I. Operation of Single and 6-Stage Automatic Sample Changer Holders
Laboratory / Work Group
Location
Number of Pages
Author's Name
Lab Manager’s Name
Trainer’s Name
Creation Date
Revision Date
Table of Contents
Shared Equipment Authority, Rice University
Space Science Building, Room B06
37
W.V. Knowles
Richard Crouse
Richard Crouse
4/15/2006
4/30//2014
1. INTRODUCTION ................................................................................................................................... 2
2. SAFETY EQUIPMENT REQUIREMENTS ........................................................................................ 2
3. OUTSTANDING HAZARDS ................................................................................................................. 3
4. REQUIRED EQUIPMENT .................................................................................................................... 4
5. RAW MATERIAL QUALITY ............................................................................................................... 4
6. VERIFICATION / CALIBRATION...................................................................................................... 4
7. START-UP PROCEDURES .......................................... ОШИБКА! ЗАКЛАДКА НЕ ОПРЕДЕЛЕНА.
7.1
S TART -U P P ROCEDURE .......................................................................................................................... 4
7.3
G ENERATION OF XRAYS ...................................................................................................................... 5
8. CONTINUING OPERATION PROCEDURE ..................................................................................... 7
8.1
S IGN THE L OGBOOK .............................................................................................................................. 7
8.2
O PENING /C LOSING THE XRD D OORS W HILE THE XRAY G ENERATOR IS O N ....................................... 8
8.3
S AMPLE P REPARATION ......................................................................................................................... 9
8.3.1 Sample Packing Procedures ......................................................................................................... 9
8.3.2 Common Errors in Sample Preparation ......................................................................................13
8.4
L OADING S AMPLE ( S ) INTO THE
XRD… ...............................................................................................14
8.4.1 …for the Single Sample Holder ...................................................................................................14
8.4.2 …for the 6-Stage Auto Sample Changer ......................................................................................16
8.5
THE G ONIOMETER C ONFIGURATION FOR XRAY B EAM C OLLIMATION ................................................18
8.5.1 Hardware Identification ..............................................................................................................18
8.5.2 "What Slit Size Should I Use?" ....................................................................................................19
8.6
A NALYSIS C ONDITIONS .......................................................................................................................25
8.6.1 General Guidelines ......................................................................................................................25
8.6.2 Software: Main Screen of Standard Measurement .....................................................................27
8.6.3 Software: Scan Condition Window of Standard Measurement ...................................................28
8.7
S TARTING THE A NALYSIS ....................................................................................................................31
9. SHUTDOWN PROCEDURES ..............................................................................................................32
9.1
T ERMINATING A R UN E ARLY ...............................................................................................................32
9.2
R ETURNING XRD TO I DLE A FTER S AMPLE A NALYSIS .........................................................................33
9.3
S HUTDOWN AND P OWER O FF ...............................................................................................................33
10. EMERGENCY SHUT-DOWN PROCEDURE ..................................................................................34
11. MAINTENANCE .................................................................................................................................34
12. TROUBLESHOOTING .......................................................................................................................34
13. DISPOSAL OF WASTE ......................................................................................................................35
14. INSTRUMENT DETAILS...................................................................................................................35
14.1
T ECHNICAL S PECIFICATIONS .............................................................................................................35
15. CONTACT LIST ..................................................................................................................................36
16. REVISION LOG .......................................................... ОШИБКА! ЗАКЛАДКА НЕ ОПРЕДЕЛЕНА.

Powder XRD Operating Procedure
1. Introduction
This procedure is intended for general user training only. It does not cover maintenance or complex procedures for advanced users.
The unit is a Rigaku Ultima II vertical

-

powder diffractometer using Cu K  radiation (

= 1.5418 Å) with Bragg-Brentano para-focusing optics (series of fixed and movable slits). A water chiller system is used to cool the x-ray tube (Haskris, model
RW100). The principal application of this system is phase analysis of polycrystalline samples. See Section 14.2: Technical Specifications for equipment details such as available 2

scanning range, filters, slits, etc . (Definition: θ-θ geometry means that both the x-ray tube and detector move simultaneously while the specimen is fixed; in contrast,
θ-2θ geometry means the x-ray tube is fixed and the specimen moves at ½ the rate of the detector to maintain the θ-2θ geometry.)
Three different sample attachments can be used on this instrument: 1) single sample holder, 2) 6-stage automatic sample changer, and 3) in situ high temperature chamber. This procedure explains use of both the single sample holder and 6-stage automatic sample changer. Separate procedures explain how to (i) switch between sample holders and (ii) install and operate the in situ high temperature chamber.
Using the single sample holder configuration provides the most straightforward operation and highest flexibility in sample preparation. This is because numerous options exist for sample mounting and sample volumes are relatively small. The 6-stage automatic sample holder is convenient for unattended analysis of multiple samples but it requires high sample volumes. During use of both attachments, the sample is open to the atmosphere ( i.e.
, room temperature, air, relative humidity, etc .) without the ability to control the environment.
2. Safety Equipment Requirements
Safety Equipment Must be used during...
X-ray exposure badge
Radiation meter
Latex gloves
Safety glasses
Area monitoring of each XRD
Whenever desired to test background levels
Sample handling. You are responsible for understanding the health risks associated with your own samples!
Risk of flying debris during sample preparation

Powder XRD Operating Procedure
3. Outstanding Hazards
Outstanding
Hazard
X-Rays
High Voltage
Fire
Precaution
Background:
The United States governmental office responsible for regulating x-ray exposure is the Food and Drug Administration’s Bureau of Radiological Health. The 1968
‘Radiation Control for Health and Safety Act of 1968’ (Public Law 90-602) established maximum limits for whole body exposure of x-rays:

0.1 REM (Roentgen Equivalent Man) per day

3 REM per 13 weeks

5 REM per year
Skin erythema (reddening of the skin) occurs with a local dose of approximately
300 REM; skin destruction (burns) result from doses ≥ 500 REM. X-ray diffraction and spectrographic tubes generate dose rates between 100,000 and
1,000,000 REM/hr, thus only a short exposure to the primary beam of analytical instruments is required to cause severe skin burns. However, operators should realize that the intensity from a scattered beam is MUCH LESS than the direct beam.
Precautions:
1.
The manager of Rice's X-ray Diffraction Facility has insured this unit meets or exceeds the local radiation safety standards through a system of regular inspections.
2.
This analytical x-ray equipment is manufactured with numerous safety devices and interlocks to protect the user.
3.
Each user must: a.
Receive an acceptable amount of training in radiation safety as approved by the radiation protection supervisor, b.
Demonstrate competence to use this machine, c.
Receive approval of the radiation protection supervisor and sign endorsement form before operating this machine independently.
Background
The unit is connected to 208VAC. A high voltage transformer converts this to
60,000VAC for operation of the x-ray generator. Exposure to this electric potential can cause severe burns and/or death.
Precautions
1.
Follow the instructions in this manual for operating the electrical system of this instrument.
2.
If a serious electrical problem (smoke or sparks) arises, do not try to fix the problem. Depress the Emergency RED Button and contact the XRD Facilities manager for assistance.
1.
Remove all personnel from danger area.
2.
Pull nearest fire alarm to activate fire alarm system.
3.
Call Campus Police (x6000). You are in Space Science B06.
4.
Know where the extinguishers are located and how to use them. Attempt to contain fires if possible without personal risk.
5.
Refer to the Rice University Fire Procedure for more information.

