Trying to combine selected samples

Mike Jercinovic · August 20, 2015, 01:19:28 PM

This is me today...
www.youtube.com/watch?v=nXKeNKvl-J4

So someone (Calvin) is probing today and has run a set of analyses in a domain, but the SD is not great so he wants to run some more points. I say "no problem Calvin, just run more as a new sample and we will combine them in Analyze." We have done this before. Once he has finished, we go into Analyze and highlight the two samples. We try "Combine the selected samples into a new sample" which is what I thought we used to do. We get the following...

Warning in AnalyzeCombineSamples: sample Un 52 MT-09-96_m22 core additional does not contain the same number of data rows as combined sample Un 50 MT-09-96_m22 core
Warning in AnalyzeCombineSamples: element u is already present in the combined sample and will not be loaded again
Warning in AnalyzeCombineSamples: element k is already present in the combined sample and will not be loaded again
Warning in AnalyzeCombineSamples: element th is already present in the combined sample and will not be loaded again
Warning in AnalyzeCombineSamples: element Ca is already present in the combined sample and will not be loaded again
Warning in AnalyzeCombineSamples: element S is already present in the combined sample and will not be loaded again
Warning in AnalyzeCombineSamples: element P is already present in the combined sample and will not be loaded again
...and so on for the rest of the 26 elements in the samples

in the new "combined" new sample, it only has the data from the first one. I realize at this point that what it apparently is doing is combining samples if there are new elements only. I don't see the importance of the warning about having a difference number of data rows. OK, so now we move to the "Combine Selected Samples" button, at which time Calvin says, looking at the Analyze window..."what's the difference between Combine analysis lines and Combine Data lines, oh and data rows as it says in the warning?" So he wants to know why we say analysis lines, data lines, and data rows and why are these not the same things...I don't know because now I am confused too. You just have to click them to see what they do. Alright, so now if we highlight the two analyses we want to combine and we click the yellow "Combine Selected Samples", it does what we want, that is it looks at the 5 points run in one sample, and 4 points in the other, and treats them all as a single nine point (line, row, whatever) analysis. That's fine except there is not a way to have these put together into a single sample analysis for output. Oh well we can do this offline I suppose, so the real question I guess I have is the use of Combine the Selected Samples into a New Sample. It does not combine the selected samples into a new sample unless there are only new elements in the second sample. If anyone has some clarification on this, I would appreciate it.

John Donovan · August 20, 2015, 03:36:41 PM

Quote from: Mike Jercinovic on August 20, 2015, 01:19:28 PM
...Oh well we can do this offline I suppose, so the real question I guess I have is the use of Combine the Selected Samples into a New Sample. It does not combine the selected samples into a new sample unless there are only new elements in the second sample. If anyone has some clarification on this, I would appreciate it.

Hi Mike,
I agree the buttons could be labeled better. Basically the "Combine Samples" button combines elements from multiple samples (duplicate elements are skipped). While the "Combine Analyses" button just combines lines from multiple samples into a single sample (must be the same elements).

If you hold the mouse over the buttons there is a bit more explanation that will pop up. See attached screen shot below...
john

Mike Jercinovic · August 21, 2015, 06:19:52 AM

OK thanks John. There is not a "Combine Analyses" button, but there is a "Combine Analysis Lines From Selected Samples" button. This works, but what would be really great here would be to be able to take this combined result and create a new sample in the way that "Combine the selected samples into a New Sample" works for additional elements.

John Donovan · August 21, 2015, 07:52:33 AM

Quote from: Mike Jercinovic on August 21, 2015, 06:19:52 AM
OK thanks John. There is not a "Combine Analyses" button, but there is a "Combine Analysis Lines From Selected Samples" button. This works, but what would be really great here would be to be able to take this combined result and create a new sample in the way that "Combine the selected samples into a New Sample" works for additional elements.

Hi Mike,
Yes, I was "paraphrasing"!

Anything is possible, but why go to the trouble to make it into a new sample? You do know about right clicking any selected samples in the Analyze! sample list?

Mike Jercinovic · August 21, 2015, 09:10:59 AM

For us, having the combined data in a new sample would allow that dataset to be output with everything else when completing the session. There are only three output options via the right click in Analyze, and none of them are for U, Th, Pb geochron. We will just do this offline.

John Donovan · July 16, 2022, 05:38:58 PM

So this might be a slightly esoteric feature in Probe for EPMA, but it can be very useful. Anyway we made a small tweak to it for John Fournelle and Will Nachlas. What am I talking about? The Combine Selected Samples button from the Analyze! window.

