Contacts: Paul Carpenter Dr. Jeff Catalano Dr. Brad Jolliff
The Bruker d8 Advance X-ray diffractometer is a theta-theta instrument that is configured for analysis of powder samples. This instrument is configured with a Cu x-ray tube, a number of slits and filters, a rotating sample holder, and a position sensitive LynxEyeXE detector. It is used for routine identification of unknown materials, cell refinement work, quantitative phase analysis, structure determination, and other applications.
The d8 diffractometer unit houses the diffraction goniometer assembly, x-ray tube, high voltage power supply, cooling water circuit, (eventually an environmental high temperature cell), and intelligent electronics system that is used to monitor and run the equipment. Everything is monitored and controlled by either on-board electronics or the Bruker PC that runs the Measurement Server and Diffrac.Suite software.
For further general information about the Bruker d8 Advance, see the Bruker PDF Manuals.
The Bruker d8 diffractometer has a number of capabilities which are summarized in this instruction document but are discussed more completely in the Bruker manuals. You should download these manuals and refer to the complete discussion in order to fully understand the capabilities (Bruker PDF Manuals).
The Measurement Server application is started first and attempts to connect via ethernet to the Bruker d8. Once this connection is made, all subsequent actions are handled by the Measurement Suite software.
For full details see the Bruker Measurement Server section.
The Measurement Suite program (called Diffrac.Suite or Diffrac.Measurement Suite in the documentation) contains all components necessary to run the diffractometer and acquire data. Processing of the data is performed using the Diffrac.Eva and Topas programs.
The Measurement Suite manual contains a complete discussion of the components of the program, see: Bruker PDF Manuals.
The components of the Measurement Suite are the icons on the left side of the Measurement Suite main window:
The Bruker Diffrac.Eva program is used for the evaluation or processing of xrd data.
There are two manuals for Eva. The Diffrac.Eva manual contains a complete discussion of the components of the program, and the Diffrac.Eva tutorial has some examples of how to use the program, located here: Bruker PDF Manuals.
Capabilities of the Diffrac.Eva program are:
Bruker uses the Topas program which has a graphical user interface as well as a scripted capability called launch mode. The Topas manuals for the Bruker version are located here: Bruker PDF Manuals.
Capabilities of the Topas program are:
The Bruker d8 instrument is always in a power-on state. The x-ray tube is also in a power-on state but the tube power is set to a standby condition (20 kV and 5 mA). This is different from the Rigaku you are used to where we turn the x-ray tube off when not using the instrument. Therefore, it is important to remember that we do not turn off the x-ray power at the conclusion of a run. Secondly, if the high voltage is off or the instrument is turned off, that is not a routine state and you need to get Paul Carpenter / Jeff Catalano / Brad Jolliff to investigate.
As part of your training you are required to understand the location and function of controls on the Bruker d8.
The following sections outline the default setup for the Bruker d8 in terms of slits and filters (if any) that should be used for routine work.
From left to right as you view the instrument, the hardware layout is as follows.
Here is what modules A and B look like with the default 0.6 mm and Ni 0.0125 filters in place:
This is what the sample anti-scatter fin looks like when configured on the instrument. You need to have been instructed by Carpenter on how to mount the anti-scatter fin, if you have not done it before, get help.
If you need to use the fin:
This is what the Lynxeye 2.5 degree Soller slit looks like and how it is situated in the Lynxeye assembly--this sequence shows how to remove it.
Be very careful when handling the Soller slit, do not damage the metal foils or allow dust to get into the slit array.
See Inventory of Slits and Filters for configurations
Use Commander Davinci mode to determine the current slits and filters that are installed on the Bruker d8. All slits and filters have an electronic chip that the Bruker uses to identify the hardware and its position on the instrument.
For the Davinci image shown above, the system is reading (from left to right, in a V-shaped path):
Note the following:
The Wizard software is built in to the Diffrac.Suite software and is accessed using the Wizard icon that is on the top left side of the Diffrac.Suite window. The Wizard is used to generate a Bruker .bsml file which is used to run the XRD job from the Diffrac.Suite software, and is used to generate a Bruker .brml (and .raw) output file that contains the scan data.
The Wizard control is used to perform both simple and complex XRD runs, and the capabilities are listed below (you will not necessarily use all the capabilities).
It is important to understand the distinction between an experiment (procedures) file and a results (data) file:
The Wizard pdf manual is found here: Bruker PDF Manuals..
