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***IMPORTANT*** Select 'LiveTime" for Test End section (Figure 22D). Not selecting 'LiveTime' will not complete spectrum measurements properly.

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Figure 22. Innov-X Set Up Screen. A. Set Up tab B. Test Condition button C. Test Time area D. Test End section E. Save button

The behavior of the Test Time settings is as follows. If the minimum time is set to 1 s and the maximum time is set to 30 s (as shown in Figure 22, arrow C), the pXRF will scan until it determines that it has a good profile (via manufacturer-defined quality conditions) and stop measuring before it gets to 30 s. However, even if the pXRF has not reached a "good profile," it will stop at the maximum time.
If the user wants to ensure the pXRF measures for the same time on each measurement, set the minimum and maximum time to the same number (e.g., Beam 1 Min = 30, Beam 1 Max = 30). We do not recommend measurement times below 30 seconds, and longer times may be necessary to get good resolution of weak lines.

Naming the Sample for Measurement

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. A. Current run number, B. Click on the blue "…" to enter test information (see Figure 24)

The measurement naming window will appear (Figure Fig. 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:

• Run Number: A sequential number increased by +1 with every measurement, ex: 1, 2, 3… This number should start at 1 for the first measurement of the expedition. This should be unique throughout the expedition, so the use of a logsheet is highly recommended.
• Sample Name: Sample name according to the sample or section half label. Ex: 366-U1234A-20F1-W.
• Text ID: Unique database identifier for each sample or section half located under the barcode on the label. Ex: SHLF8638181
• Offset for SHLF: The point where a measurement was taken, measured as distance from the top of the section. Leave this field blank for discrete samples. Note: Be sure to enter one single number, not a range. (Example:  Wrong 100-101, Correct: 100.5)
• Comment: A brief description of the measurement. An optional field.

First enter the run number manually. Then put the cursor in the 'Sample Name' field and scan the label with a barcode scanner. This will populate the 'Sample Name' and 'Text ID' fields. If measuring a section half enter the offset in 'Offset for SHLF'; leave this field blank for discrete measurements.

Important! Click Save in the lower right portion of the screen (Fig. 24, arrow B).

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 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.

If the user needs additional fields to describe the sample or the measurements being done, the technician can modify the method to enable up to 11 additional user-defined fields. To see how to add fields refer to the section 'How to Add Fields to Sample Information Window'.

pXRF User Interface

The pXRF User Interface allows you to perform analysis controlled directly from the gundevice. This is NOT recommended.

The DELTA's user interface starts with the start-up radiation safety and initialization screens (Figure Fig. 25). Read the radiation safety notice screen, and then confirm that you are a certified user.

Figure 25. Start-up Radiation safety and initialization screens. 

System initialization begins immediately after confirmation (Figure Fig. 26). The analyzer launches a test screen using the previously selected mode.

 Figure 26. Initialization and test screens.

Performing a Cal Check

Before sample testing can begin, a Cal Check needs to be performed. This will be shown by a "Cal Check Required" message located on the bottom left of the screen. A Cal Check measurement tells the gun device to measure the stainless steel disk located in the stand. This is an internal calibration which ensures the gun device is measuring properly.
Note: Cal Checks must be performed when the analyzer requests the procedure (once when the program is started, and once after every ten hours of testing). The Start Test button and trigger are disabled until a successful Cal Check is achieved. The Cal Check can be run any time during software operation, except during a test. When the Cal Check is in progress, the X-ray indicator light assembly blinks. This indicates that the X-ray tube is energized.

To perform a manual Cal Check: Place the analyzer it the DELTA docking station. Tap the Cal Check button.
Note: The deadman trigger are overridden when the analyzer is mounted in the docking station. If necessary, unlock the software trigger lock by tapping the Lock button at the top of the screen.
If the "Cal Check – Passed" message appears on the Results screen, the analyzer is ready for sample testing. If the Cal Check refer to the 'CalCheck fails' section in 'Troubleshooting'.

