OPERATING MANUAL
Philips XRG – X-Ray Goniometer System
INDIANA UNIVERSITY
Department of Geological Sciences
Written by R. Ensman
Contributions By: C. Shriner, P. Levy, B. Mertz & K. DeHart
1
OPERATING MANUAL FOR THE PHILIPS XRG-3100
COMPUTER-CONTROLLED X-RAY DIFFRACTION UNIT
Rev. January 10, 2010
Table of Contents:
page
Principles of Crystallography Using X-Ray Diffraction
3
Safety Precautions for Using X-Ray Equipment
3
Sample Preparation
5
Operation of the X-Ray Generator and Goniometer Instrumentation
Preliminary Checks
Turn on the AC Line Power
Turn on the X-Ray Generator
Shut down the Generator
8
9
9
16
Startup Procedure for Databox / Computer Control
12
System – Operational Verification
13
Running Samples
14
Presentation of Results Using JADE Software
17
Optimization of Goniometer and Signal Conditioning Parameters
Calibration of 2 Goniometer Readout
Optimization of Signal Conditioning Parameters
XRG Maintenance / Scheduling
Condensed Operating Instructions
Sample XRG Printout for Alpha Quartz
20
22
23
24
26
(See a separate Operating and Maintenance Log 3-ring binder for notes)
Revision : 8/15/2011
file name:
2
XRG Manual Ha.docx
Principles of Crystallography Using X-Ray Diffraction
1. A collimated beam of monochromatic x-ray photons directed at the surface of a finely divided
mineral or kaolin sample will be diffracted at various angles that depend upon the mineral content
of the sample.
2. The intensity of the diffracted beam and the angle between the incident and diffracted beam (2)
can be used to identify a mineral or minerals present in the sample.
3. The relative intensity of peaks (usually two or more) and their corresponding 2 angles can be
compared with spectra of known pure minerals to help determine the composition and relative
percentages of complex mineral mixtures.
Safety Precautions for Using Single Layer Shielded X-Ray Equipment
1.
The Philips XRG-3100 X-Ray Diffractometer utilizes radiation that is readily absorbed by soft tissue.
Severe damage to skin and/or longer term cancer risks is a possibility due to prolonged exposure or
cumulative exposure over time.
2. The XRG-3100 system was designed many years ago and thus presents a higher risk source of radiation
exposure than the double radiation shielding used in modern instrumentation. Additional lead sheet
shielding has been added over the years to shield potential “hot spots” (very narrow beams of
radiation).
3. However, extra precautions that are to be taken by operators are:
a.
All operators must wear a radiation
badge (finger, film type) on their hand
likely to be used close to the x-ray
beam. Periodic badge testing will be
responsibility of the machine
supervisor.
most
the
b. At the start of each
machine use, with the beam ON,
a sample in place and the shutter
open, a radiation monitor
(Scintillometer – Model 3 by
Ludlum Co.) must be used to
scan all areas where the beam
will pass to look for leakage.
3
4. Proper use of the Ludlum Model 3 Scintillometer will include:
a. Use the mode switch to select Battery Test –
observe that the battery voltage is adequate.
b. Select the Sensitivity mode at the “x1” position
and be sure that the Audio feature is
ON –
to preclude having to watch the meter while
moving the probe around the area.
c. Normal background radiation readings will fall
200–400 Counts (beeps) Per Minute (CPM)
Readings substantially above background are
reported to qualified service personnel before
continuing with instrument use.
4
in the
range.
to be
Sample Preparation – Sample Carrier: Back Loading Method for Powdered Samples:
1. Materials Needed:
a. Tape – masking or transparent, XRG sample holders, razor blade, glass slide (frosted), mortar
and pestle, No. 150 mesh or equivalent sieve.
2. Procedure:
a. Grind the sample to a fine powder and sift it through the sieve.
b. Remove the metal backing plate from a XRG sample holder.
c. Tape a glass slide (frosted is better) onto the front of the sample holder.
5
d.
Load sifted sample into the open back of the holder.
e. Use a razor blade to pack the sample into the
holder and remove any excess.
f.
Snap on the backing plate and press down.
6
g. Turn the sample holder over and press down on the glass slide.
h. Slide the glass plate off the sample /holder and hold it upside down to ensure the stability of the
packing.
i.
