you probably only want to do this with 13C enriched samples or to suppress the small 13C satellites)

Software setup:

  1. Recall standard 19F parameters.
  2. then type dn=’C13’ dof=(your value from the 13C spectrum)
  3. rf(1,3,2)

Hardware setup:

  1. Terminate the cable labeled "Console Output #2" with the big black terminator.
  2. Connect the cable labeled "Console Output #3" to the input at magnet stand "B Band Amp" (from where you took off the cable labeled "Console Output #2").

 

When you are done, you have to set the instrument back to standard conditions!

Here is how to:

  1. Terminate the cable labeled "Console Output #3" with the big black terminator.
  2. Connect the cable labeled "Console Output #2" to the input at magnet stand "B Band Amp" (from where you took off the cable labeled "Console Output #2").

The software changes will be undone automatically, when you set up a new experiment.