Setting Parameters

Tap the Home button  . You are now in the main measurement window. First set the Mode in which you'd like to measure in. The gun device has a Geochemical and Soil Mode. Each one has different scanning parameters which preferentially pick up some elements better than others. The gun device will remember the chosen mode and does not have to be chosen each time a new measurement is taken or the Gun device is turned off/on.

To access the Modes click on 'Mode' button  . This directs you to the 'Mode' Screen where you can choose between the Geochemistry and Soil modes (Figure Fig. 27). Click on each to see it's corresponding features and select the one best for your analysis.

Figure 27. Mode Screen (Mining Plus corresponds to Geochemistry mode).

Now that the Mode is set, establish the measuring time for each beam. Each Mode has preset measuring times but these are changeable. To access the Measurement Time, in the Mode Setup screen click on 'Test Condition.'
 In the Test Conditions screen, tap the Test/Tools button  . This brings you to the Test Setup screen (Figure Fig. 28). Enter the Minimum and Maximum time currently set for each beam (Figure Fig. 28). Adjust the settings to your liking and click 'Save'.

Figure 28. Test Setup screen.

Note: If the minimum time is set to 1 and the maximum to 30, if the gun device determines it has a good profile in less than 30 seconds it will stop actively measuring. If you want to ensure it measures for the full time, set the minimum and maximum time to the same number. Ex: Minimum 30s and Maximum 30s

Naming a Measurement

Staying in the Test Setup screen, tap the Label Defaults button located in the bottom left corner.  

This is where you can manually input sample information. Editable fields are as follows: Run Number, Sample Name, Text ID, SHLF Offset, and Comment (optional field).
Run Number: A sequential number increased by +1 with every measurement, ex: 1, 2, 3… This number will start at 1 for the measurement of the expedition.
Sample Name: Sample Name according to the sample or section half label. Ex: 366-U1234A-20F1-W
Text ID: Unique 11 digit ID for each sample or section half located under the barcode on the label.
Offset for SHLF: The point where a measurement is made on a section half, measured as distance from the top of the section. This field will only have a value for section half measurements.
Comment: A brief description of the measurement. An optional field.
Click 'Save' in the lower right portion of the screen. If you do not click save the information will revert back to the prior run and there will be two measurements with the same name. The measurements are parsed by time so measurements will not overwrite one another there will just be multiple measurements with the same information.

Preparing the Sample for Measurement

Discrete Measurement

1. Open the mount door. The measurement window should lay flush with the bottom interior of the sample chamber.
2. Insert the discrete sample oriented face down towards the X-ray beam. ALWAYS make sure only smooth, flat surfaces go on the X-ray window. The pXRF has a very thin Prolene window that can be easily torn and is the only barrier between the beryllium window and the sample. If the window becomes torn stop measuring immediately and replace the window. The Beryllium window is very fragile and brittle, any particles coming into contact with it can ruin the window and make the pXRF unable to measure accurately.
3. Close the mount door, and make sure the shielded mount is firmly and safely attached to the analyzer. The discrete sample is ready to be analyzed.

Warning! NEVER activate the X-ray source when the Flex Stand door is open! The Sample Chamber door does not have a safety trigger and the pXRF will continue to emit X-Rays if the door is open.

Section Half Measurement

1. Locate the area on the section half to be measured. If measuring sediment, make sure that section portion has a layer of Ultralene® film on it. Put a layer of GLAD® wrap on the rest of the core that the lead shield might touch. We do not want to contaminate the core or pXRF. If hard rock, make sure that the section is dry and perfectly cleaned before measuring (a Ultralene® film may not be necessary).
2. Place the shield over the core so the point of measurement is centered. Use the plexiglass view-finder to help find this spot.
3. 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.
4. 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 the green Start button located on the bottom left of the screen as shown in Figure Fig. 29 (arrow D), below. The measurement can be started in either the Test Information (Figure Fig. 24) or Analysis window (Figure Fig. 29). 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 (

Fig. 30). Start the test by pulling the trigger or tapping the Start Test button Image Modified.

Figure 30. Start and mid-way through an active test.

The results are displayed immediately upon test completion. Tap the Spectral Plot button to view the spectrum results (

Fig.31). Make sure each measurement has its own spectrum results. If results are being averaged the spectrum graph will appear blank.