This feature is normally utilized when you analyze some elements under one set of conditions, and then analyze different elements using a different set of beam conditions, for example, major elements at one beam condition and then minor/trace elements at a different beam condition.

Now normally one would just acquire the data for both the major and minor/trace elements using different conditions in a single sample at acquisition time, using the Combined Conditions feature as discussed in this topic:

https://smf.probesoftware.com/index.php?topic=5.0

But sometimes one wants to acquire the elements at different beam conditions as separate samples. You can ask Will and John why that might be.

Anyway, when doing this, one merely selects two or more samples from the Analyze! window and clicks the Combine Selected Samples button. Probe for EPMA then combines the samples into a separate (temporary) sample and calculates the composition as seen here:

Combined Analytical Condition Arrays:
ELEM: Si Zr Hf Hf Hf
CONDN: 1 1 1 1 1
CONDO: 1 1 1 1 1
KILO: 17.0 17.0 17.0 17.0 17.0
CURR: 40.0 40.0 200.0 200.0 200.0
SIZE: 5.0 5.0 5.0 5.0 5.0

Un 34 (Un 34 GSJ 1, Un 136 GSJ 1), Results in Elemental Weight Percents

ELEM: Si Zr Hf Hf Hf O
TYPE: ANAL ANAL ANAL ANAL ANAL CALC
BGDS: LIN LIN LIN LIN LIN
TIME: 10.00 10.00 10.00 .00 .00 ---
BEAM: 50.27 50.27 203.01 .00 .00 ---
AGGR: 3 ---

ELEM: Si Zr Hf Hf Hf O SUM
XRAY: (ka) (la) (ma) (ma) (ma) ()
1581 15.030 48.785 .607 .000 .000 34.347 98.769
1582 15.128 49.162 .609 .000 .000 34.591 99.489
1583 15.330 49.732 .590 .000 .000 35.018 100.670
1584 15.421 49.337 .593 .000 .000 34.984 100.335
1585 15.334 49.468 .591 .000 .000 34.930 100.323
1586 15.187 49.152 .573 .000 .000 34.648 99.559

AVER: 15.238 49.273 .594 .000 .000 34.753 99.858
SDEV: .148 .322 .013 .000 .000 .267 .709
SERR: .060 .131 .005 .000 .000 .109
%RSD: .97 .65 2.21 .0000 .0000 .77
STDS: 391 391 387 0 0 ---

STKF: .1356 .4170 .6346 .0000 .0000 ---
STCT: 149578.4 21265.3316584.2 .0 .0 ---

UNKF: .1343 .4111 .0053 .0000 .0000 ---
UNCT: 148129.9 20965.8 2649.5 .0 .0 ---
UNBG: 1140.9 111.8 1699.4 .0 .0 ---

ZCOR: 1.1350 1.1985 1.1177 .0000 .0000 ---
KRAW: .9903 .9859 .0084 .0000 .0000 ---
PKBG: 130.92 188.86 2.56 .00 .00 ---

In this example the Si and Zr were acquired at 40 nA, while 3 channels were utilized to acquire Hf at 200 nA, and then the "aggregate" feature was utilized to aggregate the Hf intensities from the three Hf channels as discussed here:

https://smf.probesoftware.com/index.php?topic=155.0

This all works fine. That is the software acquires each of the samples at all the conditions (normally used for thin film acquisition), or it can acquire all the samples at each condition (normally used for the constant k-ratio acquisition). You get to decide. See this new "Run Multiple Setups One at a Time" feature here:

Then for quantification you simply combine the samples with different beam conditions in the Analyze! window using the Combine Selected Sample button as shown below.

Anyway, then John and Will asked me if they could utilize the "Use All Matrix Corrections" checkbox with this combined analysis feature. This is where the software runs the selected samples using all 10 matrix corrections supported in PFE. However, it didn't work for combined analyses in PFE until today.

