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Before running the NIST standard, carefully remove the anti-air scatter screen. Failure to do this may result in a Be careful not to hit any of the limit switches within he XRD as this will cause error and possible collision of the motorized drives. The screen is only removed when running the corundum standard to allow a larger range of angles without any interference. The anti-air scatter screen should always be on when running samples. (Look at Review the video on Desktop/XRD_ICP Prep Documents/Bruker TRAINING VIDEOS to see this done before proceeding).

1. Make sure the Xray generator is off (Key on front is in off position and Red 'Xray is On' lights are off.
2. With two people, carefully remove the cover over the sample staging area, making sure not to hit any wires. The cover is not fastened to the base and will lift off directly.
3. Open D4 Tools and click "Online Status".
4. Click the computer icon to connect with the configuration files in the instrument.
5. Click "Positioning Drives" and "Sample Changer Y" direction.
6. Click "Go", enter "360", and hit "Enter". The sample changer will move in the Y-direction to position 360. This allows you to open the front door and remove to the XRD and gain access to the anti-air scatter screen.
7. Open the front door with a socket wrench (tools specific for the XRD are on the XRD Sample Area). Loosen the two bolts on the door and slide the bolts to their opposite side. Carefully let down the door.
8. Remove the anti-air scatter screen (Figure 33). Using an Allen wrench, unscrew the four screws holding up the anti-air scatter screen. These screws are very tiny and easy to drop inside the D4. Be very careful while unscrewing them. The screws are the main support for the screen, so hold onto the screen while removing the screws or else it can fall.
9. When the screws are removed, take off the screen without hitting the theta drives. If the theta drive is knocked, the instrument may signal a hard limit switch error.
10. Close the front door and use the socket wrench to slide the bolts back to their original position and tighten. Go back to the software and move the Y-drive back to Position 1. (Enter "1", "Go", and press "Enter".)

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Figure 33. Anti-air scatter screen in place inside the instrument (top image) and after being removed (btm image).

Scanning the NIST 1976 Standard and Verifying QA/QC, homing the axis inside the XRD.

Running the Scan

Run the scan as you would for a sample. With D4 Tools closed, open XRD Commander. Initialize the drives and click on the "Create Jobs" tab. Enter the sample position. The corundum standard does not have a text ID, so name it with an informative convention (e.g., Corundum NIST 1976 X342X396). Make the sure the name matches the name entered in the "Raw File" column. The parameter file, Corundum QAQC continuous 20 to 130.dql, is found at Local Disk C: >DIFFDAT1>DIFFDAT1_old computer pre March 2013>DIFFDAT1. Under the "Raw File" tab, set the path to the DATA>IN folder; this scan will not be uploaded to the LIMS database.

Click Start Start and wait for the scan to finish.

Processing the Scan

1. Open scan in EVA (remember the QAQC parameter file Corundum QAQC continuous 20 to 130.dql ran without the anti-air scatter screen).
2. Subtract the background (do not append, just simply close background menu) (Figure 2934).
3. 3 .Strip Kα₂ and Append (Figure 35).

Figure 2934: EVA diffractogram.
The arrow points to the Background Subtract tool.

3 .Strip Kα₂ and Append (Figure 30).

Figure 3035: EVA diffractogram with the background subtracted. (1) Dropdown Menu to Append Scan
(2) Strip Kα2 Tool 

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4. In the "Data Tree" panel there are two scans: Background Subtracted Scan and Kα2 Subtracted Scan (Figure 3136). For both of these scans, you will "Create Area" and "Append Area" for four angle ranges. This will insert area information as a subtree entry under that scan.

Figure 3136: Diffractogram with two scans in Data Tree panel. Top arrow points to the Background Subtracted scan. The bottom arrow points to the Kα2 scan 

5. Select the area around each peak as shown below in Figure 3237. Click on either scan so that it is highlighted (Figure 3237). Then click "Create Area" (Figure 32–237–2). A New window will pop up where you can enter the left angle and right angle (Figure 32–337–3, 3234-4).

