Author Topic: Multiple background "sharing"  (Read 14798 times)

Karsten Goemann

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Multiple background "sharing"
« on: July 04, 2013, 07:19:02 PM »
I was wondering if it would somehow be possible to "share" off-peak measurements between elements when doing multi-point background type work. I find when doing REEs with multi-point backgrounds I end up using the same absolute off-peak positions for some neighbouring elements and it seems a waste to use those counts only for one element at a time. That way time could be saved during acquisition and/or background measurement statistics could be improved.

Almost like a calibration curve sort of approach.

As far as can see so far this would have limitations similar to multi-point backgrounds in general (absorption edges, point selection for fitting...), but I expect the main issue would be how to handle this software-wise?

Cheers,

Karsten

John Donovan

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Re: Multiple background "sharing"
« Reply #1 on: July 07, 2013, 09:50:56 AM »
Hi Karsten,
Yes, exactly, a software implementation issue.

Since the dominant paradigm in the software is that each element is treated separately, there would have to be a sort of global table that these off-peak intensities would get stored in, and the user would have to view, select and assign them on a global basis.  Kind of like the MAN dialog, but for off-peaks.  A lot of work!

Essentially it would be a 4th (!) bgd method (in addition to the already existing off-peak, MAN and multi-point bgd methods).

I will have to ruminate on this for a while and see if I can think of some clever method to implement this.
john
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Mike Jercinovic

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Multipoint background funtionality
« Reply #2 on: May 22, 2014, 01:46:21 PM »
OK, maybe we can start to think about increasing the efficiency and power of minor and trace element EPMA by expanding the capability of the multipoint background. 
Here is an example we deal with a lot in geochronology applications - The measurement of U in the presence of Th in monazite, xenotime, etc. is tricky business (lets assume we are not going to use Uranium La at high voltage).  U Ma is severely overlapped by Th Mb, and is further compromised by the Ar K edge if P10 is used.  U Mb is generally preferred due to less spectral interference and actually greater intensity than UMa in most circumstances (see attached figure).
 
Without getting into absorption edge issues in very high Th compositions, the remaining problem is the boundary fluorescence of potassium near interfaces with K-feldspar or micas.  The first-order interference of K with UMb is minor, but in the trace element realm, it's a problem, causing "too many" apparent U counts and therefore a slightly younger age at the rim (hooray, we just discovered a new event!).  So this is dealt with nicely as a mutual interference problem between UMb and KKa.  So now it is interesting because the best way to characterize this complex background region is via the multipoint acquisition.  Works fantastically well (see second attachment), but here is the problem, we measure all these background points for the U measurement, and characterize the background in this spectral region very accurately.  If we want to do a K measurement the same way on the same spectrometer, we would have to re-collect this multipoint acquisition.  So why not use that regressed background data (from the U measurement) for the K measurement on the same spectrometer also - just move the peak position from U to K?  Why do an independent background acquisition for K - we already have the data!  In fact, if I wanted too, I could use the ThMg line with this same background measurement, just at a different wavelength for the analytical line?  This could be very powerfully applied in other minor element situations where measured lines are in the same spectral region (REEs?).

It seems odd to me when we measure the full suite of rare earths to measure 15 analytical lines that we have to do 30 background acquisitions in the classical two-point interpolation method (two backgrounds per element), when we could probably characterize broad ranges of background very accurately with less than half that actual number of background measurements with a multipoint approach.

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Re: Multiple background "sharing"
« Reply #3 on: May 22, 2014, 10:07:29 PM »
Hi Mike,
You guys are killing me!   :'(

I do agree though, the ideas you and Karsten present above are totally valid. These concepts would save x% time, if implemented...

But implementation is the problem. Consider that this proposed shift from a "single" element model to a "sparse spectrum" model is a paradigm shift similar in magnitude to the "instrument centric" to "sample centric" approach I take in our software as described here:

http://probesoftware.com/download/Instru-vs-sample-centric.ppsx.