Now you can get all the matrix corrections for the samples selected using the Combined Selected Samples button as seen here:

Summary of All Calculated (averaged) Matrix Corrections:
(Un 34 GSJ 1, Un 136 GSJ 1)
LINEMU Henke (LBL, 1985) < 10KeV / CITZMU > 10KeV

Elemental Weight Percents:
ELEM: Si Zr Hf Hf Hf O TOTAL
1 15.238 49.273 .594 .000 .000 34.753 99.858 Armstrong/Love Scott (default)
2 15.234 49.256 .610 .000 .000 34.746 99.846 Conventional Philibert/Duncumb-Reed
3 15.238 49.272 .606 .000 .000 34.755 99.872 Heinrich/Duncumb-Reed
4 15.232 49.253 .616 .000 .000 34.743 99.844 Love-Scott I
5 15.234 49.260 .616 .000 .000 34.748 99.859 Love-Scott II
6 15.220 49.214 .652 .000 .000 34.722 99.809 Packwood Phi(pz) (EPQ-91)
7 15.241 49.281 .587 .000 .000 34.758 99.867 Bastin (original) Phi(pz)
8 15.240 49.282 .607 .000 .000 34.761 99.890 Bastin PROZA Phi(pz) (EPQ-91)
9 15.234 49.258 .610 .000 .000 34.746 99.847 Pouchou and Pichoir-Full (PAP)
10 15.233 49.254 .615 .000 .000 34.745 99.848 Pouchou and Pichoir-Simplified (XPP)

AVER: 15.235 49.260 .611 .000 .000 34.748 99.854
SDEV: .006 .020 .017 .000 .000 .011 .021
SERR: .002 .006 .005 .000 .000 .003

MIN: 15.220 49.214 .587 .000 .000 34.722 99.809
MAX: 15.241 49.282 .652 .000 .000 34.761 99.890

I guess this might be useful to others as well.

wonachlas · July 19, 2022, 02:02:49 PM

John,

Thanks for looking into this. I noticed a quirk when using the "Combine the Selected Samples into a New Sample" button to combine a routine for major elements at 20 nA with a routine for trace elements at 200 nA. I am using the 200 micron aperture, not the normal 150 micron beam regulation aperture, so I am setting the beam current manually by changing C2 condenser lens and reading the measured Faraday current. For this I am selecting "Do Not Set Conditions during Acquisition" in the Acquisition Options window. I first noticed a problem when I did not update the beam current in the Analytical Conditions window. When I combined the trace element measurement that was acquired at 200 nA (199.6 nA actual) but still reads the default 20 nA in the Analytical Conditions, it uses the current from only the first 20 nA condition instead of the 199.6 nA measured current from the second sample. The calculated result of this measurement shows all the trace elements are too high.

Analytical Conditions set to 20 nA, traces actually measured at 200 nA

Combined Analytical Condition Arrays:
ELEM: Si Al Ca Ti F Fe Ce Nd Zr Y Nb Ce Nd
CONDN: 1 1 1 1 1 1 1 1 1 1 1 1 1
CONDO: 1 1 1 1 1 1 1 1 1 1 1 1 1
KILO: 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0
CURR: 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0
SIZE: 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0

Un 96 (Un 35 test 8_108 Ttn RM_majors, Un 36 test 8_108 Ttn RM_t, Results in Elemental Weight Percents

ELEM: Si Al Ca Ti F Fe Ce Nd Zr Y Nb Ce Nd O
TYPE: ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL CALC
BGDS: LIN LIN LIN LIN EXP LIN LIN LIN LIN LIN LIN LIN LIN
TIME: 10.00 10.00 10.00 10.00 10.00 10.00 60.00 60.00 40.00 40.00 40.00 .00 .00 ---
BEAM: 19.87 19.87 19.87 19.87 19.87 19.87 19.87 19.87 19.87 19.87 19.87 .00 .00 ---
AGGR: 2 2 ---

ELEM: Si Al Ca Ti F Fe Ce Nd Zr Y Nb Ce Nd O SUM
XRAY: (ka) (ka) (ka) (ka) (ka) (ka) (la) (la) (la) (la) (la) (la) (la) ()
827 14.883 .680 19.763 20.956 .479 1.032 3.244 1.840 .233 1.045 .896 .000 .000 41.359 106.411

AVER: 14.883 .680 19.763 20.956 .479 1.032 3.244 1.840 .233 1.045 .896 .000 .000 41.359 106.411
SDEV: .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000
SERR: .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000
%RSD: .00 .00 .00 .00 .00 .00 .00 .00 .00 .00 .00 .0000 .0000 .00
STDS: 9710 5633 9710 9710 1050 5533 356 364 5607 800 9706 0 0 ---