Figure 3237: Create Area for Scan Angles. (1) Arrow points to scan name (2) Create Area tool (3) Left Angle entry field (4) Right Angle entry field

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6. After you enter in both angles click again on the left angle. This populates the rest of the fields. When all fields are populated, you can click on "Append Area" (Figure 3338). Do this for each of the following angle ranges for both scans:

• 25.576°2θ (24.7°–26.2°2θ)
• 35.149°2θ (34.0°–36.2°2θ)
• 88.993°2θ (88.1°–89.7°2θ)
• 126.8–129.0 (angle range is not necessary but recommended). 

Figure 3338: Create Area Window A. Append this Area button. 

7. Right-click on the "Area List #" subheader for background-subtracted scan and select "Create and Area Column View" (Figure 34). Do the same for the Kα₂ appended scan. This creates another tab on top with the Area data in column format.

Figure 3439: Data Tree panel Scan Area list. 

8. Open the QAQC corundum standard Equipment Verification 3.3.xls Excel spreadsheet.  QAQC Corundum std Equipment Verification X384.xls on the XRD computer. Figure 40.

Image AddedFigure 40: QAQC Verification Spreadsheet. Zeroing the goniometer.

9. Instructions provided by the vender can be found via the Instruction cell in the QAQC sheet. Enter your name and date and select "Vantec-1" for the detector .8(Figure 40A). Enter the following values into the spreadsheet (Figure 35, Figure 36)appropriate columns:

• For 2θ 2Theta Obs, use the Chord. Mid values from the Kα₂ appended scan areas (Figure 31–141–1)
• For I Obs, use Net Area from the background subtracted scan areas (Figure 32–142–1)
• For FWHM, use the FWHM from the Kα₂ appended scan areas (Figure 31–141–1)

Figure 3141: Kα₂ subtracted Scan Area column view. (1) Chord Mid value (2) FWHM value

Figure 3242: Background Subtracted scan area column view. (3) Net Area value

10. The QAQC verification spreadsheet has the calculations already embedded. 

11. Enter the XRD's Current Zi into the QAQC verification spreadsheet (Figure 40B). The current Vi value is found in the Configuration program on the desktop (icon Figure 43). Open Config program, Password is DIFFRAC. Click Motorized Drives > 2 Theta. Use the value under Zero Reference - Home of the Axis (Figure 44).

If the RED "ZI correction must be applied" shows upup (Figure 40C), you will need to open the Configuration and adjust enter the corrected Vi into the Config program. This will adjust the home position for the 2Theta drive. If there is no message just save the worksheet under a new name (Expedition) and no more action is needed. 

Apply ZI

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Correction to the XRD

 1. Open the Configuration Program on the desktop (Figure 3343). Password DIFFRAC.

Figure 3343. Configuration program icon

 2. In the left side panel navigate to Motorized Drives > 2Theta (Figure 3444). In this window go to Zero Reference - Home of the Axis. Enter the corrected ZI value from the excel spreadsheet into the 'Zero' space (Figure 3444).

Image Removed

Image AddedFigure 3444. Configuration 2Theta page

3. Select 'File' > 'Save and Download' or click on the red CNF arrow. 

DO NOT CHECK THE BOX FOR THE PSD CONTROLLER. Downloading the config file to the PSD Controller corrupts the Controller. For more information see the Troubleshooting section. Always backup the config.file on the server. With ONLY the 'Save Configuration' and 'Download Configuration to Diffractometer' boxes checked select 'OK' (Figure 3545). The new configuration will take a moment to download to the Diffractometer. 

Figure 3545. Save and Download Configuration page. Correct settings to save

Now that the scan is complete put the Anti Air Scatter Screen back on. Move the y drive to the 350 position and open the front door (instructions above Removing the Anti Air scatter Screen section). Line up the Screen with the screw holes. There is a small divet and you will feel the Screen settle into place when positioned correctly. Then carefully put on the screws. When the Screen is back in place close the door and put the cover back on the base. Turn the XRay generator back on with the Key on the front of the instrument.