Ready for insertion into the XRG Goniometer for analysis. (See section on Running Samples)
7
Operation of the X-Ray Generator and Goniometer Instrumentation
Preliminary Checks:
1. Be sure the water pressure gages for water cooling system for the X-ray generator reads in the
range of 40- 65 PSI. Check the gauges behind the X-ray generator – before (inlet) and after
(outlet) the filter. A pressure greater than ~30 PSI is necessary for generator operation.
a. Inlet and outlet valves handles are to be turned to a position parallel to the piping to permit
water flow. With the X-Ray beam ON, if the input pressure is 10 PSI (or more) than the
outlet pressure, the water filter probably needs to be changed.
b. Note that generator interlocks measuring water flow will turn off the X-Rays, if the pressure
falls below ~25 PSI.
2. Observe the setting of the Goniometer’s 2ϴ angle indicator to ensure that it reads +2.00
(degrees) or greater.
Observe that the 2ϴ angle displayed is
40.00 degrees.
a. Operating Less than 2 will increase the possibility of a direct x-ray beam impinging onto
the detector – this may well damage the scintillator and/or photomultiplier detector.
[NOTE: In an emergency, the Goniometer scan motor can be stopped immediately by
shutting off the Data Box power switch.]
b. If needed, engage the adjustment handle (push in) and
manually adjust the 2ϴ indicator dial to a suitable starting
angle. The Data Box Power Switch must be OFF to
enable manual 2ϴ adjustment.
8
Turn On the AC Line Power:
1. Turn ON the main power for the X-ray generator and the power supply that services the X-ray
signal processing electronics, the Goniometer angle controller (Databox) and the Goniometer
stepping motor by pushing the handle up on the grey switch box mounted on the east wall.
a. This enables AC power to the X-ray generator and powers a multi-voltage power supply,
located in the lower section of the electronics cabinet, which powers the NIM Bin (holding
the electronics signal modules and the DATABOX NIM module).
Turn on the X-RAY Generator:
1. Be sure that the KV is set to 25 (minimum setting) and the MA to 10 (starting).
2. Turn on the Power key switch (clockwise) on the left side of the generator control panel and notice
that the red X-RAYS OFF light comes ON.
9
3. Notice that none of the Overload or
Fault lamps will have come on.
However, if one or more does come on,
try restarting (step 2). If unsuccessful,
call a maintenance technician for help.
4. Be sure that the Current Control Switch (at the right end of the
panel) is set to OPERATE (not to Minimum MA) and use the
DISPLAY button switch to set the Panel Meter display to KV.
.
5. Be sure that the sample compartment cover is on and
to lock it in place and that the mechanical beam shutter
has enabled the beam shutter – an audible click will be
the cover is rotated.
turned CW
mechanism
noticed as
5. Push the X-RAYS ON button (the second switch to
the right of the key switch) and hold until the KV panel
meter reading stabilizes at 25 KV.
Observe that the yellow X_RAYS ON
lamp sitting on top of the generator has
turned ON. Know that, if the light bulb
inside of the yellow shroud burns out, the
beam shutter will not open.
10
Obser
ON sa
the ge
Know
of the
beam
6. Bring up the KV (high voltage) SLOWLY (5 KV steps) to 45 KV maximum (for a copper, (CU), anode
x-ray tube) by pushing the vertical stepping switch down and waiting for the Panel Meter to stabilize
after each increment before proceeding.
7. Toggle the DISPLAY switch to indicate MA (Milliamperes) and use
stepping switch to SLOWLY increase the current in one milliampere
toggle both digit switches at once in going from 19 to 20 MA. Do not
MA for a Cu x-ray tube.
a. Using less than 20 MA may prolong the life of the x-ray tube,
reduce the intensity of the X-Ray beam and diffraction peak
the MA
steps –
exceed 20
but will
heights.)
Observe that the Shutter Light
(orange plastic cover) at the
output of the X-ray tube is OFF –
indicating that the beam shutter
remains Closed – though enabled.
8. Push the Shutter Open button on the right side of the
Generator Panel.
9. Observe that the
orange X-Ray
beam light at the X-Ray
source comes
ON and know that an X-Ray beam is now passing into the sample
compartment.
10. Refer to the Safety Precautions section in this manual – specifically part 3 and use the X-Ray beam
detection meter / Scintillometer to check for radiation leaks before beginning a series of sample runs.