The following steps summarize how to use the Wizard to set up a basic XRD experiment, which is then run from Diffrac.Suite.
Here is an example of parameters entered for a scan from 5-60 degrees, with a 0.019 degree step size, a 0.5 second per step count time, with sample rotation turned on (15 rotations per minute), with a coupled two-theta / theta scan.
Summary of how to acquire data on the Bruker d8 Advance:
To run the job that you created using the Wizard, use the following instructions.
The Commander interface is the main interface to XRD data collection during a scan.
Once you have started a job running using the Start Jobs window, switch to the Commander window to view the progress of an XRD scan. You can scale and zoom the scan image during acquisition.
If you observe a yellow alert icon next to any of the goniometer drives or the sample spinner, you will typically need to initialize the drive that has the alert icon. This seems to happen frequently for the sample rotation drive and is not a problem to collect data with the drive not initialized. Here is an example of the drives checked for initialization (left image) and after the initialization sequence (right image), where the goniometer searches for the initialization positions and incrementally aligns to them. Note that these positions are not at integer degree values:
When a run is started, it takes some time before the data are plotted on the display screen because the Lynxeye detector starts below the requested start position and collects data until a sufficient number of channels have been measured for display. Do not cancel the run during this initial part of the scan, just wait for the data to appear.
It is possible to run the d8 from the Commander window directly by entering the run parameters into the fields on the lower right of the window. If you run a sample this way you will need to explicitly save the data to a file at the end of acquisition by using the File menu.
When your run is finished, the d8 is left at the current axis position. The d8 indicator light changes from blue to green and the red led lights on the X-ray tube are turned off. This means you can use the sample exchange procedure to run additional samples. You have about 10 minutes to do a sample exchange before the Commander automatically ramps the X-ray tube back down to standby conditions.
Please be sure to do the following at the end of your session.
You do not need to turn the Bruker d8 tube back to standby conditions, this is done automatically after 10 minutes, so please do not attempt to change the kV and mA values in the Commander window.
The Bruker Diffrac.Eva program is used for the evaluation and processing of xrd scan data, primarily for search-match identification of unknowns. The program is relatively easy to use, and has two manuals that are very helpful in learning how to do things.
Please note we are using Eva version 7 as of 8-2023. You will need to use the Eva manuals in some cases as there are improvements and differences in the interface.
There are two manuals for Eva:
The Diffrac.Eva manuals are also located here: Bruker PDF Manuals.
The Diffrac.Eva tutorial files are located on Bragg and Rietveld in the following location: C:\ProgramData\Bruker AXS\Tutorials\EVA. These are the .raw files that are referred to in the Eva tutorial manual.
After the search is complete the list of match results is displayed. The
The Bruker Topas program is used for advanced processing of xrd scan data, primarily for Rietveld refinement of xrd scans. The program is fairly advanced and requires time to master. There are three manuals that are very helpful in learning how to do things. There are also a number of papers, presentations and tutorials in the Drive D XRD Resources directory on the Rietveld computer
New! We now have Topas version 5 which has several nice improvements; see the Topas manuals for more information.
Here is a summary of the roles that Diffrac.Eva and Topas play in processing of powder diffraction data:
The Eva software is used for basic xrd pattern processing, including search-match and phase identification using the ICDD PDF5+ or COD database files. It has utilities for pattern display and simplified approaches to quantitative analysis, estimation of amorphous content, and compensation for variable unit cell parameters for visual comparision with an expermental powder xrd pattern. One uses Eva to identify a single phase material or all phases present in a multiphase mixture.
The Bruker Topas software is used for advanced powder xrd processing, including Rietveld refinement by whole pattern processing and least squares fitting of peaks defined by structure files to the observed xrd pattern. Assuming that a material has been identified by Eva, the Topas program is used to refine the cell parameters (dimensions and angles), particle size, strain parameters, site occupancies (and atomic positions for single phase refinements), amorphous component, and other parameters. For multiphase mixtures, quantitative analysis is performed using structure files for the known phases and the weight percent of each component in the crystalline fraction is determined by refinement. There are two modes used to run Topas, the GUI interface which is user friendly and can be used to do a lot, and the launch mode, which uses an .inp file and allows for more sophisticated applications. The .inp file contains Topas macros and one needs to be familiar with the Topas Technical Manual to understand the macro language structure. One does not use Topas to identify materials as there is no search match capability.