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Health, Safety, and Environment

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If X-rays have not been turned on in longer than 24 hours (is this correct? I thought it was >120 hrs) you must turn on tube conditioning to avoid damaging the X-ray tube. In D4 Tools select the icon with the computer and plug. THis connects the program to the instrument. Click on the XRay generator green button on the status screen, this will show the screen in Figure 3646. Or Select "X-RAY" under the Instrument tree.  Then select Utilities -> X-Ray Utilities -> Tube Conditioning ON/OFF (Figure 36Figure46).

Figure 3646: D4 Tools X-ray subtree window. (A) X-ray subtree button (B) Utilities command (C) Standing kV and mA

Only click on tube conditioning on/off once. In the bottom right corner of the screen you should see a message 'Tube Conditioning On' (Figure 37).

Figure 3747: Tube Conditioning On Indicator

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A parameter file tells the D4 the conditions that a sample will run under. This is a DQL file made with the XRD Wizard program. The parameter file includes scan settings, scan parameters, generator settings, and beam optics. Some of these settings are constant because they are hardware features of our D4.
To start, double-click the XRD Wizard icon on the Desktop (Figure 3848).

Figure 3848. XRD Wizard Desktop Icon

An empty gray screen will open. There options on the top bar to either open a preexisting file or open a completely blank sheet. It is better to open and edit an old file and save it under a new name. Many settings are fixed, and editing a file reduces the chance of entering in a wrong value.
After a file (new or old) is opened, this first screen will open (Figure 3949). Change the "Operator" to your name and click "OK" at the bottom of the page. You can click "Update" to get the current date and time.

Figure 3949: First page of parameter file setup.

 The second page declares the detector and PSD electronic window (Figure 4050). These settings are PSD: VANTEC-1 and 3. Do not deviate from these values. Click "OK" and continue to Scan Settings.

Figure 4050: Detector declaration.

 Scan Settings includes Scan Type and Sample Rotation (Figure 4151). Scan Type should stay set to "Locked Coupled". This is a hardware setting indicating that the theta and 2theta positions move together. Under Sample Rotation, the Spinner can be set on or off. This spinner spins the sample while being scanned. This is typically on because it captures all potential angles of the sample giving a complete image of the material. Rotation Speed is set to 30 rpm and .5 rps (you only have to enter in one of these fields). Click "OK" and continue to scan parameters.

Figure 4151: Scan Settings parameter window.

Scan Parameters includes the scanned angle range, angle step size, number of steps, time per step, and delay time (Figure 4252). Adjust the angle range depending on the material and scientific objectives. For example, if looking for clays, set a low angle (3°–30°). The step size determines how much the goniometer will move before recording more data. The number of steps will adjust itself based the step size and angle range. Time/Step controls how long each step is measured. The Delay Time will add in an amount of time to wait before scanning the next sample. The machine does have limits on these settings and if something is entered outside of its range it will alert you. Click "OK" and move onto Generator Settings. At low angles (2–4°2theta) there is a very sharp peak. This is caused by beam overspill onto the sample holder and into the detector.

Figure 4252: Scan Parameters window.

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Generator Settings contains the X-Ray Tube Configuration and Generator Configuration (Figure 4353). The X-Ray Tube values are constant. You can adjust the kV and mA in the Generator Settings. The voltage is typically between 30 and 40 kV and the current is 40 mA. Lowering these values too far can reduce peak intensity. Click "OK" and continue to the Beam Optics window.

Figure 4353: Generator Settings window.

The Beam Optics settings lists the Divergence Slit and AntiScattering Slit (Figure 4454). Both of these are constant values based on our hardware setup. The Divergence Slit should be set to .300°. Click "OK" and you will have finished all the settings and will loop back to the first window.

Figure 4454: Beam Optics window.  

Save the file under a new name to the path Local Disk C: > DIFFDAT1 > DIFFDAT1_old computer pre March 2013. You can print this file by clicking the "Report" tab at the top the subtree window and then clicking the print icon. Occasionally scientists will ask for a printout of the settings to put in their reports.

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