This procedure completes the steps for start-up of the X-Ray Generator and attainment of
beam. Next - go to: Running Samples, Goniometer 2 Calibration or Generator ShutDown Procedure.
11
Startup Procedure for DATABOX - Computer Control and Data Acquisition
1. Turn ON the power to the Computer, if it is not already ON.
a. NOTE: The current computer in
(9/2010) must be left ON at all
to ensure proper startup
communication with the DataBox
module. If the computer power is
to be OFF, communication with the
DataBox can be established by
following the instructions for
“Restarting the communications
between the DataBox and the
Computer” – see below:
use
times
found
link
2. Turn ON the Monitor and the Printer.
a. Note, that if the computer, monitor and printer are all that will be used to view or manipulate
data already taken, bypass steps 3 & 4.
3. Turn ON the AC Line power at the breaker box which will turn
on the NIM BIN power supply – the bottom unit in the relay rack
cabinet.
4. Turn ON (UP) the NIM BIN signal
electronics - Switch #1 (at the lower
of the NIM BIN) and the power to the
DATABOX – Switch #2 (on the
– which also powers the Goniometer
motor used to change 2 .
left end
Databox)
stepper
5. Restarting the communications link between the DataBox and the Computer.
If the Databox program will not communicate with the DataBox, this will likely be the result of
having turned the computer off after its last use and communication between the DATABOX and
the Computer has been lost. Go to the device manager on the computer (via: Start, Settings,
Control Panel, System, double click and then to Device Manager) and delete both COM1 and
COM2 ports. Then reboot the computer after being sure that the DataBox power is ON.
The computer should automatically find the appropriate port and restore the link.
12
System – Operational Verification
1. Enter the Databox program using the computer cursor. (Note: The Databox NIM module must be
ON at this point.)
2. Set Steps/Degree – Type “S” (if not on screen) and enter 200 (a “normal” selection). Type – RTN
(Enter)
3. Determine the 2 angle as displayed on the
Goniometer counter and dial – to the nearest
degrees.
(The 2 angle in the photo now
0.005
reads
40.00 degrees.)
a. Notice that the counter display will “turn
early as the dial is rotated in the CW
direction; and may cause confusion as to
actual 2 setting. For example: if the
is 4.35 degrees, this is the correct angle.
reading is 5.85, the angle is actually 4.85
5.xx has turned over early).
over”
the
reading
If the
(the
4. Enter the Starting Angle – “A” and enter the 2 angle as read. (Note: following zeros need not be
entered.) Do not set 2 at less than 2 or more than 50 degrees! Type – RTN
5. Enter the 2 angle at “G” The angle to which you want the Goniometer to GO (usually the starting
angle for a run.) Do not set 2 at less than 2 or more than 50 degrees! Type – RTN (The stepper
motor on the Goniometer should drive the detector to the selected 2 angle and stop precisely at that
destination. If true, angle drive calibration is verified.
a. For an Emergency Shutdown - If there is a
malfunction or an erroneous 2 has been entered, it is
possible that the X-ray detector or the Goniometer
be damaged. Stop the slewing Goniometer motor at
by turning off the Databox power switch - #2.
6. Enter a Title – at the “T” prompt. The Title may be as
and descriptive as needed.
7. Type “E” for Enter and then RTN to go to the Edit Mode.
13
may
once
long
RUNNING SAMPLES:
1. Close the Beam Shutter – using the white pushbutton on the right side of the generator panel.
[photo 12] Notice that the orange beam shutter light is OFF and know that the X-Ray beam is
OFF.
2. Open the Sample Compartment cover, release
friction lock by turning the small knurled knob
degrees CCW, then turn the cover CCW until
mechanical shutter is released and pull the cover
you. {This mechanical shutter lockout is a
secondary mechanism to ensure that the x-ray
blocked from entering the sample
compartment.}
the
~180
the
toward
beam is
3. Remove any sample holder in the chamber by
pushing down on the spring clip with a spatula or similar tool
and remove the sample holder. With a damp tissue wipe out
any residual sample powder from the chamber.
4. Insert a new sample/holder using the reverse
procedure above – being sure that the sample is
centered on the holder pedestal. Release the spring
clip carefully and replace the chamber cover with a
CW rotation and lock it in place with modest CW
tension on the locking screw.