Image Removed

Image AddedFigure 31. Completed test and results. Results shown as both a list and as a spectrum. 

Processing Sample Results

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 device to the laptop. PC Users jump ahead to 'Exporting Results'.

pXRF Interface

If using the pXRF interface at this point the laptop needs to be turned on and logged in as pXRF host. Then connect the gun device to the computer using the micro-USB cable. Open the software icon. Click on the 'Import Data Only' Button. This allows data storage on the computer. Do NOT click 'Import to PC' as this removes all configurations from the gundevice. Then login with:
Username: innovx
Password: 1776

Exporting Results – All Users

The gun device writes one file per day that contains all the measurements taken in that 24-hour period. Until that file is exported the measurements are not permanently attached to the file.
Important! If files have not been exported DO NOT disconnect the gundevice, turn off the software, or turn off the gundevice; otherwise those un-exported measurements will be lost. For this reason, be sure to keep an eye on remaining battery life (or use the AC power adapter to provide continuous power to the pXRF).

If running from the computer and communication error occurs FIRST export data and then restart system to clear errors. So long as the gun device is not unpluged and the data is NOT imported on start up the data should remain/ stored locally. If data is imported when software is restarted the data will be over written and lost, that is why it is best to export both .csv and spm files before clearing errors.

To export a file, click Set Up on the top right corner of the screen (Fig. 29). Click Data Management located on the left hand panel as shown in Figure 32, arrow B.

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Figure 32. Accessing the Data Management Screen. A. Set Up tab B. Data Management Button

Once .

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 32, arrow A. 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 32, aboveat arrow B, the Data button is selected).

• Data: reduced data will be exported; extension is .csv.
• Spectra: raw data and metadata will be exported; extension is .spm.

Export a data file and a spectra file for each file. It is important that the filename be the same for both files. For example, follow this naming convention: MM-DD-YYYY.extension, examples shown here:

• Data File: 07-23-2017.csv
• Spectra File: 07-23-2017.spm

Note 1: Data files will default to ExportData-07-23-2017.csv and Spectra files will default to ExportSpm-07-23-2017.csv. In order for MUT to be able to upload data, the Spectra file extension needs to be changed like with the extension .spm (like shown above) before the file is exported in order to match the exported .csv file (i.e., the Data File).

Note 2: There is a maximum limit of data saved in the .spm file. A maximum of 129 128 runs can be saved. It does not seem to be a maximum number of runs saved for the .csv file.

Other file types are possible, but are not our normal procedure; talk to the technician if you need a different file type.

Figure 3332. 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 3332, 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, but with the .spm file extension. 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 (recommended); however, the measurements will still be written to the same date file. A  pop-up window will ask you to 'overwrite' the already existing file. Click , click 'YES'. The measurements are appended to the same date file, not overwritten.. If you are unsure if you are overwriting previous samples from earlier in the day (if you weren't the first user of the day, but you selected 'Import Data Only'), add your initials to the file name to save. 

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 X-Ray Lab technician.
Open MegaUploadaTron (MUT). If the file(s) are not yet in the DATA > IN folder; 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. If the files are not listed in MUT, it is possible that one Excel file is open. Close all Excel files if the case.
Check the boxes for the files to be uploaded. The Misc column identifies files that have not been uploaded as shown in Figure 3433.

Figure 3433. MUT XRF Uploader.

Click Upload in the bottom right of the window. This brings up the pXRF Pre-upload Form as shown below in Figure 3534. This form lists all measurements and allows files to be edited. The fields in white are editable: Run Number, Sample Name, TextID, Offset for SHLF, and Comment. Measurements can also be checked or unchecked to upload or not upload to LIMS. Cross check measurements with the log sheets and make edits as necessary.