Powder XRD Operating Procedure
4. Required Equipment
This list excludes standard hardware attachments but includes consumable items for a
“basic user” as used on a daily basis.
Equipment Purpose Location
Mortar and pestle
Glass microscope slides
Sample preparation
Use flat surface of slides to press powders into sample holders
Sample Mounting Table
Sample Mounting Table
Double-sided tape
Wax paper
Mounting surface for small amounts of powder sample
Clean surface for sample preparation
Cleaning of used slides
Sample Mounting Table
Sample Mounting Table
Scotch pads Sink area
Compressed air cans Cleaning of spilled powder samples from the 6-stage autosampler turret
Sample Mounting Table
5. Raw Material Quality
Raw Material Quality does not apply to this procedure.
6. Verification / Calibration
These standards are available for use. All standards other than the Si crystal must be obtained from the XRD Facilities Manager.
Material
Silicon crystal "setting jig"
LaB
6
(NIST 660a)
Details

Used on a weekly and monthly basis to calibrated the XRD

Rigaku/MSC does not call this a "standard" because it is not rigorously quality-controlled (in contrast to NIST standards)

Do not touch this crystal with bare hands! Use gloves. Skin oils can compromise the integrity of the crystal.

Used for quantifying instrumental contributions to peak broadening ( i.e.
, instrument error).
.
7.1 Start-Up Procedure
This procedure only needs to be performed when the XRD is turned off before use.
If the instrument is already on and ready for use, skip to Section 8: Continuing
Operation. For the current section, the order of operations is very important. Failure to follow this procedure stepwise may result in needing to shut down the equipment and
“reboot”.

Powder XRD Operating Procedure
Figure 7.1a: Haskris chiller Figure 7.1b: Front control panels of XRD
Step
1
2
3
Action
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Turn on the computer and monitor. Windows XP Log In information:
1.
User name = Rice Univ. user Name on AD Rice server
2.
Password = Rice Univ Password
3.
Click OK.
Turn ON the Haskris chiller by pushing the black rocker power switch into the UP position (located on front of chiller, upper right corner) (Figure 7.1a). Check the following status indicators on the chiller to verify proper operation:
1.
Tank water level indicator light should illuminate ORANGE (full).
2.
Power indicator light should illuminate RED.
3.
Water flow on flowmeter should be ~1.5 gpm; GREEN Arrow.
Located in the back of the Haskris chiller is the deionizer indicator with red and green LEDs (Figure
7.1a). Observe which color LED is illuminated:
1.
If GREEN, system is OK. No further action required.
2.
If RED, make a note in maintenance logbook (date, user, problem description) and notify the XRD
Facilities Manager. Operation can continue however.
4 Verify the front sliding doors to the XRD are closed.
5
6
7
Make sure the 3-position shutter toggle switches on the front Shutter panel are in their proper orientations:
1.
Left = CLOSE
2.
Right = EXT. (computer control)
Turn ON (flip into the UP position) the 3 circuit breakers, located behind the two lower front panel doors
(Figure 7.1b):
1.
Right side: ELB1 and ELB2
2.
Left side: POWER
Push the square white ON button on the x-ray panel on the front of the XRD (Figure 7.1b). The following should occur:
1.
White LED on front panel labeled POWER will illuminate.
2.
Green READY lamp on "Christmas Tree" array (on top of XRD) will illuminate.
7.2
Generation of X-rays

Powder XRD Operating Procedure
The x-ray tube lifetime is highly dependent upon operating conditions. At typical sample analysis power outputs, 40 kV x 40 mA, the tube lifetime is ~2000 hours; reducing the tube power to Stand-By level, 20kV x 2mA, increases the lifetime by over
100%. Please use 40 kV x 40 mA power setting for sample analysis and return to
Stand-by level when your operating session is finished.
Step
1
Action
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Start the x-ray generation control software from the Windows Desktop of the computer by double-clicking the "XG Operation" icon. The dialog box in the left figure below should open and is known as the "control view":
If instead the dialog box in the right figure opens (known as the "monitor view"), revert back to the control view by doing one of the following:
1.
Single-clicking the 3 rd button from the left, or
2.
From the drop down menu, select OPTION → CONTROL.
2 Make sure the sliding front doors to the XRD are both closed.
3
Turn on the x-ray source from the "XG Operation" control view by single-clicking the button with the radiation symbol. The following should occur:
1.
A loud, low-pitched "thunk" sound is heard.
2.
Red X-RAY lamp on "Christmas Tree" array (on top of XRD) will illuminate.
3.
Radiation button on the control view should turn from black to red/yellow.
Troubleshooting
If the x-ray generator does not turn on, look at the color of the "server icon" in the
Windows system tray (bottom right corner of computer screen):
1.
Blue = OK.
2.
Red or green = NOT READY. a.
To reset the server, right-click on "server icon" and select INITIALIZE. b.
Wait ~30 seconds while server icon flashes between red and green. When server is reinitialized, "server icon" will turn blue. c.
Attempt to turn on the x-ray source again via the XG Operation control view window. If still unsuccessful, request help.

Powder XRD Operating Procedure
Step
Action
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4
"Slow age" the x-ray tube by slowly ramping power to the x-ray tube for 30 minutes.
1.
Single-click the button on the XG Operation control view showing the picture of a frying pan. The following will occur: a.
Power will start ramping (voltage 20→40 kV; current 2→40 mA) b.
Button with frying pan will turn from gray (OFF) to yellow (ON).
2.
Do not do use this feature unless the X-ray Tube has been OFF for an extended period and it is now cold.
3.
When the 30 minute aging period is finished, the image on button will revert to its
OFF picture.
8. Standard Measurement Operation Procedure
8.1 Sign the Logbook
Signing the logbook serves several purposes. First, it assists in accurate bookkeeping for
Rice SEA (charge rates). Second, it helps the XRD Facilities Manager to monitor instrument usage in order to better understand user trends. Third, it greatly assists in troubleshooting of equipment problems when they occur. Please make a note of any problems in the far right column (Notes/Comments); if no problems please indicate
“OK” in this column.
Step
Action
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1
All users must be registered with the SEA.
1.
New user information sheet
2.
SEA users agreement
2 Sign in to the user logbook (date, name, time start/stop, etc.)

