Rigaku D/Max 2200PC Ultima III

Basic Operations Guide

Manual No. BOG-U3-v2

February 2006
 Table of Contents
Section 1: Cooling System Maintenance and Operation……………………..…...1-12
Addendum: Water Quality Documentation……………………………..…………13-15
Section 2: System Power-up…………………………………………..…………16-20
Section 3: Configuration of Hardware and Software with
Focusing Optics………………………………………………………21-30
Section 4: Automatic Alignment with Focusing Optics………………………....31-45

Optional Instrument Configurations

Section 5: System Configuration and Alignment with Parallel

Beam Optics…………………………………………...……………..46-60
Section 6: System Configuration and Alignment with Focusing Optics
and Diffracted Beam Monochromator……………………………......61-71
Section 7: System Configuration and Alignment with Parallel Beam Optics
and Diffracted Beam Monochromator……………………………......72-73

Service Evaluation Record…………………………..………………………….……………...74

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Section 1: Cooling System Maintenance and

Operations

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Before we power up the generator, always check the condition of the water in the chiller. The
reason for this is that we would like to catch any water quality issues before pumping
contaminants through the x-ray tube. For sake of illustration this section addresses the routine
chiller maintenance issues using a small water-to-water chiller. The same methodology can be
applied to air-to-water chillers and larger chillers, as the water quality issues are essentially the
same.

Step 1. Cooling System Inspection

a. Remove the reservoir cover and visually inspect (see Figure 1.1)
b. Water level – the water level should be above the float switch level.
c. Water quality: the water in the reservoir should be clean and clear, free of algae-like
substances, bacteria, corrosion debris.
d. In-tank filter: the nylon filter elements should be white and free of particulate and all
other forms of debris.
e. Reservoir sediment: blue CuS chips in the bottom of the reservoir can help suppress
algae growth however, a few chips is plenty. Otherwise the bottom of the reservoir
should be free of all particulate matter.

Figure 1.1. The reservoir cover has been removed in this picture to allow for inspection of the
reservoir, filter, and general water quality.

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In the case shown below (Figure 1.2), the filter is significantly discolored due to the
accumulation of algae-like debris and a fair amount of particulate debris has accumulated at the
bottom of the reservoir (Figure 1.3).

Contaminated
Filter
Figure 1.2. The in-tank filter has turned black as a consequence of accumulated algae-like
debris.

Particulate debris
accumulation at the
bottom of the reservoir

Figure 1.3. Organic debris has accumulated at the bottom of the chiller reservoir.

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For cases where the water in the reservoir is found to be clean and clear skip ahead to Step 3.

Step 2. Flush the Cooling System.

a. Drain the contaminated water into a suitable container (see Figure 1.4)
b. Disconnect and clean the in-tank filter – rinse under running water and/or gently
brush with a soft bristled brush to remove attached debris. You can safely soak the
filter in warm soapy water with a little household bleach to kill algae while cleaning
the reservoir out. The filter is made of nylon and won’t be harmed by soap or bleach.
c. Flush the system with TAP water. Depending upon how dirty the reservoir and
cooling system are you may have to flush the system several times to eliminate water
borne contaminants. {The reason for flushing the system with tap water is twofold.
First, tap water is typically less expensive than distilled water, which matters more
when the system has to be flushed several times. Second, tap water usually (not
always) contains some residual chlorine, which can help to kill most type of algae and
waterborne bacteria.}

Figure 1.4. Disconnect the reservoir hose and drain the reservoir contents into a suitable
container.

d. Wipe debris out of the reservoir after each flush using paper towels (see Figures 1.5
and 1.6 below). This will help to minimize the number of flush cycles required to
clean out the cooling system.

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Figure 1.5. This image shows the debris remaining on the bottom of the reservoir after the tank
has been drained. In some cases, algae may adhere to the walls and condenser plumbing so it is
a good idea to wipe down these parts too.

Figure 1.6. This image shows that a significant amount of residue can be removed quickly with
paper towels.

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e. After reattaching the drain hose, in-tank filter and refilling the reservoir start the
chiller again. In many cases, contaminated water that was trapped in the lines will
pollute the new water in the reservoir (see Figure 1.7). Let the system run for a few
minutes then repeat the flushing process described above. If the cooling system is
severely contaminated you may choose to add APPROVED chemicals to the cooling
system to help speed along the flushing process. DO NOT USE unapproved
chemicals in the cooling system as even a few minutes of exposure can be sufficient
to destroy components in the water path (e.g., pump seals, hose materials, flow
sensors). Approved water additives are described in the addendum to this section.

Figure 1.7. This image shows the water in the reservoir after the first flush cycle and a few
minutes of operation. Sometimes it takes several flush cycles before the chiller will run clean.

Step 3. Inspect and Clean the Internal Filter (X-ray Tube)

It is assumed that the instrument has power at this point and that the control PC has been booted-
up. If this is not the case, power up the instrument (NOT the generator though) and PC. To
power up the instrument make sure that the “Emergency Stop” is fully released, the main breaker
(lower right-rear corner) is closed (full up position) and that the power “ON” button (left side of
control panel on the instrument). The green “Ready” LED (below the “XRAYS” label) should
be on.
Drive the tube axis to 75 degrees using “Manual Measurement” (see Figure 1.8)
a. Double click on the Rigaku folder located on the PC desktop.
b. Double click on the Right Measurement folder
c. Double click on the Manual Measurement icon
d. Under the Control Axis pull down menu select the “Theta S” axis.

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e. Under the “Control” pull down menu select “Initialize” then click “Execute”.
f. Under the “Control” pull down menu select “Move”.
g. Type 75 in the position window then press the “Execute” button. Figure 1.9 shows the
final position of the tube arm prior to removal of the x-ray tube.
h. Remove the X-ray tube (See Figure 1.10).

Figure 1.8. This screen shot shows the mouse operations used to open the Manual Measurement
program and move the tube axis (named Theta S) to 75 degrees.

