Bruker Fourier 300 Manual de usuario

Bruker Fourier 300 Guide

Loading a sample

•Check your solvent height. For best shimming homogeneity, the sample height should be 5 cm.

•Wipe the exterior of the tube clean using a Kimwipe.

•If present, remove the cap from the top of the magnet bore.

•

•Type “ej” in the command line at the bottom of the screen to turn the lift on.

•

•Use the depth gauge to adjust the spinner height on the tube.

•Carefully place your sample into the bore. Make sure air flow is on before releasing sample!

•Type “ij” to turn off the lift.



Experiment Set-up

•Click on the ‘Start’ tab in the TopSpin Menu bar

•

•Select by clicking on it.

•

•Give your experiment a NAME and an experiment number (EXPNO)

•Make sure your data directory (DIR) is set to C:\data\student\nmr

•Press the “Select” button next to Experiment, and choose which NMR experiment you will

carry out.

•

•Once you have clicked on the experiment you wish to run, be sure to click the “Set selected item

in editor” button.

!Note: If you change the parameter folder to nmr\par\user, you will be presented with a much

more manageable set of experiments!

•Choose the correct solvent from the drop down menu next to “Set solvent”.

•Enter a Title for your experiment.

•Click on

•Click on the ‘Acquire’ tab in the TopSpin menu bar.

•

•Type lock in the command line at the bottom of the screen, or click on the “Lock” button.

Select your deuterated solvent from the list that appears.

•

•Click on the “OK” button, and wait for the lock routine to finish. At the bottom left corner of

the screen, a message “lockn: finished” should appear.

•Select by clicking on the icon.

•Wait for the shimming to finish before continuing. It should take about 1-minute to shim. The

message “gradshimau: finished” will appear in the lower left corner of the screen once gradient-

shimming is complete.

•Note: shimming only needs to be performed once per sample. If you run a 13C experiment

after a 1H experiment, this step can be omitted.

•Select by clicking on it

•NOTE: This will load the pulse width and power levels in to the parameter set.

Acquisition

•Select by clicking on it.

•Click on Close if the following window appears:

•Wait for the receiver gain auto-adjust (rga) procedure to finish before continuing. The message

“rga: finished” will appear in the lower left corner of the screen once the receiver gain has been

automatically set.

•Select by clicking on it.

•NOTE: The 1H (16 scans) experiment will take ~2 minutes.

Processing

•Click on the ‘Process’ tab in the TopSpin Menu bar.

•

•Click on

•NOTE: This executes a processing program including commands such as an exponential

window function ‘em’, Fourier transformation ‘ft’, an automatic phase correction ‘apk’ and a

baseline correction ‘abs’.

•

•Expand the spectrum to include all peaks. This can be done by left clicking inside the spectrum

window, and dragging from one side to the other, and then letting go of the mouse button.

•

•Another option is to click the button, and type in the desired left and right ppm values.

•

•Spectrum intensity (vertical-zoom) can be increased/decreased by pushing the mouse scroll-

wheel forwards/backwards.

•You can also use the icons below:

•

•The following toolbar icons can be used to manipulate the spectrum.

•

!"#$%&'(#)*'+#,-%

•If you are using an internal standard such as TMS (tetramethyl silane), you can set the position

of a particular peak quite easily.

•Zoom in on the peak whose position you wish to set.

•Click on the Calib. Axis. Button.

•

•Left click on the peak you wish to set.

•

•Type in the peak position in the dialog box the appears.

./'0%.#10#-2%

•Click the peak picking button on the toolbar.

•Drag the cursor over the tip of a peak to select it. The green box only needs to enclose the tip of

the peak—dragging the box to the baseline may cause noise to be identified as peaks.

•

•Click the save and return button when you are done picking peaks.

•If you wish to pick additional peaks, be sure that the select region icon ( ) is highlighted.

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