Xrd+manual.pdf

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//xraysrv.wustl.edu/web/xrd/xrd_manual.html#Laboratory_Safety_Document[11/15/2011 6:19:30 PM]

X-ray Diffraction Online Manual

Paul Carpenter, Earth and Planetary Sciences, Washington University

nstructions -- Rigaku Dmax/A Using MDI Datascan and Jade

Contents

1. Sample Preparation2. XRD Instrument Startup3. Calibration Procedure4. XRD Sample Exchange

5. Performing a Routine Scan6. Jade Program Procedures7. XRD Instrument Shutdown8. XRD Utility Programs9. Laboratory Safety Document (Appendix 4 of Blue Book)

Sample Preparation for an XRD run

1. Obtain representative sample.2. Grind sample to ~10 micron grain size, best grind is in acetone or isopropanol (i.e., not dry).3. Approximately 80-100 mg of powder required.4. We use the NIST Si (111) standard for routine external calibration, which is adequate for most

identification of unknowns.If an internal standard is required, use smallamount of CaF2Fluorite.

5. Load sample into glass 5g holder. Sample should completely occupy the square glass well.If you do not have enough powder you can try to arrange a dike of material parallel to the longdimension of the slide with powder in the center of the well.The glass slides do not leave the lab. If you need to order your own:Rigaku USA, Cindy Acuff 281-363-1033 ext. 137, part number 9200/5G Rect 0.5mm 10 slides pkg$92 per set of 10.

6. Sample must be flush with top surface of glass slide:If sample is above surface of slide then positive z-axis displacement error will move the XRDspectrum to higher anglesIf sample is below surface of slide then negative z-axis displacement error will move XRD spectrumlower angles.

7. Avoiding preferred orientation by excessive agitation of sample.8. Hygroscopic or other reactive powders may be sealed using Saran wrap, Kapton x-ray film, etc. to

reduce reaction with the atmosphere.9. Other capabilities include RIR method (use 1 micron Al2O3as internal reference standard, acquire

standard XRD spectra, use FullPat or similar program to fit sample spectra to standards).


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XRD Instrument Startup Checklist

1. On the Rigaku Generator Enclosurea. Confirm that all x-ray shield doors are closed:

The inner door should be all the way to the left, in the slot.The outer door should be set with the two red dots exactlylined up.

b. Check that the POWER and X-RAY READY white lamps are lit (they are dim and not easy tosee).

c. Check that the kV (Voltage) and mA (Current) control knobs are at their minimum settings:Both knobs should be fully counterclockwise with the kV set to 20 kV and the mA sto 2 mA.

d. Check that the LOAD switch is set to 1.5.e. Confirm that the SHUTTER 2 control switch is in the CLOSE position.

We use only shutter 2 (on the right) and shutter 1 is not engaged or used and cannot beopened.

2. Databox (red rack on table to the left of the computer):a. Check that the MINIBIN POWER SUPPLY POWER switch is ON and red lamp is lit.b. Check that the HIGH VOLTAGE ORTEC 556 module POWER switch is ON, the LED is glowing a

the METER reads 0.90 kV.

c. If the meter reads below 0.90, turn off the High Voltage Power Supply using theswitch at the lower left. Wait 5 seconds, then turn back on. If the meter does not re0.90 get Paul Carpenter.

d. Confirm that the DATABOX module switch is in the ON position.

3. XRD Computer:a. Confirm that the XRD computer and DELL monitor are on.b. If you need to log on, use the instructions in the written logbook.

4. Printera. Confirm that the printer is on with a Ready status.

5. Enter your user information in the User Excel Sheet:a. The XRD Usage Excel spreadsheet launches at login, but can be lanunched from a desktop icb. Enter your name, email, advisor, 1st 4 digits of department charge code (NOT campus box

number),user code (eps=Earth Planetary Sci, wu=all other Wash Univ departments, ext=other universcomm=commercial.

c. Read the instrument odometer value from the Hour Meter located at the lower right inside thRigaku hutch and enter this in the spreadsheet (do not use copy, please type in the value).