Processing with Topas includes the identification and fitting of diffraction peaks, assignment of hkl indices and cell refinement, identification of the space group, determination of the crystal structure, and utlimately Rietveld refinement of the structure and aspects of the powder. Corrections are made for the instrumental contribution to the shape of diffraction peaks, strain broadening, differential x-ray microabsorption (multiphase materials), preferred orientation, among others. For materials with unknown structures, the methods of simulated annealing and charge flipping are available to solve the structure. The program has been very successful in solving crystal structures using laboratory powder diffraction data as well as synchrotron data on very large protein crystals. The largest known unit cell (Mo2P2O4) was solved using single crystal data in Topas. Multiple data files can be simultaneously refined so that neutron and x-ray data can be used.
You will need to use several resources in order to confidently run the Topas software. There are pdf manuals for the Topas software that you can download, and also several Bruker powerpoint presentations that cover aspects of Topas refinement. I have also provided a basic step-by-step procedure which illustrates how to do a Topas Rietveld refinement.
There are three manuals for Topas version 5:
The following steps show how to do basic Topas Rietveld refinement of a powder xrd pattern.
Use File - Load Scan Files to navigate to your scan file and load it. You will load the .raw file, not the .brml file generated by the Bruker software. Very important, note that .raw file has no instrument settings. The range.def file in the Topas5 directory contains default settings for our Bruker d8 Advance. These settings include the goniometer radius (280 mm), the slits typically used (two Soller slits with 2.5 degree acceptance), and the LynxEyeXE detector parameters (3 degree acceptance).
The example file used here is for a quartz sample. If you are processing a file acquired on a different instrument, you will need to edit the instrumental parameters and save your Topas project so that those parameters are used in the refinement.
This window shows the default settings for refinement of XRD scans acquired on the WUSTL Bruker d8 Advance. These values are read from the range.def file in the Topas5 folder and assigned by default to all loaded scan data. The settings are as follows, listed top to bottom when the loaded XRD scan file is selected in the tree window:
The Emission Profile settings are used to specify the X-ray wavelength of the tube source. The WUSTL Bruker d8 uses a Cu X-ray tube and one can select from the default lamda file which has the wavelength values for Cu Kα1 and Kα2, or other lamda files that contain a more complete listing of the Cu Kα peak bundles. Note that we refine using the Cu Kα peaks in order to fit the doublet seen in the XRD scan.
This shows the background settings before refinement. After refinement, the fields will be populated with the parameters for the polynomial and 1/x parameters.
This shows the instrument parameters used for refinement. The WUSTL Bruker d8 has a goniometer radius of 280 mm, LynxEyeXE position sensitive detector with 3 degree acceptance angle, 2.5 degree Soller slits, and we use the Full axial model for instrument correction.
Always use Lorentz Polarization correction. For PSD with no monochromator use value of 0 fixed. If processing tutorial files with data acquired on a Bragg Brentano instrument with a monochromator, will need to use value specified in the tutorial.
Normally only a subset of the XRD scan range is used for refinement. This reduces the effect of poor counting statistics at higher angles on the refinement. Here you can set the range that is specifically used.
Refinement using Topas requires that you have atomic position data. The easiest procedure is to load this atomic position data into Topas using the Load STR command. Files with a .str extension are in the format required for Topas to read in and use. The latest version of the ICDD PDF5+ database utility on the Rietveld computer allows you to save ICDD card data from the File menu (File - Save PDF card, then select the Topas structure format from the file type pull-down menu). This .str file exported from the ICDD database can then be used to perform refinements.
Topas Structure .str files are located on Drive C in the Topas5 folder, Structure Database subfolder. These .str files have been exported from the PDF5+ program. The .str file is a text file having the Topas script language structure, and contains information such as the space group, cell dimensions, axial angles, cation and anion site xyz values, site occupancy, and other commands used in the Rietveld fitting procedure.
There is a dedicated User Structures folder that each research group should use to store .str files exported from the PDF5+ program. It is recommended that when you export a .str file, you add the phase name at the beginning of the file name and keep the ICDD card number so that you can easily identify the phase by inspection.
You can also use .cif files for Rietveld refinement. The Crystallography Open Database can be used to convert atomic position coordinates to Topas .str structure files. This has been done for Topas5 and the directory COD database for Topas contains COD structure files in the Topas .str format. Finally, if no .str file can be found, or if no ICDD structure data can be used to generate a Topas .str file, then you can use a Crystallography Information Format file with a .cif extension to perform Topas refinements. Note that there is some variation in .cif file formatting and one potential problem is that the cation and anion element symbols may not be read into Topas correctly and you will need to enter them in the sites field.