Powder XRD Operating Procedure
8.2 Opening/Closing the XRD Doors While the X-ray Generator is On
The critical components of this entire assembly are the mechanical position sensors installed on each horizontally sliding Access Door on the front of the XRD. These sensors work like switches—when the DOOR OPEN button is depressed, the X-rays will remain ON while working in the sample area; if the DOOR OPEN button
depressed before opening the doors, these sensors immediately switch off the power to the x-ray tube; x-rays OFF.
Step
Action
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1
2
3
CAUTION!
Failure to follow this procedure correctly will result in immediate power loss to the x-ray tube. Permanent and potentially catastrophic damage can occur to the x-ray tube. The replacement cost of an x-ray tube is ~$3,500.00.
Be sure you are logged in to the computer and the “server” icon has BLUE color background.
Press the yellow DOOR OPEN button on the front panel of the
XRD EVERY TIME the doors are to be opened while the x-rays are on.
The buzzer will sound a long, constant alarm for ~3 seconds. Do NOT open the doors while alarm in constant state; x-rays will turn OFF!
4 When the buzzer starts beeping, wait for 3-4 beeps before opening the doors.
5
6
7
8
Grab the black handle on the right door and give it a gentle but firm tug to the right. When it opens, slide it gently to the right. Firm pressure on the left door, pushing to the left, will cause it to slide open if required for additional access.
CAUTION: Bumping or pulling extremely hard on the handle can cause the doors to jump up and down in their tracks which can cause the x-rays to turn
OFF. Please open the door carefully and gently.
The alarm will beep the whole time the doors are open. This alerts users in the lab that the x-ray door is OPEN.
If an analysis scan was underway before the doors were opened, this opening of the doors will temporarily suspend the run and close the x-ray shutter. After the doors are closed, the shutter will open and the run will resume. No data loss should occur.
When finished working inside the sample area, gently slide each door closed.
The Door Alarm will silence once both doors are closed.
CAUTION: Be careful not to push them so hard as to collide and jump out of their tracks. Again, there is a potential that the door sensors will "think" the doors are being opened improperly and will immediate turn OFF the X-rays.

Powder XRD Operating Procedure
8.3 Sample Preparation
8.3.1 Sample Packing Procedures
Step
Action
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1
Standard sample holder; ALWAYS CLEAN BEFORE AND AFTER USE.
1.
Why use this holder? a.
Advantages i.
Sample preparation is simple. ii.
Low sensitivity to impurities remaining on slide from previous run because of large sample volume for current sample. b.
Disadvantages i.
X-ray transparent samples (low absorption coefficient) may be affected by background interference from holder. ii.
Possibility of sample contamination from run-to-run if slides are not cleaned properly. iii.
Holders must remain in XRD Facility, so samples cannot be prepared ahead of time. iv.
Glass slides are $80/ea, so be careful!
2.
Holder specifications: a.
Rectangular: 3 mm thick glass slides with 21×19 mm (L×W) indentations for packing of powder samples. Two indentation depths are available (0.2 mm,
0.5 mm). b.
Round: 24 mm inside diameter aluminum disk, 1mm or 2 mm deep, with solid back.
3.
Place a clean empty holder on a flat surface.
4.
Using wax paper or paper towels underneath holder aids cleanup and sample recovery after sample makeup.
5.
Put on latex gloves, if necessary.
6.
Pour in just enough powder sample to fill cavity.
7.
Using a clean microscope slide, pack the powder into the cavity as tightly as possible. a.
Fill the indentation fully. Any patches not covered by sample will contribute to background interference from the holder. b.
When finished, carefully lift holder and look at the edge profile. Top surface of powder should be flat and at same elevation as top of holder. c.
Depending on the sample's physical properties and static electricity, samples occasionally prefer to stick to the compression slide instead of staying in the holder. In this case, after packing it is often effective to not lift the compression slide off the holder but rather to laterally shift the slide sideways away from the cavity.
8.
When finished packing, scrape excess powder from the free surfaces of the holder onto the underlying paper. Recover excess sample as desired.
For single sample stage For 6-stage automatic sample changer

Powder XRD Operating Procedure
Step
Action
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2
Back-filled holder ALWAYS CLEAN BEFORE AND AFTER USE.
1.
Why use this holder? a.
Advantages i.
If samples are x-ray transparent (low absorption coefficient) and experience background interference from the standard top loading holders, then these holders avoids that interference. ii.
High sample volume helps to obtain high measurement intensities. iii.
Low probability of cross-contamination from sample-to-sample. iv.
Sample holder is aluminum (cheap) and nearly indestructible. b.
Disadvantages i.
Large sample volumes required. ii.
Sometimes difficult to pack powder tight enough to become "selfsupporting". iii.
Holders must remain in XRD Facility, so samples cannot be prepared ahead of time.
2.
Holder specifications: a.
Rectangular: 1.6 mm thick aluminum plates with a 21×19 mm (L×W) hole near one end. b.
Round: 24 mm inside diameter aluminum disk, 1.5 mm deep, without back.
3.
Place empty holder on a flat, mobile surface such as a microscope slide.
4.
Using wax paper or paper towels underneath holder aids cleanup and sample recovery after sample makeup.
5.
Put on latex gloves, if necessary.
6.
Pour in just enough powder sample to fill cavity.
7.
Using a clean microscope slide, pack the powder into the cavity as tightly as possible.
8.
When finished packing, scrape excess powder off edges of holder onto underlying paper. Recover excess sample as desired.
9.
While holding onto "slide sandwich" (glass/aluminum/glass), carefully invert the stack.
10.
Remove top slide to expose the sample surface that was originally on the bottom during the packing process.
11.
Remove bottom slide. If sample holds in place… a.
Rectangular holder: No problem, so load sample as-is. Otherwise, the glass slide can be taped to the bottom of the holder and the entire assembly loaded into the XRD b.
Round holder: Must use a different holder design for analyzing sample. The
6-stage automatic sample changer cannot accommodate a glass slide taped to the bottom of the holder disk.
For single sample stage For 6-stage automatic sample changer

Powder XRD Operating Procedure
Step
Action
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3
Zero background holder. ALWAYS CLEAN BEFORE AND AFTER USE.
1.
Why use this holder? a.
Advantages: i.
This holder is cut from silicon, parallel to (510), which has no diffraction reflections in the typical scan range for the instrument’s 2-theta. ii.
Often allows collection of decent diffraction patterns from VERY small sample volumes, depending upon crystallinity of sample. b.
Disadvantages i.
Smaller sample volume capacity (than other holders) leads to lower measurement intensity (smaller peaks). ii.
Very sensitive to impurities. Improper cleaning from previous runs can easily lead to cross-contamination for subsequent samples. iii.
Holder must remain in XRD Facility, so samples cannot be prepared ahead of time. iv.
Expensive, ~$500.00 replacement cost.
2.
PRIOR TO USE, IT IS RECOMMENDED THAT A QUICK SCAN IS
PERFORMED ON EMPTY HOLDER TO VERIFY IT IS CLEAN.
3.
Same procedure as for the top loading holders (see above).
Maintenance note: If the silicon crystal pops out of the aluminum holder, refer to
Section 12: Troubleshooting.