14
5. Set Experimental Parameters:
a. Type I (Initial 2) and enter the Initial/Starting 2 degrees for the run. RTN. Note: One
can scan a desired range of angles beginning either at the highest or the lowest.
b. Type F (Final 2) and enter the final/ending angle for the run. RTN.
c. Type S, then enter the Step Size (see table below), then RTN.
d. Type C, then enter the Count Time for each successive angle, then RTN.
2 STEP Size (Degrees) Count Time (seconds)
Degrees per Minute
.03
1
~2
.06
2
~2
.01
1
~ 0.6
.02
2
~ 0.6
.02
1
~ 1.2
.10
1
~5
.01
6
0.1
.03 / 1 is the default step / count parameter.
e. Type E, then RTN to go back to the monitor mode.
f. Type S to start the run.

When prompted for a Title, enter a new title, then RTN or press RTN for the previously
entered title. The title will display and data collection will begin.

For a real-time display, press F7 (Press ESC to exit real-time). To change display
parameters, press PGUP.
g. When Data collection is complete, press F8 to quick dump the data into MDI format (this is
an ASCII format).

The file name for this format must be short and without “_” or spaces. No suffix is
needed.

With certain runs (multiple sequences) the quick dump command will give an error
message. For this situation, use F4, then RTN to download the data (use the default file
name supplied, since it is only a temporary assignment) then proceed to save it in the
MDI format by pressing F8 and your own short and unique file name.

Press ALT-F7 to retrieve the dump as a display, if desired.
15
h. To run additional samples, with the same parameters - Close the shutter, Replace the
sample, Open the shutter, type T, then enter a new title, then RTN and Press S and RTN to
start the run.
i. To run additional samples with different parameters, Press E (Edit) then RTN and Press P
(for previous session) to go back to step 5 above to enter the new parameter(s).
To Shut Down the XRG System:
1. Close the Shutter and Remove the Sample – replace the sample compartment cover.
2. Reduce the HV current in one mA steps to 10 mA (starting setting).
3. Toggle the digital display selector to read KV and bring down the voltage in one KV steps to 25 kV
(the minimum setting).
4. Push the X-RAYS OFF button.
5. Turn off the Generator with the Key Switch.
6. Turn off the Databox NIM module with switch #2.
7. Turn off the NIM Bin electronics rack with switch #1.
8. Turn off the main AC Line power switch box on the east wall.
9. Fill out the System Log Book noting the hours used, date, operator and enter any malfunctions
noted in the Maintenance Notes section, etc.
16
Presentation of Results Using JADE Software
JADE (program) COMPUTER PROTOCOLS
For use with XRG Instrumentation
1. Opening files.
a. To open a file, go to File -> Open.
i. Files are automatically placed in the “Databox” file when saved out of Databox, they
must be manually moved to other files (e.g. “Clay Lab”, etc)
ii. After selecting a file, click on “New Plot” to open.
iii. You may also choose to “overlay” one plot over another through this window.
2. Analyzing data
a. Zoom window controls
i. The zoom window is the window that opens automatically when a file is opened – it
shows a graph of the XRD findings.
ii. On the right side of the graph, there are several controls for the graph’s properties.
1. When the mouse is placed over these buttons, what they control will be
shown on the top, blue, bar of Jade. Each of these buttons does at least two
things – one for left-clicking, another for right-clicking.
2. The “Reset” button can only reset the screen back through one change, i.e., if
you to a background elimination, then do a 2nd elimination, the reset will
return you to the graph of the 1st elimination, not the original data.
b. There is a data-edit horizontal toolbar located above the zoom window.
i. The buttons are, left from right:
1. Cursor
2. Peak-edit I
3. Peak-edit II
4. Peak-paint
5. Background-edit
6. Data-edit
7. K-alpha2 edit
8. Profile fitting
9. Cubic indexing cursor
c. Background-editing
i. To filter out the background, click on either Analyze  Fit Background, or left-click
the “BG” button on the uppermost toolbar, or right-click on the Background-edit
(BE) button.
1. By left-clicking on the “BE” button, you can manually fit a background
curve.
ii. Double-clicking on the “BG” button will re-fit the graph to correct for the
background.