Right click on the pattern name or select Load STR from the command pane.
You may wish to compare the .str file with the grid window in Topas to see how the data is loaded into Topas for use in the refinement. The .str file contains data and keywords, but also has variable declaration (including use of the ! flag to inhibit refinement of that parameter), and constraints on the limits that a parameter may obtain during refinement (this can be seen for crystal size and cell axial size values).
Here is the display of quartz structure file parameters after the quart.str structure file was loaded. Again, parameters to be refined are shown in red. The cell axis values are to be refined and will also be assigned to the variables a_quartz and c_quartz. The crystal size has a nominal value of 1000 nm, is to be refined, and can range from a minimum of 32 nm to a maximum that has no limit. Note that if the crystal size L value was refined initially, then the refined value can be fixed; the size parameter can also be turned on and off with the "Use" checkbox.
Quartz unit cell parameters are as-loaded, red color indicates refinable quantity. Crystal size is default number and has minimum limit of 32 nm. Note variables used for cell paremeters (a_quartz, c_quartz, etc.) which can be used in Topas macro for reporting or other processing.
The refinement is initiated using the red play button, and typically you are given the choice of accepting or rejecting the refinement results. This is based on a visual inspection of the refined spectrum in case something goes wrong.
Option to accept refinement.
A 3rd order Chebychev polynomial was used, with 1/X bkg to treat increase in background intensity at low 2θ angles.
Most samples do not precisely fill the sample holder so that the sample is on the Roland circle of the goniometer. This excess or deficient sample z-axis location causes the XRD scan to shift to higher or lower 2θ values, respectively. The Sample displacement correction is enabled here and corrects for the offset residual during refinement. This value is in mm, so here the offset is 94 um deficient to the Z=0 reference surface.
Values for site positions x y z for quartz structure. The blue color indicates a special position that must be described using code =1/4 =2/3 etc.
Codes for site positions x y z for quartz structure. The position for Si4+ is special and set to exactly 2/3 using =2/3 code. Note variable names x1_quartz etc. here !x1_quartz means variable that is fixed (not being refined); removal of the ! mark makes that parameter refinable.
Quantitative analysis is the determination of the weight percent of phases in a multiphase sample.
The example used is the Bchips sample that is used for EVA search-match demonstrations, it is a mixture of calcite, dolomite, and quartz, with a minor amount of clinochlore (chlorite).
It is very important to understand the following:
Remember that quantitative analysis can be reduced to the following steps:
To do this, load a scan pattern as outlined previously, set the proper refinement parameters, and load an .str structure file for each phase that has been identified in the sample. You will use the Bruker EVA program to perform search-match and identify those phases, and you must do this before proceeding to using Topas for quantitative analysis.
Here is the EVA program with the Bchips .raw XRD scan loaded, and showing the results of the Search-Match procedure. The sample contains calcite, dolomite, quartz, and a minor contaminant of the chlorite mineral clinochlore. Note that the EVA match results are based on cards that may or may not have atomic coordinates. The clinochlore card initially matched does not have coordinates.
Now using the PDF5+ utility program: We search for the mineral "clinochlore" in the name field of the PDF5+ main window, and select a card that has peaks at the correct position (this is done by inspection of the synthetic pattern and the 2-theta peak listing on the card), and also has the required atomic coordinates as seen here using the Structure button on the left (cards with no atomic positions have no values when this data is viewed). The search results also has a column with a check mark to indicate which cards have atomic coordinates. We confirm this card is appropriate by loading it into EVA using the match by number selection on the left side and compare with the Bchips peak positions as we do for normal Search-Match procedures.
Here is the EVA Search-Match display for the Bchips XRD scan with card matches for calcite, dolomite, quartz. and the clinochlore card matched using SM on the pattern but which does not have atomic coordinates (and is unchecked here), and the clinocholore card found using name search in the PDF5+ program and loaded into EVA using the card number.
Once the correct card is identified in this way, we export it from the PDF5+ program using the Export drop down menu at the upper left of the card display and save it as a Topas *.str structure file.
This structure file should be saved to the User structures directory located on drive C:
C:\Topas5\Structures\User Structures\Your Group folder\Your folder.
Now launch the Topas Rietveld Refinement program. You will need to resize the program to look like this, which includes moving the boundary of the right pane to the left as shown, if you don't resize then you will not be able to see the refinement control button.
Refer back to the Topas instructions for general controls on the refinement setup.