Figure 1.9. This photograph shows the tube axis inclined at approximately 75 degrees. This
will make it easier to uninstall the X-ray tube and will also help to prevent water from dripping
down into the tube tower.

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Figure 1.10. Left: the X-ray tube before being removed from the tube tower. Right: A standard
screwdriver is used to remove the two screws that attach the tube to the tower assembly.

Note: The X-ray tube should be handled carefully. Whenever possible it is best practice to hold
the tube by the stainless steel water jacket. For example, when the tube is being removed from
the tube tower it is natural to hold the tube by the stainless steel water jacket. However, in order
to inspect the internal filter inside the water jacket an alternate method of holding the tube is
required. Under no circumstance should human hands touch the Beryllium windows.
Furthermore, it is highly undesirable to touch the body of the x-ray tube with bare hands as the
oils and other debris transferred to the tube body can cause electrical arcing when the tube is
energized. Powder-free latex gloves can be used when handling the x-ray tube or alternately lint
free paper wipes can be used as shown in Figure 1.11 below.

Be X-ray windows
Figure 1.11. Left: shows lint-free paper being used to keep the tube clean during handling.
Right: the four Allen screws are removed to release the water jacket from the body of the x-ray
tube.

i. Release the four Allen screws attaching the water jacket to the body of the x-ray tube.

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j. Inspect the individual parts – look for dirt, debris, corrosion, excessive oxidation of
the cooled anode surface, flat spots on the O-rings, evidence of water leakage, etc.
(see Figure 1.12). Replace O-rings as needed (replacement O-rings are normally
included in the accessory kit delivered with the instrument).

Figure 1.12. Left: shows modest oxidation of the wet side of the anode. The direction of the
oxidation patch matches the line direction of the x-ray source. Right: water jacket assembly
with spray nozzle.

k. Remove the spray nozzle by gently pulling the brass nozzle straight up and remove
the brass mesh filter inside (see Figure 1.13).
l. Inspect and clean the filter as needed (see Figure 1.14). The water treatment
document appended to the end of this section offers some suggestions as to how to go
about cleaning the internal filter. Needless to say, handle and clean the filter with due
care as this part is not normally considered to be consumable (no extra filters are
included in the accessory kit delivered with the instrument).

Figure 1.13. This image shows the spray nozzle being removed from the water jacket assembly.

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Figure 1.14. Left: Substantial blockage of the internal filter. Right: The same filter is shown
after cleaning.

m. Reassemble the water jacket (see Figure 1.15).

a. Insert brass mesh filter
b. Install spray nozzle

Figure 1.15. Left: re-install brass filter inside nozzle mount. Right: align notch in the base of
the nozzle with locator pin at base of nozzle mount.

n. Attach the water jacket to the tube body (see Figure 1.16).
a. Reseat O-rings to ensure a good water seal
b. Rotationally align the screw holes in the water jacket with the corresponding
holes in the tube body.
c. Tighten the attachment screws just enough to slightly compress the O-rings
(Note: over tightening the screws can damage the O-rings).
o. Install the tube in the tube tower (see Figure 1.17)
a. Align the pin & corresponding pinhole on the tube assembly.
b. Tighten the attachment screws enough to achieve a good water seal.

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Figure 1.16. Left: the screw holes in the water jacket are not lined up with the holes in the tube
body. Right: the water jacket was rotated 90 degrees clockwise so that the screw holes in both
part lined up then the attachment screws were attached.

Figure 1.17. Left: the pin hole on the tube assembly is aligned with the pin on the tower. Right:
the attachment screws are tightened just enough to provide a good water seal.

p. Refill the chiller reservoir with distilled water and reinstall the in-tank filter (if not
currently installed) (Figure 1.18).
q. Consult the operators manual for proper temperature (~68 F) and pump pressure (40-
55 psi) settings.
r. Turn the chiller power switch on.
s. Check to make sure that there are no leaks around the x-ray tube.
t. Check to make sure that the chiller is performing within the specified operational
limits.
u. Re-install the reservoir cover and replace side panels and top cover of the chiller unit.

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Figure 1.18. This photograph shows the chiller reservoir after being flushed and cleaned several
times. The in-tank filter has also been cleaned and re-installed.

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ADDENDUM

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Section 2: System Power-up

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Prior to beginning this phase in the procedure it is assumed that the chiller and x-ray tube have
been inspected and cleaned (as needed). The instrument PC should be already on before
proceeding.

Step 4. Power Up the X-ray Generator.

a. Use the mouse to double-click on each of the numbered programs shown in
Figure 2.1 below.

Figure 2.1 The image above shows the mouse operations used to open the x-ray generator
control software (named “XG Operation”).

b. Click on the icon shown in

Figure 2.2 to change the
view displayed for the
generator control.

F
Figure 2.2. Click on the third icon as shown above.

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c. Verify that the Hand icon is highlighted in Yellow (see Figure 2.3). If it is not use
the mouse to click on it. This will turn on instrument power (power to move the
goniometer axes)

Figure 2.3. Click on the Hand icon if it is not already active (yellow highlights will appear on
the button when instrument power is “ON”.

d. Click on the radiation icon (see Figure 2.4) – this will power up the generator to
20kV and 2 mA.

Figure 2.4. Left: Click on radiation symbol. Right: Radiation icon changes color when the
generator is on and the power settings are displayed in the horizontal scroll bars.

e. Click on the “Option” menu then select “Property (see Figure 2.5).
f. Select the Tab labeled “Aging data”.
Note: At this point you will start to make decisions based upon the details of the instrument that
you are working on. For new tubes (or tubes that haven’t been used for a month or more) you
will select or setup an aging program that will gradually outgas the filament. Alternately, for X-
ray tubes that have been used recently, the goal of the aging process is to gradually ramp the
power up in order to achieve thermal equilibrium at measurement power (e.g. 40kV and 44mA).
When out gassing a new tube typically the kV settings will be incremented in sequential time
steps with the mA setting being left at a relatively low value initially. This procedure allows
adsorbed gasses time to release from the surface of the filament. The kV and mA values can be
increased in an alternating time steps (e.g. kV first, then mA) when thermally aging a tube for
every day use since both power settings contribute to the overall operating temperature of the
tube. Examples of each type of aging cycle are given in Figures 2.6 & 2.7.