17
d. Peak list
i. Jade can automatically find peaks in the data. To do this, press F2, or go to Analyze
 Find Peaks.
ii. This will open the “Peak Search and Labeling Dialog,” which allows changing the
search parameters, including filter length, and labeling options. Click “Find” for Jade
to scan for peaks.
iii. To read the peaks as a list, click View  List Reports  Peak List Report.
1. From the Peak List Report, you can delete peaks that are unnecessary or
caused by background noise
e. Comparing data with PDF files
i. On the top toolbar, there is a space to type in either the mineral name (i.e.
“QUARTZ”) or the mineral ID#. Press return, and a new toolbar will appear with the
mineral name, and lines will appear on the graph corresponding to the mineral’s
peaks.
ii. You can then enter other minerals, to make multiple comparisons.
1. To keep a mineral’s peaks visible, you must “tag” it using the button that
looks like a push-pin. Clicking on the ‘?” button will open a settings window.
iii. If a mineral has been tagged, a printout will include that mineral’s peaks as a bar
running beneath the graph of your sample’s data.
iv. View  List Reports  Peak ID (Extended) or Peak ID (Compact) will show your
data’s peaks with the corresponding mineral’s peaks and show the differences
between them.
f. Search/Match
i. This allows for the computer to compare your data to its own database of minerals,
and determine possible matches
ii. Can be accessed either by clicking the “S/M” button or via the top toolbar.
1. Clicking on this will open a window with various setting that can be changed
– since this computer has only one database of minerals, it is important not to
change that setting.
iii. After beginning the Search/Match run, a message may come up stating that the
background noise must be eliminated, allow Jade to do this automatically.
iv. The “hit list” will show various potential matches, and which peaks appear to
correspond in the data. There are various filtering options you may use to alter the
data.
18
g. Printing
i. You can print the “zoom window” directly just by pressing the print button on the
top of the screen. There are also print buttons for Peak List Report and Search/Match
Report windows. Under the File button there is a Print Plot button which prints the
current “zoom window” and a Print Report button that expands to who printable
reports including the Peak List report which we usually print on the back of each
printout.
ii. File  Print Setup allows you to make several changes to the page that will be
printed.
NOTE:
1. An important note: because of the printer’s settings, light colors do not print
well. Once you are in print setup you can press the setup button and choose
black and white under Plot Color Settings.
2. The buttons at the top of the print setup screen allow you to add arrows,
shapes and text. For example to add text click the button all the way to the
right with the “a and b” on it. Then click anywhere on the pattern and a text
cursor will appear. Type the text you want to add and press enter.
3. There are five buttons on the bottom left that show small pictures of what the
pattern printout will look like. Pushing these will change the style of the
printout. Not all are always available. Some require stick bars from using
the mineral identifying features and some require more than one pattern in a
printout.
a. The top button gives a standard printout. Any patterns and stick bars
are printed in one band.
b. The second button prints all patterns in a single band with a separate
band on the bottom for stick bars.
c. The third button is the same as the top button but splits the band into
two sections. All patterns and stick bars are overlaid together.
d. The fourth button prints each x-ray pattern in its own band with stick
bars overlaying the pattern.
e. The fifth button prints each x-ray pattern in its own band with a
separate band at the bottom for stick bars.
19
Optimization of Goniometer and Signal Conditioning Parameters
The procedures and parameter adjustments described in this section are normally left to an
instrumentation specialist, electronics engineer and/or computer specialist, as applicable.
Begin with the section on: Operation of the X-Ray Generator and Goniometer Instrumentation.
Calibration of the 2 angle readout for the Goniometer:
1. Insert a known standard sample (-quartz or other standard desired) into the sample chamber (see
section Running Samples - 1-4).
2. Note that the following NIM modules are in place and properly connected together – back panel:
Detector Power Supply, Amplifier, Threshold and Window, Rate/Level Meter. The following
parameter settings are those considered nominal.
a. Detector Voltage – SCINTillation
0.6 KV + 50 Volts (FINE)
KV –
b. Amplifier Gain – x 128 ; Input
(at bottom of module)
– Scint.
Select
c. Baseline/Threshold – 0.45 ;
Window - ~4/10 (not critical)
d. Baseline Control – INTernal,
INTEGrate
e. Clock Signal - OFF– OFF
Mode –
f. Rate Meter Range – as needed (~
Time Constant – 1-2 seconds;
%Supp. - ?, AUDio – ON or OFF
desired.
