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Figure 4. AC battery source inserted into pXRF
You
You can now turn on the gun. Press the power button on the top of the analyzer for a couple of seconds (Figure 5).
Figure 5. pXRF power button outlined in red. pXRF is off.
The button will illuminate green when on, as shown below in Figure 6.
Figure 5. pXRF power button outlined in red. pXRF is off. 
Figure 6. pXRF turned on
The following step is only applicable at this stage if controlling the pXRF through the computer. If choosing to use the pXRF alone move on to 'Discrete Samples'. The pXRF interface users will use the laptop during the 'Export Files' Section later on.
Open the dedicated pXRF laptop and login to the computer with the following:
user: XRFHost
Password: B113@iodp.
To operate the gun and have it correctly write files administrator privileges are needed. If you login with something different, such as 'daq' 'daq', there are no administrator privileges and the gun will not work properly.
Connect the pXRF to the computer via the micro USB cord (Figure 7). Micro USB ports are very fragile so take care when plugging in or removing.
Figure 7. pXRF connected to laptop via micro USB cable. A. micro USB port. B. Laptop usb port
Discrete Samples
Figure 8: FlexStand components. A. FlexStand Base B. Sample ChamberTo To set up the discrete sample station collect the FlexStand Base and shielded sample chamber (Figure 8).
Figure 8: FlexStand components. A. FlexStand Base B. Sample Chamber
2. Place the back of the analyzer into the indented portion of the FlexStand Base. The analyzer nose will point into the air as in Figure 9. Take note of the two indents in the analyzer nose.
Figure 9. pXRF in FlexStand base. Red arrow indicating two indents on analyzer nose 
nose
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3. On the Sample chamber there are two pegs and a release handle (Figure 10). The release handle controls the pegs.
Figure 10. Bottom of Sample Chamber. A. Two pegs B. Release handle
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4. The two pegs will fit into the two indents on the analyzer nozzle. Orient the sample chamber so the pegs will fit into the holes and lower the chamber over the nose (Figure 11). The pegs will snap in when inserted.
Figure 11. Sample Chamber resting over pXRF nose.
Note: The Olympus DELTA Flex Stand can be set up in a second orientation, with the instrument standing upright. This is not recommended on board, because the samples are more likely to rock with ship's motion and give inconsistent results.
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5. When it is time to remove the sample chamber pull the release handle and while holding the handle, lift off the sample chamber (Figure 12)
Figure 12. Release handle being pulled
Section Halves
In preparing for section half analysis, consider the safety requirements of the instrument. Prepare the area carefully, ensure everyone working with or around the instrument understands X-ray safety, and use the lead drape to protect from scattered X-rays. When the pXRF is in contact with a section half, most of the X-ray energy is absorbed by the sediment/rock. The scattered radiation is at a low (but measurable) level, so maintain reasonable distance between the pXRF and the user. Do not place your hands close to the nose of the instrument; keep them on the grip/trigger area or butt of the instrument.
Remember ALARA: keep your exposure As Low As is Reasonably Achievable.
Set up an aluminum core tray to hold the unwrapped section half (you will wrap it with Ultralene later, but GLAD® Plastic Wrap is thick enough to interfere with measurements. Place the core tray far enough back from the edge of the bench that the pXRF will be several feet away from the operator.- Put a long ruler next to the aluminum tray to measure the measurement offset.
- Place the docking station to the side of the core tray.
- Collect the rubber lead impregnated shield. When it is time to take a measurement the pXRF will lock in to the mat as shown in Figure 13.
Figure 13. pXRF being lowered into section half shielding. pXRF oriented with indents facing set screws.
Again, please note that it will be necessary to cover the core surface with Ultralene film and GLAD® Plastic Wrap in order to protect the nose of the instrument and the underside of the shield from contamination. See Preparing Section Halves, below.
Important! Do not measure the core section half without covering it with film!
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Sample Preparation
Sample preparation is split into two main categories: discrete samples and section halves.