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Figure 2.5. The image shows the numbered mouse operations shown above are used to gain
access to the Aging data tables.

Figure 2.6. The mouse is used to select ”The Present condition” from the pull down menu so
that the generator remains at the last power level programmed into the “Aging data” table.

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Figure 2.7. Left: The image shows the name of the aging table (New Target 2) along with
power and time step values for a typical out gassing aging cycle. Right: The image shows typical
power and time step values for a thermal aging cycle used to bring the tube into thermal
equilibrium at operating power for standard measurements.

Note: Tube suppliers will typically provide an out gassing power/time schedule in the
paperwork associated with the replacement tube. It is always preferable to use the manufacturers
aging schedule when one is available.
Note: After a new tube (or infrequently used tube) has been through an out gassing aging cycle
once it can be aged using a thermal aging cycle provided that the tube is used regularly.
Note: Any tube that has not been used for a period of several weeks (or longer) should be aged
using an out gassing power/time schedule to reduce the risk of damaging the tube (filament). In
general, the longer the period of inactivity the longer the dwell time for each power step.
New aging programs can be created by clicking on the “New” button and entering a name in the
text field of the dialog box that appears. Correspondingly, any user created aging schedule can
be removed from the pull down menu by first selecting the program then clicking on the
“Delete” button. The default aging schedules can be edited but can not be deleted. Aging data
table entries can be edited by using the mouse to select a cell, then type the new value and press
the “Enter” button on the keyboard to register the changed value. Once a suitable aging program
has been defined and selected click the “OK” button at the bottom of the dialog box.

Figure 2.8. Left: Click on the aging icon to initiate the aging cycle. Right: The aging icon
changes color while the program is running and the power levels changes automatically.

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Section 3: Configuration of Hardware and

Software with Focusing Optics

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At this point in the procedure the instrument and control PC should be on and the X-ray
generator should be at normal operating power (e.g., 40kV, 44 mA). It is advisable to power
down the generator however, if you need to remove any of the incident beam optical components
in order to prevent accidental exposure to x-rays. In this section hardware configuration will be
verified. Not all Ultima III’s will have exactly the same configuration as shown in the
photographs below. In some instances the detail of how components are attached will be a little
different depending upon the components installed on a particular instrument (e.g., either thumb
screws or Allen screws may be used to attach the detector box to the detector arm depending
upon whether the in-plane arm has been installed on the goniometer). However, in all cases the
same basic sequence of steps should be followed in terms of checking/setting up proper hardware
and software configurations.

Step 5. Verify Installation and Proper Mechanical Positioning of All Optical Components.
a. Open the lower left door on the instrument and turn “OFF” the RCD 3 controller power
(SERVO AMP unit on left side of left cabinet). This will ensure that none of the
motorize electrical connections are live while we check connections.
b. Check the power/communication cables for the CBO (2 connections), Div Slit (1
connection), detector optic box and Scintillation detector (1 connection – always live
700V, DO NOT disconnect unless the “Emergency Stop” button has been depressed.) as
shown in Figure 3.1. The incident beam optical components are shown in Figure 3.2.

Figure 3.1. This image shows an Ultima III with the following accessories attached: Cross
Beam Optic, computer controlled slit assemblies, standard sample stage, in-plane arm
goniometer and Scintillation detector.

Figure 3.2. Left: shutter assembly and tube arm with all other optical components removed.
Mechanical reference surfaces used to mechanically position the incident beam optics assembly
are highlighted in RED. Right: Labeled incident beam optical components are shown.

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c. Make sure that the incident beam optic is

properly inserted into the shutter
assembly*. The external shutter is
normally open when a primary optic is
properly installed. In Figure 3.3 the
external shutter was manually opened
half way to demonstrate the function of
the external shutter. DO NOT EVER
attempt to mechanically open the
secondary shutter while the generator is
turned ON as this would be a
RADIATION SAFETY HAZARD. If
the generator is currently at measurement Figure 3.3. The external shutter aperture
power (e.g., 40kV, 44mA), place your is being opened by pressing the spring-
hand on top of the tube. If the top of the loaded button down. The entry aperture
tube is noticeably warm/hot power down of the primary incident beam optic (Empty
the generator and clean the X-ray tube beam path or CBO) has to be inserted into
filter (see STEP 3 for further details). the shutter opening to hold this outer
shutter open. The optic reference surfaces
*The X-ray generator should always be powered should be in contact with both of the
OFF prior to removal of the primary incident reference surfaces highlighted in RED in
beam optic. Figure 3.2.

d. Verify that the incident beam PSA box is

fully attached to the primary optic (check
to make sure that the Allen screws are
snug).

Figure 3.4. The incident beam PSA box is

attached to the primary optic using two
Allen screws. The PSA optic does not have
to be uninstalled to check the tightness of
the screws but the Div Slit assembly will
have to be removed.

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e. Now the BB selection slit and 5 degree

PSA should be installed in the positions
shown in Figure 3.5.

