Quote from: Probeman on March 13, 2026, 04:02:19 PM...And yes, there are a few "black holes" in the periodic table that may require a roughly similar matrix, e.g., Si Ka in Hf due to disagreement in mass absorption coefficients.  But geological silicates and oxides are pretty well handled by modern matrix corrections."

While Andrew Ducharme and I are waiting for some time on the instrument, I decided to take a look back at some old runs I did on our old SX50 (which has long been scrapped), and see if I examined any of the synthetic silicates standards we had obtained from various sources when I was at UC Berkeley. I found the following run from 2014 when I was still using differential PHA tuning, which we now know produces less accurate results as described here:

https://smf.probesoftware.com/index.php?topic=1831.msg13978#msg13978

So while we wait to re-run these materials using SiO2 as the primary standard on our Sx100, here are the results from the Evaluate program for Si Ka in these materials:

https://smf.probesoftware.com/index.php?topic=340.0

2  St   12 Set   1 MgO synthetic                         
3  St   14 Set   1 SiO2 synthetic                        
4  St   16 Set   1 ThSiO4 (Thorite)                      
5  St   19 Set   1 HfSiO4 (Hafnon)                       
6  St   25 Set   1 MnO synthetic                         
7  St  257 Set   1 Zircon crystal (synthetic)            
8  St  263 Set   1 Fe2SiO4 (synthetic fayalite)          
9  St  272 Set   1 Ni2SiO4 (synthetic)                   
10  St  273 Set   1 Mg2SiO4 (magnesium olivine) synthetic
11  St  274 Set   1 Co2SiO4 (cobalt olivine) synthetic   
12  St  275 Set   1 Mn2SiO4 (manganese olivine) synthetic
13  St  358 Set   1 Diopside (Chesterman)                
14  St  386 Set   1 Alamosite (PbSiO3)                   

The big outlier is Si Ka in HfSiO4 (hafnon) synthesized by John Hanchar. Note the 45% relative accuracy in the quant:

St   19 Set   2 HfSiO4 (Hafnon), Results in Elemental Weight Percents

SPEC:       Th      Hf      Pb      Co      Ni      Zr      Al      Ca      Ti       O
TYPE:     SPEC    SPEC    SPEC    SPEC    SPEC    SPEC    SPEC    SPEC    SPEC    SPEC

AVER:     .000  65.967    .000    .000    .000    .000    .000    .000    .000  23.653
SDEV:     .000    .000    .000    .000    .000    .000    .000    .000    .000    .000
 
ELEM:       Si      Mg      Mn      Fe
BGDS:      MAN     MAN     MAN     MAN
TIME:    60.00   60.00   60.00   60.00
BEAM:    30.13   30.13   30.13   30.13

ELEM:       Si      Mg      Mn      Fe   SUM  
    86  15.092    .026    .043    .032 104.813
    87  15.126    .024    .030    .035 104.835
    88  15.122    .029    .038    .039 104.848
    89  15.094    .027    .039    .031 104.811
    90  15.078    .025    .047    .030 104.799

AVER:   15.102    .026    .040    .034 104.821
SDEV:     .021    .002    .006    .004    .020
SERR:     .009    .001    .003    .002
%RSD:      .14    6.98   15.97   10.86

PUBL:   10.380    n.a.    n.a.    n.a. 100.000
%VAR:    45.49     ---     ---     ---
DIFF:    4.722     ---     ---     ---
STDS:       14      12      25     395

STKF:    .3884   .4222   .7420   .6869
STCT:  1002.33  906.18  379.64  336.38

UNKF:    .0565   .0002   .0004   .0004
UNCT:   145.83     .35     .21     .18
UNBG:     2.03    1.43     .89    1.10

ZCOR:   2.6725  1.6261   .9765   .9241
KRAW:    .1455   .0004   .0005   .0005
PKBG:    72.96    1.24    1.23    1.16

This is because of the large absorption correction due to the Si Ka line being near the Hf M edge. The MAC from FFAST is only very slightly better. Remember in cases of large absorption corrections our matrix corrections are only as good as our mass absorption coefficients!