Powder XRD Operating Procedure
Step
Action
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4
Microscope slide for solid residue after solvent evaporation
1.
Why use this holder? a.
Advantages i.
Convenient for wet samples (sols, gels) that require solvent evaporation. ii.
Can be prepared ahead of time--especially useful for samples requiring lengthy preparation procedures. iii.
Sample slides can be saved after analysis for future repeat analysis. iv.
Slides are cheap. b.
Disadvantages i.
Poor option for powder samples. ii.
Low sample concentration or crystallinity can lead to time consuming preparations that require multiple iterations of dripping and drying. iii.
Thick sample spots lead to 2

shifts on diffraction pattern. iv.
Evaporation of solvent can lead to preferred orientation of sample. See
Section 8.3.2: Common Errors in Sample Preparation for more details.
2.
If template cannot be found, make a new one: a.
Place back-filled holder on top of clean microscope slide, aligning top edges as shown in the figure below. b.
Use marker to trace around the inside of the aluminum holder opening. c.
Mark the end of the slide that will be inserted into XRD sample holder.
3.
Get new, clean microscope slide and align it on top of template slide.
4.
Apply sample drops to sample area as necessary.
5.
Label opposite end of sample slide for identification purposes. Never allow sample material to slide under the Sample Holder.
6.
Two slides (blank slide below) will be necessary to securely mount into Sample
Holder.
7.
Save sample slide until analysis. Template is still clean and ready for reuse.

Powder XRD Operating Procedure
8.3.2 Common Errors in Sample Preparation
Step
Action
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1
Sample displacement



Probably the most common and largest source of error in diffraction data.
Sample sits above or below the Measuring Circle (top of Sample Holder plane).
Peak positions will shift ~0.01° (2 
) for every ~60
 m elevation offset.
2
3
4
5


Sample flatness (closely related to sample displacement)


Top surface of sample should be as flat as possible.
Peaks shift towards lower 2

Peaks broaden asymmetrically.
Maximum effect is at small 2

angles.
Sample transparency

Error is caused by diffraction from below the surface of a low absorbing sample.


Asymmetrically broadens peaks.
Maximum effect is at 90° (2 
).
Sample particle size

Particles must be small enough to:
– allow x-rays to penetrate to core.
– pack to provide a flat surface.

To minimize re-absorption of reflected x-rays within the sample, the general rule is that powder particulate sizes should be <45
 m diameter (325 mesh screen or finer). If the sample has heavy elements, 500 mesh or smaller particle sizes may be necessary.
Preferred orientation

The sample's crystals line-up or stack in such a way that certain reflections appear more intense than normal.

Commonly observed in the following materials:
– clays and mica
– graphite
– thin film samples obtained by evaporating a solvent to dryness

Special sample preparation may be required. The use of the round Sample holders in the 6-Position Stage and rotating while being exposed to the x-ray beam will reduce this problem.

Powder XRD Operating Procedure
8.4 Loading Sample(s) into the XRD…
8.4.1 …for the Single Sample Holder
Be sure the x-ray power is at full power level (40kV x 40 mA) and that no samples are currently being analyzed.
Step
Action
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1
Press the yellow DOOR OPEN button on the front panel of the XRD (see Figure 7.1b).
Wait until the alarm begins intermittent cycling (2-3 seconds).
NOTE: A steady alarm that does not begin to cycle after a few seconds indicates that the computer and instrument are not linked together. Computer log-in and server background BLUE required at all times.
2 Open the sliding doors at the front of the XRD.
3
Locate the single sample holder attachment in the center of the goniometer.
4
Maintenance note: If either or both sides of the spring clip have gotten bent and are too loose, place two fingers under the springs and press upward. Contact Lab Manager if broken or damaged.
Loading the sample holder. If the aluminum back-filled sample holder is being used with self-supporting powder, handle very gently; bumping the holder too hard may cause sample to fall out, leading to sample loss and a mess in the XRD.
1.
If using the aluminum back-filled holder: a.
Hold a plastic weighing dish underneath the sample during loading. b.
Carefully slide edge of holder between spring clip and attachment base.
2.
If using a Standard Top-Fill holder: a.
Carefully slide edge of holder between spring clip and attachment base.
3.
Gently push all the way back.
4.
Inspect powder sample. If top surface was disturbed during loading, remove and repack.

Powder XRD Operating Procedure
Step
Action
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5
Check alignment of holder
1.
Edges of sample holder should align with the endpoints of the diameter of the semicircular base.
2.
Sample displacement due to lateral misalignment (solid vs dotted lines in figure below) leads to analysis errors. Refer to Section 8.3.2 Common Errors in Sample
Preparation for more details.

Powder XRD Operating Procedure
…for the 6-Stage Auto Sample Changer (D/Max East XRD)
Although not difficult, this procedure requires very close attention to detail because it is easy to mix up samples when distracted. Refer to Figure 8.4.2 for an image of the autosampler.
Figure 8.4.2: Top-down view of the 6-stage auto sample changer

Powder XRD Operating Procedure
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Confirm that the 6-stage auto sample changer has been installed and previously aligned (recorded in logbook). If not, contact the XRD Lab manager to facilitate the installation and alignment of this attachment.
Below is a list of useful items to assist in loading the 6-stage auto sample changer.
3
4
Sit down at a sample preparation area that is clean and uncluttered with lots of space for spreading out.
Arrange up to six samples (in their original vials) in the numerical order in which they will be loaded. This numerical scheme will carry through sample loading and software setup.
5 Orient the sample carrying tray so that the red tape (reference mark) is on the left side.
6
1.
If using the top loading holders (with solid backs), flip them over and arrange numerically. Numbers and depth are engraved on back.
2.
If using the back-filled holders (no backs), these are hard to label. Just be careful.
7 Make a list of sample locations (slots #1-6) and sample identities.
8
9
10
One at a time, press each sample into its respective holder per Section 8.3.1: Sample
Packing Procedures . To avoid cross-contamination and sample mix-up, completely rebottle all stray powder from each sample before opening the next sample.
As each sample holder is finished, transfer it immediately to the sample carrying tray.
Fill the tray from left to right, being careful not to skip numbers, samples, or slots.
At the XRD, make sure a sufficient number of sample slots are vacant on the 6-stage auto changer. If not, remove the necessary items.
1.
Press the DOOR OPEN button on the XRD, wait for the alarm to start beeping.
2.
Open the sliding doors at the front of the XRD.
3.
Remove items from the autosampler.
4.
Use a compressed air can to carefully blow away any stray powder on the autosampler. Please try to contain as much dust as possible.
11 SLOWLY carry sample tray to XRD.

