Part 3. Bruker D8 Standard Operating Procedure (SOP)
Operating Procedures
XRD Safety and General User Responsibilities
Emergency Instrument Shutdown
Turning on the D8 Instrument
Running the D8 Instrument
Normal Instrument Shutdown
Turning on the Sol-X Detector
Calibrating the Sol-X Detector
Putting the Sol-X into Standby Mode
(Note: This item needs updating)
(Note: This item needs updating)
(Note: This item needs updating)
XRD Safety and General User Responsibilities
CAUTION: X-ray Generating Equipment!!
The Bruker D8 ADVANCE XRD uses a high voltage power supply to generate x-ray
radiation. Before using the Bruker D8 ADVANCE XRD all users must be certified by
the College of Science and Engineering Radiation Safety Officer (Linda Vadura, ext. 86892, lvadura@sfsu.edu) in x-ray safety. In addition, training in the use of this
equipment by one of the instrument principle investigators must administered prior to
authorized use of the equipment.
See Part 2 of this document which outlines X-Ray Safety and Training and follow these
instructions prior to use of this equipment.
In case of an accident or emergency contact SFSU Campus Police at:
911 or 338-2222
Emergency Instrument Shutdown
NOTICE: In the event of an instrument malfunction, fire, earthquake, or
other emergency the Bruker D8 can be shut down rapidly using the
Emergency Instrument Shutdown procedure below. Do not use this
procedure for routine shut down of the instrument.
1. Hit the red Emergency Stop button on either rounded front corner of the D8
instrument cabinet. X-Rays are no longer being generated, but the storage
capacitors in the generator will continue to hold electrical charge for >15 minutes.
2. Turn off power to other parts of the instrument by depressing the red "0" button
on the rounded right-hand corner of the instrument.
3. Turn off electrical power to the Haskris water chiller and water valves to the city
water supply.
Turning on the D8 Instrument
1. Haskris water chiller.
o Open water supply to the Haskris water chiller (3 valves). Verify that no
leaks are occurring and that all valves are open.
o
Turn ON Haskris power (ON/OFF switch front panel). Note water flow meter
and temperature settings and record these values. The pump motor sounds
should be audible. The instrument requires a flow rate of at least one
gal/minute and a water pressure of 70 to 75 psi.
o
2. Turn on the PC computer monitor and the computer. Wait until the computer is
fully booted.
Username: BrukerAdministrator
Password: Bruker (case sensitive)
3. Power on the D8. Be sure that power to the D8 goniometer and the detector are
turned off. Reset the X-ray generator by twisting the red Emergency Stop buttons
on both rounded corners of the instrument. Power to the D8 is controlled by the
round red "0" (off) button and green "1" (on) button on the rounded right-hand
corner of the instrument.
Turn D8 power ON
Turn Fan ON
Turn D8 light ON
(Round green "1" (on) button on right corner panel)
(Round green fan button on left corner panel)
(Round green light button on left corner button panel)
4. Open D8 TOOLS Software (on PC desktop)
a) Click “On-Line Status” →
b) Click "On Line Refresh ON/OFF" icon (last icon on the left)
→ D8 Instrument status page appears (see Figure 1)
c) Click “Instrument Status” ; On menu tree
d) click → Drives
→ Theta (click → "Adjust" button) (see  icon)
→ 2Theta (click → "Adjust" button) (see  icon)
→ spinner (click → "Adjust" button) (see  icon)
e) Click “Alarm (red box)”
f) Click “X-Ray Generator” tree
Note: Because X-ray generator is off, capture register will have "alarms"
(red boxes) that must be cleared before running samples. This is normal.
On line Refresh ON/OFF
Figure 1. D8 Tools Instrument status page (Online Refresh ON/OFF button
is circled)
5. To turn on X-ray generator.
Rotate HIGH VOLTAGE lever clockwise (toward ON) for ~5 seconds.
X-ray alarm boxes (red) should go off after a few seconds Note: "X-RAYS
ON” lights goes on the light ring on top of the D8 and on LED panel on corner of
the instrument.
1. Close the D8 TOOLS page
6. If the Sol-X detector is being used, open the “MSPA-32” program (icon on
desktop).
Running the D8 Instrument
1.
Select “DIFFRACPLUS Measurement” icon on the desktop.
2.
Open up “XRD Commander” (opens data collection software—see Figure 2)
Figure 2. XRD Commander Page in DIFFRACPLUS Measurement software.
Circled items referred to in SOP.
Primary optic
X-ray power
Start angle
Detector
Scan type
Start
Stop angle
7. Set Up for Data Collection
a) Click → "Primary Optic" (Figure 2, circled). Choose either Bragg Brentano OR
Goebel mirror (depending on which unit is installed)
b) Ramp up X-ray generator power (at start up power = 20 kV, 5 mA)
Enter values and hit "set":
1-Enter 30 kV, 10 mA, hit "set", and wait 2-3 minutes
2-Enter 40 kV, 15 mA, hit "set", and wait 2-3 minutes
3-Enter 40 kV, 30 mA, hit "set", and wait 2-3 minutes
4-Enter 40 kV, 40 mA, hit "set", and wait 2-3 minutes
c) Choose scan type → "locked coupled" (Figure 2, circled).
11.
Select detector in DETAILS tab (at bottom)
[Note: "DETAILS" is actually the detector menu page]
Choose detector type (scintillation or Sol-X)
Note: If running the Solex detector, see detailed instructions later in this SOP.
Click
12.