Figure 3534. MUT pXRF Pre-Upload Form. A indicates the selection boxes. B. Editable fields

Keep a close eye out for duplicate lines. It is easy to inadvertently create multiple measurements with the same name, if the Save button isn't pressed when identifying the sample (see Naming the Sample for Measurement, above).
If any changes need to be made to the editable fields or if scientists require a different file type, from the MUT main screen, click Options > Set active analyses… to open the Configure Active Analyses window as shown in Figure 3635. Follow the prompts in the window and select Handheld X-Ray Fluorescence Analysis to see the configurable options. The option wheel icon will only appear when the analysis type is on the Active uploaders side and is highlighted.

Figure 3635. Configure Active Analyses screen (pXRF shown active).
 

Once the wheel is clicked, the window in Figure 37 appears36 appears.

Figure 3736. MUT Settings for pXRF Analysis.

These settings determine what MUT is searching for to validate the data before upload. These values are editable, but it is strongly recommended to have a developer assist you with this. If other labels (see Naming the Sample for Measurement, above) are enabled in the Olympus Innov-X software, those columns can be added here. Add the column name to the EditableColumns value exactly as it appears in the Innov-X menu.

Quality Assurance/Quality Control

This measurement is highly affected by surface conditions, the heterogeneity of the sample, the size of the features in a heterogeneous sample, and the quality of the instrument-sample connection. Even a slight tilt of the instrument, for example, may have a significant effect on data quality.
It is highly recommended for the scientist to develop a quality control plan, to measure known standards for discrete samples (see Measuring Accuracy for Discrete Samples below). This is not possible for section half measurements; the user cannot judge accuracy of the elemental chemistry on section halves—only precision by measuring some of the positions more than once. (Be sure to label deliberate duplicates carefully!)
When measuring discrete samples for quantitative elemental chemistry, it is important to follow good laboratory practices: bracket the elements of interest (wherever possible) by the standards, ensure that samples are uniformly made (so that packing density is not an issue), etc.
When measuring section halves, unfortunately, the instrument cannot make quantitative measurements without significant post-pXRF work. In general terms, this means taking a representative number of discrete samples for each lithology, measuring them by another method like ICP-AES, and then calibrating the pXRF data for that lithology. Differences in moisture content, porosity, composition, surface smoothness (for good contact for the pXRF) will all have an impact—often a strong impact—on the quality of the results.
That being said, the power of pXRF for qualitative measurements of sediment and hard rock is very great (presuming heterogeneity is accounted for). A technique of evaluating elemental peak ratios can help to normalize results (but not quantify) for variances in physical properties, for example, and downhole trending can be displayed (similar to XRF Core Scanner results).

Measuring Accuracy for Discrete Samples

It is not straightforward to determine accuracy for section halves, so this section applies to discrete samples. Calibration curves can be created by measuring powdered rock and sediment reference materials whose elemental responses bracket the samples.
Properly calibrated energy-dispersive XRF results, on homogenized and consistently-packed samples (or pressed pellets or flux fusion beads), can be expected to produce results of similar data quality to that of ICP-AES. (The detection limits are quite different, of course.)
It is recommended to measure some of the standard reference materials as unknowns during the analytical process in order to characterize the accuracy of the method. If all of the variables are properly controlled, accuracy of ±5% or better should be achievable.

Available pXRF cups with standard reference materials for calibration curve are:

Write the list here of rock standards used for X391

BE-N, BCS-CRM-368, BCS-CRM-393, LKSD-1, LKSD-4, JR-1, RGM-1, JB-2, JP-1, DTS-1, BIR-1, OKUM, NKT-1, JA-1, JA-2, DTS-2b, MRG-1, SO-3, Nod A-1, AGV-1, JB-3, DNC-1, JG-1a, CGL-001, UB-N. The mounted pXRF standards are located in a drawer in the Phys Props area of the Core Lab.

QAQC STANDARDS: Scientists should regularly measure pXRF standards for measurement accuracy during the day. Two flagged standards are available: BHVO-2 (Basalt, Hawaiian Volcanic) and BCR-2 (Basalt, Columbia River) (Fig. 37). More information on QA/QC can be found at /wiki/spaces/LN/pages/7338176581. 7338176581.

