Professional Documents
Culture Documents
Working up 1H 1D data:
MNova automatically FTs your data. If you would like to see your fid, you may do so
under the
icon.
Window function (mathematical function called apodization applied to raw fid): click
the
icon to get a list of functions. Use a matched filter for 1H 1Ds, which is an exponential
that is the inverse of the acquisition time (on Homer/Athena AQ = 2.7 sec; on Hermes at = 4
sec). Other functions may be used as well. To see what they do to your spectrum make sure the
interactive box is checked in the lower right of the GUI. (Mnova applies the apodization that
has been defined on the spectrometer, although not for Homer/Athena data.)
is useful in 1H 1Ds, because it adds digital resolution to the data (ie. you
Zero filling
can easier observe fine splitting). MNova automatically does one zero fill. You can find the
icon by clicking on the Fourier Transformation
options. In the GUI that appears,
you have the option of changing Spectrum size, if you want more zero fills (Original size is the
number of points in the raw data). However, dont use more than two zero fills.
Phase correction: MNova does an automatic phase correction, but if you increase the
intensity of your spectrum (
Baseline correction: this must be done for integrations to be correct. Click on the arrow
by
and then
to get an interactive GUI for applying the correction. A dark blue line
will show how the polynomial chosen will fit your baseline. Use either Bernstein polynomial
Fit or Polynomial Fit and you may change the polynomial to better fit your baseline. In some
cases, Whitaker baseline correction works well (ie. for very heterogeneous mixtures that may
have large aggregates), but be careful since it will remove broad lines.
Referencing: click on
to reference TMS or any other solvent peak (L shortcut).
The GUI that pops up allows you to annotate the peak with any text.
Peak picking: Click on the arrow by
threshold
option (K shortcut) is nice, because it allows you to select groups of peaks with
Integration
(I shortcut), which allows you to define the integration regions yourself. The
first integral that you define, will automatically be normalized to 1.0. To change this, R-click on
the integral that you want normalized and Edit Integral. In the GUI change the normalized value
and click on Apply to All at bottom.
Multiplet analysis: The arrow by
shows that you may either do this automatically
on the entire spectrum or you may choose the multiplet regions yourself. The analysis works
better if you choose the multiplets by clicking on
by one. When you select a multiplet, make sure the horizontal line that appears is below your
peaks that you want analyzed (or close to the baseline).
Manipulating integrations and multiplets: move the cursor over the integral or over the
multiplet definition box and R-click. You may manually Edit Multiplet features or delete certain
multiplets. You may change your integration normalization values from here also.
to
Phase correction: MNova does a good job here for most 13C 1Ds. If youd like to correct
the phase (ie. if you see some dips below baseline), go to
and
Click on
to change the cursor to zoom mode and select the region you want to zoom
in on. Z-shortcut works best: 1st Z is horizontal zoom, 2nd Z is vertical zoom, 3rd Z is in both
dimensions (hit Esc to get your cursor back to normal).
Zooming out may be done by clicking on
icon or using Shift-Z, which puts the
cursor in zoom out mode. Click on the spectrum to zoom out.
The Full Spectrum icon
will get the entire spectrum back in horizontal (ppm) and
vertical (intensity) dimensions. The F shortcut will get the entire spectrum back in the horizontal
(ppm) dimension. While the H shortcut or
to the top of the page.
Some like to see the entire spectrum, while zooming in on particular regions. Go to View
-> Full View, which brings up a small box with the whole spectrum and the zoomed in part
highlighted in blue. You may click and drag the blue region to different parts of your spectrum.
Helpful for getting to different parts quickly. You may also drag the Full View box around, to
check out how it can get plugged in to different parts of the window.
icon and then select the region of your spectrum that
Spectrum insert: E shortcut or
you want the insert of. You may manipulate the insert the same way you would the entire
spectrum (using the above shortcuts), just make sure the insert is selected.
Cutting parts of the spectrum: If you have large baseline regions, you may click on
icon (X shortcut), which puts your cursor in scissor mode and you may cut certain regions out of
view. The scale at the bottom will reflect the cut. Use the V shortcut to get the cursor into
restore mode and highlight the cut that you want restored.
Change annotation features, such as font: Look at icons in lower left to get to different
annotation features. Here you can change the font, font size, super and subscript, etc.
Spectrum title: This automatically gets added in the upper left corner of your spectrum
(except for Bruker AC data). To change this text or to add line breaks (so its lower than the top
of the page), R-click on background and go to
of the Title. In this GUI you can add line breaks at the beginning or change the text.
3) In order to phase each slice of the array, you must break the array into the individual spectra.
Click Stack > Extract All Spectra to perform this operation. Give MNova time as this is an
intensive process, especially if you have >100 slices. After the extraction, you can delete the old
array page as it may distract you later on.
4) Perform the proper phasing for each spectrum.
5) To recombine them into a stack plot, click over to the pages section and hit Ctrl-A (Cmd-A for
Mac) to select all the spectra. Next, hit Stack > Stack Spectra and a next page containing your
stacked spectrum should appear.
6) To apply a baseline correction to each spectrum in the array select the page and hit
Processing > Baseline > Baseline Correction.
7) Finally, you can integrate each spectrum in the array by selecting one spectrum (preferably
with both reactants and starting material) and use
on the left menu to select Active
Spectrum. Integrate the regions of choice and onced finished, you can export these integrals to
a .txt file by clicking File > Save As. Under Format you see you can change it to MestraNova
Integral Regions or Script: Integral Table Series among others containing the word
integration. I primarily use Script: Integral Table Series and I open the text file in Excel. For
understanding the text file, see the end of the page.
For Non-Arrayed Kinetics
1) Begin by phasing and referencing each spectrum.
2) Follow directions from step 5-7 above.
Absolute Integration
1
8729.96218
3.10418
27099.39158
0.67411
5884.94555
0.6703
5851.71054