Performing Integrated WDS and EDS Acquisition in PFE

[John Donovan]

You can get the MSCOMCTL.OCX file from the (still available) IDE directly from Microsoft here: Microsoft website

And extract the required .OCX file by unzipping the .msi file using 7zip.

You then place the .OCX file in C:/Windows/SystemWOW64/ and register the component via an administrative console with

Code Select Expand

regsvr32 C:\Windows\SysWOW64\MSCOMCTL.OCX 
It could of course also be something to do with one of the dependencies for this file (which might hopefully also be in the .msi file above), or something completely different!

Update: Yanan Liu at Univ Toronto, recently tried these steps on her JEOL 8230 and is still not able to obtain non-zero net intensities. But it was certainly worth a try!  

JEOL Japan is continuing looking into this issue... so if your 8230/8530 EDS interface is still returning non-zero net intensities, you might want to wait to upgrade your JEOL software until this is fixed.

One additional observation is that JEOL added this get net intensity function call towards the end of the development of the LibEDSIS.dll file, so maybe at some point these late changes were not included in the latest JEOL PC-SEM software? 

But again, please note this zero net intensities issue does NOT affect the newer JEOL iSP100/iHP200F instruments which use a completely different interface for EDS integration.

That might explain why the get spectrum calls all work, but just not the get net intensity call.

[John Donovan]

Ryan McAleer makes some suggestions for getting the best results from the JEOL EDS interface on iSP100/iHP200F instruments:

1. You should run a single EDS spectrum acquisition in the JEOL software prior to any EDS acquisitions with Probe for EPMA. Doing seems to get the JEOL software interface into a correct state. Just one EDS acquisition for each time starting the JEOL software. 

2. To avoid issues with the Faraday cup inserting before the WDS acquisitions are finished, you must uncheck the "Insert PCD after reservation execution is completed" [PFE will prompt you about this once per run]

3. The user should run a single EDS acquisition after they change the EDS time constant in Probe for EPMA. This is to ensure that these EDS conditions are properly saved for subsequent EDS element analyses. Or one can just set the EDS time constant they want in both JEOL (Analysis-->EDS analysis basic conditions) and Probe for EPMA. Otherwise the documented time constant on that first point will be incorrectly saved [we are looking into why this occurs].

4. If there is any hangup during EDS comm, RESTART the JEOL COMPUTER.  If you just restart the software (either through "ResetEPMA" or through the task manager) the "reservation" of the EDS will not clear and you will run into a variety of problems.

[Joe Boesenberg]

John

Given my continuing issues with my TAP crystals, I was trying to do a mini WDS-EDS run yesterday for olivine. Just Fe and Mn on WDS and Si and Mg on EDS. A couple questions since Scott B. is out in the field.

1) PfE asks a question about "Do I want to output the EDS data?" just before starting the Standards analysis. I said yes, but am not sure this is correct?

2) As far as the EDS correction procedure, I want the Bruker phi-rho-z procedure, correct? This is what is recommended by Bruker when using standards, but I am not sure if PfE is doing the analysis of the spectra independently or is Bruker doing the analysis and then outputting it to PfE.

3) Also, to process the data in Analyze, why does PfE need to connect to the EDS? If that connection is not established, PfE doesn't do any calculation of the data and I seem to lose whatever EDS data I had after I try to reconnect. Is there a specific option in PfE that should be check marked to save the spectra other than "Acquire EDS data".

4) Where is the saved EDS spectra for an individual run (mdb file) located? Is the spectra saved within the mdb file?

Thanks.
Joe

[John Donovan]

Given my continuing issues with my TAP crystals, I was trying to do a mini WDS-EDS run yesterday for olivine. Just Fe and Mn on WDS and Si and Mg on EDS. A couple questions since Scott B. is out in the field.

1) PfE asks a question about "Do I want to output the EDS data?" just before starting the Standards analysis. I said yes, but am not sure this is correct?

Good questions.

As you know, when PFE runs automated data acquisition it outputs the raw data for every point automatically to the log window. This takes only a fraction of a second for WDS data, but when EDS data is being acquired, it calls the EDS interface (JEOL, Thermo or Bruker) to obtain the EDS net intensities. This takes a bit longer since the EDS software has to do a peak deconvolution.

Also since all the data in the sample is output for each new data point, all the EDS points in the current sample are output each time, which, if the sample contains hundreds of points, can take a few seconds or many more depending on the number of points. During a long automated run these repeated EDS net intensity calculations can add up to increase the automated acquisition time.

So this question is just asking if you really want to run these EDS net intensity calculations during the automated acquisition, so you can reduce the amount of time it takes to run the automated acquisition with EDS elements.

