SAFETY OPERATING PROCEDURES Reliotron III Cathodoluminescence Instrument DO NOT USE THIS MACHINE UNLESS YOU HAVE BEEN INDUCTED IN ITS SAFE USE AND OPERATION AND HAVE SIGNED AN INDUCTION FORM PERSONAL PROTECTIVE EQUIPMENT CLOSED TOE SHOES MUST BE WORN IN THIS AREA PRE-OPERATIONAL SAFETY CHECKS Check Workspace to ensure no SLIPS / TRIPS / HAZARDS are present. Check that the assembly of cables as in Section III.01 has been completed. Familiarise yourself with the parts of the equipment i.e.: Reliotron Chamber, microscope and camera, Reliotron Control Panel, Pump. See Photographs below. www.monash.edu/ohs/

SAFETY OPERATING PROCEDURES Reliotron III Cathodoluminescence Instrument SAFETY OPERATING PROCEDURES GETTING STARTED To get the most out of your session on the CL it is best to load the sample in the sample holder and look at the thinsection through the microscope first. You can become familiar with the minerals and determine which area you are hoping to get a CL image from. Before starting, it is important to adjust the microscope and the optics specifically for your sample, in addition to determining an accurate scale. Turn the on the computer and log on. Turn the camera on by pressing the button on the Nikon Digital Sight DS-U3 box. Start the program ‘NIS Elements F”. (Shortcut is on the desk top). Select “Nikon DS-U3” when prompted. Turn on the microscope. The switch is located on LHS of microscope base. Turn dial up (also on LHS) to increase the amount of transmitted light. To load your sample see section on SAMPLE LOADING. www.monash.edu/ohs/

SAFETY OPERATING PROCEDURES Reliotron III Cathodoluminescence Instrument SAFETY OPERATING PROCEDURES SCALING: The microscope is an Olympus SZH and uses a GWH 10X-D eyepiece. See the scale chart below for the field of view measurements and total magnification determined by different objective sizes. In the program ‘NIS Elements F ‘, Select Camera > Calibrate. Make sure objective is on a sensible number like 20x or 10x. Double check it is sensible using the scale ruler. Place the scale bar next to the focussed thinsection. Remember 1mm-1000 mm. www.monash.edu/ohs/

SAFETY OPERATING PROCEDURES Reliotron III Cathodoluminescence Instrument SAFETY OPERATING PROCEDURES INITIAL OPERATION AND FAMILIARIZATION To start with do not pump down the chamber, instead leave it vented at atmospheric pressure. There will therefore be no discharge in the electron gun when the HV is turned on. Turn the control knobs all the way Counter Clock wise Turn the mode selector switch to the “Pump” position. In this position, the beam voltage cannot be turned on. 3. Turn power on, on wall, both switches, pump and console. 4. Turn on Transformer. The instrument is from USA therefore a transformer is needed to convert to the correct Voltage. 3 Console Transformer 5. 4. 5. Turn on the “ Main power” on the control console (but not the high Voltage). The vacuum gauge should read approx. 760 Torr which is atmospheric pressure. 6. Turn the “Mode” switch to the “Manual” position. www.monash.edu/ohs/

SAFETY OPERATING PROCEDURES Reliotron III Cathodoluminescence Instrument SAFETY OPERATING PROCEDURES 7. Turn on the beam voltage by pushing the “High Voltage” switch/button. The red indicator light should come on and a low reading, about -1 kV should appear on kV meter. The beam current (mA) meter will read a few microamperes. 7. 8. Turn up the “High Voltage” control and note that the kV meter reading will increase smoothly and the mA reading will also increase. Stop at about -5kV. PREPARATION FOR PUMP DOWN PROCEDURE AND SAMPLE LOADING Turn DOWN the “High Voltage” control and then turn OFF the “High Voltage” switch/button. Turn the mode selector back to the “Pump” position. SAMPLE LOADING Remove the draw from the chamber, check that the chamber and 2”x3” glass slide is on the bottom of the tray. Elevate sample if needed, in any convenient arrangement as long as it is stable. Place one or more thin sections or thin slabs onto the 2”x3” glass slide, making sure that the thin sections face up so the beam can strike them. www.monash.edu/ohs/