6. Sample Exchange Procedure for Startup:a. Place the SHUTTER 2 control switch in the CLOSE position.

This protects you from x-ray exposure.

b. Confirm that the rectangular SHUTTER lamp on tube tower is not illuminated red.c. Turn the FS (Fail Safe) RELEASE key clockwise and release, you should see a flashing red lig

above the key and hear a loud beeping sound.d. Slide both front doors fully to the right.e. If you are performing a Si 111 calibration, the NIST Silicon sample should be run first.

The Silicon standard is kept in the tray to the left of the Rigaku goniometer, in the hutch.Please be careful with the sample, the NIST Silicon powder is expensive.

f. Unscrew the sample/goniometer cover plate and CAREFULLY place the sample mount under ttwo spring clips:The glass slide is inserted with the glass portion first and the sample portion away from theclips.


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g. Replace the metal sample chamber cover. GENTLY screw in the retaining screw and make suthe cover is not tilted away at the bottom.

h. Slide the innermost door all the way left into the groove.i. Slowly slide the outer door to the left and use your left finger to keep from overshooting the

dot position, line the two red dots exactly.DO NOT SLIDE THE DOOR PAST THE RED DOT

j. The override flashing red light will stop illuminating and the audible beeping sound will stop.k. You are now ready to turn on the X-ray tube.

7. Turning on the X-ray tube:NOTE: The x-ray tube is turned ON by pressing down the ON switch.The x-ray tube is turned OFF by pressing down on the OFF switch.Each switch is used for only one function (they do not toggle).Procedure:

a. Press down and release the white X-RAY ON toggle switch. You will hear a loud click as the hvoltage is turned on.

b. This should illuminate two red x-ray lamps:One is located above the X-ray power switchThe other is the X-ray warning lamp located inside the hutch.

c. These warning lamps provide positive protection and disable the tube from operating if a lamburned out.

d. The kV meter should read 20kV and the mA meter should read 2mA (Tube Voltage/CurrentMeters).

8. Raising the high voltage kV:

When turning the tube ON, we raise the kV voltage FIRST, then the mA current SECONDNOTE: The operating voltage for XRD scans is 35 kV.You should take about 30-45 seconds turning the voltage from 20 to 35 kV as follows.Procedure:

a. Turn the kV knob clockwise one click at a time.b. Do not delay between clicks, that is, do not stay in between click settings.c. When the kV reaches 35 (at the black line), you are ready to raise the mA current.

9. Raising the tube current mA:When turning the tube ON, we raise the kV voltage FIRST, then the mA current SECONDNOTE: The operating current for XRD scans is 35 mA.You should take about 30-45 seconds turning the current from 2 to 35 mA as follows.Procedure:

a. Turn the mA knob clockwise one click at a time.b. Do not delay between clicks, that is, do not stay in between click settings.c. If you delay between the 25 and 27 mA click settings this may cause the Rigaku to overload.

If an overload occurs there may be a loud buzzer or a circuit breaker will be tripped.Get Paul Carpenter if this happens.

d. When the mA reaches 35 (at the black line), you are ready to run your sample.

10. Leave the shutter closed until you have set up the computer for a routine scan.

Calibration Procedure

We use the Silicon (111) reflection to perform a routine calibration of the XRD goniometer.his sets the goniometer to the theoretical position for Si (111), 28.443 degrees two theta.he calibration scan should be performed every 1-2 days. If you are doing routine identification ofnknowns it is not as important compared to collection of cell data, etc.his is a community laboratory, so when in doubt, perform the calibration scan for quality control.


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1. Calibration Procedure:a. Use the Sample Exchange Procedure to change samples and put the NIST Silicon sample in t

sample chamber.b. Launch the MDI Datascan program.c. Open the menu: Control - MDI Databox, this opens the MDI Databox window:

d. On the MDI Databox window, select the menu Function - Scan Line, this opens the Scan Li(2Theta/Theta) window:

e. The window should already have the following settings for the Si (111) calibration scan:Symmetrical scan centered around 28.443 degreesStep size of 0.004 degrees and count time of 2 secondsIt should be populated with these values and is ready to run.

f. Open the shutter: Shutter 2 switch from Close to Open.g. Click on the Scan button in the Scan Line window.h. Datascan will acquire the data and shows the cursor at the theoretical value for the Si (111)

peak.