Figure 3.5. Left: BB selection slit, PSA, 10 mm H.L. Slit. Right:

the Bragg-Brentano (BB) selection slit and incident beam PSA are
installed.

f. Install/check the Div Slit assembly. There

are two different designs the older design
is shown in Figure 3.6. Here you
set/check the mechanical positioning by
aligning two reference marks (circled in
Red) then tighten the thumb screw using
the J-bar tool shown. On the newer design
there are two flat reference surfaces
similar to those on the CBO assembly that
match two perpendicular reference
surfaces on the detector arm. To properly
align the newer Div Sit assembly just slide
the assembly along the horizontal Figure 3.6. This image shows the
reference surface until it engages the mechanical reference marks used to
vertical reference surface, then mechanically align the divergence slit
tighten the Allen screw. assembly.

g. Install/verify the 10mm H.L. slit in the

top part of the Div Slit assembly. A
properly assembled incident beam
optical assembly should look similar
to one of the captions in Figure 3.7

Figure 3.7. Left: CBO incident beam optical

assembly with position of the H.L. slit circled
in RED. Right: Empty Beam Path incident
beam optical assembly.

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h. Verify that the standard stage has been installed properly (see Figure 3.8)
a. The stage inserts into the goniometer and is attached using three thumb screws.
b. A flat support should be installed in the sample position and the rotational
orientation of the stage should be adjusted using a level. Tighten the thumb
screws to preserve the level orientation of the stage (see Figure 3.9).

Figure 3.8. Left: this photo shows the attachment mounting surface on the goniometer. Right:
Standard sample stage, (3) thumb screws and J-bar screw tool tightening tool.

Figure 3.9. After the stage is leveled, the thumbscrews are cinched up to provide enough
friction to preserve the rotational positioning of the stage.

i. Verify the mechanical positioning and electrical connections for the detector optics (see
Figures 3.10 & 3.11).
j. Adjust the position of components as needed (see Figure 3.12).

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Figure 3.10. Left: Important reference marks on the detector arm. Right: Detector optic box
and Scintillation detector.

Figure 3.11. The captions in this figure show the bottom of the detector optic box while
mounted on the detector arm. Left: Mechanically misaligned. Right: Mechanically aligned.

Figure 3.12. Left: Loosen/tighten screws to adjust mechanical location of detector box. Right:
Loosen/tighten Allen screws to adjust location of detector.

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k. Open detector box and verify that the 5 deg PSA has been installed with the parallel foils
vertically oriented (see Figure 3.13). Also make sure that the notch in the PSA properly
engages one of the two pin positions within the detector box.

Figure 3.13. Left: Flex the latch in the direction indicated to open the detector box. Right:
Insert the PSA in the forward or aft position making sure that the notch in the PSA housing
engages the alignment pin in the optic box base.

Step 6. Verify That The Software Settings Match The Hardware Configuration Settings.
a. Double click on the Rigaku icon. This will open a dialog box containing four programs
(see Figure 3.14).
b. Double click on “Control” which will open another dialog box containing another four
programs.
c. Double-click on “Rigaku Control Panel” which opens a third dialog with four programs.
d. Double-click on “RINT 2200 Right System” (see Figure 3.15).

Note: the fourth icon in the “Rigaku Control Panel” has a very similar name but the icon looks
like a wrench. This is a utility program used by installation engineers to install software modules
corresponding to physical pieces of hardware purchased with the system. This utility only needs
to be used when new hardware is added to the system or in instances where the software has
been reloaded from the installation CDs.

e. Check/set all of the system construction settings (settings on the first tab of the dialog
box) to the values shown in Figure 3.16. As you select each component you will notice
that the picture in the lower right corner changes accordingly. Pay particular attention to
the following items:
a. “Differential” and “Do Not Execute” MUST be selected in the “Detector
Property” dialog – these settings will impact the automated alignment
procedure to be performed shortly.

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Figure 3.14. The arrows and numbers indicate the sequence of mouse operations used to pen the
“Rigaku Control Panel” utility.

Figure 3.15. Double-click on the RINT 2200 Right System” icon.

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Figure 3.16. The gold arrow cursor symbols indicate mouse operations that you should perform
in order to verify that all software settings are correct.

b. If a CBO is mounted on the instrument, the “Incident monochro” pull

down menu must be set to “Use” and “CBO unit” Must be set in the
Property window. When the Empty beam path optic is installed the “Not
used” option should be selected.
c. In the ”Slit” pulldown menu select Auto Variable slit (Focus), then click
on the “Property” button to the right. Verify that the “DivSlit and “SctSlit
tables have all of the same angular settings. The RecSlit table should have
different values all of which are listed in units of (mm).
f. Click on the second tab (labeled “X-ray beam type”) and select the settings shown
in Figure 3.17.
g. Click on the third tab (labeled “Geometry system”) and select the settings shown
in Figure 3.18 then click the “OK” button at the bottom of the dialog box.
h. The RINT 2200 Right…. Dialog will close and another small dialog box will
open asking whether you want to write the configuration changes to the Registry.
Click on the “Yes” button.

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Figure 3.17. The gold arrows in this figure indicate mouse operations for specifying the proper
settings.

Figure 3.18. The gold arrows in this figure indicate mouse operations for specifying the proper
settings.

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Section 4: Automatic Alignment with

Focusing Optics

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The instrument should be on and the generator should have been at measurement power (e.g., 40
kV & 44 mA) for at least 30 minutes. In addition, the PC should be on and the x-ray optics
should be set for focusing measurements. Inspect cabling – make sure that arms can move freely
Step 7. Focusing Optics Alignment.
a. Open the “Automatic Alignment” program using the mouse operations shown in Figure
4.1.

Figure 4.1. The numbers and gold arrows indicate the mouse operations used to open the
“Automatic Alignment…” program.

b. The “Automatic Alignment” program uses Active X components which MS Windows XP

automatically blocks. Thus, for the “Automatic Alignment” program to work you have to
follow the numbered sequence of steps shown in Figure 4.2.
c. Verify that the software settings displayed in the log window (lower right corner of the
Automatic Alignment dialog) are set correctly (see Figure 4.3).
d. Select the 2Theta, Theta and Profile Measurement check boxes (1), set the power settings
to standard measurement values *# and click “Execute”(see Figure 4.4).