For example, each element would have to be measured under the same PHA conditions to "share" backgrounds. Then there's the question of peak integrals...

Also I estimate the amount of work necessary for this "sparse spectrum" implementation would be larger than the MPB implementation was (~6 months of work).  But rather than open up new vistas for further investigation, I suspect it will only save some time. Could I be convinced otherwise? Of course. But I would sure like to see a more tangible rationale than merely saving time.

I've got several current projects that will improve accuracy and precision (while also reducing acquisition time) and they seem more attractive to me at the moment (see attachment below).

I'm willing to discuss it.   :)
« Last Edit: May 23, 2014, 08:36:04 AM by John Donovan »
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Philipp Poeml

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Re: Multiple background "sharing"
« Reply #4 on: July 03, 2014, 06:46:13 AM »
I just programmed 48 lines into PfE all with multipont background. I really would like to have this feature. Now the software will measure 48 x 4 background positions. In my case it could measure 4 x 4 and that would be it. Saves a HUGE amount of time.

If one day you find the time John...

Cheers
Ph

Mike Jercinovic

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Re: Multiple background "sharing"
« Reply #5 on: July 03, 2014, 08:06:43 AM »
Yes, I realize there may be a lot of work in implementation, but we should be talking about this seriously.  I mention the U-Mb K-Ka measurement, which in monazite becomes more than an efficiency argument, but is also an accuracy question because of beam exposure time on a beam sensitive material.  This is an important justification for the on peak time fraction too.  Efficiency, however, is a very good reason when you are talking about doubling (or more) the analysis time for trace element analysis.  Those of us who deal a lot with commercial customers are always working this aspect to maintain an attractive cost structure.  To them, they don't want to hear so much about being sample-centric as much as being customer-centric...not that our academic or government customers are that much less cost/efficiency conscious.  Believe me, I think about this every time I write another proposal support letter where they want to know how much it is going to cost to do a full monazite work-up per thin section for their budget.  As such, we simply just don't do as good a job with U and K measurements as we think we could do if this background sharing was possible.

Anette von der Handt

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Re: Multiple background "sharing"
« Reply #6 on: July 03, 2014, 10:24:15 AM »
Hi,
Wouldn't it be possible to have an offline processing work-around solution for the time being? Like only program the 4X4 backgrounds, run the other elements only on the peak, export the data, copy background counts to the other elements and import the data again. Not elegant, and definitely would need a script to make it truly efficient.
« Last Edit: July 03, 2014, 11:13:41 AM by John Donovan »
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Re: Multiple background "sharing"
« Reply #7 on: July 03, 2014, 11:22:17 AM »
Hi,
Wouldn't it be possible to have an offline processing work-around solution for the time being? Like only program the 4X4 backgrounds, run the other elements only on the peak, export the data, copy background counts to the other elements and import the data again. Not elegant, and definitely would need a script to make it truly efficient.

Well, of course almost everything is possible... but practical?  That is tougher. However, has anyone ever noticed that the bathroom is a great place to get new ideas?   ;)    Here's mine:

The problem as I see it is in creating an entire new infrastructure to handle this multi-element off-peak implementation. But what if we could use a software infrastructure that already exists?  Hmmm...

For example, we already have a multi-point background array. So what if the user acquires normal off-peak backgrounds on a number of elements on the same spectrometer, using the same crystal, using the same PHA settings? And then what if there was a flag that the user could flip that would force the data routines to automatically search for other elements on the same spectro/crystal/PHA combination and load their off-peak intensities into the multi-point arrays, along with the off-peak intensities from the element in question?

So, it would be a sort of "dynamic" multi-point background correction which utilizes multiple elements off-peaks.  Let's chat about this at IUMAS...