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Load the samples onto the 6-Position Auto-sampler.
Carefully mount each numerically-labeled sample holder onto the proper autosampler mounting ring (labeled #1-6). a.
NOTE: Latex gloves can get "pinched" between the sample holder and mounting ring because of their magnetic attraction. When this happens, removing your hand causes the glove to "snap" out. The holder subsequently slams into the turret and commonly disturbs the powder packing. If this happens, remove the holder and repack.
13 Close the XRD doors.
8.5 Goniometer Configuration for X-ray Beam Collimation
8.5.1 Hardware Identification
The items described in this section are introduced and discussed only briefly. For detailed installation instructions, refer to the big blue ring binder labeled "RINT2000/PC
Series Instruction Manuals, Rigaku Corporation" which is composed of numerous small manuals.
Throughout the following discussion, refer to Figure 8.5.1a for a schematic layout of goniometer hardware. Most of the x-ray beams which irradiate the sample travel at a slight angle to the plane of the focusing circle. If this angle of inclination is too large, the resolution of the diffracted x-rays and precision of diffraction angle will be lowered. To minimize this angle of inclination, divergence Soller slits (parallel plates arranged parallel to the plane of the diffractometer circle), a manual divergence height-limiting slit, and an automatic divergence slit (arranged perpendicular to the diffractometer circle) create a beam of incident x-rays that are approximately parallel. After colliding with the specimen, scattered x-rays do not perfectly reflect exactly congruent to the angle of incidence. To correct this scatter, multiple devices are used in series: a manual divergence height-limiting slit (optional), an automatic scattering slit, receiving Soller slits, and an automatic receiving slit. Used together, these accessories provide a nearly parallel beam of x-rays to the monochromator. One final slit, the manual receiving monochromator slit, corrects minor divergences created by the monochromator. Table
8.5.1 lists the relevant components of Figure 8.5.1a as well as the control mechanism of each.
Figure 8.3.1a Schematic of goniometer layout

Powder XRD Operating Procedure
Table 8.5.1: Goniometer components and control mechanism
Abbreviation from
Figure 8.5.1a
DSS
DHLS
DS
F (optional)
RHLS (optional)
SS
RSS
RS
RMS
Component Description
Divergence Soller slits
Divergence height-limiting slit
(variable) Divergence slit
Filter
Receiving height-limiting slit
(variable) Scattering slit
Receiving Soller slits
(variable) Receiving slit
Receiving monochromator slit
Control Mechanism
Manually switchable
Manually switchable
Computer-controlled
Manually switchable
Manually switchable
Computer-controlled
Manually switchable
Computer-controlled
Manually switchable
Figure 8.5.1b: Overall goniometer view

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8.5.2 "What Slit Size Should I Use?"
While not specific rules of operation, this section lists general guidelines to help a researcher identify an appropriate equipment configuration for sample analysis.
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General Guidelines
1.
Wide slits give higher intensity but lower resolution.
2.
Narrow slits give lower intensity but higher resolution.
3.
Use narrow slits if your sample is very small.
4.
Keep a personal log of the configuration of the manually switchable components for each sample you analyze because the software does not save this information
( i.e.
, divergence and receiving Soller slits, divergence height limiting slit, filters, receiving height-limiting slit, and receiving monochromator slit). This is especially important with shared equipment because you never know what configuration the person before you used. Always check the slits, ect.
Slit Mode and Sample Width. The variable slits (divergence, scattering, and receiving) installed on this instrument allow a great deal of flexibility in how a sample can be analyzed.
1.
Fixed slit / variable sample irradiation area. a.
User specifies the widths of the divergence, scatter, and receiving slits which remain constant during the scan. Based on geometrical considerations, the irradiation width of the sample changes as 2

moves. b.
This is the historical method of analysis.
2.
Fixed correction/ variable sample irradiation area. a.
User specifies the divergence and receiving slits which remain constant during the scan. After the software is told to start but before data collection, the appropriate scattering slit width is calculated by the computer based on the divergence and receiving slit widths. The scattering slit automatically adjusts to the calculated width and then remains fixed during the entire scan. As such, it is still a "fixed slit / variable sample irradiation width" mode as above.
3.
Variable slit / fixed sample irradiation width. Preferred Setting for best results.
a.
The computer automatically adjusts the opening of the Divergence and
Scattering slits as necessary (as a function of 2

position) to maintain a constant sample irradiation width (area parallel to the X-ray Beam axis) as specified by the user. The receiving slit width is still user-specified.

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Soller slits (divergence and receiving)
1.
The so-called focused beam optics of this instrument results in x-rays emitting from a point source and falling upon the sample at a slant. If the slanting angle is great, the resolution and accuracy of the measured diffraction angle decrease. The
Soller slits are used to reduce the slanting angle.
2.
The Soller slits consist of thin metal foils that are layered at equal intervals and parallel to the plane of the focusing circle.
3.
There are two sets of Soller slits available, one set of which is always installed.
Both the divergence and receiving slits must be of the same type: a.
"Standard thin film" (vertical foils) [default] b.
"Thin film distortion" (horizontal foils)
4.
The spacing of the metal foils are designed so that the angular aperture of the xrays will be: a.
5° for "standard thin film" b.
0.5° for "thin film distortion"
5.
For complete installation details, refer to yellow manual (p.18-21) in blue binder labeled:
Cat. No. 2185C101
RINT Ultima+/PC Series
Theta-Theta Wide-Angle Goniometer Instruction Manual
Manual No. ME12029A05
Vertical Soller slits Horizontal Soller slits

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Divergence height-limiting slit
1.
This manually switchable slit (in combination with the computer-controlled divergence variable slit) establishes the horizontal divergence angle of the x-rays, and therefore determines the area of the sample to be irradiated by x-ray beams.
2.
Four optional slits: 1.2 mm, 2.0 mm, 5.0 mm, and 10.0 mm (OPEN).
3.
Compared to smaller slits, using bigger slits will cause: a.
Measured intensity to be higher because more sample is irradiated. b.
Broader peaks and loss of peak profile sensitivity due to scattering effects caused by more coincident x-rays. c.
Higher background interference from sample holder if sample size is small.

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Divergence slit
1.
The divergence slit limits the total irradiation area of the sample by chopping the horizontal divergence angle of incident x-rays.
2.
The best width for this slit is truly found by trial and error.
3.
Modes of operation a.
Fixed and Fixed Corrected: i.
Seven discrete options: 0.05 mm, 0.17mm, 0.25mm, 0.5mm, 1mm, 2mm, and open ii.
[default] = 1mm b.
Variable: i.
Moves continuously and automatically as a function of 2

Background
6
The figure above shows both the theoretical and measured the relationship between sample irradiation length versus °2θ for several different divergence slits. Notice that for a 1° slit, a length of 2.5 cm is reached at 13° 2θ. At lower angles, the sample intercepts only part of the beam resulting in reduced beam intensity per unit area of sample surface and increases the likelihood of background scatter from the sample holder. At higher 2θ angles, less area is irradiated which has the effect of decreasing diffraction intensity. The depth of penetration of the beam becomes commensurably deeper with higher angles. This effectively increases background as well as a sample displacement effect. The theta-compensating divergence slit
( i.e.
, operated in variable mode) is designed to lessen high-angle intensity loss and displacement effects and low-angle background scattering. One must always recall however, that the standard form of reporting relative intensity is with fixed-slit conditions and that variable slit data must be appropriately corrected when analyzing in Jade.
Filter or receiving height-limiting slit
1.
This slot is commonly left empty [default] .