i. If a change to the position is identified by Datascan a dialog will be presented with the changin degrees 2 theta.

j. You can alternatively move the cursor to position it better (for example, to a symmetricposition).

k. After doing this, the goniometer is driven to a position that compensates for the smallcalibration error.The calibration is assumed to be linear over the range of 2 theta and this is typically valid.

l. The calibration scan leaves the goniometer at the end of the scan range.You do not need to drive the goniometer to 20 degrees because the Routine Scan procedurestart at the requested scan position.

m. You can now perform the sample exchange to run your sample.


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Sample Exchange Procedure

1. Sample Exchange Procedure with X-ray Tube Turned On:a. Close the shutter: Place the SHUTTER 2 control switch in the CLOSE position.

This protects you from x-ray exposure.

b. Confirm that the rectangular SHUTTER lamp on tube tower is not illuminated red.c. Turn the FS (Fail Safe) RELEASE key clockwise and release, you should see a flashin

red light above the key and hear a loud beeping sound.d. Confirm the audible beeping -- if you open the doors without turning the FS release key this

turn off the X-ray tube. Please do not do this!e. Slide both front doors fully to the right.f. Unscrew the sample/goniometer cover plate and place it on the foam pad.g. Remove the existing sample from the sample chamber.h. Place your next sample mount under the two spring clips:

The glass slide is inserted with the glass portion first and the sample portion away from theclips.

i. Replace the metal sample chamber cover. GENTLY screw in the retaining screw and make su

the cover is not tilted away at the bottom.j. Slide the innermost door all the way left into the groove.k. Slowlyslide the outer door to the left and use your left finger to keep from overshooting the

red dot position, line the two red dots exactly.

DO NOT SLIDE THE DOOR PAST THE RED DOTl. The override flashing red light will stop illuminating and the audible beeping sound will stop.

m. You are now ready to run the sample.

Performing a Routine Scan

he Datascan program is used to run Routine Scan, which acquires an XRD scan from the starting anglehe ending angle at a specified step size and count time, and writes the data to your data file in your foocated in the My Documents directory.

he Routine Scan procedure writes the data to an *.mdi file automatically, you do not need to save thecan from Datascan.he Jade program can be used to load the scan data at any time, it will load what you have acquired soar.

ou will need to do the following:

et the path to point to your foldereuse or create a scan job to acquire the datanter the scan settings for the routine scan (start, end, step size, time, file name, and comment)un the scan

1. Performing a Routine Scan:a. Launch the MDI Datascan program.b. Select menu Scan - Routine Scan(Do not use Quick Scan). This opens the Setup Scan

window:


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c. Click on the Browsebutton and navigate to your folder in the My Documents folder.

Please use the following protocol for your user folders:My Documents: Lastname: Lastname date: Lastname Sample specific foldersFor example, in My Documents folder:

Lastname Firstname: master folder for all your XRD dataMake a new folder: Lastname 10-5-2011Make a sample specific folder such as: Lastname quartz scansThis allows us to put files into the correct destination folder.

d. Confirm that the path is correct in the Setup Scans window before proceeding.The window above shows the correct path using this protocol.

e. Next, click on the inverted new page icon (next to last icon on right) in the upper right of theSetup Scans window to clear the previous scan job. Confirm that you do want to do this.

f. Now click on the New Scan Jobbutton in the Setup Scans window.This opens the New Scan Job window:

g. Click on the New Rangebutton. This opens the New Scan Range window:


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h. Enter the start angle, end angle, step size (default is 0.04 degrees), and count time (default

second per step).The calculated run time is displayed in the lower left of the window.Click on Ok to close this window.

i. Data File ID: Enter the windows file name that will be used for the data output.Please use the following format:Lastname date letter: Carpenter 10-5-2011a for example.

j. Comment: Suggest the following protocol -- when you export the data as a text file, yourcomment will be in the header of that file.Sample name, scan range, step size, count time

Example: Quartz 1AB24 15-70 degrees, 0.04 degree step, 1 second per stepThis comment will tell you all information when you export the scan ascii data from Jade.k. The completed scan job window should look like this:

l. Click on Ok to close the New Scan Job window.The completed scan job setup should look like this:


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m. If the scan job is all correct, you are ready to run the scan.n. Open the shutter: Shutter 2 from Close to Open.o. In the Setup Scans window, click Startto begin the scan.

p. The scan should now proceed until completed.q. Additional information about Datascan:

If you forget to open the shutter, click on the stop sign, wait for Datascan to reset, then restthe scan.Please do not change the preferences.If you need to do a scan from a low angle position or to a position above 90 degrees, pleasesee Carpenter for instructions.