Image AddedFigure 37. QAQC Rock Standards used for pXRF data accuracy: BHVO-2 and BCR-2

Please use the following Text_ID when measuring the standards for QA/QC to see in QCViewer:

BHVO2 : OTHR10999061 (QAQC XRAYPXRF pXRF_BHVO 2)

BCR-2 : OTHR10999071 (QAQC XRAYPXRF pXRF_BCR 2)

QCViewer can be found at: http://ship.iodp.tamu.edu/QCViewer/#/qcviewer

Measuring Precision

Precision measurements are quite straightforward for pXRF for both discrete samples, but for section halves there are complications that must be discussed.

Discrete Samples

Discrete sample precision is expected to be quite high, with percent differences <1% for replicate measurements of either samples or standards. Differences higher than that may represent non-homogenous packing of sample cups.

Section Halves

If the pXRF is not moved between measurements, precision will be very high (similar to that for discrete samples). However, if the pXRF if moved and is not placed in the exact same spot as the previous measurement, the precision is likely to be significantly lower, depending on the characteristics of the core section in question.
It may be quite useful, therefore, for the user to make such measurements, attempting to place the pXRF back in the same place, in order to define some of the limits of the precision of the measurement.

Maintenance and Troubleshooting

Maintenance

It is important to keep the pXRF clean and if the Prolene® window becomes dirty (or breaks), it should be replaced immediately. For instructions on how to replace the Prolene® Window please refer to the Olympus 'DELTA_Family--User—International' User Manual found on the laptop.
Keep the batteries away from extreme temperatures, and talk to the ET's about the best way to promote long battery life.  
Mini-USB ports are very easy to damage, so take care to protect it against force from the side (i.e., pulling the cable sideways).  The cables are somewhat easy to damage, but the biggest concern is the port itself.  Use a zip tie to secure the cable to the handle of the gun device to prevent it from moving.

Delete Files from Software

In the Set Up > Data Management area select the box next to 'Delete'. Then select the files to be deleted. A blue 'Delete' button will appear at the bottom of the screen. Click the 'delete' button. Restart the software to see be removed.

Replace Ultralene Window

It is critical during the process to keep the surrounding area and analyzer clean. Do not touch any internal components or allow anything inside the analyzer.

1. Turn off the analyzer and make sure the surrounding area is clean.
2. Collect a Prolene® Measurement window from the bin labeled 'XRF Supplies'device briefcase, a small Phillips head screwdriver, and a box of KimWipes
3. Orient the analyzer so the nose is pointing sideways. This will help minimize the likelihood of anything falling into the analyzer.
4. Remove the two screws on the plate using the Philipps Phillips Head screwdriver (Figure Fig. 38)

Figure 38. XRF nozzle showing ultralene window replacement

5. Swing the face plate outward. The film window is now exposed.

6. Remove the damaged window.

7. Take the new window, grabbing it by the edges, and place it on the plate. Orient the window so the backside (side fully covered with film) facing upward.

8. Double check the white window spacer and black rubber gasket are seated properly, and then rotate the hinged plate upwards.

9. Insert the screws and tighten until snug.

Directions and images for this section were provided by Olympus Delta Family User Manual. For more details on this procedure please refer to the 'DELTA_Family—User—International Guide'.

Add User Defined Fields

1. Go to 'Setup' tab at the top and then 'Result Test Info' in the left panel.
2. Select 'Customize..'
3. Labels with the Red Check are enabled. Select the 'enable' box next to the next Test label number.
4. On the right side select the appropriate test label number from the dropdown.
5. Define the 'style' from the next dropdown as 'text', 'fixed list', 'auto incrementing order'.
6. Give the test label a name.

The label is now created and it has to be setup for being exported.

1. In the left panel go to 'Data Management'
2. Select 'Customize' underneath the Data and Spectra boxes.
3. Under the 'Fields' panel select the test label number you just made from the 'Not Exported' panel. Then click the left pointing arrow to move it into the exported field.
4. Click the 'Up' button to move the label into position. The vertical order transposes left to right in the .csv and lore report.
5. Click 'Save' at the bottom of the screen.

User Factor

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.