Important Notes regarding refinement and quantitative analysis
Use File menu to load scan data, this will be the .raw scan file saved from a diffraction run. It is a good idea to unzoom the spectrum by right clicking in the scan display area and selecting unzoom. Remember that the refinement is context sensitive and if you are zoomed in on the spectrum, only that region will be refined.
Expand the tree for this scan file to show the controls (Corrections, Background etc.). Here the basic instrument and background settings are displayed.
Here the Corrections are displayed. In general you should refine the Sample Displacement Error because the powder sample is typically higher or lower than the surface of the sample holder. You should not in general refine the zero position as that has been accurately set for the instrument and it is more likely there is a sample displacement error. You may need to refine sample displacement initially and then set to fixed for refinements that are not converging properly.
Here Miscellaneous has been selected in order to restrict the scan range for refinement. In general, you should use the portion of scan range above low angle background curvature which has no diffraction peaks, and set the upper limit to avoid peaks that have comparatively poor counting statistics and are overlapped because these do not contribute to accurate refinement. Here the range has been set to 10 - 54 degrees.
Now load the .str files to be used for refinement. This is done by right clicking on the scan file name (here Bchips.raw with the blue square) and selecting Load STR (do not select Load Structure), or click on the scan file name to highlight and select Load STR from below the tree area. You can load multiple .str files by multiple selection in the dialog window or add them sequentially. Here the .str files for calcite, dolomite, and quartz have been loaded.
The Structures/HKL Phases folder allows you to select which phases to "use" in the refinement. You can also select the "use" checkbox for each phase. Here the calcite structure folder has been opened and the "use" switch, space group number (click on this to see the space group descriptors), the unit cell dimensions which are shown in red for refinable quantities (some structures do not have refinement turned on and should not be refined), and the "Scale" checkbox which will fit the intensity of peaks during refinement and should be turned on.
The Wt% Rietveld value will show the weight percent of the phase here and on the main scan window at far right. The unit cell mass and volume are known quantities and the refined values allow the calculation of weight % of the phase.
Click on the Microstructure button to open this window, which allows you to turn on refinement of Lorentzian particle size calculation and other paramenters (see the Topas Technical Manual for these topics). In general you should use the Lorentzian refinement to correct for particle size effects. If the refined peaks are sharp and narrow compared to the scan data peaks, then particle size refinement is necessary.
Here the Sites folder has been selected. This shows the crystallographically distinct sites, their coordinates in relative unit cell distance, the cation present under the Atom heading along with the valence, the occupancy, and thermal Beq value (see Topas Technical Manual for information on Beq). The use of the =0 and =1/4 is required to avoid roundoff error in unit cell coordinates and these are denoted as "special positions". Again, if a .cif file was used, check to be sure that the Atom entries have been populated; to change them click on the field and select the atom and valence from the popup menu that opens.
Samples that exhibit preferred orientation (acicular or platy materials) may have a peak that is higher than the calculated intensity from the refinement. Fitted intensities are expected to scale according to diffraction from randomly oriented particles. Structure files may include a declared HKL which is a likely reflection to exhibit higher intensity due to preferred orientation. The HKL values are for the peak in question, the "use" checkbox is used to turn the correction on and off, and the fix vs. refine keyword is used to refine or use a previously refined value. You will observe that the declared peak will be fitted independently during refinement with preferred orientation turned on.
With the .str structure files loaded and parameters checked, it is now time to refine the Bchips pattern. Do this by clicking on the red "play" button on the Topas controller at upper right. The "play" button refines to convergence and the "play until end" button refines to completion as determined by the user.
After refinement, a "Refinement Converged" dialog box is opened. The calculated spectrum is shown in red and compared to the blue XRD scan data. If selected for display, the residual is shown below as seen in this display, and can be used to determine the quality of the fit. If the fit is good, click on "Yes" to keep the refined results, but if the refinement did not converge, click on No to identify where the problem might be.
You can select the scan data to be displayed by selecting these items from the View menu.
To get a screen capture of the scan area with the phase wt%, right click in the scan window and click on the entry to copy a bitmap of the scan area to the clipboard.
The weight percent of each phase is displayed at the far right of the scan window. You can use the snipping tool to capture that display for pasting into Powerpoint etc. (there does not seem to be any other place where the phase weight percents are listed).
To view the calculated XRD fit for each phase, hover the mouse pointer over the phase name at the far right of the XRD scan display. This will show the calculated intensity for that phase only.
The following windows show the calculated spectra for calcite, dolomite, and quartz. To return to the main fitted display, click anywhere in the scan window.