Jade Procedures

About the Jade Program and Documentation

he Jade program is a powerful but fairly complicated program and there is no manual specifically desigo walk you through procedures. There is an extensive help file that is hyperlinked and is the source fornformation regarding all the capabilities of the program; you can make a copy of the Jade help file (it ishe pub folder on the XRD computer and is also available here: Jade Helpdo not try to launch the help se right-click and save to your computer. This is a windows help-format file; if using Vista or Windows ou will need to download the windows help file viewer utility from Microsoft. There is now also a pdfersion of each section of the help file that is in a zip file (note that these documents do not have

unctioning links but they can be viewed on any computer).

ade Help Files -- pdf version

Here are the links to the pdf versions of the Jade Help file subsections (note that they do notave active internal links):

Jade Installation and Version FeaturesJade User InterfaceGetting Data Into JadeGetting Data Out of Jade
http://xraysrv.wustl.edu/web/xrd/xrd_files/http://xraysrv.wustl.edu/web/xrd/xrd_files/1%20Jade%20Installation.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/2%20Jade%20User%20Interface.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/3%20Getting%20Data%20Into%20Jade.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/4%20Getting%20Data%20Out%20of%20Jade.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/4%20Getting%20Data%20Out%20of%20Jade.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/3%20Getting%20Data%20Into%20Jade.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/2%20Jade%20User%20Interface.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/1%20Jade%20Installation.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/


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Basic pattern processingICDD PDF & NIST Crystal Data AccessSearch Match for Phase IdentificationAdvanced Pattern ProcessingCalculate XRD Powder PatternsVisualize Crystal Structures in 3DMiscellaneous Topics (Datascan)

Basic XRD Pattern Processing Using Jade

asic pattern processing involves the following procedures:

Loading the XRD scan into JadeIdentifying the background points, subtracting the background, and stripping the Cu Ka2 componIdentifying the peaksSetting up and running the Search-Match procedureComparing results of the Search-Match hit list and loading additional ICDD cards for comparisonCapturing images of the SM displayExporting the XRD data scan as an ascii file for import into other software

ere is a step by step sequence for basic XRD pattern processing as outlined above:

1. Use the menu File - Patternsto load your .mdi file into Jade for processing.a. Navigate to your folder with the data file.

Make sure that the file filter in the window is set to display files with an *.mdi extension or ywill not be able to see them in the Patterns dialog window.
http://xraysrv.wustl.edu/web/xrd/xrd_files/5%20Basic%20Pattern%20Processing.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/6%20ICDD%20PDF%20&%20NIST%20Crystal%20Data%20Access.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/7%20Search%20Match%20for%20Phase%20Identification.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/8%20Advanced%20Pattern%20Processing.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/10%20Calculate%20XRD%20Powder%20Patterns.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/11%20Visualize%20Crystal%20Structures%20in%203D.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/13%20Miscellaneous%20Topics.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/13%20Miscellaneous%20Topics.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/11%20Visualize%20Crystal%20Structures%20in%203D.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/10%20Calculate%20XRD%20Powder%20Patterns.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/8%20Advanced%20Pattern%20Processing.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/7%20Search%20Match%20for%20Phase%20Identification.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/6%20ICDD%20PDF%20&%20NIST%20Crystal%20Data%20Access.pdfhttp://xraysrv.wustl.edu/web/xrd/xrd_files/5%20Basic%20Pattern%20Processing.pdf


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b. If you need to export the raw data file, do that now:c. Use File - Save - Primary Pattern as *.txtto save your raw data.