All data from the handheld pXRF should be considered qualitative (like the big XRF Core Scanners back on shore at the GCR) unless the scientists do the HUGE amount of work to measure representative materials, a representative sample of the samples (see Note 2 below), adjust for differentials in moisture content, etc. In other words, the standards are powders mounted in the XRF cups, while the section halves or TSBs are not in that form. The XRF data get from each of those (powder mounts, section halves, and TSB) are all going to be different and have different concentration-to-count ratios.

Note 1: we prefer uploading the data without any correction factors (slope, intercept) included because there’s no easy way to export that information from the gun device and then upload and/or qualify the LIMS data with those factors. This especially applies to section halves and/or discrete samples (e.g., CUBE or TSB samples). See Note 3 below about powdered samples and powder mounts.

Note 2: grain size/spot size is a big issue for the pXRF because the spot size is 8 mm (or 10 mm) for our gundevice.

Note 3: If you take the time to create powders so that the samples and standards are in the same form factor and are prepared the same way, then you can run the standards, determine the slope/intercept values to correct the inherent instrument calibration to your sample set, enter those into the gun device software, and then produce quantitative data from the powder samples. This requires a good hand at creating the XRF cups so they’re (a) consistently full (you want at least 1 cm of powder to be “infinite” depth for the X-rays), (b) consistently made, and (c) don’t have air gaps. Once you have the cups filled, you measure them using the test stand (samples upside down on the instrument nose and inside the shielded cover) and you can get quantified data.
Note 3 *only* works when you’re comparing like to like. You should *not* attempt to use powdered standards to quantify non-powdered samples.

Troubleshooting

Indicator Bar shows a 'CommError'

This indicates a Communication Error between the pXRF and the computer. If this error shows up at the initial startup window, close and restart the software. The gun device must be connected via the micro-USB cable before turning on the software. If this error shows up while the software is already open, close and restart the software. In this instance the connection between the analyzer and computer was broken, either through the cable being unplugged or the Gun device turned off. 

Do not click 'Import Data Only' when you restartre-open the software without turning off the computer and the pXRF device. Click 'Start' directly. The data will be lost otherwise (overwritten if the file name is not changed). See "Computer Interface" above.

Files are missing from the Data Management Panel

This could be a range of issues:

1. (Most Likely) Connection between the analyzer and computer was broken before files were exported. If a file is not exported before the communication is broken, either intentionally or unintentionally, the measurements are not saved.
2. The memory card on the XRF Gun device was too full and the gun device started deleting files
3. The software versions on the PC and the analyzer do not match.

Looking through the results tab and it shows no or a partial list of samples

A 'filter' has likely been applied to the results display. Select 'Filter' in the lower right hand corner and adjust as needed to include the results.

Cal Check Fails

Go through these steps:
Remove the gun device and clean the stainless steel disk and Prolene® window. Try to measure again. If it still fails, restart the software and gun device then try again (make sure to export any data first). If it still fails, replace the stainless steel disk and measure again. If none of this resolves the issue, then contact Olympus and David Houpt.

Health, Safety, and Environment

Handheld XRF Analyzer Safety Design

To control X-ray emissions, and thereby minimize the possibility of accidental exposure, the Olympus DELTA Premium pXRF analyzer has a standard safety interlock structure consisting of two features listed below. Be sure to understand the software trigger lock setting to understand whether the trigger is "armed" or not.

Software proximity sensor

Within two seconds of starting a test, the analyzer attempts to detect backscatter radiation from the sample. If it fails to detect this backscatter radiation (i.e., no sample is detected), the test aborts to prevent accidental exposure. Upon an abort action, the filter wheel returns to the 0 position, the X-rays shut off (the tube current decreases to 0.0 µA), and the red light stops blinking. If the probe is pulled away from the sample while a test is in progress, testing will stop and X-rays will shut off.
This safety works slightly differently inside the sample chamber. If the pXRF starts measuring inside of the sample chamber without a sample inside the X-rays will continue emitting until it switches to Beam 2. At the start of the second beam the analyzer will abort the measurement. Beam 1 is a higher voltage and the analyzer detects the x-rays bouncing off the walls in there. If a run was started but a sample was not put in the chamber it is NOT SAFE to open the sample chamber door.

