lab-2 - Lab #2 1D 1H Double Resonance (Selective...

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1D 1 H double-resonance lab CHEM 4190/6190/8189 1 Lab #2 1D 1 H Double Resonance (Selective Decoupling) operation of the 400 MHz instrument using automated sample insertion (robot) and automated locking and shimming collection of 1D 1 H spectra retrieving data, peak picking, peak integration, plotting selective decoupling and spectral analysis Login -the operator screen should be in view when you first sit down at the spectrometer console: -from the list of operators (pull-down menu), select chem6190 -there is no password for this account -click OK chem6190
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1D 1 H double-resonance lab CHEM 4190/6190/8189 2 Sample slot selection -if the tray panel is not present, click the “ O ” located above and to the left of the black spectral display window to display the tray panel
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1D 1 H double-resonance lab CHEM 4190/6190/8189 3 -the tray panel represents the sample tray located on top of the white platform next to the magnet -the X in the upper left of the sample tray will toggle the display back to the black spectral display window -the numbered circles on the tray panel correspond to sample slots in the sample tray -sample slots that appear in color on the tray panel are NOT available for use -also, sample slot 50 is never available for use (this slot is reserved for a standard sample) -sample slots that appear gray on the tray panel may be available for use, but this must be confirmed (see below) -you also can click on this arrow which will pop up a small window that tells you what sample currently is in the magnet
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1D 1 H double-resonance lab CHEM 4190/6190/8189 4 -click the switch to #50 button at the top of the screen -if nothing happens, this means that any of the gray slots can be used -if there is a sample in the magnet already, the robot will take it out and replace it with sample 50. At this point, all gray slots are now available for use ( the robot is slow, so be patient ) - choose one of the available ( gray ) slots. You must confirm that this slot is empty by checking the sample tray
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1D 1 H double-resonance lab CHEM 4190/6190/8189 5 Sample placement -hold the sample tube near the middle of the tube and in a vertical position -push the tube through the hole on the large end of a sample spinner turbine - NEVER push on the top of the tube -the bottom of the tube should be pushed slightly through the bottom (small) end of the spinner turbine -set the tube/spinner assembly in the black sample depth gauge in the sample tray -push the tube (by its sides, NOT from the top) down until it stops -the tube is now properly positioned in the spinner turbine -now you can place your tube/spinner assembly in one of the open slots (on the sample tray, the slot number is to the right of the slot/hole) Experiment selection -you can select from among the experiment tabs the one corresponding to the experiment that you will be acquiring -in our case, we will select std 1D -click Proton -this will load the appropriate parameters for collecting a simple 1D 1 H experiment
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1D 1 H double-resonance lab CHEM 4190/6190/8189 6 -in window below, new sample and Proton
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lab-2 - Lab #2 1D 1H Double Resonance (Selective...

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