STKF: .1202 .2685 .2040 .2088 .5101 .6459 .5229 .5268 .4201 .3663 .5961 .0000 .0000 ---
STCT: 9683.1 22214.2 9637.7 12186.0 19589.5 5886.5 2217.0 2532.0 1842.7 1441.0 3185.2 .0 .0 ---

UNKF: .1217 .0048 .1966 .1816 .0009 .0089 .0246 .0135 .0018 .0080 .0073 .0000 .0000 ---
UNCT: 9803.8 396.4 9286.0 10599.6 35.4 81.2 104.2 64.8 8.1 31.3 38.8 .0 .0 ---
UNBG: 113.4 61.0 45.5 80.3 23.8 17.1 95.3 115.4 39.5 33.6 52.2 .0 .0 ---

ZCOR: 1.2229 1.4201 1.0052 1.1541 5.1983 1.1581 1.3197 1.3639 1.2654 1.3121 1.2342 .0000 .0000 ---
KRAW: 1.0125 .0178 .9635 .8698 .0018 .0138 .0470 .0256 .0044 .0218 .0122 .0000 .0000 ---
PKBG: 87.47 7.50 205.16 133.07 2.48 5.75 2.09 1.56 1.20 1.93 1.74 .00 .00 ---
INT%: ---- ---- ---- ---- ---- ---- ---- ---- ---- ---- ---- ---- ---- ---

The second output shows what happens when I correctly update the Analytical Conditions to match the actual conditions:

Analytical Conditions set to 200 nA, traces actually measured at 200 nA

Un 95 (Un 35 test 9_108 Ttn RM_majors, Un 36 test 9_108 Ttn RM_t, Results in Elemental Weight Percents
Combined Analytical Condition Arrays:
ELEM: Si Al Ca Ti F Fe Ce Nd Zr Y Nb Ce Nd
CONDN: 1 1 1 1 1 1 1 1 1 1 1 1 1
CONDO: 1 1 1 1 1 1 1 1 1 1 1 1 1
KILO: 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0
CURR: 20.0 20.0 20.0 20.0 20.0 20.0 200.0 200.0 200.0 200.0 200.0 200.0 200.0
SIZE: 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0

ELEM: Si Al Ca Ti F Fe Ce Nd Zr Y Nb Ce Nd O
TYPE: ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL CALC
BGDS: LIN LIN LIN LIN EXP LIN LIN LIN LIN LIN LIN LIN LIN
TIME: 10.00 10.00 10.00 10.00 10.00 10.00 60.00 60.00 40.00 40.00 40.00 .00 .00 ---
BEAM: 19.87 19.87 19.87 19.87 19.87 19.87 199.61 199.61 199.61 199.61 199.61 .00 .00 ---
AGGR: 2 2 ---

ELEM: Si Al Ca Ti F Fe Ce Nd Zr Y Nb Ce Nd O SUM
XRAY: (ka) (ka) (ka) (ka) (ka) (ka) (la) (la) (la) (la) (la) (la) (la) ()
826 14.618 .662 19.801 21.839 .503 1.046 .325 .185 .023 .103 .088 .000 .000 40.199 99.392

AVER: 14.618 .662 19.801 21.839 .503 1.046 .325 .185 .023 .103 .088 .000 .000 40.199 99.392
SDEV: .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000
SERR: .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000
%RSD: .00 .00 .00 .00 .00 .00 .00 .00 .00 .00 .00 .0000 .0000 .00
STDS: 9710 5633 9710 5502 1050 5533 356 364 5607 800 9706 0 0 ---

STKF: .1202 .2685 .2040 .5548 .5101 .6459 .5229 .5268 .4201 .3663 .5961 .0000 .0000 ---
STCT: 9683.1 22214.2 9637.7 31476.6 19589.5 5886.5 2217.0 2532.0 1842.7 1441.0 3185.2 .0 .0 ---

UNKF: .1217 .0048 .1966 .1868 .0009 .0089 .0024 .0013 .0002 .0008 .0007 .0000 .0000 ---
UNCT: 9803.8 396.4 9286.0 10599.6 35.4 81.2 10.3 6.4 .8 3.1 3.8 .0 .0 ---
UNBG: 113.4 61.0 45.5 80.3 23.8 17.1 9.4 11.4 3.9 3.3 5.2 .0 .0 ---

ZCOR: 1.2012 1.3820 1.0072 1.1690 5.4640 1.1732 1.3366 1.3863 1.2583 1.3026 1.2221 .0000 .0000 ---
KRAW: 1.0125 .0178 .9635 .3367 .0018 .0138 .0047 .0025 .0004 .0022 .0012 .0000 .0000 ---
PKBG: 87.47 7.50 205.16 133.07 2.48 5.75 2.09 1.56 1.20 1.93 1.74 .00 .00 ---
INT%: ---- ---- ---- ---- ---- ---- ---- ---- ---- ---- ---- ---- ---- ---

As a final test, I selected 21 nA for the second condition, and it uses the correct 199.6 measured current.