SAFETY OPERATING PROCEDURES Reliotron III Cathodoluminescence Instrument SAFETY OPERATING PROCEDURES PUMP DOWN PROCEDURE Close the pump valve. IMPORTANT: Ensure Steps 3, 4 and 5 have been followed from the INITIAL OPERATION AND FAMILIARIZATION page. Turn on the mechanical pump. Vent Cap Drawer Check the “vent” cap is closed (finger tight is sufficient). Push drawer firmly into the chamber until the pump noise is clearly lower, indicating that it has sealed. The chamber will now pump down and the progress can be followed with the TC gauge pressure readout on the front panel. www.monash.edu/ohs/

SAFETY OPERATING PROCEDURES Reliotron III Cathodoluminescence Instrument SAFETY OPERATING PROCEDURES OPERATION INSTRUCTIONS: BEAM TURN ON When the pressure has reached a value of 100-150 millitorr, it is possible to turn on the electron gun. To do this follow the instructions below. This CL machine has been operating best at 70 mTorr. Turn the “High Voltage” adjust and the “Focus” adjust to zero. (Counter clockwise?) Turn the “Mode” switch to “Manual”. Push the “High Voltage” switch- it should light and a low value of high voltage should be indicated on the meter, -1 to -1.5 kV. Beam current will also be indicated. Slowly adjust (increase) the “High Voltage” adjust while looking at the beam current meter, maintain the beam current at less than 0.5 mA. Carbonate samples will luminesce at approximately -06.0 kV. Note: Sometimes the beam current will not come on at first and as you continue to adjust the “High Voltage” it may come on suddenly at a high value. This is common in cold cathode electron guns. If this happens adjust back to a lower value of high voltage. www.monash.edu/ohs/

SAFETY OPERATING PROCEDURES Reliotron III Cathodoluminescence Instrument SAFETY OPERATING PROCEDURES Pause for a moment and observe the beam current meter, If the system is still pumping down, the current should be continuously decreasing for a given value of HV. Follow up with Massimo: Beam current decreases with decreasing chamber pressure (further away from atmospheric pressure) and increases with increasing chamber pressure (closer to atmospheric pressure). ???? You should be able to see a luminescence from the sample at about 5 kV. Adjust the deflection magnets and the slide to bring the beam onto the sample. If there is no CL visible, try increasing the voltage to 10 kV, keeping the current below 80% of full scale. ???? For tips on Beam current adjust see section VII.05 For tips on focussing and defocussing the electron beam see section VII.06. Follow up with Massimo, is the purge valve the same as the vent cap. BEAM TURN OFF BETWEEN SAMPLES To change samples, please follow these steps: Turn off the beam voltage and reduce the HV adjust to zero. Close the pump valve. Vent the chamber completely with the purge valve. Move the specimen tray so it is near the front of the chamber and slide out the drawer part way. Exchange the sample. Tighten the purge valve press the drawer back in to place, pump down and follow the procedures already given for turning the beam on. www.monash.edu/ohs/

SAFETY OPERATING PROCEDURES Reliotron III Cathodoluminescence Instrument SAFETY OPERATING PROCEDURES TURN OFF PROCEDURE-END OF SESSION Turn off the beam voltage and reduce the HV adjust to zero. Close the pump valve. Vent the chamber completely with the purge valve. Move the specimen tray so it is near the front of the chamber and slide out the drawer part way. Turn pump off After the pump is turned off, and with the purge valve still open and/or the chamber drawer open, open the pump valve, slowly. You will hear a rush of air into the pump hose, which is still under vacuum. This procedure vents the hose. This is important as if the hose is not vented, there a partial vacuum will remain even though the pump is turned off. This may lead to pump oil being sucked from the pump into the hose or even into the chamber. www.monash.edu/ohs/