If you say "Yes" it outputs the EDS net intensities for each point acquisition which takes a bit longer. If you say "No", it won't hurt anything, but the EDS net intensities won't get automatically calculated and stored in your probe database. You might also want to read this topic from the beginning as it has lots of information on this topic:

https://smf.probesoftware.com/index.php?topic=79.0

After writing all the above I found this post:

https://smf.probesoftware.com/index.php?topic=42.msg8432#msg8432

2) As far as the EDS correction procedure, I want the Bruker phi-rho-z procedure, correct? This is what is recommended by Bruker when using standards, but I am not sure if PfE is doing the analysis of the spectra independently or is Bruker doing the analysis and then outputting it to PfE.

When PFE asks for net intensities from the EDS interface, the EDS software calculates the composition depending on the vendor model for deconvolution. Some vendors use a filter fit, some vendors model the continuum and the latter method does depend on the quantification used by the EDS vendor, but only to the extent that the composition affects the continuum modeling.

In other words, the matrix correction model in the EDS software doesn't affect the EDS net intensity calculations much at all.  Of course once PFE obtains the EDS net intensities, then both the WDS and EDS net intensities are calculated using the matrix corrections selected in Probe for EPMA. See here:

https://smf.probesoftware.com/index.php?topic=482.msg2826#msg2826

Finally I should note that because Probe for EPMA handles the matrix corrections for both EDS and WDS elements, it can perform spectral interference corrections from EDS on WDS elements or WDS on EDS elements:

https://smf.probesoftware.com/index.php?topic=482.0

3) Also, to process the data in Analyze, why does PfE need to connect to the EDS? If that connection is not established, PfE doesn't do any calculation of the data and I seem to lose whatever EDS data I had after I try to reconnect. Is there a specific option in PfE that should be check marked to save the spectra other than "Acquire EDS data".

Your EDS data is still there if you don't have a connection to the EDS interface on your data re-processing computer, but you'll want to turn on the Use Stored EDS Net Intensities option here from the Analytical | Analysis Options menu dialog:



That of course assumes that the EDS net intensities have already been calculated and stored.

So for example, if you answer "No" to the question: "Do I want to output the EDS data?" when acquiring your automated EDS (and WDS) elements, the EDS net intensities will not have been calculated and stored in the probe database during the automated acquisition.

That's not an issue when you're still connected to the EDS interface and start calculating analyses from say the Analyze! window, because the EDS net intensities will be automatically obtained from the EDS interface, stored in your probe database and the composition calculated.

But if you finish your automated acquisition and then immediately take the MDB file to another computer that does not have the EDS interface, there will be no EDS net intensities stored for the EDS elements.  So if you answered "No" to that question, what you want to do when the automation is finished is to select all your samples in the Analyze! window and click the "Raw Data" button while you are still connected to the EDS interface.

Then the software will calculate net intensities for all your points and store them in the MDB probe database.  Once that is done you can move the MDB file to another computer (that doesn't have the JEOL/Thermo/Bruker EDS software installed), and then go to the Analytical | Analysis Options menu dialog and select the Use Stored EDS Net Intensities as described above...

Then the software will utilize the already stored EDS net intensities even if the EDS interface is no longer present. Of course the best thing is to install the Thermo/Bruker software in "demo" mode on your off-line computers and then you can interface to the Bruker EDS software for off-line re-processing (the JEOL software cannot be installed off-line).

4) Where is the saved EDS spectra for an individual run (mdb file) located? Is the spectra saved within the mdb file?

The EDS spectra data is stored in the probe MDB data for your run. You can view it any time from the Run | Display and Export EDS Spectra menu dialog:

https://smf.probesoftware.com/index.php?topic=40.msg8739#msg8739

Let us know if you have further questions.

[Ben Buse]

Hi, very interesting reading how PFE incorporates EDS signal. Given the EDS manufacturer provides the net intensity do we see some EDS manufacturers provide better net intensity? How much does the accuracy of the data vary from manufacturer to manufacturer?

[Nicholas Ritchie]

Hi, very interesting reading how PFE incorporates EDS signal. Given the EDS manufacturer provides the net intensity do we see some EDS manufacturers provide better net intensity? How much does the accuracy of the data vary from manufacturer to manufacturer?

Great question.  Maybe we could do a study?

[John Donovan]

JEOL Japan is continuing looking into this issue... so if your 8230/8530 EDS interface is still returning non-zero net intensities, you might want to wait to upgrade your JEOL software until this is fixed.

One additional observation is that JEOL added this get net intensity function call towards the end of the development of the LibEDSIS.dll file, so maybe at some point these late changes were not included in the latest JEOL PC-SEM software? 

But again, please note this zero net intensities issue does NOT affect the newer JEOL iSP100/iHP200F instruments which use a completely different interface for EDS integration.

