FTIR: Perkin Elmer Spectrum One FTIR Spectrophotometer

 

OPERATION OF THE PERKIN ELMER SPECTRUM ONE FTIR SPECTROMETER

  1. At the IR computer, click Start ⇒  Programs  ⇒  PerkinElmer Applications  ⇒  Spectrum

    At the Login window, select Open Lab as the user and click “OK”
     
  2. Your sample will be placed on the dark dot at the center of the thick, flat, metal stage on the IR instrument.  (This dot is actually a diamond crystal).   The metal stage should not be moved.  The stage may have a thin metal plate with a conical depression and hole in the center of it that rests on top of the stage. The diamond can be seen through the hole in the depression on the top plate.  The top plate with the conical depression is used for solid samples.   There is also a small anvil on an arm that can swing over the stage. 

    Check to see that the stage, the diamond, the top plate with conical depression, and the tip of the anvil are clean.  If any part is dirty or you suspect it is dirty, swab it with a Kimwipe wetted with acetone from the small dispenser by the instrument.   Allow the surfaces to dry for a few seconds. 
     
  3. (a) For liquid samples, simply place a drop of your sample on the diamond crystyal.  Do not use the removable top plate.   Keep the anvil swung off to the side.  If your sample evaporates readily, commence quickly with the data acquisition step. (If the sample evaporates too readily, covering the sample with a microscope slide cover slip can slow the evaporation.  Usually this is not necessary, however.)

    (b)  For solid samples, check that the top plate with the depression is mounted on the stage, then place just enough of your solid sample in the conical depression to cover the diamond.   Swing the anvil over the sample and screw it down using the knurled knob until the anvil gently makes contact with the solid.  You will adjust the force from the anvil in following steps. 
     
  4. Click on "Scan" at the top of the IR software window.  This will begin a Preview scan of your sample.  

    (a)  For liquid samples, click "Scan" immediately again to begin the acquisition of data. 

    (b)  For solid samples, carefully tighten the anvil as it presses the sample in the conical depression by turning the knurled knob until the bar graph in the Force Guage display is approximately 1/2 to 2/3 of the way across the guage.  Then click "Scan" to begin acquiring the data. 

    Data aquisition is complete when the bar graph reads 100%. 
     
  5. Save your data file in the file folder specified by your instructor.   Name the file according to the naming conventions also given by your instructor (usually your last name, course number, sample name, and lab manual experiment number).    Click "Save." 
     
  6. Click “Peaks” (on commands bar) to label strongest peaks with their frequencies. If the strongest absorption peak reaches the bottom of the graph, vertically compress the spectrum slightly by using the left side of the “Expd Y” (on commands bar).
     
  7. To print the sample name, your name, or other information on the spectrum, click “ABC Text” (on commands bar) and type your entry. Then click “OK”.
     
  8. Click “Save. ”
     
  9. Click “Print”, which will produce a copy of your spectrum on the printer by the Open Lab instructor’s desk.   Be sure that the specified printer is the one in the Open Lab. 
     
  10. Then click “Close” under “File” to ready the machine for the next user. DO NOT EXIT, except at the end of a day, AS THIS WILL REQUIRE THAT A NEW BACKGROUND BE OBTAINED, which is time consuming and should not be necessary more than once or twice a day.

                                                                                                                                                                                           Prepared by Charles Anderson, v 1.0, 2/02;  Updated by Fryhle 09/17/2012