*# The default power settings used by Rigaku are (40kV, 44mA). However, the instrument can be
used at any power setting between (20kV, 2mA) and the upper limit power rating for the tube
((e.g., 2kW for normal focus Cu tubes). The power settings used during alignment should match
the power settings used for routine measurement. Aligning the instrument with generator settings
other than those used for standard measurements can lead to systematic sources of error in
diffraction data. There are two reasons for this. First the power settings directly influence the

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Figure 4.2. The numbered mouse operations indicate the steps required to enable the
“Automatic Alignment” program.

Figure 4.3. The “Automatic Alignment” program modifies the alignment process based upon
the software configuration of the instrument (circled in RED).

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Figure 4.4. The numbered steps and gold arrows indicate mouse operations used to initiate
the Automatic Alignment process.

steady-state operating temperature of the X-ray tube, which influences the positioning of the
anode via thermal expansion. Aside from this, the kV setting determines how deeply the
electron beam (emanating from the filament) will penetrate into the surface of the anode, which
directly influences the characteristic depth into the surface of the anode from which the nominal
X-ray beam emanates. Both of these factors contribute to the observed peak positions.
Consequently, both of these factors are normally accommodated during alignment operations.

e. A dialog box will appear prompting you to verify that the tube has been at power for 30
minutes, that the BB selection slit has been installed and that a suitable number of Cu
absorbers are inserted (see Figure 4.5). Click the “OK” button after completing the
requested operations.
f. The next dialog box that appears relates to the HV/PHA test which we have not selected
(yet, but we will later). Thus, we can ignore this dialog box temporarily and just click
“OK” (see Figure 4.5).
g. Read the instructions carefully in the next dialog box. Skipping a step here will likely
result in alignment failure (see Figure 4.5).
h. The software is requesting that you install the parts shown in Figure 4.6. Press the
“Door” button on the front panel of the instrument. The button should flash on/off then it
is OK to open the radiation enclosure doors. Once the Center Slit and Absorbers have
been properly installed and the radiation enclosure door has been closed (flashing light
will turn off), click the “OK” button.

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Figure 4.5. Each of the popup dialogs shown will appear sequentially.
Critical details are highlighted in RED.

Figure 4.6. Left: Center slit being installed in the sample position. Right: Cu absorbers
being installed in the detector optics box.

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i. The instrument will initialize all motorize axes then immediately proceed to performing
the first series of measurements (see Figure 4.7). When these tests are complete the
software will prompt you to remove the center slit (see Figure 4.8).

Figure 4.7. Prior to the onset of alignment measurements the instrument initializes each
motorized axis.

Figure 4.8. After performing the first measurement the software will stop and prompt the
user to remove the center slit prior to the onset of the second set of measurements.

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j. Verify that the sample position is empty as indicated in Figures 4.9. This instruction is
critical as it relates to the first measurement in the “Theta Alignment” series. Any object
installed in the sample position will distort the measured beam position.

Figure 4.9. At the end of the 2Theta measurement series the program will uncheck the
2Theta test (circled in RED), then prompt the user to install the Alignment jig.
k. Press the “Door” button, open the radiation enclosure and install the alignment jig as
indicated in Figures 4.10 and 4.11. Close the radiation enclosure door(s) then use the
mouse to click on the “OK” button.

Figure 4.10. The direct beam position is indicated by the blue + in the plot shown above.
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Figure 4.11. Left: the Alignment jig referred to in the software is normally stored in a box
labeled Setting Jig. Right: Install the alignment jig in the sample position as shown above.

l. Press the “Door” button on the radiation enclosure, open the door(s), open the detector
optics box and remove the Cu absorbers (see Figure 4.6). The next test (Profile
Measurement) is a diffraction experiment rather than a direct beam measurement. Thus,
if you forget to remove the absorber the displayed data will exhibit a flat intensity profile
(i.e. no observable diffraction peak) and the alignment test will fail.
m. Close the detector optics box; verify that the alignment jig is still in the sample position;
close the radiation enclosure door and click on the “OK” button (see Figure 4.12).

Figure 4.12. The “Theta Alignment” series is now complete and the instructions presented in
the dialog relate to the last measurement (Profile Measurement).

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n. Using the mouse, follow the numbered sequence shown in Figure 4.13 to save and
print the alignment results.

Figure 4.13. The optical alignment of the instrument is now complete.

Step 8. Calibrate the Detector Electronics.

a. Use the mouse to select the check box next to “HV/PHA Alignment”, verify
generator power settings, then click “Execute”.

Figure 4.14. The settings associated with detector calibration are circled in RED.

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b. Click the “OK” button in the first dialog that appears (see Figure 4.15). These
instructions pertain to the optical alignment test series just completed.

Figure 4.15. The instructions in this dialog relate to the optical alignment tests preformed
earlier.
c. Read and complete the instructions in this dialog prior to clicking the “OK”
button (see Figure 4.16).

Figure 4.16. The instructions in this dialog relate directly to detector calibration.

d. Use the mouse to perform the numbered steps shown in Figure 4.17. The printout
should appear similar to Figure 4.18.

Figure 4.17. The numbers indicate mouse operations that will save and print the alignment
results.
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Figure 4.18. The results of the HV/PHA tests are circled in RED.

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e. Next we will perform the “Counting Loss” correction experiment. The circuit
used to count photons (based upon the HV/PHA settings determined above) takes
a finite amount of time per photon to process the electrical signal produced as it
interacts with the detector. Correspondingly, at very high count rates (e.g. in
excess of 100,000 cps) some signals are lost while previously detected signals are
still being electronically processed. The “Counting Los” experiment determines
correction coefficients needed to compensate for these losses so that the detector
response becomes linear up to approximately 700, 000 cps. To initiate this
experiment perform the mouse operations indicated in Figure 4.19.

Figure 4.19. The mouse operations used to perform the “Counting Loss” correction
experiment are shown above.