It is possible to have several .str files loaded into Topas and use a subset of them. Select the Structures/HKL Phases to see a list of the structures currently loaded into the Topas project. The "use" checkbox allows you to select structures for refinement. Here the crystal size refinement is listed at the top, and the weight percent or amplitude scaling is shown at the bottom. This allows these two sets of parameters to be selected independantly.
It is important to understand that the structure file may not contain the full inventory of elements that are in the phases you are processing. For example, a scan on an ankerite (Mg,Fe,Mn dolomitic carbonate) nominally requires a structure file with the species Ca, Mg, Fe, and Mn listed in the file with their presence declared in the sites display. It is possible however, to refine using structure files for calcite, magnesite, siderite, and rhodochrosite to accomplish this. These structures would be fitted and the weight percent data used to calculate the composition of the natural sample being fitted.
For the Bchips example, it was shown in the EVA instructions how to sequentially perform Search-Match of the XRD scan. First the SM procedure was used to match the calcite, dolomite, and quartz peaks, and then those peaks were masked and the spectrum searched again in order to match the low angle peaks which allows the identification of the chlorite mineral clinochlore. Again, the identification of phases is done using EVA, but the quantitative analysis is done using Topas.
The low angle region of the Topas scan window shows that peaks are present from clinochlore. A .str file can be exported from the PDF5+ database by searching for cards with the phase name "clinochlore", selecting a card which has atomic coordinates, and exporting it as a Topas .str file.
Now the .str structure file for clinochlore has been added to the project, and inspected prior to fitting. It is selected for fitting with the "use" checkbox.
This is now the final refinement for the Bchips example, with calcite, dolomite, quartz, and clinochlore all fitted, and the results shown in the scan window. Note that the scan range for fitting avoids the concave down portion of the scan at low angles. The background model used must not overcorrect the background in the range from 10-18 degrees or the clinochlore concentration will be underestimated. The calculated paricle size for each phase is listed in the upper window, and the phase concentrations are shown at the far right of the main scan window.
A Topas project file contains the current XRD scan data, the structure files, and settings used for refinement. Once you have set up all these items, you should use File Save Project As to save the project. As you work on a project, save it periodically so that if the refinement blows up, you can reload the project and start over. Some divergences result in a situation that cannot be recovered from because multiple parameters have refined to bad values.
If you have additional XRD scans to process with the current project setup, then first save the project with a new name. To load the new XRD scan, select the scan name in the tree window (it has the blue square next to it), right click, and select Replace Scan Data, then navigate to the location of the .raw XRD scan and select it. You can immediately perform the refinement to the extent that all structures and refinement parameters are close enough for the new scan.
Refinement of multiple XRD scans. It is possible to load many XRD scans into the current project. However, you need to select one scan for refinement at a time, this is done by clicking on the colored square next to the scan file name to fill the square, and deselecting all the other scans. Otherwise you fit all scans at once and any variables that are duplicated will cause an error message. It is easier to use one project per scan and use Replace Scan Data to load a new XRD scan file.
Refinement of multiple XRD scans and combined data sets (synchrotron and lab-based diffraction data). The Topas documentation indicates that a refinement can be done on multiple data sets simultaneously. There is no example for this.
The Bruker d8 has excellent long-term calibration stability and has a guaranteed specification for both diffraction peak position and peak intensity using the NIST 1976a Corundum sample mount. It is not necessary to perform daily checks of calibration as we have done on the older Rigaku DMAX/A, so this step is optional.
If the calibration needs to be checked, use the following setup to perform a run using NIST 1976a.
NIST 1976a Calibration Check:
The Bruker has an extensive set of sensors and monitors all aspects of the safety interlocks, tube conditions, the water cooling circuit, and so on.
The most likely problem is an interruption of cooling water from the Haskris chiller system which is not an emergency condition.
Most problems that are detected by the Bruker will result in:
These sensors are used to shut down any system that has an error condition, so the system has built-in protection. For these reasons you should not have to take action under normal circumstances where the instrument has some problem regarding equipment parameters.
The following events require immediate action:
If there is a real emergency, do the following:
If there is water leaking from the braided vinyl tubing connected to the Bruker from the building water supply (this is from the Haskris chiller in the 4th floor penthouse) then you should do the following:
STOP. These instructions are only for rebooting the Bruker d8 hardware after a change has been sent to the diffractometer, it is not part of normal operating procedures.