Edit by John: Another idea somewhat along the lines that Anette suggested: write some code that, for the selected samples, searches for any additional off-peak backgrounds from other elements (same spectro/xtal/PHA) (within some range criteria?) which is then written to the sample multi-point background (MPB) arrays. The sample could then be treated just as any other normally acquired MPB sample.

Of course, this could not be used for samples already with MPB intensities, only those with off-peak intensities.... dang, someone owes me a beer!
« Last Edit: July 03, 2014, 01:33:29 PM by John Donovan »
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Re: Multiple background "sharing"
« Reply #8 on: July 03, 2014, 03:56:32 PM »
Ok, I took a look at the code and this shouldn't be all that hard, maybe a few days work.

Let's discuss some of these ideas at IUMAS and decide what kind of parameters (such as the spectrometer range) need to be specified.
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Karsten Goemann

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Re: Multiple background "sharing"
« Reply #9 on: July 03, 2014, 04:20:40 PM »
John, I think that is a great idea. Spectro range is probably the main parameter. It would be important that the same options are available for processing, e.g. forcing specific backgrounds in/out, but if it is treated as a "normal" multi-bg measurement after the background data has been copied from the off-peak to the multi-peak database that should be the case, right?

Edit by John: Yes, I think that should all follow.
« Last Edit: July 03, 2014, 06:53:56 PM by John Donovan »

Mike Jercinovic

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Re: Multiple background "sharing"
« Reply #10 on: July 04, 2014, 09:13:20 AM »
This is all starting to sound very interesting!

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Re: Multiple background "sharing"
« Reply #11 on: August 15, 2014, 03:43:10 PM »
OK, I have a beta version of the "shared" background method implemented in v. 10.4.4 of Probe for EPMA.

To test this you'll need several elements measured on the same spectrometer at the same keV, using the same crystal. Acquire normal off-peak bgds as you typically might for a number of elements that are positionally grouped somewhat together in the spectrometer range, though one could use the entire spectrometer range in principle.

Then go to the Analyze! window and click the Data button to see the normal on and off-peak intensities as seen here:



Now click the Search For "Shared" Bgds button and the program will search for other elements which might have off-peak intensities measured on the same spectrometer/crystal combination and if so, the program will save them to the multi-point background arrays as seen here:



Now, go to the Run | Display MultiPoint Background Intensities menu and you will see the "shared" backgrounds for La La as seen here:



and for Ce La as seen here:



Note that all element peak intensities are now utilizing multiple off-peak bgds. To return your sample to its original state you can use the Remove "Shared" Bgds button as seen here:

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Probeman

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Re: Multiple background "sharing"
« Reply #12 on: August 16, 2014, 10:51:39 AM »
Here's a "quant" example of shared backgrounds on pyrite where both K and Cl share the same crystal, spectrometer, etc *and* were acquired at different beam currents (the code seems to handle it fine).

First, just the normal off-peak intensities:

On-Peak (off-peak corrected) or MAN On-Peak X-ray Counts (cps/1nA) (and Faraday Current):
ELEM:    na ka   si ka    k ka   al ka   mg ka   fe ka   ca ka    s ka   cl ka   ti ka    p ka    f ka
BGD:       MAN     MAN     OFF     MAN     MAN     MAN     MAN     OFF     OFF     OFF     OFF     OFF
SPEC:        1       2       3       4       1       5       2       2       3       5       4       1
CRYST:     TAP    LPET    LPET     TAP     TAP     LIF    LPET    LPET    LPET     LIF     TAP     TAP
ORDER:       1       1       1       1       2       1       2       3       2       2       2       3
  146G    1.20    4.27     .12    2.06    1.59  429.61    4.95  101.40    -.04     .15    -.06    -.02
  147G    1.07    4.16     .06    2.16    1.53  431.27    4.98  100.90     .04     .08    -.05     .02