What I did at the time was to empirically measure the MAC for Si Ka in Hf using the method of Pouchou:

https://smf.probesoftware.com/index.php?topic=1340.msg9631#msg9631

After utilizing this experimental MAC from the EMPMAC.DAT file:

we now obtain these results:



Here for comparison is the HfSiO4 again:

St   19 Set   2 HfSiO4 (Hafnon), Results in Elemental Weight Percents

SPEC:       Th      Hf      Pb      Co      Ni      Zr      Al      Ca      Ti       O
TYPE:     SPEC    SPEC    SPEC    SPEC    SPEC    SPEC    SPEC    SPEC    SPEC    SPEC

AVER:     .000  65.967    .000    .000    .000    .000    .000    .000    .000  23.653
SDEV:     .000    .000    .000    .000    .000    .000    .000    .000    .000    .000
 
ELEM:       Si      Mg      Mn      Fe
BGDS:      MAN     MAN     MAN     MAN
TIME:    60.00   60.00   60.00   60.00
BEAM:    30.13   30.13   30.13   30.13

ELEM:       Si      Mg      Mn      Fe   SUM  
    86  10.924    .027    .039    .027 100.636
    87  10.950    .024    .025    .030 100.649
    88  10.947    .029    .034    .034 100.664
    89  10.925    .027    .035    .026 100.633
    90  10.914    .025    .042    .025 100.625

AVER:   10.932    .026    .035    .028 100.641
SDEV:     .016    .002    .006    .004    .015
SERR:     .007    .001    .003    .002
%RSD:      .14    7.01   17.95   12.71

PUBL:   10.380    n.a.    n.a.    n.a. 100.000
%VAR:     5.32     ---     ---     ---
DIFF:     .552     ---     ---     ---
STDS:       14      12      25     395

STKF:    .3884   .4222   .7420   .6869
STCT:  1002.33  906.18  379.64  336.38

UNKF:    .0562   .0002   .0004   .0003
UNCT:   145.00     .34     .18     .15
UNBG:     2.85    1.43     .91    1.13

ZCOR:   1.9456  1.6431   .9672   .9145
KRAW:    .1447   .0004   .0005   .0005
PKBG:    51.81    1.24    1.20    1.13

5% accuracy is a lot better than 45%!

The other silicates are all around ~1 to 2% accuracy. Can't wait to re-run these materials using integral PHA mode on a more modern instrument.

Quote from: anenburg on Today at 12:14:46 AM

Quote from: John Donovan on November 27, 2024, 06:02:13 PMHey, would someone be willing to acquire an x-ray map of an As,Pb sulfide and try to quantify it?   

Here's pyrite with some As zoning in it:

As K line mapped on LIF.
Same thing, Pb EDS map:

The galena shows up very well in the As map. As counts on galena are actually much higher, I truncated the max values so the As zoning in pyrite is actually visible.

I do not see any scale for concentrations in your maps.

Is this a map from a Probe for EPMA/CalcImage project?  Would it be possible to share the MDB, GRD and CIP files with me so I can look into it more?

Quote from: Les Moore on April 09, 2026, 05:20:35 PMThere's an added factor that would favor SDD over FC, recovery time.  Try mapping something with SiC in it with a Si Ka at 200nA with bidirectional mapping and you will see a saw tooth effect on the boundaries. The massive change in countrate must be saturating the detector such that it won't reliably measure the Si Ka when it drops back down.
 

Could you share a picture?

Excellent observation about saturation... but completely wrong tree to bark. What you are saturating is rather the preamplifier and not the gas flow chamber itself. Also, did this observation happened with correct PHA settings to compensate the PHA shift? The PHA shift will happen gradually at transition of grain boundary, as discharging the feedback capacitor (which gets near-full charged during very high count rate) of preamplifier needs some time.
This thread is about preamplifier design which is the weakest part in currently used GFPC. Replace the outdated preamplifier + shapping oamps and discrete pulse counters, and give modern electronics to GFPC and it will leave SDD in the dust with the performance.