2. Perform background subtraction and strip Cu ka2 component:a. Use Analyze - Fit Background...to open the background dialog:


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b. Reset the options to their default values by clicking on the I icon.c. If necessary, change the background mesh spacing using the radio buttons.

d. Make sure that the Strip Ka2 checkbox is selected.e. To perform the background and Ka2 strip, click on the icon that is a down-pointing arrow witan underline.

f. If you want to save the background corrected file use File - Save to do so.

3. Find the peaks using Find Peaks:a. Use Analyze - Find Peaksto open the Peakfinder dialog:


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b. Reset the options to their default values by clicking on the I icon.c. To find the peaks, click on the icon that looks like a play button

d. Inspect the spectrum. If there are peaks without a dashed centroid marker that do not appeain the list, then you will need to use the manual peaking tool to index them.You can also adjust the threshold values to bring a low intensity peak into the acceptance ranfor the peakfinder algorithm.

e. If you want to save the peak list, use the disk icon to do so.

4. Set up the Search Match Routine:a. Use the menu Identify - Search/Match Setupto open the Search Match dialog:


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b. Reset the options to their default values by clicking on the I icon.c. Select the appropriate ICDD file from the left side of the window.

d. Start your Search-Match procedure without constraints (such as chemistry).If you need to apply constraints you can add them from the Search-Match window.e. When you have completed the selections, click on the SM icon to run the Search-Match

procedure.f. This will open up a new window with the Search-Match display and hit list:


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5. Inspect the Search Match Results in the Search-Match Window:

a. The hit list is ranked in decreasing order of the fit parameter.b. Use the up/down arrows to highlight each hit and compare the marker lines with your peaks the scan.

c. Check the box next to hits that you want to keep. These will also now appear as ribbons on display.

d. Click on the ribbon to change the color to one that humans can see.e. This display uses a context sensitive mode.

If you select an area for zooming, you need to use the icon that looks like a window to workback incrementally to the original "focus" range of your scan.

f. To remove unwanted hits from the list, use the X icon which will be located on the lower leftright.

g. You can load any ICDD card for comparison in the hit list using the text box at the top of the

screen.h. Peaks can be labelled with the currently selected hit using labelling icons at the top of thescreen.

i. Use the MWSnap utility to capture an image of the Search-Match display for export. The prinutility does not produce an exact copy of the display.

j. You can rerun the Search-Match routine from this window and change constraints.k. See the help document for more information on basic pattern processing and Search-Match

procedures.

Other Jade Capabilities


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here are a number of other capabilities that the Jade software has (please see the help file for morenformation):

Cell refinementGenerating a synthetic XRD spectrum from input dataDisplay of 3D rendered structures (also have site license for Diamond 3D)Comparing results of the Search-Match hit list and loading additional ICDD cards for comparisonCapturing images of the SM displayExporting the XRD data scan as an ascii file for import into other software

XRD Instrument Shutdown Checklist

1. Perform the Sample Exchange Procedure:a. Place the SHUTTER 2 control switch in the CLOSE position.

This protects you from x-ray exposure.b. Confirm that the rectangular SHUTTER lamp on tube tower is not illuminated red.c. Turn the FS (Fail Safe) RELEASE key clockwise and release, you should see a flashing red lig

above the key and hear a loud beeping sound.d. Slide both front doors fully to the right.e. Unscrew the sample/goniometer cover plate and remove your sample.

Leave the sample chamber cover on the foam pad.f. Slide the innermost door all the way left into the groove.g. Slowly slide the outer door to the left and use your left finger to keep from overshooting the

dot position, line the two red dots exactly.

DO NOT SLIDE THE DOOR PAST THE RED DOTh. The override flashing red light will stop illuminating and the audible beeping sound will stop.i. You are now ready to turn down the X-ray tube current then kV.

2. Lowering the tube current mA:When turning the tube OFF, we lower the mA current FIRST, then we lower the kVSECOND.You should take about 30-45 seconds lowering the current from 35 to 2 mA as follows.Procedure:

a. Turn the mA knob counterclockwise one click at a time.b. Do not delay between clicks, that is, do not stay in between click settings.c. If you delay between the 25 and 27 mA click settings this may cause the Rigaku to overload.