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Once dry, samples are ground into a talc-like powder. Grinding is accomplished by three methods: agate mortar and pestle, SPEX Mixer/Mill®, or SPEX Shatterbox®. The specific grinding method used is dependent on sample hardness. For more details on grinding methods refer to the XRD User Guide and ICP Hard Rock Prep User Guide.
Loading Samples into an XRF Sample Cup
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- Powdered & dried sample
- Scoopula
- XRF sample cups (32 mm Double Open Ended)
- SPEX Ultralene thin film (0.16 mil; 4 µm thick)
- Whatman Filter Paper Circles (32mm) or Parafilm M® film
- Foam plug
Figure 14. Mortar and pestle along with scoopula. XRF Sample Cup components denoted with red arrows A. Open-end Ring B. Cup C. Cap D. Ultralene® film box E. Whatman Filter Paper F. Foam plug inserts
Foam plug inserts
- Figure 15. Ultralene® covering of one side of cup
A XRF Sample cup has three components: cup, ring, and cap. Take a piece of Ultralene® film and stretch it over one end of the cup. Place the open ring over the film and cup and snap it firmly onto the cup. This will create a tight window on one end of the sample cup (Figure 15). Ultralene® is very thin and prone to ripping. Check for rips before and after sample powder is added.
Figure 15. Ultralene® covering of one side of cup
2. Flip this unit upside down and begin to load the sample into the cup. Remember that the discrete sample will be back loaded. A couple centimeters of sample is sufficient. The sample layer cannot be too thin, or X-ray penetration (and the results) will be inconsistent. Make sure the powder is evenly dispersed, maintaining a relatively flat, even surface.
3. Next place a barrier layer on top of the powder, either Whatman Filter Paper or Parafilm. This creates a seal that prevents contamination and keeps powder secured in place. Take a piece of Whatman filter paper and put it on the powder or cut a square of parafilm, wrap it over the end of the foam plug and put inside the cup. Press down evenly until it is firmly on the powder.
4. Insert the foam plug. Take care not to insert it too quickly and cause air displacement that might disturb the powder. Depending on how much sample has been loaded into the sample cup; a couple centimeters of the foam may need to be chopped off.
5. Once you have filled the unit properly, place another piece of Ultralene® film across the back of the sample cup and snap the closed cap on the cup. If you have over-filled the sample cup, this is the point where the film will break, so examine both sides of the cup after you snap the lid on.
6. It is important to create some outward "bowing" of the film so that the powder stays well-packed and stationary. Cracks, gaps, or inconsistent filling of the powder will create inconsistent results. Be careful, however, not to pack too tightly or the Ultralene® film will break and you will have to start over.
Your finished product should look like the cup in Figure 16.
Figure 16. Properly filled XRF cup; note the slight bulge of the powder.Your finished product should look like the cup in Figure 16.
Put a sample label onto the cup. Remove excess Ultralene to help the label stick. The discrete sample is now ready for analysis.
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Important! Even a small amount of sediment on top of the thin film will be transferred to the pXRF, and will affect the measurement of the next core section half.
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Starting the Software
Note: Independent of sample type (discrete or section half) all samples follow the same procedures for taking and storing XRF data.
The computer interface and the pXRF interface are different. Follow the appropriate instructions.
Computer Interface
Getting Started
Figure 17. Innov-X software icon.Double-click the Innov-X Delta Advanced PC Software icon on the desktop (Figure 17) to launch the software.
Figure 1817. Innov-X Start-up Screen 
software icon.
The initial start-up window will appear (Figure 18, below); click the Import Data Only button. Import Data Only moves only the analytical data from the pXRF to the PC. If the pXRF was just turned on then wait a moment and select 'Close Device App' then continue with 'Import Data Only'. The PC Software will not let you continue on if the Device Application is active.
Figure 18. Innov-X Start-up Screen
Important! Do not click the Import to PC button!
The Import to PC button overwrites the saved method on the PC with the method stored on the pXRF unit. This is likely to be factory settings and not the methods needed for the analysis, so it is a very undesirable action.
Once the Import Data Only button has been clicked, the Start button will become active after a brief pause to sync the instrument with the software. Click Start. The login screen appears (Figure 19). Enter the following information:
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