Some Bruker settings are saved to the instrument and a reboot is required for those changes that affect hardware components. These instructions cover the reboot procedure. These steps are for users who have been authorized to reboot the d8.
Bruker d8 Reboot Procedure:
STOP. These instructions are only for turning the Bruker back on after a system shutdown.
If the Bruker has been complete turned off, the startup sequence is used to bring the unit back up to operating condition. These steps are for users who have been authorized to turn the system on or off.
Bruker d8 Cold Startup Sequence:
STOP. These instructions are only for shutting the Bruker completely off. We normally leave it turned on with the x-ray tube set to 20 kV and 5 mA. Do not use these instructions unless you have specifically been told to do so.
Bruker d8 Full Shutdown Sequence:
The Measurement Server application is started first and attempts to connect via ethernet to the Bruker d8. Once this connection is made, all subsequent actions are handled by the Measurement Suite software.
Here the Measurement Server window shows the configuration when the server has connected to the d8 Advance, and is currently idle with no active jobs.
On the Bragg control computer confirm that the Measurement Server is running and connected to the Bruker d8:
These are the Bruker supplied manuals for the d8 Advance, Diffrac.Measurement Suite operating software, Diffrac.Eva data processing software, Topas, and utility programs.
The following information covers the available instrumentation in the lab, and the computers that are used for data acquisition and data processing.
There are currently two XRD systems in the lab, the Rigaku and Bruker XRD instruments, and additionally the new XRD workstation. The scheduling of these resources is done as follows.
The Bragg PC computer is used for both data acquisition using the Bruker d8, and for processing of data. The main capabilities are listed below.
The Rietveld PC computer is a high performance PC with 16 gb RAM and high speed SATA6 hard drives. The main capabilities are listed below.
The Rietveld PC computer has a directory of resources for XRD users, located in the XRD Users directory on drive D. The materials are listed below and are available for you to copy; please do not move them from their folders.
These resources include journal papers, powerpoint presentations, tutorials, and other materials that are topically centered on Rietveld refinement using the Topas program. There is also information about XRD quantitative analysis and crystal structure determination. Be aware that these materials are being organized and may be reclassified as time goes on.
The Bruker d8 Advance is configured with the X-ray tube in line mode. This means the X-ray beam is 1" in y-axis and approximately 2 mm in x-axis direction, so that when the sample holder is rotated, a circular 1" area is irradiated by the X-ray beam.
We have several sample holder types for the Bruker d8, including powder sample holders provided by the lab, and thin-film sample holders which your research group will need to have made (Chemistry machine shop, Jim Linders, jlinders@wustl.edu). These are described as follows.
Please note that your research group will need to have these holders machined.
Thin-film sample holders (machined aluminum).
The Earth and Planetary Science Bruker d8 Advance is made available to selected members of the EPS department, Washington University, other non-profit organizations, and commercial clients. Users are permitted to use the instrument subject to the following requirements:
Please note that users are trained approximately once a month in group sessions only. Be prepared to spend approximately 3 hours in these training sessions and come prepared to use the software by reviewing the procedures in this web document including the Bruker pdf manuals. You will be asked to demonstrate your knowledge of these procedures and your ability to follow them during and after the training session. If you do not demonstrate adequate knowledge you will not be able to use the instrument.
Each research group has a "main user" that is the person responsible for helping new users by running samples during the period between training sessions. Contact Paul Carpenter to be added to the list for the next training session. You cannot be trained by another user.
In order to add you as a new user, Paul Carpenter needs the following information:
A current EHS training certification is required to use any laboratory at WUSTL.
Use of the EPS XRD lab is not authorized without a current certification and entry in the lab blue book.
If you have not taken the laboratory safety EHS training, go to the EHS web site and see the instructions for EHS training using the Learn@Work web site:
Environmental Health and Safety web site
Learn@Work web site
To obtain proof of your EHS on-line training, you can access your electronic information on the Learn@Work web site:
The XRD lab is available for use during normal weekdays from approximately 9am-5pm. It is also necessary for Paul Carpenter or a designated person to be available for supervision of your time in the lab. The lab is closed on weekends and holidays.
The building and hall require electronic key card access so that lab is not available on nights and weekends except to EPS personnel. Please remember this when scheduling time on the calendar. The XRD laboratory is kept locked because it is an environment where ionizing radiation is used. For routine users a key can be obtained for entry into the lab. Please use one key for your research group (let Carpenter know if you are a user in a new group that does not have a key).
Current fee structure established 2024 after no increase in rates since 2013.