Analytical Conditions set to 21 nA, traces actually measured at 200 nA

Combined Analytical Condition Arrays:
ELEM: Si Al Ca Ti F Fe Ce Nd Zr Y Nb Ce Nd
CONDN: 1 1 1 1 1 1 1 1 1 1 1 1 1
CONDO: 1 1 1 1 1 1 1 1 1 1 1 1 1
KILO: 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0 15.0
CURR: 20.0 20.0 20.0 20.0 20.0 20.0 21.0 21.0 21.0 21.0 21.0 21.0 21.0
SIZE: 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0

Un 97 (Un 35 test 10_108 Ttn RM_majors, Un 36 test 10_108 Ttn RM, Results in Elemental Weight Percents

ELEM: Si Al Ca Ti F Fe Ce Nd Zr Y Nb Ce Nd O
TYPE: ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL ANAL CALC
BGDS: LIN LIN LIN LIN EXP LIN LIN LIN LIN LIN LIN LIN LIN
TIME: 10.00 10.00 10.00 10.00 10.00 10.00 60.00 60.00 40.00 40.00 40.00 .00 .00 ---
BEAM: 19.87 19.87 19.87 19.87 19.87 19.87 199.61 199.61 199.61 199.61 199.61 .00 .00 ---
AGGR: 2 2 ---

ELEM: Si Al Ca Ti F Fe Ce Nd Zr Y Nb Ce Nd O SUM
XRAY: (ka) (ka) (ka) (ka) (ka) (ka) (la) (la) (la) (la) (la) (la) (la) ()
828 14.618 .662 19.801 21.839 .503 1.046 .325 .185 .023 .103 .088 .000 .000 40.199 99.392

AVER: 14.618 .662 19.801 21.839 .503 1.046 .325 .185 .023 .103 .088 .000 .000 40.199 99.392
SDEV: .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000
SERR: .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000 .000
%RSD: .00 .00 .00 .00 .00 .00 .00 .00 .00 .00 .00 .0000 .0000 .00
STDS: 9710 5633 9710 5502 1050 5533 356 364 5607 800 9706 0 0 ---

STKF: .1202 .2685 .2040 .5548 .5101 .6459 .5229 .5268 .4201 .3663 .5961 .0000 .0000 ---
STCT: 9683.1 22214.2 9637.7 31476.6 19589.5 5886.5 2217.0 2532.0 1842.7 1441.0 3185.2 .0 .0 ---

UNKF: .1217 .0048 .1966 .1868 .0009 .0089 .0024 .0013 .0002 .0008 .0007 .0000 .0000 ---
UNCT: 9803.8 396.4 9286.0 10599.6 35.4 81.2 10.3 6.4 .8 3.1 3.8 .0 .0 ---
UNBG: 113.4 61.0 45.5 80.3 23.8 17.1 9.4 11.4 3.9 3.3 5.2 .0 .0 ---

ZCOR: 1.2012 1.3820 1.0072 1.1690 5.4640 1.1732 1.3366 1.3863 1.2583 1.3026 1.2221 .0000 .0000 ---
KRAW: 1.0125 .0178 .9635 .3367 .0018 .0138 .0047 .0025 .0004 .0022 .0012 .0000 .0000 ---
PKBG: 87.47 7.50 205.16 133.07 2.48 5.75 2.09 1.56 1.20 1.93 1.74 .00 .00 ---
INT%: ---- ---- ---- ---- ---- ---- ---- ---- ---- ---- ---- ---- ---- ---

It appears that as long as the beam current is specified to be different between the two conditions, it will correctly use the measured currents from each of the separate conditions.

I acknowledge this is mostly a user-related error associated with "Do Not Set Analytical Conditions", but still something that could introduce problems and would be obscured if the dataset was not appropriate to notice it.

John Donovan · July 19, 2022, 02:25:01 PM

Be sure to use the "Tt" text format when displaying quant data so the columns line up nicely (I edited your post for this).

Not sure what we can do to help prevent this user error. Are you suggesting we need to check something during this sort of acquisition? Not sure what that might be.