→ "set detector"
To run a quick scan of your sample:
Push DOOR OPEN button
(Square Green button on right corner button panel)
CAREFULLY Open glass doors to the D8 and LOAD YOUR SAMPLE.
Close doors (should hear a "clunk" as doors lock)
14.
click
→
ADJUST tab [Note: this is the Data collection main page]
Enter the START and STOP angles and the increments in the
appropriate fields
click
→
START
[This will run a single scan of your sample]
To run a long scan, set up a JOB file in XRD WIZARD
click
→ XRD Wizard
→ Create a .dql file
→ Go thru the windows (menu) and click on appropriate values
[Note: Can run in XRD Wizard or Commander, but easier to set up a .dql file w/ run
parameters and run in commander]
click
→ "JOBS" tab at bottom of the window. Open your .dql file and run.
Normal Instrument Shutdown
1. In the Immediate Measurement program, set the generator power to 20 kV and 5
mA. Hit the Start button. When data collection has started, hit the Stop button.
Exit the Immediate Measurment program. Shut Down the PC computer.
2. Shut down the D8 controller by depressing the "0" button on the right side of the
rounded column of the instrument. Note that doing this will also shut down the Xray generator. X Rays are no longer being generated, but the storage capacitors in
the generator will continue to hold an electrical charge for at least 15 minutes.
3. On the generator control panel, depress and hold the heater button for at least 5
seconds or until the green lamp on the button is lit.
4. After 5 more minutes, turn the generator switch key to the "0" position, turning
off the generator.
5. Close water valves between the water chiller and the instrument. If there are no
other instruments using the water chiller then turn off the electrical power to the
water chiller and close the water valves between the chiller and the city water
supply.
Emergency Instrument Shutdown
4. Hit the red Emergency Stop button on either rounded front corner of the D8
instrument cabinet. X-Rays are no longer being generated, but the storage
capacitors in the generator will continue to hold electrical charge for >15 minutes.
5. Turn off power to other parts of the instrument by depressing the red "0" button
on the rounded right-hand corner of the instrument.
6. Turn off electrical power to the Haskris water chiller and water valves to the city
water supply.
Turning on the Sol-X Detector
1. Turn on power Sol-X detector controller. The controller is beneath the instrument
on the front upper right hand side. The switch on the far right side of the
controller should be in the up (I) position.
2. The display should now read "Ip-OK DC-OK" on one line and "Ready: Press F1"
on the second line. If not, press Start button (F1) until this message appears.
3. Press the Start button (F1). The controller will begin a sequence of events to
power up the detector. The different steps in the power up sequence will take
about one and a half hours.
4. The display on the controller should now read "Chan 2048 Real" on one line and
"Story" on the second line.
Calibrating the Sol-X Detector
1. Log onto the computer and open the "Immediate Measurement" program.
Initialize all axes of the goniometer by hitting the small goniometer icon on the
toolbar (hit the icon on the right). In the instrument controls on the left side of the
screen set Theta to 17.57, 2Theta to 35.14, the slit to 0.1, Phi to 90, Chi, X, and Y
to 0, Z to -0.090, kV to 40, mA to 40. Drive the instrument to these positions by
hitting the middle goniometer icon.
2. Place the corrundum, Al2O3, sample on the instrument. In the Immediate
Measurement program change the starting 2Theta to 35.14, the ending 2Theta to
36.00, and the scan mode to locked coupled. Hit the Start button on the program
window. When measurement begins, hit the Stop button. Drive the instrument
back to the proper starting position by hitting the middle goniometer icon. This
program will not be used again until it is closed at the end of this procedure.
3. Open the MSPA program. In the MSPA program hit the STOP button, the
CLEAR RAM button and the Yes button in the pop up screen. Select the boxes
next to the Cycle Read and Auto Scale so that they read On.
4. Press the START and READ RAM buttons. After about 5 seconds, a spectrum
with one strong peak should appear.
5. Electronic Calibrtion. In the upper window, using the left mouse button, drag
across the peak. After you drag across the peak, the peak will appear in the lower
window in a larger scale. In the lower window, drag across the center 2/3 to 3/4 of
the peak. This region will be highlighted and the peak maximum will be
automatically calculated.
6. Press the 1 button and then the CALIBRATION button. In the pop up box type
8.048 (keV) for Energy 1 and 0 for Energy 2. Press the OK button.
7. Press the SHOW button. In the fifth column (the second column labeled keV),
check that the number is below 0.40. Select the OK. button. If this number is
higher than 0.40 contact the lab director.
8. Setting the DAC Window (Discriminator). In the lower window, position the
mouse under the left side of the peak near the baseline. Hold the Shift key down
and click on the left mouse button. This sets the low energy channel for the
discriminator window(670-690). Move the mouse to the right side of the peak and
click the right mouse button while holding down the Shift key. This sets the
channel for the high energy channel for the discriminator window(745-755). The
MSPA program can now be closed.
9. In the Immediate Measurement program, close the shutter and remove the
corrundum sample from the instrument. Close the program, and log off the
computer.
Putting the Sol-X into Standby Mode
Every two to three weeks put the SOL-X into standby mode for at least 24 hours in order
to prolong the life of the detector and aid in maintaining constant, reproducible data from
the detector.
1. From the menu of the SOL-X press the STOP button.
2. The display will show "Stop? F1-NO F2-Yes." Press the STOP button again. If
you do not want toput the SOL-X into standby mode, press the START button
instead of the STOP button.
3. The detector display will show a 5 minute timer. When the timer is complete, the
display will show "STOP: HV-OFF ALL OFF PRESS F2." Now press the STOP
button and the SOL-X will be in standby mode.