10-5K);
as
20
3. Start up the XRG System – see section Operation of the X-Ray Goniometer and
Goniometer Instrumentation - through Startup Procedure for Databox – step 3.
4. Select two or three (better) major 2 diffraction peak angles listed in the literature for the calibration
standard sample chosen. (For Alpha Quartz these are: 50.20, 39.52, 36.52, 26.68 and 20.85
degrees).
and
angle for
the
to
5. Turn the mechanical 2 angle counter dial
vernier dial by hand to near the desired
the first diffraction calibration peak. (As
handle is rotated, push in the crank handle
engage the vernier with the 2 gear train.)
6. Adjust the Amplifier Gain or the Rate
Meter
Range switch to obtain a working
deflection of the Rate Meter and then
manually
rotate the vernier dial setting back and forth
through
the radiation peak (highest rate meter
deflection. (Adjust the rate meter range and the time constant to obtain the highest possible meter
deflection.)

Note: The most accurate calibration procedure will result from approaching the final peak
angle from the same direction (CW or CCW) as will be used to scan samples. This is
because there is a small but finite back-lash in the gearing of the Goniometer – less than
0.02 deg.
7. Write down the 2 angle observed to the nearest 0.005 degree and compare this result with the
literature value to determine the error and its sign.
8. In like manner, determine the magnitude and direction of the error for the other calibration peaks.
9. If the errors are found to be significant, mechanically adjust the vernier dial relative to the
Goniometer gearing to minimize the net error by:
a. Turn on the power to the Databox, which will of
gear train.
the
b. Loosen the three screws in the face of the vernier
and push in on the handle shaft until the friction
between the shaft and the dial is broken. Rotate
to the desired position and retighten the screws.
dial
fit
the dial
10. Recheck the error at each of the calibration peaks.
21
Optimization of the Signal Conditioning Parameters:
1. Set the Voltage to the Detector: a photomultiplier tube that detects light pulses coming from a
scintillator crystal as a function of X-Ray intensity.
a. On the Scintillator NIM module,
the SCINT. KV selector to 0 .6
and the vernier dial to a nominal
Volts (0.50 of full scale). Settings
to 1000 volts are possible, but the
signal to noise ratio will fall near
nominal setting of 650 Volts.
adjust
KV
50
of 450
best
this
b. Set the Gain of the Signal
Amplifier Module (Nominal
is x 128 to x 512). This module
not substantially change the signal
noise ratio as a function of gain.
setting
will
to
2. Set the Baseline/Threshold dial to a level that exceeds the background noise from the
photomultiplier and the previous signal conditioning modules – this setting will depend on the PM
voltage and Gain settings. Nominally, a setting of 0.4 to 1 (full scale of 10.0) will work. If the
Threshold is set too high, some of the weaker pulses from the diffracted x-ray beam will be
rejected, too low and PM noise will dominate. (0.40 to 0.45 works well.)
3. Set the pulse height window to a value that will not exclude the strongest x-ray pulses, as detected
by observing the rate meter. (Little effect will be noted if only diffracted X-Ray pulses are
dominate.)
4. Adjust the Rate Meter Range and Time Constant settings to obtain sufficient pointer deflections to
optimize signal levels.
5. Note that: The signal going to the Databox Module is derived from the output of the Baseline and
Window Module and is not affected by any adjustments of the Rate Meter module. The Databox
Input signal is applied at the back of the module and can be accessed (in parallel) at the front panel
– marked Input.
22
XRG Maintenance / Scheduling:
Daily: During each session of use – by the Operator.
Each user should run a standard sample (Alpha Quartz) or a user selected standard similar to the series of
samples being investigated. Prudently – run the standard first (and, perhaps, last).
Any deviation from expected results or aberrant operation of the instrument should be reported in the
separate Maintenance Logbook and/or directly to the Instrument Supervisor.
Quarterly: Conducted by the Instrument Supervisor or a designee.
Review all comments written by users in the XRG Operations Logbook and take action as necessary.
Semi Annually: Conducted by the Instrument Supervisor or a designee.
Run an Alpha Quartz Standard to confirm the 2 calibration of the Goniometer by comparing the results
with previous data: angular and peak amplitude . The procedure and major useful diffraction angles are
listed on Page 21, section 4.