The "CURR:" beam currents line merely note the specified beam currents and are for documentation purposes and not utilized in any calculations, while the measured beam currents on the "BEAM:" line are what are actually utilized for the beam normalization.

This all reminds me of back in the day (~1980s) when we did almost everything manually, but people would occasionally forget to do something, so I started writing automation code so that these sorts of mistakes could be avoided.

Remind me again why you can't just use the combined conditions sample feature in Probe for EPMA to automate this sort of multiple beam condition acquisition?

wonachlas · July 20, 2022, 08:17:37 AM

It seems there is a trigger to use the measured beam current only if the CURR is specified to be different. For the example where both were specified to be 20 nA, it did not use the measured current from the second sample, only from the first. If you could modify it so that it automatically uses the measured current when combining two samples, that might prevent future users from encountering this problem.

There are many reasons to use different apertures other than the regulating aperture. If I am running long (>15 hr) runs at very high beam current, this can contaminate the regulating aperture and reduce its useful lifetime, so I will use the 200 um instead. If I am working at super high beam current, I might use no aperture in position. If I am trying to get the smallest possible spot diameter or working at very low beam current, I will use the smallest aperture (70 um). It is faster to change between C2 values than wait for beam regulation when switching currents. The source has excellent stability, so even with the 150 um aperture I am often working with beam regulation off, anyway. No doubt that I use combined conditions for many projects when appropriate, but for some it is not.

John Donovan · July 20, 2022, 08:54:49 AM

Huh. I think I would still just use "Combined Conditions" acquisition method and just clean the beam regulator aperture a bit more often!

OK I think I found the problem. It was getting confused because you had the same specified beam currents, but different measured beam currents on different elements.

Yes. It doesn't force a combined condition sample just because the measured beam currents are different, because for different samples they often are a little different due to beam drift.

So we put a test version of Probewin.exe in the PFE Dropbox where it just forces this flag for any "combined analyses" sample. This should not hurt when the beam currents are similar, but it should help when they are different.

Please grab it, and let me know if this works better for you.

John Donovan · August 26, 2024, 10:32:50 AM

I'm not sure if others will find this useful but Scott Boroughs recently requested that we add a "duplicate sample" feature in Probe for EPMA so one could create multiple copies of a sample for testing different calculation options for unanalyzed elements.

After thinking about it a bit we decide to modify the existing "Combine the Selected Samples into a New Sample" button to allow for a simple duplication if only a single sample is selected:

Previously this button asked if one wants to combine elements or data lines from multiple selected samples into a new sample, but now if only a single sample is selected, it merely asks if you want to duplicate the selected sample.

John Donovan · January 16, 2025, 09:58:20 AM

Just a quick note to point out the two ways one can combine samples run under different conditions with different elements in the Probe for EPMA Analyze! window.

The Combine Samples feature can be performed two different ways:

Either way you can combine either elements (or data lines) for various purposes. In the following example Scott Boroughs acquired some elements at 15 keV (using TDI to correct for beam sensitivity) and some elements at 25 keV (again using TDI) including Br Ka.

Combining them using either method yields this output (note the different keVs):

Code Select

Un   92 (Un   60  10Br, Un   88  10Br)
(Magnification (analytical) = 300000),        Beam Mode = Analog  Spot
(Magnification (default) =      100, Magnification (imaging) =    100)
Image Shift (X,Y):                                         .00,    .00

Formula Based on Sum of Cations = .000   Oxygen Calc. by Stoichiometry
Number of Data Lines:  20             Number of 'Good' Data Lines:  20
First/Last Date-Time: 12/12/2024 02:11:46 PM to 12/12/2024 02:53:45 PM
WARNING- Using Time Dependent Intensity (TDI) Element Correction

Average Total Oxygen:       43.860     Average Total Weight%:   96.454
Average Calculated Oxygen:  43.860     Average Atomic Number:   11.352
Average Excess Oxygen:        .000     Average Atomic Weight:   20.442
Oxygen Equiv. from Halogen:   .173  Halogen Corrected Oxygen:   43.686
Average ZAF Iteration:        3.00     Average Quant Iterate:     5.00

Oxygen Calculated by Cation Stoichiometry and Included in the Matrix Correction
Oxygen Equivalent from Halogens (F/Cl/Br/I), was not Subtracted in the Matrix Correction (because oxygen from halogens was greater than zero)
WARNING- Duplicate analyzed elements are present in the sample matrix!!
Use Aggregate Intensity option or Disable Quant feature for accurate matrix correction.

