How to acquire a 1D spectrum on the DPX300: revised September 25, 2008

Commands shown in bold are typed at the command prompt followed by return. Commands in brackets [command] are accessed from the left menu, the sequence [command1]->[command2] refers to the top pulldown menu.

Indented paragraphs in italic cover additional commands and options which are not necessary for the standard procedure.

1) Sample setup:

• -Sign your name in the logbook.

• -Measure sample height in gauge, make sure it is at 18mm.

• -ej to remove standard, insert your sample. If standard came not up, and you are not sure where the standard is, do not insert your sample.

• -ij to lower your sample into magnet.

• -type lock, select your solvent from the list and wait until lock signal is in the upper third of the screen.

If lock is not found or lock signal is very noisy, type rsh last to read in the latest shim file and type lock again.

• -Select [Window]->[BSMS Panel] from the top menu (or type bsmsdisp).

In the BSMS window, Select [Shim]

Select the desired shim by clicking on the icon, which will be displayed in yellow. On the [ +/- ] button click with the left mouse button to decrease the shim current, or the middle mouse button (wheel) to increase. Continue adjusting in that direction where you see an increase in the lock signal, until you achieve a maximum signal. If the lock signal moves outside the upper end of the screen select lock gain and decrease the value until the lock signal is back on the screen. Start with z, then cycle z², z and finally z³,z²,z until no further improvement is achieved.

When finished with shimming, exit the BSMS window by selecting [Display]->[Exit] from the BSMS main window.

For automatic shimming, use the command quickshim for a quick, 1-2 min shimming, or longshim for a more thorough adjustment (will take at least 5 minutes).

On samples with a single strong proton signal (no-D samples etc) the gradient shimming can be performed with the command gradshim

2) Acquisition setup

• -Type new. Define name (name) and experiment number (expno). You can chose any experiment number, but the data set name should start with your initials, i. e. hfmycompound for user Holger Försterling. Avoid special characters like * / \ & $ % < > in the file name. It is ok to use - _ [ ].
• -Exit the window with save to keep the settings.

Make sure you have an empty window

• - Type rpar experiment all to read the parameter file for your experiment. For example, to do a standard proton, you type rpar h1.hf all.

For a listing of all parameter sets defined by me type rpar *.hf, for a list of all parameter sets type just rpar without argument.

Some important experiments available are:

h1.hf 1D standard Proton, 16 scans

c13.hf 1D standard C-13, 1024 scans

c13dept135.hf 1D C-13 DEPT-135, CH and CH₃ up, CH₂ down.

cosy.hf 2D ¹H/¹H COSY, 1 scan, ~5 min.

hsqc.hf 2D ¹H/¹³C correlation (HSQC) (30 min.)

hsqc_ed.hf 2D ¹H/¹³C correlation with editing: CH,CH₃ positive, CH₂ negative

hmbc.hf 2D ¹H/¹³C multiple (2-3) bond correlation

noesy.hf 2D ¹H/¹H NOESY

noe1d.hf 1D ¹H/¹H NOE

An complete updated listing can be found next to the spectrometer.

Important parameters :

sw spectral width in ppm

o1p center of your acquisition window in ppm

ns number of accumulations

d1 relaxation delay

use eda to get a listing of all acquisition parameters

ased will give a listing of all acquisition parameters used by that specific experiment

Single experiment:

• -type rga to adjust the receiver gain

You can check the receiver gain by typing rg, for proton spectra the value should be normally below 1000.

• -start the experiment by typing zg.

Multiple experiments (same sample):

• -Define the next experiment by repeating new, rpar as described above. Keep the experiment name, but increase the number by one. Repeat this until you have defined all experiments.
• -Return to your first data set by typing re expno, where expno stands for the experiment number of your first data set in the series (typically 1).
• -Start acquisition by typing run : You will be prompted for the number of experiments you have defined.
• - Using run will automatically control spin on/off dependent on the experiment and will switch to the standard file after completion. This will protect you from the next user accidently overwriting your data.

Other useful acquisition commands :

expt calculates the time required for the experiment

tr saves the current acquisition while the experiment is still in progress. It allows you to process (see below) and preview a spectrum while continuing to acquire data.

halt halt the current acquisition prior to finishing and save the fid.

go Append to an existing experiment.

acqu or [Acquire]->[observe fid window] from the top menu switch to the acquisition display window to display the fid.

3) Processing

• -Type ef to perform exponential multiplication and fourier transform.

lb allows to adjust your line broadening, a larger lb yields a better signal to noise at the expense of resolution. Standard values are 0.3 for proton and 1 for carbon

edp accesses all processing parameters..

• -apk performs an automatic phase correction.

You can du a manual phase correction by selecting [Phase] from the left menu

• -abs performs an automatic baseline correction.

[*2],[/2],[*8],[/8] Adjust vertical scaling of spectrum sisplay

[<>] [><] Adjust horizontal scaling

[->] [<-] Move spectrum left or right.

[] [|<>|] Reset vertical and horizontal scaling

Click with left mouse button on spectrum to get a cursor on spectrum. Now use middle mouse button to select your display limits. Use left mouse button to release mouse again.

[integrate] (left menu) enters the integration routine. Use the left mouse button to get an arrow on the spectrum. Use the middle mouse button to define your integration limits.

To calibrate an integral, move the integration arrow onto the desired integral and click the left mouse button while under that integral. The integral is now marked with an asterix. Select [calib] from the left menu and type the value for that integral.

Finally use the left mouse button to get back to the normal cursor. Exit to the main menu by hitting [return] and selecting [save intrng and return].

• -[DP1] Define plot region. You will be prompted the left and right plot limit in ppm. The default is the region displayed on the screen

• -setti set plot title. This command calls up a text editor.

• -cy set y-scaling for highest peak in spectrum. Default 12 cm. You can also set it interactively from the [Utilities] menu (left menu, option [cy])

• -mi adjust minimum threshold for peak picking (in cm) if necessary You can also set it interactively from the [Utilities] menu (left menu, option [mi])

edg Access all plotting parameters. Lets you control the plot layout

• -view gives a preview of the plot

• -plot send the plot to the printer.

xwinplot calls the plot editor for more advanced plots.

4) Finishing:

• -ej eject your sample, insert standard

• -ij to lower down standard

• -finish automatically executes the following commands:

rsh last read standard shim file

lock cdcl3 lock on standard

re standard 1 read in default data set. This will protect you from your data to be overwritten by the next user.

• -Finish your log book entry.