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8
Scattering slit
1.
The scattering slit limits the scattered x-rays entering the counter. It prevents the background from increasing and also prevents ghosts from occurring.
2.
In so-called focused beam optics, the scattering slit width is normally set equal to the divergence slit width.
3.
Modes of operation a.
Fixed: [default] i.
Seven discrete options: 0.05 mm, 0.17mm, 0.25mm, 0.5mm, 1mm, 2mm, and open b.
Fixed Corrected: i.
The proper slit width gets calculated automatically based on the divergence and receiving slit widths, automatically adjusts to this calculated width and then remains fixed throughout the scan. c.
Variable: i.
Moves continuously, automatically, and equally to the divergence slit as a function of 2

. Uniform sample irradiation at specified width setting.
Receiving slit
1.
The receiving slit limits the width of the diffracted x-rays entering the counter. Its primary use is to determine the minimum step size (sampling width) of the sample. a.
Increasing the width of the receiving slit general increases the peak height and width and decreases the ability to resolve peaks. b.
See table for minimum recommended step sizes for a given receiving slit.
i.
OK: Desired step size ≥ minimum step size from table ii.
BAD: Desired step size < minimum step size → pick new slit width c.
RECOMMENDATION: If using continuous scan mode for your analysis, the spreadsheet labeled "XRD CALCULATORS" on the Windows Desktop includes a tab called "Scan Conditions". Use this spreadsheet to determine conditions for your scan. After a step size is determined, use the table below to determine the proper receiving slit.
2.
Modes of operation a.
In all modes of operation (fixed, fixed correction, or variable), this slit width is user-specified and fixed. b.
This slit is "variable" in that it automatically moves to the user-specified position prior to scanning, but then it remains fixed during analysis ( i.e.
, no hardware needs to be installed).
Slit Width Minimum Recommended Step Size
[mm] [2

]
0.05
0.15
0.002°
0.005°
0.3
0.6
1
2
0.01°
0.02°
0.034°
0.068°

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.
8.6 Analysis Conditions
8.6.1 General Guidelines
While not rules of operation, this section lists general guidelines to help a researcher identify an appropriate analysis conditions.
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Spreadsheet
On the Windows Desktop is an Excel spreadsheet labeled "XRD CALCULATORS".
If the XRD will be operated in continuous mode (see below), the SCAN
CONDITIONS tab on the spreadsheet can help you design your experiment.
A good idea:
If you have a sample that you have not previously measured, it is strongly recommended to first make a quick scan with large step size (0.1 or 0.2° 2 
) and a short time per step (0.5-2 seconds/step) over a wide angular range to see where the reflections are and how intense they are. Afterwards, slits, step sizes, scan speeds, etc. can be adjusted as/if necessary to make more precise measurements. It will help you to get high quality data and save you a lot of time.

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Scan mode (3 options)
1.
Continuous (general-quick scans) a.
Data is collected continuously as the angular position is continuously increased. Intensity results should be given in COUNTS (benefits Jade). b.
User-specified parameters: i.
Step size or "sampling width" (deg 2

)
(1) Some experts recommend that the step size (in deg 2

) should be of the order of the (scan speed)/250 ii.
Scan speed (deg 2

/min)
(1) Typical scan speeds are 0.5-2.0°/min (2

) c.
Pros/cons i.
Continuous scans are faster than stepwise scans. ii.
Since goniometer always moves, data is less likely to be undersampled.
2.
Fixed Time (FT) (good quality scan and improved statistics) a.
The goniometer moves stepwise in discrete increments to each angular position and stays there while the data is collected. Intensity results will be given in counts. b.
User-specified parameters: i.
Step size or "sampling width" (deg 2

) ii.
Count time (seconds/step)
(1) Typical fixed times are 0.5-2.0 seconds/step c.
Pros/cons i.
Stepwise scans are more accurate than continuous scans. ii.
If step size is too large for the receiving slit, data can be undersampled.
3.
Fixed Count (this method seldom used) a.
The goniometer moves stepwise in discrete increments to each angular position and stays there until enough counts have been collected. No data is collected while slewing between steps. b.
User-specified parameters: i.
Step size or "sampling width" (deg 2

) ii.
Count value (# of counts) c.
Pros/cons i.
Useful for quantitative analysis where high counting statistics are required ii.
Speed cannot be determined, only estimated.
Remember:

Smaller step size gives better angular resolution but potentially more noise


Longer dwell time per scan gives better statistics (reduces noise)

Measuring time = time per step * (stop angle – start angle) / step size
"Counts per second" or "cps" = counts/time per step

The scan speed and step size that one should use depends on sample size and the crystalline quality of the sample. Generally, one can say that a small sample of poor crystalline quality takes longer to measure than a large sample of good crystalline quality.

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Comparing data from different samples


Use the same angular range (x-axis)
Regardless what mode was used to collect the data, comparison of samples requires all y-axes to be rescaled to "counts per second", not "counts".

Use the same type of intensity scale (y-axis): linear, square root, or logarithmic.

Measuring time = time per step * (stop angle – start angle) / step size
8.6.2 Software: Main Screen of Standard Measurement
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From the Windows Desktop, double-click the "Standard Measurement" icon to start the analysis software.
2
The main screen of Standard Measurement will open.
3
4
If you have a personal analysis condition profile already saved (*.mcd file), load it from the drop down menu: File → Open.
Parameters to enter on the main screen of Standard Measurement:
1.
Each row represents a different data file. A data file can contain one or multiple scans from the same sample.
2.
Use: Each row where Use = YES will be analyzed. Set all unused rows to NO, making sure to scroll down so as not to miss any.
3.
Print: YES will print data file to local printer at end of scan.
4.
Browse: Single-click the Browse button and specify where to save the data.
5.
Sample Name: Text message only, appears in Jade header.

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Attach and Sample: These columns appear only when the 6-stage auto sample changer is installed.
1.
Sample specifies on which of the 6 positions the sample sits.
2.
Double-clicking in the Attach box for each sample opens the Auto Sample
Changer window. a.
The number in the Attach box from the main screen (see figure above) is tied to a tab with that same number in the Auto Sample Changer window below. b.
Each of 10 tabs are available for setting different autosampler conditions. c.
Available conditions for the autosampler: i.
None: No rotation before or during scan. ii.
Fixed: Sample rotates to a fixed angle before analysis, then remains stationary at this angle throughout scan. iii.
Step move: Sample rotates stepwise through a user-specified range at a given step size. A full scan is collected at each step before advancing to the next step increment. iv.
Rotate: Sample rotates continuously during the scan at a user-specified rotation speed (0-120 rpm).
3.
Exit window when finished.
6
7
Condition: Double-clicking in the Condition box for each sample opens the Scan
Conditions window of Standard Measurement. Refer to Section 8.4.3: Software –
Scan Condition Window of Standard Measurement for more details.
Ending Process (list box): User specifies what state the equipment should return to at the completion of the sample scan.
1.
Present condition [default] : Leaves power on and x-ray energized.
8.6.3 Software: Scan Condition Window of Standard Measurement
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The Scan Condition window actually has two screens, but these are poorly labeled.
You just have to visually recognize which one you are on. For purposes of this discussion, call them #1 and #2. The user can switch back and forth between them by clicking the horizontal scroll bar (at bottom of the window).