Instrument Rate
|
Additional Operator as necessary |
Material use fee
|
|
| Earth, Environmental, and Planetary Sciences |
$36 |
$36 |
$20 |
| Washington University (non-EPS) | $36 |
$36 |
$20 |
| Other Universities and Non-profit Organizations (external) |
$48 |
$48 |
$25 |
| Commercial Users |
$102 |
$102 |
$30 |
The link below should allow you to access the XRD Resources folder on the WUSTL Box site. There is a large collection of powerpoint files, journal and other pdf documents, and video presentations on many aspects of X-ray powder diffraction analysis. There are also several XRD short course documents that can be used to improve your knowledge of XRD analysis. Enjoy!
Link to Box folder: WUSTL Box Folder: XRD Resources
This section summarizes the technique of Powder X-ray Diffraction and provides some links to further information, see also the reference list for more complete treatment.
Important points:
The technique is summarized as follows:
Here are links to information about Powder X-ray Diffraction and related topics.
There are general references to powder x-ray diffraction and more modern references which highlight the widespread use of Rietveld refinement in processing powder patterns.
All of these references are currently listed in the Washington University Library catalog. Here they are ordered by date.
The Bruker d8 X-ray Diffractometer is supported by NSF grant funds and user fees. Please include the following information in the acknowledgements section of published papers that use data acquired on this system. You can use the following statement:
Use of the Bruker d8 Advance X-ray diffractometer in Earth and Planetary Sciences at Washington University in St. Louis is supported by the National Science Foundation, award no. NSF EAR-1161543.
Use: In this lab, we work with an instrument that generates X-rays. Exposure to X-rays is harmful to you even though you can not see them or necessarily feel their effects. Our instrument has an annual radiation survey and the results are in the laboratory blue book for the current and past year surveys. The sheilding and safety interlock system permit us to work without the requirement of dosimetry badges. During normal operation, you will not be exposed to harmful levels of radiation.
It is important for you to follow the standard operating procedure and placards on the instrument during sample exchange. Failure to do so will result in you being banned from the laboratory.
As with any radiation source, you should limit exposure time and maximize shielding and distance from the X-ray source. Note that the exposure limits during pregnancy and for minors are much lower than for routine workers. It is therefore not recommended to use any x-ray source during pregnancy or to bring children into the lab. For information concerning typical exposure levels see http://www.new.ans.org/pi/resources/dosechart/
The main concerns for safety in this lab lie with sample preparation and with cleaning (see below). For sample prep, we work mainly with powders. Most of the powders used in this lab are harmless. If your samples are harmful, you need to take appropriate precautions in handling them to prevent contamination of the lab, bench tops, and instrument. Acetone and Ethanol are present in the lab for after-analysis clean-up. The instructions here are meant to supplement the University’s Chemical Hygiene and Safety Training. After this instruction, please sign the Bluebook for the Lab indicating that you have received the annual Lab training.
OSHA requires every laboratory to have laboratory-specific training and documentation.
The following procedures are useful for XRD information.
The MDI Mineral Program can be used to find information for minerals. Launch the program and either scroll down the list or enter the mineral name. This will load information about that mineral. A pictograph of the diffraction peaks is shown at the upper left; hover the mouse over this graph to determine the 2 theta position of peaks and the start and end values for a routine scan. The data also lists at least one ICDD card for this mineral, which you can use in Jade to force a comparison in the Search Match display. This program is a quick and easy utility to determine x-ray information.
The PDF5+ program is the front end utility that can be used to call ICDD card data from the ICDD database. We get the DDview+ utility with our subscription to the PDF5+ ICDD database. There is a help file that you can copy that covers routine proceduures with the DDview+ program. There are also web based tutorials on the ICDD web site that include DDview+ information, see http://www.icdd.com for more information.
Here are some short instructions for retrieving ICDD card information:
The X-ray Diffraction Lab is located here:
Scott Rudolph Hall, Environmental, Earth, and Planetary Sciences, Room 152
For information about visitor access and parking see: WUSTL Visitor Parking.
On the WUSTL parking map Rudolph Hall is building 105.
Here is the mailing address if you are sending samples:
Paul Carpenter
Rudolph Hall Room 110
Department of Environmental, Earth, and Planetary Sciences, CB1169
Washington University
1 Brookings Drive
St. Louis, MO. 63130-4899
Email (preferred): paulc@wustl.edu
Phone: (314) 935-2585
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Document last updated on by Paul Carpenter