Combined Analytical Condition Arrays:
ELEM:       Na      Ca       S       U       B      Al      Br      Si      Th       S
CONDN:       1       1       1       1       1       1       1       1       1       1
CONDO:       1       1       1       1       1       1       1       1       1       1
KILO:     15.0    15.0    15.0    15.0    15.0    25.0    25.0    25.0    25.0    25.0
CURR:     12.0    12.0    12.0    12.0    12.0    10.0    10.0    10.0    10.0    10.0
SIZE:     12.0    12.0    12.0    12.0    12.0    12.0    12.0    12.0    12.0    12.0

Un   92 (Un   60  10Br, Un   88  10Br), Results in Elemental Weight Percents
 
ELEM:       Na      Ca       S       U       B      Al      Br      Si      Th       S       O
TYPE:     ANAL    ANAL    ANAL    ANAL    ANAL    ANAL    ANAL    ANAL    ANAL    ANAL    CALC
BGDS:      MAN     MAN     MAN     MAN     LIN     MAN     MAN     MAN     MAN     MAN
TIME:    50.00   50.00   50.00   50.00   40.00   40.00   40.00   40.00   40.00   40.00     ---
BEAM:    12.07   12.07   12.07   12.07   12.07    9.92    9.92    9.92    9.92    9.92     ---

ELEM:       Na      Ca       S       U       B      Al      Br      Si      Th       S       O   SUM  
XRAY:     (ka)    (ka)    (ka)    (ma)    (ka)    (ka)    (ka)    (ka)    (ma)    (ka)      ()
  2079  13.280   5.456    .056   -.021   1.466   5.457   1.613  25.022   -.013    .066  43.594  95.976
  2080  13.125   5.512    .056   -.007   2.028   5.395   1.793  25.223   -.003    .059  44.978  98.160
  2081  13.174   5.279    .064   -.024   1.312   5.398   1.707  25.210   -.014    .064  43.315  95.486
  2082  13.040   5.429    .057   -.025   1.274   5.443   1.796  25.113   -.013    .058  43.156  95.329
  2083  13.406   5.342    .062    .000   1.687   5.401   1.687  25.077    .009    .064  44.108  96.843
  2084  13.320   5.178    .059   -.023   1.692   5.438   1.718  25.132   -.003    .072  44.122  96.704
  2085  13.306   5.343    .059   -.017   1.339   5.449   1.751  25.283   -.026    .078  43.588  96.152
  2086  13.152   5.400    .063   -.004   1.539   5.413   1.727  24.909   -.003    .049  43.511  95.755
  2087  13.363   5.232    .059   -.010   1.370   5.405   1.829  25.207   -.008    .067  43.493  96.007
  2088  13.363   5.389    .062    .010   1.484   5.446   1.723  25.086   -.010    .074  43.725  96.352
  2089  13.393   5.365    .062   -.002   1.616   5.485   1.729  25.119   -.014    .057  44.065  96.876
  2090  13.415   5.260    .057   -.012   1.570   5.468   1.726  25.027   -.004    .074  43.825  96.406
  2091  13.295   5.477    .049   -.016   1.491   5.441   1.730  25.173   -.002    .062  43.808  96.508
  2092  13.438   5.538    .063   -.043   1.750   5.475   1.654  25.087   -.003    .082  44.436  97.477
  2093  13.218   5.347    .061   -.019   1.310   5.480   1.627  25.200   -.009    .069  43.420  95.705
  2094  13.321   5.324    .056   -.001   1.576   5.436   1.792  25.063   -.028    .062  43.823  96.425
  2095  13.563   5.411    .059   -.015   1.662   5.476   1.768  24.963   -.004    .066  44.066  97.016
  2096  13.126   5.227    .057   -.001   1.702   5.403   1.734  25.097    .002    .073  44.027  96.446
  2097  13.258   5.348    .056    .007   1.829   5.441   1.755  25.101   -.021    .074  44.442  97.290
  2098  13.319   5.250    .064   -.037   1.540   5.452   1.793  25.015   -.001    .071  43.697  96.164

