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Your finished product should look like the cup in Figure 16.
Figure 16: Sample preparation steps for discrete XRF sample. Note the slight bulge of the sample when correctly filled.
7. Put a sample label onto the cup. Remove excess Ultralene® to help the label stick. The discrete sample is now ready for analysis.
Figure 16: Sample preparation steps for discrete XRF sample. Note the slight bulge of the sample when correctly filled.
Preparing Section Halves
Note: Ultralene® film is quite expensive (about $1 US/meter) and it is not practical to cover the entire length of each core section.
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The initial start-up window will appear (Figure 18, below); click . 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. Import Data Only moves only the analytical data from the pXRF to the PC.
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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Before any measurements are taken, a Cal Check needs to be performed. A Cal Check is an internal calibration check in which the analyzer measures a particular stainless steel alloy to ensure the unit is measuring properly. A calibration check is required when the gun is turned on and every 10 hours thereafter. The information bar indicates when a Cal Check is needed by displaying “Perform a Cal Check” as shown in Figure 20, arrow B, below. It is not possible to proceed until the check is done. Place the gun in its docking station.
Note: When using the Flex Stand, it is possible to perform the Cal Check by simply placing a stainless steel disk on the instrument nose and closing the lid of the Flex Stand. An extra stainless steel disk can be found in the pXRF supplies.
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In the Analysis Window, click the blue button with the three dots located in the upper left corner as shown by the B arrow in Figure 23.
Figure 23. Analysis screen closeup. Clicking . A. Current run number, B. Click on the blue "…" to enter test information (see Figure 24)
The measurement naming The measurement naming window will appear (Figure 24, below). Enter sample information here.
Figure 24. Test Information window. IODP-defined fields are circled in red (arrow A). B. Save button. C. Start button.
This window contains fields to identify the sample. Arrow A in Figure 24 highlights the IODP-defined editable fields, defined as follows:
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If you do not click 'Save', the sample information will revert back to values entered for the previous run and the new measurement will have the same name as the previous one. The measurements are parsed by time so measurements will not overwrite one another; however, there will be multiple measurements with the same information, and the data will have to be sorted out later.
The barcode scanner have has been programmed to properly parse the different kind of label for section halves and other types of samples. The fields should fill with the label ID (e.g., 366-U1498B-23R-3-W…) and text ID (e.g., PWDR8638211). If they are not working correctly reprogram the scanners by going to IODP_SHARE > XRF > Barcode Rules and scan the rule set.
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- Locate the area on the section half to be measured. Make sure that section portion has a layer of Ultralene Ultralene® on it. Put a layer of glad GLAD® wrap on the rest of the core that the lead shield might touch. We do not want to contaminate the core or pXRF.
- Place the shield over the core so the point of measurement is centered. Use the plexiglass view-finder to help find this spot.
- Take note of the measurement position on the core using the ruler. Lower the pXRF into the shielding oriented so the two indents on the analyzer are on the same side as the tightening screws.
- Tighten the screws until it feels firm. This locks the pXRF into place and helps stabilize it. Keep a hand on the handle while measuring to ensure it does not fall.
Starting a Measurement
If the minimum time has been set to the same number as the maximum time for each beam setting (see Setting Parameters, above), the run time will be exactly what was set. If the minimum time is smaller than the maximum time, the pXRF may stop the measurement early, if the quality of the measurement satisfies its internal quality criteria. (These criteria cannot be adjusted by the end user.)
Important! Record each measurement taken on the paper log sheets provided by the technician. The log sheet will be a life-saver later in the expedition.
PC Interface
Press Press the green Start button located on the bottom left of the screen as shown in Figure 29 (arrow D), below. The measurement can be started in either the Test Information (Figure 24) or Analysis window .
(Figure 29).
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The spectral graph and elemental concentrations will populate after each beam has completed measuring.
Figure 29. Analysis window: Test completed. A. Current run number, B. To enter test information (see Figure 10), C. Test completed, D. Start Button to start next measurement
pXRF Interface
Navigate to the Test screen (Figure 30). Start the test by pulling the trigger or tapping the Start Test button. 
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Results are exported to a C:\Data > \IN Folder and then uploaded to the LORE database via Mega Uploader Tron , (or MUT). pXRF interface Users follow instructions on connecting the gun to the laptop. PC Users jump ahead to 'Exporting Results'.
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To export a file, click Set Up on the top right corner of the screen. Click Data Management located on the left hand panel as shown in Figure 32, arrow B.
Figure 32. Accessing the Data Management Screen. A. Set Up tab B. Data Management Button
Once the Data Management screen appears, files can then be exported. The results are organized by date in the window on the right hand-panel as shown in Figure 2632. Select the date-referenced file you wish to upload. Make sure the Data or Spectra button is selected (designated by the presence of a check mark; in Figure 3032, above, the Data button is selected).
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Export a data file and a spectra file for each file. It is important that the filename be the same for both files. Follow For example, follow this naming convention: ExportData-MM-DD-YYYY.extension, examples shown here:
- Data File: ExportData- 07-23-2017.csv
- Spectra File: ExportData- 07-23-2017.spm
Note: Data files will default to ExportData-07-23-2017.csv and Spectra files will defult default to (ExportSpm ExportSpm-07-23-2017.csv) in . In order for MUT to be able to upload data the Spectra file extension needs to be changed to (ExsportData-07-23-2017.spm) before like with the extension .spm (like shown above) before the file is exported in order to match the exported .csv file . Figure 33 section D. (i.e., the Data File).
Other file types are possible, but are not our normal procedure; talk to the technician if you need a different file type.
Once you have selected the type and set the file name, make sure the values are correct as shown in Figure 33.
Figure 33. Exporting a file. A. List of all stored files. B. Data or Spectra selection C. Pathway where exported data goes D. Filename E. Export button
In Figure 33, A indicates the date-referenced data files. These can be exported one by one, or multi-selected. (Or, click Select All to highlight and export all of the files, but this will be difficult to sort out.)
Arrow C indicates the destination path. This should always be set to C:\DATA\IN\. Arrow D is the filename; make sure it matches the file format defined above.
Once the data type (we suggest always starting with Data to help prevent mistakes) is selected, the date-referenced results are selected, the path set, and the filename assigned, click Export. Repeat the process for the Spectra file, again making sure the filename is the same as the Data file. The active file type has the red check mark.
After the files have been exported the measurements are attached to the file. Multiple exports can be done in the same day; however, the measurements will still be written to the same date file. The measurements are appended to the same date file, not overwritten.
Example: 10 measurements are exported at 11:00 on 03-15-2017. Then 5 new measurements are taken and exported at 15:00 on 03-15-2017. The 03-15-2017 file now has 15 measurements that are exported in spite of 10 measurements being exported earlier in the day. This may cause duplicate records to be uploaded to the LIMS database; see a technician if this occurs.
Uploading Files to LIMS
This step is done by the technician.
Open MegaUploadaTron (MUT). If the file(s) are not yet in the DATA > IN; transfer them now. MUT requires two file types per uploaded file: '.csv' and '.spm'. The filenames must be identical for MUT to recognize the two as linked and MUT will not allow an upload unless both files are present.
Check the boxes for the files to be uploaded. The Misc column identifies files that have not been uploaded as shown in Figure 34.
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The pXRF has a feature to apply linear regressions for elements, quantifying data as it is measured. It is NOT recommended for use. Data Quantification should be done outside of the software by the scientists. Please note that this feature can provide erratic results and not detect elements that are present.
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