1H NMR Analysis (ACDLab)

ACDLab/SpecManager

Import spectral data

Use 1D Macro to load the desired series of 1D 1H NMR ".fid" data files. When this is done, by default, the “group treatment” is on and ACD operations will be applied to the entire group.

Steps:

1. Click on the “1D NMR Macro” button.

2. On the “Execute Group Window”, make sure:

a) “Plate” should not be checked.

b) Check “spectra”.

c) Click on “add group”. The wild cards ("*" for numbers, "?" for letters) can be inserted in the directory mask line. The file mask should read “.fid”. Click “OK”.

3. When all of the data files are correctly listed, click “OK” to execute the group macro and load the files into ACDLab/SpecManager. Assuming that the files loaded correctly, click “OK” when the process if finished.

Pre-process the spectra

If appropriate, apply a window function. To match what TOPSPIN does automatically when processing data on the 500 MHz console, use a 0.3 Hz exponential window function prior to Fourier transform (FT).

Steps:

1. Click on “WFunctions” in the operations bar.

2. Set LB = 0.3 Hz

3. Choose “Exponential”.

4. Click “Ok”.

5. Fourier transform the FID files

6. Click on “Fourier Tr.” in the operations bar.

7. Phase correct the spectra.

8. Click on the “Phase Corr.” button on the operations bar.

9. Use the “Auto Simple” option.

10. Click on the “checkmark” to accept the result.

11. Set chemical shift reference using the TMSP peak.

12. Click on the “Reference” button on the operations bar.

13. Check the “Options” to verify that TMS is set. Both TMSP and TMS have chemical shift values of 0.000 ppm.

14. Click on “Auto”. Then click “Ok” in response to the “There are no labeled peaks available…” message if it appears.

Integrate the spectra and export the peak list

Using the “auto integrate” option:

Steps:

1. Click on the Integration operation.

2. Check the “Options”

a) Set for “Bucket Integration”

b) Set width of buckets to 0.025 ppm

c) Choose intelligent bucketing with width looseness (%) = 50 and method = sum

d) Set reference to “whole spectrum”.

e) Click “Ok”

f) Click on “Auto” to perform the integration

g) Click on the “checkmark” to accept the result.

3. Use the Series pull-down menu to bring up the table of common integrals. A right-click will allow one to save the integral table. The saved table can be imported directly into SIMCA or opened in Excel.