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3
The number in the Condition box from the main screen (see Section 8.6.2: Software –
Main Screen of Standard Measurement above) is tied to a tab (the "measurement condition") with that same number in the Scan Condition window.
1.
Tabs = "Measurement Conditions" a.
Each user may be assigned a single tab (99 tabs available). b.
Only one tab can be assigned per data file.
2.
Rows = "Scan Conditions" a.
Each tab allows 99 rows. b.
Each row can be selectively turned on or off. c.
A single data file can use either a single row or a sequence of rows. This is convenient if you want to spend your analysis time focused on a few peaks instead of large sections of background ( i.e.
, assign a row per peak).
3.
Measurement and Scan conditions do NOT get saved to your personal profile. It is important you maintain personal records of measurement conditions. Please do not disturb other users' settings.
Screen #1
Screen #2

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Parameters to enter on screen #1 of Scan Conditions:
1.
Slit mode: The selector for this is hidden. a.
Single-click button labeled “Detail >>” to open the advanced options. b.
Slit mode (list box) = Fixed, Fixed Correction [default] , or Variable c.
Single-click button labeled “Standard<<” to close advanced options
2.
Scan axis (list box): 2Theta/Theta [default] , 2Theta, Theta.
3.
Method (list box): Continuous [default] , FT (fixed time), or FC (fixed count)
4.
Counting unit (list box) = Always use COUNTS; important to Jade.
5.
Use: Each row where Use = YES will be analyzed. Set all unused rows to NO, making sure to scroll down so as not to miss any.
6.
Comment: Text message only, appears in Jade header.
7.
Start angle: Angular position (°2

) for starting the scan condition.
8.
Stop angle: Angular position (°2

) for stopping the scan condition.
9.
"Smart" columns #1 & 2: The choice of "Method" causes these columns to change accordingly.
"Method" selection
Continuous
FT
FC
"Smart" Column #1 "Smart" Column #2
Sampling Width (°2 
) Scan Speed (°2 
/min)
Step Width (°2

) Count Time (sec/step)
Step Width (°2 
) Count Value (counts)
10.
kV (list box): 20, 24, 28, 32, 36, 40 [default] , 44, 48, 52, 56, 60 kV
11.
mA (list box): 10, 20[default] , 30, 40, 50 mA + Remember to change to 40 mA .

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Parameters to enter on screen #2 of Scan Conditions: (Refer to Section 8.3.2: "What
Slit Size Should I Use?" for assistance identifying proper conditions).
1.
DivSlit (list box): Divergence slit width. See table below.
2.
DivH.L.Slit (list box): Divergence height-limiting slit width. a.
Options: 1.2, 2.0, 5.0, and 10.0 mm (open; max intensity) b.
Use 2.0 or 1.2 slit with Zero-background Sample Holder
3.
SctSlit (list box): Scattering slit. See table below.
4.
RecSlit (list box): Receiving slit width. a.
Options: 0.05, 0.15, 0.3 [default] , 0.6, 1, 2, and 10 mm (open)
5.
Offset angle: (effect unknown)
6.
hkl columns: Text message only
7.
BG condition: "Background condition" (effect unknown)
8.
Substance: Text message only
9.
Other: (inactive)
Column
Heading Fixed
Slit Mode
Fixed Correction Variable
DivSlit
SctSlit
0.5 mm, 1/6°, 1/4°,
1/2°, 1°, 2°, open
0.5 mm, 1/6°, 1/4°,
1/2°, 1°, 2°, open
0.5 mm, 1/6°, 1/4°,
1/2°, 1°, 2°, open
"Auto"
(computer-controlled)
"Variable"
(computercontrolled)
"Variable"
(computercontrolled)
6 Exit the Scan Conditions window and return to the main Sample Measurement screen.
8.7 Starting the Analysis
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1 Recheck all analysis conditions carefully, especially if starting a long series of runs.
2
Click on the icon below to start the data collection process.

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Pay close attention during the initial moments of the scan.
1.
You should hear the goniometer motors moving almost immediately. If not…
2.
Occasionally, message windows on the Windows Desktop open which halt the analysis until the user acknowledges them. For instance, a common message is a reminder to insert the proper divergence height-limiting slit. These small message boxes often get hidden underneath other open windows. If the analysis does not start after several seconds, shift the windows around to search for a potentially open box.
NOTE: Never leave the instrument until you confirm that the Safety Shutter has opened and the data scan has actually begun.
4
When the scan is ready to start:
1.
A metallic sounding "click" will be heard as the x-ray shutter is opened.
2.
The yellow SHUTTER R lamp on the "Christmas Tree" array (on top of XRD) will illuminate to show that the shutter is now open and x-rays are being emitted inside the XRD.
3.
A status window will appear to inform you what actions are occurring, as well as the Measurement Monitor to show the progress of the scan.
5
At this point, it is OK to leave the XRD unattended. However, if different divergence height-limiting slits are specified for either 1) different scan conditions on the same sample, or 2) different samples with the 6-stage auto sample changer, the sequence will stop and wait for your input before continuing.
9.1 Terminating a Run Early
Follow this procedure if an analysis scan is currently active but needs to be terminated early. In most cases, all data collected up to this point will be lost.
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1
On the Right Console dialog box with the message "Executing the measurement", single-click the BREAK button.

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2 The dialog box will notify you that the run is being stopped. Click OK.
9.2 Returning XRD to Idle After Sample Analysis “Standard Practice”
The default procedures for the XRD Facilities Lab is to bring the equipment to idle after use. This does not turn off the x-ray tube but it brings it to a minimum power setting.
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2
Exit from the Measurement Monitor (black screen with graph). When it asks for confirmation, single-click the YES button.
Locate the manual power control portion of the XG Operation window. Use the automated SET function to carefully reduce power to the x-ray tube and lengthen its useful lifetime (~2000 hours).
1.
The white text boxes should have the following setpoints: a.
Tube voltage = 20 kV b.
Tube cur. = 2 mA
2.
If the white text boxes have some other values, press the MIN. VALUE button which will set the values back to the 20 kV, 2 mA default minimum setting.
3.
Single-click the green SET button.
3
4
As the power is being decreased:
1.
The SET button will turn gray.
2.
A message will appear "Setting tube voltage and tube current" on the XG
Operation window.
3.
When finished, the SET button will turn green again.
Verify that the power is truly at the minimum setting (20 kV, 2 mA). The color bars should have changed similar to the figure below.
5
Be sure your sample is removed from the Goniometer. Log off from the computer and sign out on the paper Log Sheet.