Quote from: John Donovan on November 27, 2024, 06:02:13 PMHey, would someone be willing to acquire an x-ray map of an As,Pb sulfide and try to quantify it?   

Here's pyrite with some As zoning in it:

As K line mapped on LIF.
Same thing, Pb EDS map:

The galena shows up very well in the As map. As counts on galena are actually much higher, I truncated the max values so the As zoning in pyrite is actually visible.

There's an added factor that would favor SDD over FC, recovery time.  Try mapping something with SiC in it with a Si Ka at 200nA with bidirectional mapping and you will see a saw tooth effect on the boundaries. The massive change in countrate must be saturating the detector such that it won't reliably measure the Si Ka when it drops back down.
 

Quote from: Ben Buse on January 08, 2026, 07:37:47 AMHi Jacob, was that a Mitsubishi f940got-lwd-e controller, and do you have the program available, is it uploaded via rs232?

Sorry, I don't work there anymore. The f940got is just the touchscreen. The PLC is deeper in. A Mitsubishi FX3 something. Yes, it goes in via RS232 but you need Mitsubishi's software. At the time I wound up bypassing the touchscreen and using a few 24v buttons with indicator LEDs. 

Quote from: John Donovan on April 09, 2026, 01:51:46 PMBut yes, Anette learned a lot from getting the Bruker system up and interfaced to PFE, basically because the Bruker client/server configuration is waaaaay more complicated than it really needs to be (though it is very versatile!).

It's a little wild, isn't it? I really would like to know what strange instrument setups needed the full network client/server architecture.

Quote from: Jacob on April 09, 2026, 01:12:17 PMI'm sure my decision has caused Anette endless headaches trying to talk between Bruker, JEOL, and PfE, but I still think there's tremendous value in fast single instrument correlative automated mineralogy beyond the value of the stage scans.

I wouldn't say "endless headaches"! 

But yes, Anette learned a lot from getting the Bruker system up and interfaced to PFE, basically because the Bruker client/server configuration is waaaaay more complicated than it really needs to be (though it is very versatile!).

In the end she was able to write up a really nice set of configuration notes that we now distribute to customers buying the Bruker EDS with Probe for EPMA.  So that was a good outcome!

Software integration will always suffer with a third vendor in the mix. The Bruker team isn't always as responsive as they could be, especially to niche applications.

That said, when faced with the same dilemma, I chose to go with a dual Bruker EDS setup on the UBC iHP200F when we purchased it. One of the biggest reasons was so that we could integrate the Bruker AMICS (https://www.bruker.com/en/products-and-solutions/elemental-analyzers/eds-wds-ebsd-SEM-Micro-XRF/software-amics-automated-mineralogy-system.html) into the system. I'm sure there's value to combined stage WDS/EDS scans, but weighing it against the value of a full automated mineralogy system, I'd take the latter.

I'm sure my decision has caused Anette endless headaches trying to talk between Bruker, JEOL, and PfE, but I still think there's tremendous value in fast single instrument correlative automated mineralogy beyond the value of the stage scans.

I asked Google: "why does Microsoft Defender think that .mdb files are dangerous?" and it replied:

QuoteMicrosoft Defender flags .mdb (Microsoft Access Database) files as dangerous because they can contain malicious VBA macros, embedded scripts, or exploit vulnerabilities in the Jet Database engine to execute arbitrary code. As files capable of active scripting and data manipulation, they are classified as risky, particularly when downloaded or shared, to prevent trojans, ransomware, and unauthorized system access.

It's the same reason why Microsoft renamed the old Excel .XLS files to .XLSX (without macros) and .XLSM (with macros).

If you get this error (I do not with McAfee anti-virus), please follow Andrew Locock's instructions above.

By the way, all Probe for EPMA and CalcZAF MDB database files do NOT contain any macros, only static tables!