|
TCNJ Chemistry Instrumentation
Operating Instructions
HP5970MSD
General Instructions
1) Turn on the heater and electronics if they are not already on (switch is located on front panel of 5970 MSD).
2) Check to see that vacuum is about 10-5 torr and helium is running through the column. Look for the "column head pressure" gauge on the front of the HP 5890 Series II GC.
3) Adjust the column head pressure to the desired setting by slowly turning the black knob underneath the gauge clockwise (10-15 psi for a typical analysis).
4) Set the GC oven temperature to the initial temperature you will be using for your analysis. Press the grey "Oven Temp" button on the front of the HP 5890 GC, enter the temperature value using the keypad, and press Enter.
Autotuning
1) The square "buttons" on the monitor correspond to the function keys on the keyboard (F1-F8). Press F8 until you see the button labeled Autotune on the monitor.
2) Press F1 to begin autotuning. Press F1 for full autotune.
3) Open the calibration valve on the far left side of the 5970 MSD. Press return. At this point, the autotune should proceed and you should see the instrument conducting a series of tests. If you don't, see below for further instructions and possible error messages that may appear.
NOTE: Sometimes you will see an error that says "Mass Spectrometer IO Check Failure "IOTEST"". If you see this error, the heater and electronics are not turned on. Turn them on using the switch on the front panel of the 5970 MSD. Hit F8 to quit, close the calibration valve on the far left side of the 5970 MSD, and repeat steps 2-3.
NOTE: Sometimes you will see an error that says "Mass Spectrometer Status. There is no emission current. Difficulty in the mass filter electronics. Difficulty with the +/- 5 volts supply. There was an excessive signal level. Party fault has occurred." If you see this error, press F8 to exit. At this point, the autotune should proceed and you should see the instrument conducting a series of tests. An autotune report should also print automatically.
Setting Up Acquisition Parameters
A) GC Method Parameters
1) Press F8 until you see the button labeled Data Acquisition on the monitor. Press F2. Press F2 again to edit parameters.
2) Press F3 to edit the GC parameters (Edit Temp Zones).
3) Use the tab button to toggle between fields. Using the keyboard, enter the desired run time, equilibration time, oven temperature program, initial GC temperature (table on bottom left, first "Setpt" value), injector temperature (table on bottom right, first "Setpt" value), and detector/interface temperature (table on bottom right, second "Setpt" value). If you are changing the previous values, make sure to overwrite them completely with you new values. Press F8 to exit.
B) MS Parameters
1) Press F2 to edit parameters. Press F2 again to edit the MS parameters (Edit Acq Params).
2) Use the tab button to toggle between fields. Using the keyboard, enter the desired solvent delay, mass range, threshold, and sampling rate. If you are changing the previous values, make sure to overwrite them completely with you new values. Press F8 to exit.
Loading and Storing Parameters
1) Press F5 to load and store your parameters.
2) Press F6 to store your parameters. A message appears that says, "Parameters successfully stored".
3) Press F5. Press F5 again to load your parameters.
4) Check that the parameters have been loaded by pushing the "Oven Temp", "Inj A Temp", and "Det B Temp" buttons on the 5890 GC.
Starting the Analysis
1) Press F1 to prepare for injection. A message will appear asking if you want to overwrite the data file. Press F1 for Yes, or press F4 for No then enter a new filename. Make sure to include the proper file extension after the filename.
2) When the 5890 GC is ready for sample injection, the GC display will read "awaiting run start".
3) Inject ~0.2uL of sample into the GC quickly and immediately press the "start" button on the GC.
4) Wait for the analysis to finish, or press F8 to stop the run once all of the compounds are eluted from the column.
Looking at Your Data
1) Press F8 until you see the button labeled Data Editor. Press F3 to enter the data editor.
2) Press F1 to bring up the total ion chromatogram of the most recent data file acquired. If you do not see your chromatogram, press F4 to select another data file. Type "?" (without the quotes) to obtain a list of available files. Press F3 to get to the next page if necessary. Use the arrow keys and press F1 to select your data file.
3) To obtain a mass spectrum press F2. Use the arrow keys and press F1 to select the desired scan with the cursor.
4) To plot the total ion chromatogram and mass spectrum, press F7 (Environ Keys).
5) Make sure a pen is in position 1 in the plotter.
6) Press the white "Load Paper" button to raise the feeder wheels.
7) Insert a piece of paper, lining up the paper with the left edge of the plotter and the white line near the feeder wheels.
8) Press the white "Load Paper" button.
9) Press F5 to send the total ion chromatogram and mass spectrum to the plotter.
Other Data Manipulations
1) To integrate peaks in your total ion chromatogram, press F6 (Chromat Keys) when you are in the Data Editor. Press F3 to run integration. Press F4 to list the integration results. Press F5 to print the integration results.
2) To zoom into a given area of your chromatogram press F3 (Zoom) when you are in the Data Editor. Use the arrow keys to define the top left corner of the zoom area. Press F1 to select the top left corner. Use the arrow keys to draw a box around the zoom area (right, then down). Make sure you have the bottom edge of the box below the x-axis. Press F4 to move the previous corner if necessary. Press F1 to select the bottom right corner and zoom in.
3) To display a selected ion chromatogram, press F6 (Chromat Keys) when you are in the Data Editor. Press F2 (Ion Chromat). Use the tab button to toggle between fields. Using the keyboard, enter the desired time range and ion ranges. Press F1 to execute. If you want to return to the total ion chromatogram, press F8 to exit, then F1.