AVER:   13.294   5.355    .059   -.013   1.562   5.440   1.733  25.105   -.008    .067  43.860  96.454
SDEV:     .127    .099    .004    .014    .193    .029    .057    .093    .009    .008    .435    .697
SERR:     .028    .022    .001    .003    .043    .007    .013    .021    .002    .002    .097
%RSD:      .95    1.84    6.03 -103.97   12.34     .54    3.27     .37 -110.91   11.96     .99
STDS:      104      17      17    4001      43      48    7000      48     150      17     ---

STKF:    .3213   .2702   .2216   .8671   .4010   .0236   .6301   .1232   .9072   .2090     ---
STCT:   4130.0   507.0  6480.7  3089.1  1627.6  1219.3  5055.2  3686.3  5079.2  2226.0     ---

UNKF:    .0776   .0489   .0005  -.0001   .0013   .0304   .0135   .1541  -.0001   .0004     ---
UNCT:    997.5    91.7    13.7     -.3     5.2  1574.0   108.5  4608.8     -.4     4.4     ---
UNBG:      4.5     1.2     8.9     6.3     3.6    22.1    40.4     7.3     8.8     2.7     ---

ZCOR:   1.7134  1.0960  1.2587  1.3472 12.1592  1.7891  1.2807  1.6296  1.0996  1.6065     ---
KRAW:    .2415   .1808   .0021  -.0001   .0032  1.2908   .0215  1.2502  -.0001   .0020     ---
PKBG:   223.84   74.98    2.54     .95    2.50   72.09    3.68  634.63     .95    2.64     ---

TDI%:    5.440    .000    .000    .000    .000    .000    .000  -2.139    .000    .000     ---
DEV%:       .2      .0      .0      .0      .0      .0      .0      .1      .0      .0     ---
TDIF:  LOG-LIN    ----    ----    ----    ----    ----    ---- LOG-LIN    ----    ----     ---
TDIT:    59.75     .00     .00     .00     .00     .00     .00   48.60     .00     .00     ---
TDII:    1002.    ----    ----    ----    ----    ----    ----   4612.    ----    ----     ---
TDIL:     6.91    ----    ----    ----    ----    ----    ----    8.44    ----    ----     ---

Note that we did fix a minor bug that was preventing analysis of combined standard samples, but this is fixed in the latest Probe for EPMA update. Update as usual from the PFE Help menu.

The advantage of this method is that one can acquire all their samples with some elements at one keV, and then acquire different elements at a different keV (or beam current, say for trace elements) and then combine them later.

This method also allows one to acquire TDI intensities on multiple elements on the same spectrometer!

SamBroom-Fendley · January 21, 2025, 08:06:58 AM

Hello folks,

Long time reader, first time poster.

I've been playing around with combining analyses recently in order to measure minor-to-trace HREE at a higher beam current after analysing a mineral for major elements.

I would like to to know if there is a way to combine multiple pairs of analyses in one go. At present, I am selecting the two analyses I want to combine (the major elements and the trace HREE data) and combining 1 sample at a time.

What I would ideally like to do is to instruct the software to combine analyses 1-50 with analyses 51-100. So, for example, analysis 1 should be combined with analysis 51; analysis 2 should be combined with 52... and so on.

Thanks for any help

Sam

John Donovan · January 21, 2025, 09:04:41 AM

Quote from: SamBroom-Fendley on January 21, 2025, 08:06:58 AMI've been playing around with combining analyses recently in order to measure minor-to-trace HREE at a higher beam current after analysing a mineral for major elements.

I would like to to know if there is a way to combine multiple pairs of analyses in one go. At present, I am selecting the two analyses I want to combine (the major elements and the trace HREE data) and combining 1 sample at a time.

What I would ideally like to do is to instruct the software to combine analyses 1-50 with analyses 51-100. So, for example, analysis 1 should be combined with analysis 51; analysis 2 should be combined with 52... and so on.

Sorry to say there is no way to automate combining samples for analysis at this time.

What I suggest is using the "combined conditions" feature in Probe for EPMA where you can assign different beam conditions for different elements:

https://smf.probesoftware.com/index.php?topic=5.0

Click on the Combined Conditions button in the Acquire! window and assign beam conditions as desired. You'll want to group elements with similar conditions together and I also suggest acquiring the high beam current elements after the lower beam current elements.

The advantage of this method is that it doesn't depend on the reproducibility of your stage. Though you'll want to be sure that your electron column is properly aligned and the beam spot doesn't shift when changing beam currents (usually not a problem unless changing the electron energy).

SamBroom-Fendley · January 21, 2025, 12:47:04 PM

Super - thanks John.

Sam

News:

Trying to combine selected samples