AVER:     1.14    4.22     .09    2.11    1.56  430.44    4.97  101.15     .00     .12    -.05     .00
SDEV:      .09     .08     .04     .07     .04    1.17     .02     .35     .06     .05     .01     .03
1SIG:      .06     .12     .16     .07     .07    1.03     .16     .32     .03     .03     .02     .02
SIGR:     1.52     .67     .25     .90     .55    1.14     .14    1.11    1.99    1.72     .28    2.00
SERR:      .07     .06     .03     .05     .03     .83     .02     .25     .04     .03     .00     .02
%RSD:     8.24    1.87   46.03    3.09    2.53     .27     .43     .35 1486.39   41.26  -12.42    ----

Off-Peak (calculated) X-ray Counts (cps/1nA):
ELEM:    na ka   si ka    k ka   al ka   mg ka   fe ka   ca ka    s ka   cl ka   ti ka    p ka    f ka
TYPE:     NONE    NONE  LINEAR    NONE    NONE    NONE    NONE  LINEAR  LINEAR  LINEAR  LINEAR  LINEAR
  146G    ----    ----    4.82    ----    ----    ----    ----    1.04     .89     .68     .57     .26
  147G    ----    ----    5.01    ----    ----    ----    ----     .95     .79     .71     .55     .26

AVER:     ----    ----    4.92    ----    ----    ----    ----    1.00     .84     .70     .56     .26
SDEV:     ----    ----     .13    ----    ----    ----    ----     .06     .07     .02     .01     .01


And again, but this time after clicking the Search For "Shared" Bgds button:

On-Peak (off-peak corrected) or MAN On-Peak X-ray Counts (cps/1nA) (and Faraday Current):
ELEM:    na ka   si ka    k ka   al ka   mg ka   fe ka   ca ka    s ka   cl ka   ti ka    p ka    f ka
BGD:       MAN     MAN     OFF     MAN     MAN     MAN     MAN     OFF     OFF     OFF     OFF     OFF
SPEC:        1       2       3       4       1       5       2       2       3       5       4       1
CRYST:     TAP    LPET    LPET     TAP     TAP     LIF    LPET    LPET    LPET     LIF     TAP     TAP
ORDER:       1       1       1       1       2       1       2       3       2       2       2       3
  146G    1.20    4.27     .11    2.06    1.59  429.61    4.95  101.40    -.04     .15    -.06    -.02
  147G    1.07    4.16     .07    2.16    1.53  431.27    4.98  100.90     .04     .08    -.05     .02

AVER:     1.14    4.22     .09    2.11    1.56  430.44    4.97  101.15     .00     .12    -.05     .00
SDEV:      .09     .08     .03     .07     .04    1.17     .02     .35     .06     .05     .01     .03
1SIG:      .06     .12     .16     .07     .07    1.03     .16     .32     .03     .03     .02     .02
SIGR:     1.52     .67     .19     .90     .55    1.14     .14    1.11    2.05    1.72     .28    2.00
SERR:      .07     .06     .02     .05     .03     .83     .02     .25     .04     .03     .00     .02
%RSD:     8.24    1.87   31.90    3.09    2.53     .27     .43     .35-5144.27   41.26  -12.42    ----

Off-Peak (calculated) X-ray Counts (cps/1nA):
ELEM:    na ka   si ka    k ka   al ka   mg ka   fe ka   ca ka    s ka   cl ka   ti ka    p ka    f ka
TYPE:     NONE    NONE   MULTI    NONE    NONE    NONE    NONE  LINEAR   MULTI  LINEAR  LINEAR  LINEAR
COEF1:    ----    ----  8.9270    ----    ----    ----    ----    ----  1.7870    ----    ----    ----
COEF2:    ----    ----  -.0001    ----    ----    ----    ----    ----   .0000    ----    ----    ----
COEF3:    ----    ----   .0000    ----    ----    ----    ----    ----   .0000    ----    ----    ----
  146G    ----    ----    4.83    ----    ----    ----    ----    1.04     .89     .68     .57     .26
  147G    ----    ----    4.99    ----    ----    ----    ----     .95     .79     .71     .55     .26

