Performing Integrated WDS and EDS Acquisition in PFE

[JonF]

As we have mentioned previously the JEOL PC-SEM software automatically inserts the PCD (Faraday cup) after the EDS spectrum acquisition is complete (it's a feature not a bug!). 

In order to prevent the Faraday cup from being inserted before the WDS acquisition finishes (if it is using a longer acquisition time than the EDS), one must be sure to *uncheck* the "Insert PCD after the reservation execution is completed" checkbox in the JEOL software:

This came up elsewhere whilst discussing combined WDS/EDS using the older JEOL EDS interface as on the 8230/8530F EPMAs (i.e. PC-SEM as opposed to SEM Centre).

If you are doing combined WDS/EDS, you need to make sure that you have set PCD to "OFF" in the EDS Acquisition Condition window for both Spectrum and Multi Points. You can see this menu in PC-SEM in the Analysis tab, and the Condition button on the bottom right of the PC-SEM screen (in the EDS part of the window).

This will prevent the EDS from closing the PCD whilst PfE is still collecting data from the WDS (if the EDS time is less than the WDS time).

[Ben Buse]

Is there anyway to use sample setups so one sample setup uses EDS-WDS single condition; whereas another sample setup uses just WDS and combined conditions?

It doesn't seem to work because Acquistion Options are not applied with the sample setup, but apply universally.

So for combined conditions setup in Acquistion Options acquire EDS is unchecked. Which means if a EDS-WDS sample setup is run, whilst it knows it doing EDS on particular elements it doesn't acquire the spectrum

Thanks

[John Donovan]

Is there anyway to use sample setups so one sample setup uses EDS-WDS single condition; whereas another sample setup uses just WDS and combined conditions?

Yes, one cannot acquire EDS spectra on a combined condition sample.  The reason makes sense if you think about it because you don't want to change the beam conditions while an EDS spectrum is being acquired.

And yes, the EDS acquisition flag is specified on a global basis for that run.

[Ben Buse]

Thanks John for clarifying the situation.

I have a couple of questions/suggestions about workflow. And it be good to know how others find it.

(1) Instead of asking you in a pop up window when you start an analysis whether you want to extract intensities from EDS as go along or at the end, could we have a check box somewhere to set this behaviour

(2) Once intensities have been loaded into PFE in analyze window it's really slow if loads them again when checking acquired data. Having to keep going into Analytical -> Analysis Options -> To select check box 'only used eds stored net intensities' is frustrating and would be nice if more accessible. If I running secondary standards or checking standards or checking the first few analyses, I'm constantly checking and unchecking this option. Not sure as to the solution... Possibly in automate window a checkbox to say extract net intensities, and at end of automate a checkbox to say use stored intensities, or a checkbox in analysis window to say use stored intensities.

[John Donovan]

Possibly in automate window a checkbox to say extract net intensities, and at end of automate a checkbox to say use stored intensities, or a checkbox in analysis window to say use stored intensities.

I think what you want is already in Probe for EPMA.

You should simply check the "Use Stored EDS net intensities from Probe Database" in the Analytical | Analysis Options dialog:



Then Probe for EPMA will always use the net intensities that have already been extracted and stored in the run database.

If you use the "Do not use EDS spectra interface for Obtaining Net Intensities" it will skip obtaining net intensities and just use zero intensities for the quantification.

[Ben Buse]

You should simply check the "Use Stored EDS net intensities from Probe Database" in the Analytical | Analysis Options dialog:



Then Probe for EPMA will always use the net intensities that have already been extracted and stored in the run database.

Hi John, the issue I have is when this is selected it does not extract the intensities from the EDS detector during acquistion, so I have to unselect it during acquisiton.

[John Donovan]

You should simply check the "Use Stored EDS net intensities from Probe Database" in the Analytical | Analysis Options dialog:

Then Probe for EPMA will always use the net intensities that have already been extracted and stored in the run database.

Hi John, the issue I have is when this is selected it does not extract the intensities from the EDS detector during acquistion, so I have to unselect it during acquisiton.

For automation, you can click "Yes", when prompted at the start of the automation, to extract the net intensities during the automation acquisition and then they are stored. If you want to speed up the automation, just say "No" when it asks you whether to extract net intensities from the Automate! window. 

Then once the run is over, you can select all the samples from the Analyze! window and extract them off-line.

It's your choice.

[Ben Buse]

Hi John,

So to clarify

If I do the following - with use locally checked



Then in acquire window - hit start standard or unknown - I get the following



So then I have to uncheck use local intensities in order to get the intensities.

Before checking use local intensities so that it doesn't try to get them again when viewing the results.

But then having to uncheck use local intensities when I do the next analysis

The same purple error is observed during automate if I say yes to obtaining net intensities in the pop up window which could be a checkbox in the automate window

[John Donovan]

Normally Probe for EPMA gets EDS net intensities from the JEOL (or Bruker) server and stores them in your probe database when a sample is analyzed or raw data displayed. That is, if the "Only Use Stored EDS Net Intensities..." checkbox in the Analytical | Analysis Options menu dialog is NOT checked.

In order to use the EDS "stored" net intensities one has to first obtain them from the JEOL (or Bruker) server. So if you have acquired WDS data from the Automate! window, and clicked No to not obtain EDS net intensities during the automation, they won't get stored in your probe database.