Powder XRD Operating Procedure
10. Emergency Shut-Down Procedure
In the event of an emergency, immediately press the red EMERGENCY button on the front of the XRD. Power will be stopped to the entire instrument; x-rays will no longer be emitted.
Reasons FOR using the emergency shutoff:
 The x-ray Safety Shutter gets stuck open and the access door is able to open
 without shutting off the x-rays.
Electrocution risk from water contact with the XRD electrical components
(overhead leaking pipes, Haskris water line leakage, rising water in room, etc.)
Local emergencies NOT needing an emergency shutoff:
 Fire or fire alarm in the Space Science Building.
11. Maintenance
If maintenance is required for the XRD, contact the XRD Facilities Manager.

Powder XRD Operating Procedure
12. Troubleshooting
What Happened? Why? What to do?
Silicon crystal popped out of zero background holder
Spring clips on single sample holder are loose




Pressing too hard during cleaning without supporting back of holder against a flat surface
Cleaning solvents removed
Epoxy adhesive.
Normal wear-and-tear.
Improper sample mounting.
1.
NEVER use acetone. To clean outer edges of Si crystal and inner edges of aluminum holder use
Propanol.
2.
Put both items on wax paper.
3.
Flip Si crystal upside down
(indentation facing down).
4.
Wearing latex gloves, insert Si crystal into aluminum holder, press, and hold. It is important to get bottom face of Si crystal parallel to face of Al holder.
5.
Mix a small amount of 5-Minute
Epoxy and dab a small amount in
4 places on the parting surface of the aluminum and Si crystal.
6.
Cure per Epoxy instructions.
1.
Gently with two fingers apply upward pressure from below to both sides to the springs.
2.
Push upward several times.
3.
Insert the sample holder and check for a snug fit. Repeat if necessary.
Be absolutely sure the sample holder does not sag downward.
13. Disposal of Waste
You are responsible for proper disposal of your materials and cleaning of the Sample Holders after use. Please be considerate of the next user and use common sense. If your samples are hazardous, do not throw them into the general waste cans. Smaller waste containers are located next to Sample
Stations; please use these rather than the larger containers in the lab.
14. Instrument Details

Powder XRD Operating Procedure
14.1 Technical Specifications
Parameter
1 X-ray generator system
1.
Power output (continuously rated):
2.
Voltage:
3.
Current:
4.
Stability:
5.
Safety features a.
Cooling water flow and pressure detection b.
Generator overload detection c.
Tube voltage detection d.
Emergency stop switch e.
Leak current breaker
2 Radiation enclosure
1.
Steel construction with integrated lead panel direct beam stop
2.
Safety interlocked with electromagnetic shutter mechanism
3.
Sliding front access door with leaded-acrylic window
3 Cu x-ray tube and tube shield
1.
X-ray tube:
2.
Focal spot size:
3.
Tube shield :
4 Water Chiller (Haskris model RW100)
1.
Voltage:
2.
Current:
3.
Water pump (tube side):
4.
Flow meter (tube side):
5.
Water supply temperature (shell side):
6.
Safety features a.
High temperature alarm/cutoff b.
Water saver valve
5 Ultima II with theta/theta high resolution goniometer
1.
Geometry:
2.
Alignment:
3.
 s
(source) and
 d
(detector) axes control schemes:
4.
Radius:
5.
Measuring range a.
 b.
 s
/
 d
coupled s
independent c.
 d
independent
6.
Scanning speed:
7.
Rapid positioning speed:
8.
Step resolution:
9.
Step scanning width:
6 Incident (or divergence) beam optics
1.
Configuration:
2.
Soller slits, 2 options (manual) a.
"Standard thin film" vertical slits: b.
"Distortion" horizontal slits:
3.
Divergence height-limiting slits (manual):
4.
Variable divergence slit (computer-controlled):
5.
Data collection mode:
Equipment Specification
2.0 kW
20-60 kV (1 kV step)
2-50 mA (1 mA step)
± 0.01% aT
–
–
–
–
–
–
–
–
Long fine focus, 2.2 kW
0.4 mm × 12.0 mm
Electromagnetic shutter
208VAC, 1 Phase, 60 Hz
10 A
Positive displacement
Floating ball rotameter (0-2 gpm)
40-90 °F
–
–
Vertical

/

Manual or fully automated
Coupled or independent
185 mm
–
2

= -10° to 158° (0° datum pt)

2

= -3° to 79° (10° datum pt)
2

= -30° to 79° (10° datum pt)
0.001°/min to 50°/min (2

1000°/min (2

0.0001° (2 
0.001° to 45°/min (2

Bragg-Brentano para-focusing
–
5.0° axial divergence
0.5° angular divergence
1.2 mm, 2 mm, 5 mm, 10 mm
0.05 – 6.0 mm (0.01 mm step)
Fixed or variable slit

Powder XRD Operating Procedure
Parameter
7 Receiving beam optics
1.
K  filter (manual):
2.
Antiscatter slit (computer-controlled):
3.
Soller slits, 2 options (manual) a.
"Standard" vertical slits: b.
"Thin film distortion" horizontal slits:
4.
Receiving slit (computer-controlled):
8 Monochromator
1.
X-ray compatibility:
2.
Crystal composition:
3.
Geometry
4.
Crystal radius of curvature:
5.
Monochromator receiving slits:
9 Scintillation detector
1.
Linearity:
2.
Electronics (pulse height analyzer and high voltage detector)
3.
Dead time correction
10 Auto sample changer (Model ASC-6B)
1.
Allowable measuring angle range for goniometer:
2.
Sample changing system:
3.
Number of samples:
4.
Sample surface size:
5.
Sample rotation speed:
15. Contact List





For What Reason?
Emergencies (fire, injury, etc.
)
General information
Equipment problems
Building access
Billing questions
Contact Person
Rice Police
Richard Crouse
XRD Facilities Manager



Problems with SEA website
Technical support
Order replacement parts
Angelo Benedetto
SEA Scientist
Or
Richard Crouse
Rigaku Service Help
Desk
Equipment Specification
Ni for Cu radiation (optional)
0.05 – 20 mm (0.01 mm step)
–
5.0° axial divergence
0.5° angular divergence
0.05 – 10 mm (0.01 mm step)
Cu k  only graphite mosaic crystal curved
225 mm
0.45 mm, 0.6 mm, 0.8 mm
700,000 cps or better
–
–
2

= 0° to 158°
Turret rotation system
6
24 mm inside diameter
0-120 rpm
Contact Information
BRC
Phone:
Email: x6000
B08 Space Science Building
XRD lab:
Cell:
(713) 348-3279
(713) 303-4300
Fax:
Email:
(713) 348-5320 rcrouse@rice.edu
(713) 348-8207 angelo@rice.edu
Rigaku/MSC, Inc.
9009 New Trails Drive
The Woodlands, TX 77381
Office: (281) 363-1033
Front office: (281) 362-2300
Fax:
Email:
(281) 364-3628
Web: www.RigakuMSC.com