AVER:     ----    ----    4.91    ----    ----    ----    ----    1.00     .84     .70     .56     .26
SDEV:     ----    ----     .12    ----    ----    ----    ----     .06     .07     .02     .01     .01


In this particular (demo) example, the changes are slight, but consistent with what we would expect.  Let's try it on half a dozen REEs!
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Re: Multiple background "sharing"
« Reply #13 on: August 18, 2014, 05:16:43 PM »
Ok, got some quick off-peak data to test this shared bgd feature.  I tuned up Ti, V, Cr and Mn in LLIF on spec 3 and Zr, Nb and Mo on LPET using normal off-peaks.

Note that the Ti-Mn PHAs are set to different gains but the Zr-Mo PHAs are all set the same.  I just wanted to see what difference that might make- I'll need to do additional tests however. This is just a first cut with some real data.

On and Off Peak Positions:
ELEM:    ti ka    v ka   cr ka   mn ka   zr la   nb la   mo la
ONPEAK 68218.0 62147.0 56844.0 52178.0 69413.0 65459.0 61831.0
OFFSET 73.3984 62.1328 54.5156 54.9023 -25.875 -29.016 -32.949
HIPEAK 69104.3 62971.8 57402.9 53019.4 71460.6 67408.4 63629.1
LOPEAK 67346.5 61415.9 56347.3 51041.6 67882.8 64334.6 60420.1
HI-OFF 886.297 824.801 558.898 841.398 2047.61 1949.38 1798.13
LO-OFF -871.50 -731.14 -496.70 -1136.4 -1530.2 -1124.4 -1410.9

PHA Parameters:
ELEM:    ti ka    v ka   cr ka   mn ka   zr la   nb la   mo la
DEAD:     3.80    3.80    3.80    3.80    3.25    3.25    3.25
BASE:      .56     .56     .56     .56     .56     .56     .56
WINDOW    4.00    4.00    4.00    4.00    4.00    4.00    4.00
MODE:       -1      -1      -1      -1      -1      -1      -1
GAIN:     700.    650.    600.    550.    800.    800.    800.
BIAS:    1850.   1850.   1850.   1850.   1300.   1300.   1300.

Last (Current) On and Off Peak Count Times:
ELEM:    ti ka    v ka   cr ka   mn ka   zr la   nb la   mo la
BGD:       OFF     OFF     OFF     OFF     OFF     OFF     OFF
BGDS:      LIN     LIN     LIN     AVG     LIN     LIN     LIN
SPEC:        3       3       3       3       2       2       2
CRYST:    LLIF    LLIF    LLIF    LLIF    LPET    LPET    LPET
ORDER:       1       2       3       4       1       2       3
ONTIM:   30.00   20.00   15.00   25.00   60.00   25.00   25.00
HITIM:   10.00    5.00    3.00    3.00   20.00    3.00    3.00
LOTIM:   10.00    5.00    3.00    3.00   20.00    3.00    3.00
UNFAC:       2       4       2       1       2       1       1
ONTIME   60.00   80.00   30.00   25.00  120.00   25.00   25.00
HITIME   20.00   20.00    6.00    3.00   40.00    3.00    3.00
LOTIME   20.00   20.00    6.00    3.00   40.00    3.00    3.00


This is for Ti Ka where the Search for "Shared" Bgds have been found and display in the multi-point bgd dialog from the Run menu:



and here is for V Ka:



What I find interesting is that the Ti background would have the wrong slope (due to the noise in the off-peak measurement), if we didn't have this "shared" bgd feature! 

Here are data for Zr La in Nb:

« Last Edit: July 27, 2015, 05:51:22 PM by John Donovan »
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Re: Multiple background "sharing"
« Reply #14 on: August 24, 2014, 08:17:40 PM »
If anyone would like to play with the above dataset, it is attached below.
john
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