So after the automation in Automate! has completed, you will need to select all the samples from the Analyze! window (All Samples and Select All) and click the "Raw Data" button. The software will then obtain the EDS net intensities for all the samples and store them in your MDB probe database.

Once the EDS net intensities are stored in your probe database, you can check the "Only Use Stored EDS Net Intensities..." checkbox in the Analytical | Analysis Options menu dialog. Then you can your the MDB probe database file to another computer WITHOUT a connection to the JEOL (or Bruker server) and still be able to calculate EDS concentrations.

[John Donovan]

Working with Peng Jiang in Hawaii we ran some major elements on EDS (Bruker Esprit) and minor elements on WDS. Here is an analysis of a natural garnet as a secondary standard:

St  102 Set   1 Garnet, Verma (Mn), Results in Elemental Weight Percents
 
ELEM:       Si      Fe      Mg      Ca      Mn      Al       O
TYPE:     ANAL    ANAL    ANAL    ANAL    ANAL    SPEC    CALC
BGDS:      EDS     EDS     EDS     EXP     LIN
TIME:    39.98   39.98   39.98   60.00   60.00     ---     ---
BEAM:    19.84   19.84   19.84   19.84   19.84     ---     ---

ELEM:       Si      Fe      Mg      Ca      Mn      Al       O   SUM  
   112  16.589  15.708    .000    .193  19.249  11.020  38.886 101.645
   113  16.648  15.719    .001    .183  19.305  11.020  38.970 101.846
   114  16.786  15.698    .035    .171  19.238  11.020  39.119 102.067
   115  16.757  15.654    .050    .181  18.991  11.020  39.016 101.670
   116  16.821  15.710    .038    .185  19.045  11.020  39.113 101.931

AVER:   16.720  15.698    .025    .182  19.166  11.020  39.021 101.832
SDEV:     .098    .026    .023    .008    .138    .000    .099    .178
SERR:     .044    .011    .010    .004    .062    .000    .044
%RSD:      .58     .16   91.83    4.30     .72     .00     .25

PUBL:   17.240  14.020    n.a.    .170  19.050  11.020  39.077 100.577
%VAR:    -3.01   11.97     ---    7.31     .61     ---     ---
DIFF:    -.520   1.678     ---    .012    .116     ---     ---
STDS:      114     103     103     114     303     ---     ---

I cannot speak to the accuracy of this particular (natural) standard, but the analysis looks OK, but the Fe on EDS is way off.

Then we added Mn as an interfering element because Probe for EPMA can perform interference corrections whether the element is a WDS or an EDS element.  We utilized a synthetic Mn2SiO4 standard for the interference correction because it contains a known amount of the interferring element (Mn) but none of the interfered element (Fe):

St  102 Set   1 Garnet, Verma (Mn), Results in Elemental Weight Percents
 
ELEM:       Si      Fe      Mg      Ca      Mn      Al       O
TYPE:     ANAL    ANAL    ANAL    ANAL    ANAL    SPEC    CALC
BGDS:      EDS     EDS     EDS     EXP     LIN
TIME:    39.98   39.98   39.98   60.00   60.00     ---     ---
BEAM:    19.84   19.84   19.84   19.84   19.84     ---     ---

ELEM:       Si      Fe      Mg      Ca      Mn      Al       O   SUM  
   112  16.573  14.191    .000    .193  19.279  11.020  38.443  99.699
   113  16.632  14.199    .001    .183  19.335  11.020  38.525  99.895
   114  16.770  14.182    .035    .171  19.268  11.020  38.675 100.122
   115  16.741  14.158    .050    .181  19.021  11.020  38.578  99.749
   116  16.805  14.210    .037    .185  19.074  11.020  38.674 100.005

AVER:   16.704  14.188    .025    .183  19.195  11.020  38.579  99.894
SDEV:     .098    .020    .023    .008    .139    .000    .100    .175
SERR:     .044    .009    .010    .004    .062    .000    .045
%RSD:      .58     .14   91.83    4.30     .72     .00     .26

PUBL:   17.240  14.020    n.a.    .170  19.050  11.020  39.077 100.577
%VAR:    -3.11    1.20     ---    7.48     .76     ---     ---
DIFF:    -.536    .168     ---    .013    .145     ---     ---
STDS:      114     103     103     114     303     ---     ---

Much better!

[John Donovan]

Good news!  We finally fixed the problem with multiple windows popping up in the JEOL SEM Center software when extracting EDS net intensities in Probe for EPMA on JEOL iSP100 and iHP200F instruments!

Related to this issue: with the most recent version of JEOL's SEM Center (v. 1.0.10.1) software, the MEC EDS interface introduced some timing issues which we have addressed in a new MEC wrapper DLL version. Please see the attached DLL below (remember to login to see attachments!).

Once you obtain the new MEC EDS wrapper DLL (v. 1.0.51.0), simply copy it to the Probe for EPMA application folder: C:\Program Files (x86)\Probe Software\Probe for EPMA and overwrite the existing DLL.

We also updated Probe for EPMA, with a new function to close the pop up windows in the JEOL software (hence the need for a new MEC EDS wrapper DLL).  In the past, many windows would be opened in the JEOL software every time the net intensities were extracted, so this new DLL and updated Probe for EPMA fixes this issue as mentioned above.

Update Probe for EPMA using the Help menu as usual or download it from our web site Resources page:

https://www.probesoftware.com/resources/

Thank-you to all your patience in getting this all working.