SAFETY OPERATING PROCEDURES Reliotron III Cathodoluminescence Instrument SAFETY OPERATING PROCEDURES SMALL CERAIC JAW CRUSHER POTENTIAL HAZARDS AND INJURIES Low level noise Fumes from pump Electrocution X-ray exposure: an electron beam of 5-25kV or higher will produce X-rays. The CL chamber design should shield against these and the viewing window should be made of special X-ray leaded glass. Never replace this with anything except the same type of glass, from the manufacturer. DO NOT !! :Operate with gun covers off or with electronic cabinets removed. If you are pregnant or a cancer patient consult your physician before use and/or being exposed to x-ray equipment. Follow up with Massimo: Page 10 of manual; “It is advised to have an X-ray survey made with an instrument designed for low level energy detection. Date of last review: Signed: www.monash.edu/ohs/

(for cleaning microscope optics) Acetone Inhalation and skin exposure RISK ASSESSMENT SMALL ERAMIC JAW CRUSHER Reliotron III Cathodoluminescence Instrument RISK FACTOR WITHOUT CONTROLS IN PLACE CONTROLS IN PLACE TO LOWER RISK RISK FACTOR WITH CONTROLS IN PLACE HAZARD TYPE DESCRIPTION OF HAZARD PERSONS AT RISK CONSEQUENCE Negligible hearing loss LIKELIHOOD L4 Unlikely Exposure to noise 59-71 (dB9A) Current Operator, Person in Charge, Contractors. No hearing Protection required Prolonged Low level noise. > 2 Hours CONSEQUENCE C5 Negligible injury LIKELIHOOD L4 Unlikely Low Low level radiation damage. Risk to pregnant women and cancer patients Current Operator, Person in Charge, Contractors. CONSEQUENCE B5 Severe injury LIKELIHOOD L5 Unlikely High Lead Glass and sample holder prevents X-Ray emission CONSEQUENCE B5 Negligible injury LIKELIHOOD L5 Highly Unlikely Low X-ray exposure CONSEQUENCE E Negligible LIKELIHOOD L5 Highly unlikely Low Ethanol (for cleaning microscope optics) CONSEQUENCE E Negligible LIKELIHOOD L5 Highly unlikely Low Highly Flammable Current Operator. Minimum amount and fire blanket Correct storage of acetone in spray bottle, not contact with eyes and skin. CONSEQUENCE C5 Negligible injury LIKELIHOOD L4 Unlikely Low Acetone Inhalation and skin exposure (during leak testing) Highly flammable Inhalation Irritation to eyes and skin CONSEQUENCE E Negligible LIKELIHOOD L5 Highly unlikely Low Current Operator. Operation only with with gun covers on and electronics cabinets in place. CONSEQUENCE E Negligible injury LIKELIHOOD L5 Highly Unlikely Low P8 Electrical Hazard Contact resulting in current flowing through the body Electrical injury Current Operator, Person in Charge, Contractors. CONSEQUENCE A Major LIKELIHOOD L5 Highly Unlikely High Risk Assessment Completed By: Signed: www.monash.edu/ohs/

SAFETY OPERATING PROCEDURES Reliotron III Cathodoluminescence Instrument SAFETY OPERATING PROCEDURES Warning: High Voltage supplies used can cause severe electric shocks to the operator if in contact with the cathode, cable or power supply internal components during operation or test. They should never be operated with gun covers off or with electronics cabinets removed. X-ray equipment may produce radiation out of the equipment. X-rays may risk injury to an unborn child and/or may interfere with the treatment of a cancer patient. If you are pregnant or a cancer patient, consult your physician before use and/or being exposed to x-ray equipment. www.monash.edu/ohs/