Note: The “Counting Loss” button is only active when focusing optics and no diffracted beam
monochromator are specified in the “System Configuration” software.

f. The software will prompt you to install the “counting-loss correction jig” in the
sample position (see Figures 4.20 and 4.21). It is critical that all absorbers (other
than the Ni K beta filter) must be removed as these will distort the “Counting
Loss” experiment. During the course of this measurement sequence you will
notice that the software will measured several diffraction peaks and change the
generator power. This is done to generate a series of intensity values which will
subsequently be linearized (see Figure 4.22).
g. To save and print the result of this experimental series follow the steps illustrated
in Figure 4.22. The corresponding printout should appear similar to the graph
Figure 4.22.

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Figure 4.20. The numbered steps indicate the mouse operations to be performed.

Figure 4.21. Left: Polycrystalline quartz sample used for the counting loss correction
measurement. Right: Counting loss jig installed in sample position.

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Figure 4.22. The numbered steps indicate the mouse operations required to save and print the
counting loss results.
h. Now we need to tell the software to use the counting loss correction values that
were just determined. To do this close the Automatic Alignment program then
follow the numbered steps shown in Figure 4.23.

i. Since changes were made in the system configuration, the program will prompt
you to decide whether or not to save the changes – click “YES” as indicated in
Figure 4.24.

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Figure 4.23. The numbered steps indicate mouse operations used to activate the counting
loss correction for all subsequent measurements.

Figure 4.24. Save the updated system configuration information by selecting the “Yes”
button.

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Section 5: System Configuration and

Alignment with Parallel Beam Optics

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The instrument should be powered up and the generator should have been at measurement power
for at least 30 minutes. The detector electronics should have been calibrated (HV/PHA and
Counting Loss experiments – see Section 4, step 8 for further details). This section will address
the procedural sequence used to reconfigure the Ultima III hardware and software with parallel
beam optics.
Step 9. Install Parallel Beam Optical Hardware.
o. Remove the BB selection slit and install the PB selection slit. The beveled edge
of the selection slit should be
located at the bottom edge and the
slit should be inserted behind a
spring clip (See Figures 3.5 and
5.1).
p. Verify that the sample stage is level
(see Figure 3.9).
q. Open the detector optics box and
install the PB optic (see Figure 5.2).

Figure 5.1. The PB selection slit is

shown above.

Figure 5.2. Diffracted beam parallel beam optics configurations are shown. Left: High flux
configuration - 5 deg PSA (axial divergence) and 0.5 deg (radial divergence). Right: High
Resolution Configuration – Thin film PSA with a 0.11 deg. acceptance angle (radial
divergence).

Step 10. Change Software Configuration.

a. Use the mouse to perform the numbered steps shown in Figure 5.3.
b. Change the slit setting to “Auto Variable slit (Parallel)” (see Figure 5.4).
c. Select the “Geometry System” tab then select the Parallel Beam Method radio
button.
d. Click the “OK” button, then click the “Yes” button (see Figure 5.5).

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Figure 5.3. This figure shows the steps used to open the software utility where the system
configuration is specified.

Figure 5.4. This figure shows the steps used to specify parallel beam settings.

Figure 5.5. To implement changes made to the system configuration select the “Yes” button.

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Step 11. Prealign the X-ray Mirror.

a. Press the “Door” button on the front of the radiation enclosure. Wait for the light
on this button to flash then open the radiation enclosure doors (see Figure 5.6).
b. Install the fluorescent screen in the sample position as shown in Figure 5.7.

Figure 5.6. This photo shows

the “Door” button flashing Figure 5.7. The fluorescent screen
after being pressed. is installed in the sample position.
c. Turn off the fluorescent light inside the enclosure, close the doors (the button
should stop flashing) and turn off or reduce the room lighting.
d. Perform the mouse operations in Figure 5.8 in order to position the source in front
of the fluorescent screen.

Figure 5.8. This image shows the mouse operations required to properly position the x-ray
source in front of the fluorescent screen.

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e. Verify that the communication cable between the

DC motor Controller (see Figure 5.9) and the CBO
assembly is properly connected at both ends.
f. Open the shutter by pressing the “Close” (the green
LED will go out on the EXT button) and then
“Open” button. You should hear an audible click
from the shutter solenoid and the Shutter open lights
(Gold LED on the Open button, Red tube tower light
and gold Shutter R light on the safety light stack)
activate (see Figure 5.10).
g. Turn “ON” the power switch to the DC Motor
Controller then while looking through the window
of the radiation enclosure at the fluorescent screen
adjust the joystick until a bright green line appears
at the center of the screen. Figure 5.9. The DC Motor
h. Turn the power switch “OFF” and verify that the Controller shown above is
green line still appears in the center of the used to align the tilt
fluorescent screen. orientation of the x-ray
mirror optic.
i. Press the shutter “Close” button,
then press the “Ext.” button (the
green LED should light).
j. Press the “Door” button (light
should flash) and open the
radiation enclosure doors.
k. Remove the fluorescent screen and
close the enclosure doors.
Figure 5.10. Manual shutter controls are
circled in RED in this photo.

Step 12. Parallel Beam Alignment.

a. Open the “Automatic Alignment” program as indicated in Figure 5.11.
b. Verify that the software settings indicated in the lower left corner of the alignment
window are correct (see Figure 5.12).
c. Use the mouse to specify the settings shown in Figure 5.13.
d. A sequential series of dialog windows will appear with instructions that you
should perform PRIOR to clicking the “OK” button. Figure 5.14 shows the first
three and critical instructions have been underlined and annotated in RED. The
alignment parts referred to in the third dialog are shown in Figure 5.15. After
clicking on the “OK” button the instrument will perform a scan to find the angular
position of the detector relative to the X-ray source. Once this has been
determined you will optimize the mirror tilt orientation to maximize the flux
scattered toward the detector.

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Figure 5.11. Launch the Automatic Alignment” program by double clicking on the icon
shown above.

