Protocol for the SPEX 1250M Monochromotor By: Chris Dennis Created: 2008 To record beautiful spectra a proper understanding of the equipment and theory of fluorescence spectroscopy is tantamount. This manual is intended to guide the user by outlining the most basic procedures for operating this equipment well. It is advised that the user consult the user’s manual and/or spectroscopy texts for any further information and troubleshooting. Equipment The SPEX 1250M is supplemented by many peripheral instruments listed below A/D Converter (SpectraAcq2) Motor Control Unit High Voltage Power Supply (for PMT) Lock-In Amplifier (used for IR detection) Reference and Input Chopper (for use with the lock-in amplifier) Tektronix Oscilloscope (multi-purpose) Personal Computer Take a moment to review the pictures of the setup. 1. Configuration for IR or Visible Spectroscopy (Zen and the Art of Diffraction Gratings) Before you run your scan you must first decide which diffraction grating cooresponds to your desired wavelength range. The lab carries 3 diffraction gratings for the SPEX1250M. 300 grooves/mm Blazes at 3000nm 600 grooves/mm Blazes at 1500nm 1200 grooves/mm Blazes at 500nm To switch out the gratings physically you must first remove the diffraction grating housing cover located on the top of the SPEX1250M. Once you remove the four screws you will immediately see the diffraction grating turret. To remove the diffraction grating from the turret you must locate the securing lever on the back of the turret. Flip this lever down to release the grating. Now place your new grating into the turret and secure it in place with the lever. It should fit in easily, never force it in. Once you are in the software you must tell the software which grating you are using. I will walk you through that procedure when we get to the software setup section. 2. Preparing the IR Detector The IR detector must be cooled with liquid nitrogen. Place liquid N2 into the detector and let the detector cool down. You can tell when it has cooled down when the gas stops expelling from the detector. You will then need to put more Liquid N2 into the detector. You may need to periodically refill the detector. 3. Powering Up The order of powering up the equipment is extremely important. Power surges from high voltage/high amperage equipment can ruin sensitive devices. Be sure that all entrance and exit slit on the monochromator are closed. Visible: a. b. c. d. Turn on the Excitation Source (Laser, Tungsten Lamp, etc) Next, turn on the High Voltage Power Supply (950V) Next, turn on the SPEX1250M Finally, turn on the Computer a. b. c. d. e. Turn on the Excitation Source (Laser, Tungsten Lamp, etc.) Next, turn on the SPEX1250M Next, turn on the Lock-In Amplifier Next, turn on the Chopper Finally, turn on the Computer Infrared: 4. Using the Origin based SynerJY Software (Data Acquisition) Once the power-on procedure is completed and the computer is running go ahead and click on the ‘SynerJY’ icon to start the data acquisition program. The program should load and you should see this screen. Click the button that looks like a graph (circled in the picture) to begin setup. The following slides will guide you the rest of the way. Detector Selection Screen 5. Saving your data and hard work! Once your spectrum is complete it is likely you will want to transfer this data to another computer or media. To do so follow the simple instructions outlined below.