Check (and adjust) all electronic and mechanical aspects of machine operation –
Lubrication of moving parts – Goniometer drive gearing; sample compartment loading mechanisms and
mechanical shutter interlocks; cooling water filter and pressure; switches and lighted displays; standard
settings of the signal conditioning electronics panels; Computer, Monitor and Recorder operation; JADE
software functionality;
23
Philips XRG Instrument - Condensed Operating Instructions
A. X-Ray Generator Start-Up:
Reference to Manual - Page
1. Check cooling water pressure gages – normally 50-60 PSI
8
2. Mechanically and accurately set the Goniometer to a desired 2ϴ angle – greater than 2o
8
3. Check to see that the initial KV and MA settings are at 25 KV and 10 MA
9
4. Turn ON the AC Line power at the wall-mounted breaker box
9
5. Turn on the Generator using the Key Switch
9
6. Note that no overload or error lights come on
10
7. Set the Panel Meter Display modes to KV and Operate
10
8. Be sure that the sample compartment cover is on and rotated to enable the beam shutter
10
9. Push the X-Rays ON button and hold until the Panel Meter stabilizes at 25 KV
10
10. Did the X-Rays ON lamp sitting on top of the generator come ON?
10
11. Bring up the HV slowly to 45 KV in 5 KV steps.
11
12. Select MA with the Panel Meter Display push-button switch
11
13. Slowly Increase the MA from 10 to 20 (in 1 MA steps) using the MA rotary switch(s)
9 & 11
14. Push the Shutter Open switch and note that the orange “Shutter Open” lamp comes ON
15. Check for radiation leaks with the Scintillometer.
11
3, 4 & 11
16. Turn OFF the Shutter Open Switch and observe that the Orange lamp goes OFF
11
B. X-Ray Detector Instrumentation and Computer Start-Up:
1. Turn on the NIM BIN power switch (labeled #1)
12
2. Turn on the Computer, Monitor and Printer, if not already ON (the computer should be left ON) 12
3. Turn ON the Data Box NIM module using switch #2. The Goniometer should not be moving!
12
4. If the Goniometer stepper motor is running and 2ϴ is getting close to 2o or ≥ 50o,
a. Immediately turn OFF the Data Box power with switch #2! Emergency Shut-Down!
5. Bring up the DataBox program on the computer. If the program does not work, see Restart.
12&13
24
12
C. Enter the DataBox Program to Verify Program Operation:
1. Type “S” to set the Steps / Degree - 200 is a nominal value – Type Return (RTN) /Enter
13
2. Type “A” to enter the Starting 2ϴ angle (least significant “0’s” need not be entered);
a. Use the 2ϴ angle mechanically set in step A-2 above; but, not ≤ 2 or ≥50 degrees.
13
3. Type “G” (“Go To”) to enter any angle other than the Starting 2ϴ angle and type ENTER
13
a. The Goniometer should scan automatically to the “Go To” angle just entered.
4. Type “E” to exit to monitor.
5. Set Edit mode.
D. Running Samples:
1. Close the X-ray beam Shutter with the white push button – the Orange Shutter
light should go out
14
2. Open the Sample Compartment Cover and insert the sample carrier
14
3. Close the Sample Compartment Cover
14
4. Set the experimental program parameters using the DataBox program
15
5. Type “I” (Initial 2ϴ - Starting angle) and enter the desired angle – then type ENTER
15
6. Type “F” (Final 2ϴ angle desired) and type ENTER
15
7. Type “S” (Step Size) Type the angle desired – (Nominal value = 0.03o) – Type ENTER
15
8. Type “C” (Count Time) Type the time desired) – (Nominal 1 second) - Type ENTER
15
9. Type “E” (Edit Mode) Type ENTER to go back to the Monitor Mode.
15
10. Type “S” (Start ) to start the run.
11. When prompted for a Title, enter the Name of the run and then type ENTER to start the run.
15
12. For a real time display, Press F7 (ESC to exit real time) PGUP to change display parameters
15
13. When Data Collection is complete, Press F8 to dump the data – various options are available,
see Operation Manual, section 5g, p. 15
15
14. To run additional samples - same parameters - Close Shutter, exchange sample, Open Shutter
16
15. Type “T” and enter a new title
16
and Type “S” and ENTER to start the next run.
16. For running different parameters, Press E (Edit) then ENTER;
to go back to D4
25
Press P (Previous Session)
26