Figure 5.12. Verify that the software settings indicate parallel beam (see Figure 5.4).

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Figure 5.13. The numbered steps indicate mouse operations used to specify and initiate
alignment tests.

Figure 5.14. This figure shows three numbered dialog windows with critical instructions
underlined in RED.

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Figure 5.15. This image shows the alignment filters to be installed in the filter holder
positions of the detector box for all direct beam alignment measurements.
e. Read the instructions in the next dialog – they indicate how to terminate the
mirror alignment test. You will be manipulating the joystick to optimize the tilt
angle of the mirror while watching the intensity as a function of time. Once the
position of maximum intensity has been achieved you will need to terminate this
measurement.
f. Turn on the power to the DC Motor control unit.
g. Click the “OK” button shown in Figure 5.16.

Figure 5.16. The instructions shown in this window tell you how to terminate the test that
will begin when you click the “OK” button.

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h. Make small adjustments to the joystick control to change the tilt of the mirror.
Note: The intensity display takes a second or two to respond to joystick perturbations. If you
manage to lose the beam click on the “Pause” button, then repeat STEP 11. After reacquiring the
beam, you can reactivate the mirror alignment. Once the mirror position has been optimized the
scan can be terminated as illustrated in Figure 5.17.

Figure 5.17. The numbered steps shown above demonstrate the sequence of mouse
operations used to terminate the mirror alignment scan.
i. The program will prompt you to remove the Ni K beta filter (see Figure 5.18) in
preparation for the next scan. The objective of this scan is to verify that the
measured intensity approximately doubles as a result of removing the Ni filter.
Click “OK” after the filter has been removed and the enclosure doors are closed.

Figure 5.18. Left: The critical instructions are underlined in Red. Right: the Ni K beta filter
is removed from the detector box.

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j. Once you verify that the observed intensity is approximately double, turn off
power to the DC Motor Controller then terminate the scan using the steps
indicated in Figure 5.19.

Figure 5.19. The mouse operations specified in this image indicate the procedure used to
terminate the mirror alignment scan.
k. Now the software will prompt you to either repeat the mirror alignment (i.e., if the
observed intensity was not approximately double) by clicking on “Yes” or
continue to the next alignment test by clicking on “No”. When the test is
successful click “No” as shown in Figure 5.20.

Figure 5.20. Clicking on “No” will allow you to proceed to the next alignment test.

l. Follow the instructions in the dialog (see Figure 5.21) then click on “OK”.
Several preprogrammed measurements will take place.
m. Follow the instructions in presented in Figure 5.22, then click “OK”.
n. Verify that the sample position is open and click the “OK” button (see Figure
5.23).

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Figure 5.21. Left: dialog with instructions to be completed prior to clicking on the “OK”
button. Right: Photograph showing the center slit being installed in the sample position.

Figure 5.22. Prior to clicking the “OK” button, the center slit should be removed and the
Parallel beam optic (previously removed in Step 12d, see Figure 5.14) should be re-installed
in the detector optics box (see inset photo).

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Figure 5.23. The “2Theta Alignment” test series has been completed. Subsequently, the
alignment program prompts you to verify that the sample position is open.
o. The first scan in the “Theta Alignment” series is a scan of the detector position
relative to the source. Once this measurement is complete, the software will
prompt you to install the alignment jig in the sample position as shown in Figure
5.24.

Figure 5.24. The program prompt you to install the alignment jig (see inset photo) in the
sample position.

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p. The objective of the Theta Alignment” is to make the 0.00 degree orientation of
the measurement system parallel to the sample orientation. When this is
successfully completed the intensity profile will by triangular in shape (see Figure
5.25) and you will be prompted to remove all of the beam attenuating devices
previously installed. After completing these instructions click the “OK” button.
q. The program will perform a diffraction scan of the 220 reflection of Si and
compare the observed peak position and intensity values to internally defined
acceptable limits.
r. To save and print the alignment results follow the numbered steps shown in
Figure 5.26.
s. An example of the parallel beam alignment printout is given in Figure 5.27.

Figure 5.25. The Theta Alignment” measurement series is now complete and the instructions
presented relate to the last test series (Profile Measurement).

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Figure 5.26. The numbered steps in this image indicated the mouse operations used to save
and print the alignment results.

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Figure 5.27. Typical parallel beam alignment results should appear similar to the captions in
this figure.

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Section 6: System Configuration and

Alignment with Focusing Optics and a
Diffracted Beam Monochromator

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The instrument should be powered up and the generator should have been at measurement power
for at least 30 minutes. The optical configuration described in Section 3 is the assumed initial
hardware configuration. The detector electronics should have been calibrated (HV/PHA and
Counting Loss experiments – see Section 4, step 8 for further details). This section will address
the procedural sequence used to reconfigure the Ultima III with a diffracted beam
monochromator set for use with focusing optics.
Step 13. Monochromator Installation.
a. Dismount the detector form the detector arm (see Figure 3.12).
b. Disconnect the strain relief support on the High Voltage (detector power) cable.
Note: ELECTROCUTION HAZARD! NEVER disconnect the HV cable while the instrument
is powered up as there will be a live electrical potential of approximately 700V.
c. Remove the two screws
attaching the detector to the
standard bracket using a “+”
head screwdriver (see Figure
6.1).
d. Attach the monochromator
bracket to the detector.
Make sure that the screws
are tight enough that the
detector does not easily
rotate relative to the
orientation of the bracket Figure 6.1. This image shows the location of
(see Figure 6.2). the detector bracket attachment screws.
e. Assemble the
monochromator (if
needed) the
relevant parts are
shown in Figure
6.3.
a. Carefully remove
the monochromator
crystal from its
shipping box and
slide it onto the
center-post support
as shown in Figure Figure 6.2. This image shows the detector along with
6.4. Make sure that the standard bracket and the monochromator bracket.
nothing touches the
graphite crystal surface as it is quite soft and can easily be scratched or otherwise
damaged.
b. Insert a monochromator receiving slit (e.g., 0.8mm) as indicated in Figure 6.5,
then replace the removable cover and tighten the thumbscrew.
c. Before installing the monochromator, flip it over and look for the WHITE
reference line scribed on the bottom surface of the bracket (see Figure 6.6).

