Download BEAM TURN ON

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.
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SAFETY OPERATING PROCEDURES
Reliotron III Cathodoluminescence Instrument
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.
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SAFETY OPERATING PROCEDURES
Reliotron III Cathodoluminescence Instrument
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.
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SAFETY OPERATING PROCEDURES
Reliotron III Cathodoluminescence Instrument
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.
1. Turn the control knobs all the way Counter Clock wise
2. Turn the mode selector switch to the “Pump” position.
position, the beam voltage cannot be turned on.
3. Turn power on, on wall,
both switches, pump and
console.
3
Console
In this
4. Turn on Transformer. The
instrument is from USA
therefore a transformer is
needed to convert to the
correct Voltage.
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.
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SAFETY OPERATING PROCEDURES
Reliotron III Cathodoluminescence Instrument
7. Turn on the beam voltage by pushing the “High Voltage” switch/button.
7.
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.
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.
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SAFETY OPERATING PROCEDURES
Reliotron III Cathodoluminescence Instrument
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.
• 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.
Vent Cap
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Drawer
• The chamber will now pump
down and the progress can be
followed with the TC gauge
pressure readout on the front
panel.
SAFETY OPERATING PROCEDURES
Reliotron III Cathodoluminescence Instrument
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.
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.
• Carbonate samples will luminesce at approximately -06.0 kV.
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SAFETY OPERATING PROCEDURES
Reliotron III Cathodoluminescence Instrument
• 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
BEAM TURN OFF BETWEEN SAMPLES the purge valve the same as
the vent cap.
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.
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SAFETY OPERATING PROCEDURES
Reliotron III Cathodoluminescence Instrument
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.
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SAFETY OPERATING PROCEDURES
Reliotron
III Cathodoluminescence
Instrument
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 Xrays. 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:
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Signed:
RISK ASSESSMENT
Reliotron
III Cathodoluminescence
Instrument
SMALL
ERAMIC JAW CRUSHER
HAZARD
TYPE
Exposure
to noise
59-71
(dB9A)
X-ray
exposure
Ethanol
(for cleaning
microscope
optics)
DESCRIPTION PERSONS AT RISK FACTOR CONTROLS IN RISK FACTOR
PLACE
OF
RISK
WITHOUT CONTROLS
WITH CONTROLS
IN
PLACE
IN PLACE
HAZARD
TO LOWER RISK
Prolonged
Low level
noise.
> 2 Hours
Low
level
radiation
damage. Risk
to pregnant
women and
cancer
patients
Highly
Flammable
Current
Operator,
Person in
Charge,
Contractors.
CONSEQUENCE
Negligible
hearing loss
LIKELIHOOD
L4 Unlikely
CONSEQUENCE
Current
Operator, B5 Severe injury
LIKELIHOOD
Person in
L5 Unlikely
Charge,
Contractors.
High
Current
Operator.
CONSEQUENCE
E Negligible
LIKELIHOOD
L5
Highly unlikely
No hearing
Protection
required
Low
Lead Glass
and sample
holder
prevents XRay emission
Minimum
amount
and fire
blanket
Low
Acetone
Inhalation
and skin
exposure
(during leak
testing)
Highly
flammable
Inhalation
Irritation to
eyes and
skin
P8
Electrical
injury
Electrical Hazard
Contact resulting
in current
flowing through
the body
Risk Assessment Completed By:
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Current
Operator.
CONSEQUENCE
C5 Negligible
injury
LIKELIHOOD
L4 Unlikely
CONSEQUENCE
B5 Negligible
injury
LIKELIHOOD
L5 Highly Unlikely
Low
CONSEQUENCE
E Negligible
LIKELIHOOD
L5
Highly unlikely
Low
Correct storage CONSEQUENCE
CONSEQUENCE of acetone in
C5 Negligible
E Negligible
spray bottle,
injury
LIKELIHOOD
not contact
LIKELIHOOD
L5
with eyes and
L4 Unlikely
Highly unlikely
skin.
Low
Low
Current
CONSEQUENCE Operation only
with with gun
Operator,
A Major
Person in
LIKELIHOOD covers on and
electronics
Charge,
L5 Highly
cabinets in
Contractors.
Unlikely
place.
High
CONSEQUENCE
E Negligible
injury
LIKELIHOOD
L5 Highly
Unlikely
Low
Signed:
SAFETY OPERATING PROCEDURES
Reliotron III Cathodoluminescence Instrument
• 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.
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