If an overload occurs there may be a loud buzzer or a circuit breaker will be tripped.Get Paul Carpenter if this happens.

d. When the mA reaches 2 and is fully counterclockwise, you are ready to turn down the kV

3. Lowering the high voltage kV:

When turning the tube OFF, we lower the mA current FIRST, then we lower the kVSECOND.You should take about 30-45 seconds turning the voltage from 35 to 20 kV as follows.Procedure:

a. Turn the kV knob counterclockwise one click at a time.b. Do not delay between clicks, that is, do not stay in between click settings.c. When the kV reaches 20 and is fully counterclockwise, you are ready to turn off the x-ra

tube.

4. Turning off the X-ray tube:The x-ray tube is turned OFF by pressing down on the OFF switch.Each switch is used for only one function (they do not toggle).Procedure:


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a. Press down and release the white X-RAY OFF toggle switch. You will hear a loud click as the voltage is turned off.

b. This should extinguish the two red x-ray lamps.

5. On the Rigaku Generator Enclosurea. Confirm that all x-ray shield doors are closed:

The inner door should be all the way to the left, in the slot.The outer door should be set with the two red dots exactlylined up.

b. Check that the POWER and X-RAY READY white lamps are lit (they are dim and not easy to

see).c. Check that the kV (Voltage) and mA (Current) control knobs are at their minimum settings:

Both knobs should be fully counterclockwise with the kV set to 20 kV and the mA sto 2 mA.

d. Check that the LOAD switch is set to 1.5.e. Confirm that the SHUTTER 2 control switch is in the CLOSE position.

We use only shutter 2 (on the right) and shutter 1 is not engaged or used and cannot beopened.

6. Enter your ending odometer value in the User Excel Sheet:a. Read the instrument odometer value from the Hour Meter located at the lower right inside th

Rigaku hutch and enter this in the spreadsheet.

b. Save the Excel spreadsheet and leave it open for the next user. Close both the Datascan andJade programs when you are done.

XRD Utility Programs

he following procedures are useful for XRD information.

MDI Mineral Program

he MDI Mineral Program can be used to find information for minerals. Launch the program and eithercroll down the list or enter the mineral name. This will load information about that mineral. A pictographe diffraction peaks is shown at the upper left; hover the mouse over this graph to determine the 2 theosition of peaks and the start and end values for a routine scan. The data also lists at least one ICDD cor this mineral, which you can use in Jade to force a comparison in the Search Match display. Thisrogram is a quick and easy utility to determine x-ray information.

PDF+ Utility Program for ICDD Database

he PDF+ program is the front end utility that can be used to call ICDD card data from the ICDD databaWe get the DDview+ utility with our subscription to the PDF4 ICDD database. There is a help file that yoan copy that covers routine proceduures with the DDview+ program. There are also web based tutorialn the ICDD web site that include DDview+ information, see http://www.icdd.com/resources/tutorials/ f

more information.

ere are some short instructions for retrieving ICDD card information:

1. Launch PDF+ from the desktop shortcut and wait for it to load; it requires a current version of theICDD subscription to work.

2. Use File Open Card to retrieve a specific card from the database.
http://www.icdd.com/resources/tutorials/http://www.icdd.com/resources/tutorials/


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3. To find cards for an element or compound, use the periodic table mode to call up ICDD cards forspecific element lists.Note that you need to specify the correct boolean test to discriminate cards which contain only theselected elements or elements in addition to those selected.

4. When the list is loaded, double click on the card number to display the card data.5. You can use the MWSnap screen capture utility to capture any image in the PDF+ display.6. Additional constraints can be applied to the search procedure. For example, elements Si and O wit

the "only" constraint are used in the periodic table to match all Si-O compounds, and on the Nametab the mineral name "cristobalite" can be used to find only those compounds that are called by th

mineral name (this of course could be used by itself in the match procedure).