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Figure 6.3. This image shows the constituent parts that comprise the monochromator
assembly.

Figure 6.4. Left: this caption shows the exposed face of the monochromator crystal. Right:
the monochromator and support slide onto a brass center post and magnetically attaches itself
to the top support.

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Figure 6.5. The monochromator receiving slit has been installed behind a 2-pronged spring
clip.

Figure 6.6. This image shows the reference mark on the monochromator bracket that will be
used to properly position the monochromator on the detector arm.

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d. Attach the monochromator assembly to the detector arm as shown in Figure 6.7.
You only need to tighten two or three screws enough to support the weight of the
assembly. We will need to be able to laterally slide the monochromator along the
detector arm in the next step so do not fully tighten the screws yet.
Note: The Bragg angle adjustment screw is close to the position of the front attachment screw.
Adjustment of this PAINTED screw will misalign the monochromator crystal.

Figure 6.7. This image shows the monochromator assembly being installed. Two of the five
attachment screws were partially tightened to support the weight of the part while final
mechanical positioning adjustments are being made.
e. Adjust the position of the monochromator along the detector arm radius while
looking at the reference marks shown in Figure 6.8.
f. Tighten the five attachment screws (see Figure 6.9). Check to make sure that the
reference marks are still aligned and that the monochromator assembly does not
move when light hand pressure is applied.

Step 14. Software Configuration and Automatic Alignment.

a. Perform the mouse operations indicated in Figures 6.10 and 6.11.
b. Open the “Automatic Alignment” program as indicated in Figure 6.12.
c. Perform the sequentially numbered mouse operations suggested in Figure 6.13.
d. Press the “Door” button on the instrument, after the button light begins blinking
open the enclosure doors and perform the tasks indicated in Figure 6.14. Once
finished, close the enclosure doors.
e. Perform the instructions given in Figure 6.15.
f. Perform the instructions given in Figure 6.16.
g. Perform the instructions given in Figure 6.17.
h. An example alignment printout is given in Figure 6.18.

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Figure 6.8. This image shows the two reference marks that have to be mechanically aligned
in order to properly position the monochromator.

Figure 6.9. This image shows the attachment screws being tightened after the reference
marks have been aligned.

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Figure 6.10. The numbers indicated the sequence of mouse operations used to open the
system configuration software.

Figure 6.11. The numbers indicated the sequence of mouse operations used to specify the
current configuration of the hardware.

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Figure 6.12. Start the “Automatic Alignment” program by clicking on the icon circled in
RED.

Figure 6.13. The numbered steps indicate mouse operations used to initiate the Automatic
Alignment process.

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Figure 6.14. The instructions shown in this figure are related to the labeled components in
the inset photograph.

Figure 6.15. The numbered instructions correspond to the last measurement in the “2Theta
Alignment” test series and the first measurement in the “Theta Alignment” test series
respectively.

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Figure 6.16. The instructions shown above relate to the labeled component in the inset
photograph.

Figure 6.17. The numbered steps indicate mouse operations used to save and print the
alignment results.

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Figure 6.18. This image shows a typical alignment result for a system configured with
focusing optics and a diffracted beam monochromator.

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Section 7: System Configuration and

Alignment with Parallel Beam Optics and a
Diffracted Beam Monochromator

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The instrument should be powered up and the generator should have been at measurement power
for at least 30 minutes. The optical configuration described in Section 5 along with the
diffracted beam monochromator installed in Section 6 is the assumed initial hardware
configuration. The detector electronics should have been calibrated (HV/PHA and Counting
Loss experiments – see Section 4, step 8 for further details). This section will address the
procedural sequence used to align the Ultima III with a diffracted beam monochromator set for
use with parallel beam optics.
Step 15. Parallel Beam Monochromator Settings.
f. Press the “Door” button on the front panel of the instrument. After the button
light starts blinking, open the enclosure doors.
g. Remove the monochromator receiving slit (see Figure 7.1).
h. Loosen the thumbscrew on the removable monochromator cover and then remove
the cover.
i. Rotate the monochromator crystal as indicated in Figure 7.2.

Figure 7.1. This image shows the parts referred to in step 15 b and 15 c.

Figure 7.2. The monochromator crystal can be rotated 90 degrees to the “FLAT” orientation
enhancing the detection efficiency during parallel beam measurements.

j. Replace the monochromator cover and tighten the thumbscrew.

k. Close the radiation enclosure doors.
l. Change and save the system configuration settings as described in Sections 5 and
6. In particular, see Figures 5.3 and 5.4 but also remember that the
monochromator should be set as indicated in Figure 6.11 (see numbers 2 through
6 in this figure).
m. Perform the “Automatic Alignment” procedure described in Step 12 of Section 5.

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Service Evaluation Record

1. Cooling system inspected and operating correctly? Yes/No

2. Instrument and control PC power-up correctly? Yes/No

3. X-ray generator and tube powered up to measurement power? Yes/No

4. Good goniometer communication verified? Yes/No

5. Focusing optics (BB) properly installed and aligned? Yes/No

6. HV/PHA and counting loss calibrations completed? Yes/No

7. Parallel beam optics (PB) properly installed and aligned Yes/No

Optional Diffracted Beam Monochromator

8. Monochromator installed and aligned for:

a. focusing (BB) optics? Yes/No

b. parallel beam (PB) optics? Yes/No

Comments: ________________________________________________________
__________________________________________________________________
__________________________________________________________________
__________________________________________________________________

Rigaku Service Rep ________________________ Date ____________________

Customer _________________________________ Date ____________________

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