Topspin

1
Topspin

• Processing
• Relaxation time
• DOSY

2
Processing T1 in TOPSPIN

1. Select procpars tab and click on P to display
   parameters. Make the following changes
   SiF116, PH_modF2pk , PH_modF1no
2. Type xf2 to transform detection domain, then
   Type abs2 to correct the baseline
3. Select the spectrum tab
4. Click in Analysis ? T1/T2 Relaxation
   (relaxation guide appear on the right)

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Processing T1 in TOPSPIN
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Processing T1 in TOPSPIN

1. Click on Extract Slice in popup menu, click
   on Spectrum
2. Enter Slice number 1 and Click on OK
3. 1D spectrum will come on screen. If the spectra
   is not well phased, go in phase mode, phase it
   save as 2D, also save and return.

Note when you have a slice on screen, notice the
numbered button on the far right of the top
toolbar
the 1 is for the 2D relaxation, the 2 is for
the relaxation Guide, the 3 is for the 1D
slice. After Phasing the 1D slice and saving as
2D, you will need to activate 1 and reapply
Fourier transform xf2 and baseline correction
abs2
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Processing T1 in TOPSPIN

1. Click on PeaksRanges This will bring the
   integral mode
2. Define Integral regions by clicking with left
   mouse around the peaks of interest
3. Click on the Save button on integral toolbar and
   select Export Regions to Relaxation module

1. In relaxation guide, Click on Relaxation window
   enable intensity, Click OK.
2. In guide window, Click on Fitting Function
   Select uxnmrT1 in popup window
3. In guide window, Click on Start Calculation

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Processing T1 in TOPSPIN
In the toolbar on top of the active window, The 2
first button will execute calculation
calculate all peaks and give calculation result
as a Brief Report (like in figure above)
calculate the current peak
The minus and plus buttons navigate to
previous or next peak
show the full report. This can also be done by
selecting Display Report in Guide.
show/hide the text in graphic window
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Setting up DOSY 1- Pulse calibration
Sample Sucrose DSS Acetone in D2O

1. In exp1 Run proton NMR (standard) rga zg.
   Process data.
2. Create exp2 ns 1, in eda choose pulprogzg
3. Acquire data with zg and Process data with
   efp (data should be well phased) zoom on a
   signal in the center of the spectra and define
   the zoom using DP1 (this represent 90opulse
   large intensity)
4. Change the pulse length p1 (double value),
   acquire and process data (zg efp) ? click on
   plot region if the full spectra is displayed
   it will go back to the zoom region).

if the signal is null this is 180 pulse if not
try slightly different P1 pulse until null is
found (small signal with dispersion mode) Set p1
to the 90pulse value
Negative
Positive
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Setting up DOSY 2- Evaluate Relaxation time

1. In exp2 (previous page) with p1 pulse set to
   90o and ns 1 Run proton NMR zg. Process
   data efp. Get the full spectra and define it
   with DP1
2. In eda choose pulprogt1ir1d. Type d70.5
   (relaxation delay).
3. Acquire and process data zg efp (do not
   phase). The first pulse invert magnetization.
   Then during the evolution delay d7 the
   magnetization recover. If the signals are still
   negative, increase d7 re-acquire and process the
   data (zg efp) until the peak with longest
   relaxation pass through the null.
4. When longest null is found, the delay value can
   be used to evaluate longest relaxation time (d7)
   1.5 T1 (relaxation time)

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Setting up DOSY 3- DOSY 1d

1. Return to exp1 re 1 (Std H) Create new file
   exp3 (this will copy all parameters in the new
   exp) Set p1 pulse to previously calibrated 90o
   and set ns 1 Run quick proton NMR zg.
   Process data efp.
2. Zoom on the region that contain all the peaks and
   click on SW-SFO1 to narrow the window to that
   region. In eda type td16k. in edp set
   following parameters si8k, wdwem lb2
   Re-acquire, process data zg efp and phase
   correctly.
3. Create the next experiment (exp4)In eda set
   pulprogstebpgp1s1d in ased set GPZ62
   GPZ7-17,13 D200.1 P301800us
4. Adjust the gain rga, acquire and process the
   data zg efp and phase. Spectra should be
   intense.
5. Create the next experiment (exp5) In ased set
   GPZ695 and acquire and process the data zg
   efp data should be very small (if not change
   P30 and D20 in both data set exp4 and 5) and
   re-acquire the 2 experiments

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Setting up DOSY 4- DOSY 2d

1. Create new file exp6 (this will copy all
   parameters in the new exp)
2. in eda set pulprogstebpgp1s Click on button
   to change from 1D to 2D and save.
3. in eda set TDF116 (or 32) FnMODEQF
   NS8 DS4
4. Type dosy and answer questionsenter first
   gradient 2 OKenter final gradient 95
   OKEnter number of points 16 (or 32) OKRamp
   Type l (linear) OKDo you want to start
   acquisition OK

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Processing DOSY in TOPSPIN

1. Select procpars tab and click on P to display
   parameters. Make the following changes
   SiF116 (or 32) can be set to larger for
   zero filling in 2Ddosy FT),PH_modF2pkPH_modF
   1no
2. Type xf2 to fourier transform detection domain,
   then Type abs2 to do baseline correction
3. Type setdiffparm
4. Select the spectrum tab
5. Click in Analysis ? T1/T2 Relaxation
   (relaxation guide appear on the right)

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Processing DOSY in TOPSPIN

1. Click on Extract Slice in popup menu, click
   on Spectrum
2. Enter Slice number 1 and Click on OK

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Processing DOSY in TOPSPIN

1. 1D spectrum will come on screen. If the spectra
   is not well phased, go in phase mode, phase it
   save as 2D, also save and return.
2. Note when you have a slice on screen, notice the
   numbered button on the far right of the top
   toolbarthe 1 is for the 2D relaxation, the
   2 is for the relaxation Guide, the 3 is for
   the 1D slice.
3. After Phasing the 1D slice and saving as 2D, you
   will need to activate 1 and reapply Fourier
   transform xf2 and baseline correction abs2
4. Click on PeaksRanges
5. Define Integral regions by clicking with left
   mouse. Save integral with and select Export
   Regions to Relaxation module
6. In relaxation guide, Click on Relaxation window
   enable intensity, Click OK
7. In guide window, Click on Fitting Function
   Select vargrad and difflist in popup window
   OK

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Processing DOSY in TOPSPIN

1. In guide window, Click on Start Calculation.

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Processing DOSY in TOPSPIN
calculate all peaks and give calculation result
as a Brief Report (like in figure above)
calculate the current peak
The minus and plus buttons navigate to
previous or next peak
show the full report. This can also be done by
selecting Display Report in Guide.
show/hide the text in graphic window
16
Processing 2D-DOSY in TOPSPIN
Select procpars tab and click on P to display
parameters. For 2D transform do zerofilling by
settingSiF164 (or 128) Use dosy2d to get
2d transform
Sucrose
DSS
Acetone
D2O