Software trigger lock (not applicable if you are controlling the device via the software on the laptop)

After a five-minute lapse between tests (default time), the trigger automatically locks. The pXRF analyzer also has a dead man trigger protocol, in which the user is required to pull and hold the trigger for the duration of the test. When the dead man trigger is enabled, releasing the trigger prematurely will abort the test. However, it is not recommended to use the trigger—instead, trigger the measurements from the PC, and thus further away from the instrument.

Indicators and Alarms

X-ray Indicator

An X-ray indicator alerts the operator when the tube is receiving power and when X-rays are emitted from the analyzer through the measurement window. The X-ray indicator is located on the upper rear portion of the analyzer. This indicator consists of a six-element red LED array, and has three states:

X-ray Indicator Lights OFF

This signifies that the X-ray tube is disabled, and that there is no possibility of radiation exposure to you or bystanders. The instrument can be carried or set down safety safely in this condition.

X-ray Indicator Lights Continuously ON

Solid red LED array. This signifies that the X-ray tube is enabled, and that there is no radiation exposure to you or bystanders. The instrument can be carried or set down safety safely in this condition.

X-ray Indicator Lights Flashing ON and OFF

Blinking red LED array. This signifies that the X-ray tube is powered on and that the analyzer is emitting X-ray radiation through the measurement window. In this condition, the analyzer must be pointed toward a test sample and never at a human being.

Audible Alarm Protocol (not currently enabled)

When enabled, the audible signal emits three tones as a warning when the X-ray tube is about to emit X-rays. During the subsequent testing period, the audible alarm maintains a "chirping" signal throughout the duration of the test. If the pXRF is to be set up in a potentially high-traffic area (which is not recommended in the first place, but could be necessary), it is suggested to use this feature to help minimize exposure of bystanders.

Infra-Red Sensor

The pXRF has an infrared sensor that detects the presence of an object in front of the pXRF source. If no object is detected, the pXRF will not activate the source.

Radiation Safety Tips for Using the pXRF

All operators should follow minimum safety requirements discussed below. When handled properly, the amount of radiation exposure received from the pXRF will be negligible. However, the following safety tips are provided to help ensure safe and responsible use:

1. WARNING: No one but the operator should be allowed to be closer than 3 feet from the pXRF, particularly the beam port. Ignoring this warning could result in unnecessary exposure.
2. WARNING: The operator should never defeat the IR sensor in order to bypass this part of the safety circuit. Defeating this safety feature could result in over-exposure of the operator.
3. Do not allow anyone other than trained personnel to operate the pXRF.
4. Be aware of the direction that the X-rays travel when the red light is blinking and avoid placing any part of your body (e.g., eyes, hands) near the X-ray port to stabilize the instrument during operation.
5. Never hold a sample up to the X-ray port for analysis by hand; hold the instrument to the sample.
6. Establish a no-access zone at a sufficient distance from the instruments measurement window, which will allow air and distance to attenuate the beam.
7. Enclose the beam working area with protective panels (e.g., >3.0 mm stainless steel) if practical.
8. Wear an appropriate dosimeter (see the Laboratory Officer for more information on when a dosimeter is called for).
9. The operator is responsible for the security of the handheld XRF. When in use, the device should be in the operator's possession at all times (i.e., either in direct sight or a secure area).
10. Always store the instrument in a secure location when not in use.
11. During transport to and from the set up location, store the instrument in a cool, dry location.
12. WARNING: Pregnant women should not use the pXRF or work in proximity to it. See Additional Note, Pregnancy, above, for more information. Radiation exposure can be harmful to an embryo or developing fetus!

Credits

This document originated from Word document XRF_UG_v374.doc (see Archived Versions below for a pdf copy) that was written by N. Lawler and A. Armstrong. Credits for subsequent changes to this document are given in the page history.

Archived Versions

Olympus Delta pXRF User Guide - September 27, 2022

LMUG-pXRFUserGuide-230220-2004-190.pdf

XRF_UG_v374.pdf