That might explain why the get spectrum calls all work, but just not the get net intensity call.

As quoted above, several of our customers who had their JEOL EDS software updated on their 8230/8530 instrument lost the ability to obtain net intensities for data processing of integrated WDS and EDS in Probe for EPMA.

Thanks to efforts by Yanan Liu at the Univ of Toronto and her JEOL support team, they were finally able to figure out what the what was causing zero EDS net intensities to be returned:

Some good news our end: our EDS net intensity problem seems to be resolved! Thanks to our local service team and the field service engineer Tong, we are now able to get EDS intensities back and can conduct EDS-WDS combined analyses in PFE again as before!

I was told that the key adjustment was in the standard data folder setting. In PC-SEM, under Energy Calibration → Configuration → Folders tab, the "Standard data" should be set to "DrySC40E(SD30)" (screenshot attached).

Here is the screenshot:



In hindsight the solution is completely obvious...  just kidding!   

[glennpoirier]

I can confirm that the fix reported by Yunan solved the problem on my JEOL 8230 (2011 vintage). The computer was upgraded in 2022 but I only notice the net intensity problem a few months ago.
One thing to note is that you have to start the JEOL software in administrator mode to change the standard folder.

On-Peak (off-peak corrected) or EDS (bgd corrected) or MAN On-Peak X-ray Counts (cps/1nA) (and Faraday/Absorbed Currents):
ELEM:    Ca ka   Mg ka   Si ka    O ka   BEAM1   BEAM2
BGD:       EDS     EDS     EDS     EDS
SPEC:        0       0       0       0
CRYST:     EDS     EDS     EDS     EDS
ORDER:       1       1       1       1
    6G  172.01  123.05  322.33   62.54  20.050  20.060

AVER:   172.01  123.05  322.33   62.54  20.050  20.060
SDEV:      .00     .00     .00     .00    .000    .000
1SIG:      .00     .00     .00     .00
SIGR:      .00     .00     .00     .00
SERR:      .00     .00     .00     .00
%RSD:      .00     .00     .00     .00
DEAD:     ----    ----    ----    ----
DTC%:     11.5    11.5    11.5    11.5

[Ryan McAleer]

Trouble adding unanalyzed elements if EDS has been collected:

Now that the JEOL WDS/EDS integration is working pretty well (Thanks!) I'd like to collect EDS (with no elements quantified) with every WDS analysis—just to have a record, so later I could check if I missed elements, possibly use EDS for certain elements etc. This has created a minor problem with adding specified concentrations. If an EDS analysis has been collected—I can't figure out how to add an "unanalyzed element." What am I missing! 

For example, if I add Carbon in the Analyze! window after an analysis where EDS was collected, the EDS radio button is automatically selected. I couldn't figure out how to add Carbon as unanalyzed. If there is no EDS analysis collected, then WDS/EDS radio buttons are both greyed out, I can add Carbon as unanalyzed and then specify the concentration--but if EDS is selected you get "you can't specify an analyzed element"

Is it possible to add unanalyzed elements if you have collected an EDS spectrum? 

Also, unrelated, is there a way to output high and low background intensities separately vs. the single calculated off peak intensity from the 2 pts?

Thanks!

[Probeman]

Trouble adding unanalyzed elements if EDS has been collected:

Now that the JEOL WDS/EDS integration is working pretty well (Thanks!) I'd like to collect EDS (with no elements quantified) with every WDS analysis—just to have a record, so later I could check if I missed elements, possibly use EDS for certain elements etc. This has created a minor problem with adding specified concentrations. If an EDS analysis has been collected—I can't figure out how to add an "unanalyzed element." What am I missing! 

For example, if I add Carbon in the Analyze! window after an analysis where EDS was collected, the EDS radio button is automatically selected. I couldn't figure out how to add Carbon as unanalyzed. If there is no EDS analysis collected, then WDS/EDS radio buttons are both greyed out, I can add Carbon as unanalyzed and then specify the concentration--but if EDS is selected you get "you can't specify an analyzed element"

Is it possible to add unanalyzed elements if you have collected an EDS spectrum? 

Yes. In the dropdown list for the x-ray line, scroll all the way down and select the blank line.

Also, unrelated, is there a way to output high and low background intensities separately vs. the single calculated off peak intensity from the 2 pts?

I'm sure there is. Just check the PFE User's Reference manual and check the various "custom" output formats. I think there's several of them that output the raw high and low intensity data.

[Ryan McAleer]

Excellent! I was not aware of the blank line. That works!... and custom data #7 (NIST) includes the Raw high off peak AND Raw low off peak vs the calculated off peak from the two measurements. Thanks!