Laboratory Safety Document -- Appendix 4 of Blue Book

Document last updated on 11/15/2011 by Paul Carpenter

X-ray Diffractometer Lab (EPS Rooms 152-153)

se: In this lab, we work with an instrument that generates X-rays. Exposure to X-rays is harmful to yo

ven though you can not see them or necessarily feel their effects. Our instrument has an annual radiaturvey and the results are in the laboratory blue book for the current and past year surveys. The sheildind safety interlock system permit us to work without the requirement of dosimetry badges. During norperation, you will not be exposed to harmful levels of radiation.

t is important for you to follow the standard operating procedure and placards on thenstrument during sample exchange. Failure to do so will result in you being banned from theaboratory.

s with any radiation source, you should limit exposure time and maximize shielding and distance from -ray source. Note that the exposure limits during pregnancy and for minors are much lower than foroutine workers. It is therefore not recommended to use any x-ray source during pregnancy or to bring

hildren into the lab. For information concerning typical exposure levels seettp://www.new.ans.org/pi/resources/dosechart/

he main concerns for safety in this lab lie with sample preparation and with cleaning (see below). Forample prep, we work mainly with powders. Most of the powders used in this lab are harmless. If youramples are harmful, you need to take appropriate precautions in handling them to prevent contaminatif the lab, bench tops, and instrument. Acetone and Ethanol are present in the lab for after-analysis clep. The instructions here are meant to supplement the Universitys Chemical Hygiene and Safety Traininfter this instruction, please sign the Bluebook for the Lab indicating that you have received the annual raining.

OSHA requires every laboratory to have laboratory-specific training and documentation.

1. Use of Volatile Organic Chemicals, Corrosives, Flammable Materials, Epoxies, and Toxinsa. Use these chemicals only in the chemical fume hood.b. Wear appropriate eye protection, foot protection, lab coat, and gloves.

Long pants and closed-toe shoes are required; sandles are not permitted (this lab hthe potential for exposure to broken glass and high-voltage sources are prsent).

c. Store segregated by hazard class and label as Flammable, Corrosive, or Oxidizer.d. Clean up solvent spills using a towel or other absorbent.

2. Working with Powdersa. If your samples are harmful (e.g. if your samples contain Arsenic, Barium, Chromium, Lead,

Mercury, Nickel, Osmium, Selenium or Silver), you need to take appropriate precautions in
http://www.new.ans.org/pi/resources/dosechart/http://www.new.ans.org/pi/resources/dosechart/


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D Manual

handling them to avoid contaminating the lab or bench tops.b. If you use the mortar and pestle with your samples, clean it completely using the St. Peters

sandstone to remove any staining.c. If you spill, there is a spill kit in the prep lab, if needed.d. Dispose of waste properly (i.e. put in plastic baggy and remove as hazardous waste through

Environmental Health and Safety).

3. Labelling Powdersa. If you leave your samples in the lab for any period of time, they must be labeled properly.

1. The label must have your name, the date, and what the sample is composed of.2. If the sample is harmful, it should be in a secondary container that you will supply.

4. Proper Disposal of Sharps and Broken Glassa. Discard razor blades in Sharps container.b. Discard broken glass in broken glass box.

5. Use of the Chemical Fume Hood (room 153)a. The fume hood should not be used as a storage area for chemicals or equipment.b. All containers must be capped when not in use. Evaporation of chemicals is prohibited.c. Work at least 6" inside the hood with a hood sash opening of approximately 14 inches.

6. Use of Carcinogens

a. Carcinogens are not permitted in this lab during normal procedures and carcinogentraining is not routinely provided.

b. If your samples contain carcinogens, please notify lab personnel.

7. Consumption of Food and Beveragea. Consumption of food and beverage is not permitted in the sample prep lab (153).b. Beverages may be consumed in the main XRD lab (room 152) as long as the beverage is not

on the XRD console or near computer equipment.

8. The lab is equipped with an eye wash and 2 showers should you need thema. Flush your eyes for as long as you can stand it.b. Contact your supervisor or a health and safety officer to report the incident and to receive

further instructions.

9. Fire extinguishersa. The lab (152) is equipped with a fire extinguisher.b. Familiarize yourself with its location and use.

10. If you think of something that has been left off this list, please report it to the laboratory managerthat it can be incorporated in the next version of this training.

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Document last updated on 11/15/2011 by Paul Carpenter
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