Author Topic: Light Element Crystal Refractive Index Values  (Read 24690 times)

David Steele

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Re: Light Element Crystal Refractive Index Values
« Reply #15 on: November 25, 2014, 07:37:05 PM »
Hi John,
Thanks for the info and corrections....  Yes (sorry) updated the Crystals.dat file, BUT I also updated the probe.ini file re the UseLastUnknownAsWavescansetup, and other (magnification) defaults.

The log window I snipped was in theory a brand new mdb.  However because I didn't want to reinvent the wheel yet again (having done that repeatedly over the past 5 months since our initial PfE install) I did the first unk setup in Acquire then immediately did a Load File Setup from an MDB that contained the same light elements as shown.  Is this (i.e. using existing data imported via the Load File Setup) why my new MDB isn't using the updated ini and crystals info??

If yes, it seems I really have to start (again) from scratch and not import anything into ANY new MDBs to have the updated config (ini/dat) file information used.  Can you confirm (yay/nay)?

Cheers,
David 

John Donovan

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Re: Light Element Crystal Refractive Index Values
« Reply #16 on: November 25, 2014, 07:54:03 PM »
Hi John,
Thanks for the info and corrections....  Yes (sorry) updated the Crystals.dat file, BUT I also updated the probe.ini file re the UseLastUnknownAsWavescansetup, and other (magnification) defaults.
OK, but (again) you mean the Probewin.ini file!

Sorry to be so pedantic, but as a programmer I know what a single stray character can do!  Much less three!

The log window I snipped was in theory a brand new mdb.  However because I didn't want to reinvent the wheel yet again (having done that repeatedly over the past 5 months since our initial PfE install) I did the first unk setup in Acquire then immediately did a Load File Setup from an MDB that contained the same light elements as shown.  Is this (i.e. using existing data imported via the Load File Setup) why my new MDB isn't using the updated ini and crystals info??

If yes, it seems I really have to start (again) from scratch and not import anything into ANY new MDBs to have the updated config (ini/dat) file information used.  Can you confirm (yay/nay)?
If you load the file setup from another MDB file into a new MDB file, guess what you get?    ;D

Yay!
john

PS One other route is to export the element setups from the sample to the element database (SETUP.MDB) using this button:



Then from the Acquire! | Elements/cations | Element setup dialog load them into the new MDB file.  This will prevent any globals, such as your wavescan flag from the Probewin.ini file from getting into the new run, but I'm pretty sure it will still bring in the crystal 2ds because those are at the element abstraction level.
« Last Edit: November 25, 2014, 08:02:25 PM by John Donovan »
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Les Moore

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Re: Light Element Crystal Refractive Index Values
« Reply #17 on: November 25, 2014, 09:27:21 PM »
Hi guys,

If you can get your hands on an ultralow C steel, or a Ti stabilised steel (even stainless steel).  It will have Ti, C, N, Fe, Cr and Ni lines and enable you to set up a 2 parameter regression on the one sample to calculate the d value and the refractive index.

I was surprised at how different the D val was on my PC2 Xtal. Can't find the calcs so cannot share :(
Les

David Steele

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Re: Light Element Crystal Refractive Index Values
« Reply #18 on: November 26, 2014, 03:56:45 PM »
Thanks for the suggestions Les.

I've done the calcs in Excel on a line-by-line basis.  Yes, I too am surprised re the differences between 'book' (aka JEOL Inspection Certificate) and 'real' d values for the LDE1 (PC1 - ca. 60Angstrom), LDE2 (PC2 - ca. 100A) and LDEB (ca. 144A) we have on our 8530F.

I won't say too much more as I would be pre-empting what I hope to present at AMAS-XIII (Hobart, Feb 2015) re my d investigations....

PS: IMHO it is a pity JEOL don't have a ca. 45Ang xtal (aka a PC0).

Cheers,
David

David Steele

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Re: Light Element Crystal Refractive Index Values
« Reply #19 on: December 04, 2014, 04:05:52 PM »
Unfortunately my d-spacing PfE updating saga continues  >:(

I've attached the a snipit showing the log output from (yet another) brand new mdb and the crystals.dat file saved immediately before creating the new mdb....  I remain very puzzled (the polite way of saying getting very p****d off with all this now!) to know why PfE is STILL seeing the legacy d-spacings while the crystals.dat file has different (more appropriate) d values stored and saved in it.

I have not imported/loaded ANYTHING into this new mdb following John's previous posting that doing so will simply carry (unwittingly or deliberately) legacy information with the import, from an element, sample, or file setup.  I fully understand this, hence my current frustration re WT* is going on!

In addition, before modifying the crystals.dat file I deliberately closed the PfE application, then editted the crystals.dat file, then restarted the PfE application, then created the brand new mdb. Then created Un 1 as the initial setup, then the first wavescan sample (WA 1).  With the incorrect d-spacings (CRY2D) seemingly in place viz the log window output I haven't progressed any further.

"All" I want to do is rescan a few samples with the new d-spacings to check the KLM markers are much closer to the measured peaks than when using the default d-spacings  :'(

So near, yet so far.....

David

John Donovan

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Re: Light Element Crystal Refractive Index Values
« Reply #20 on: December 04, 2014, 04:19:25 PM »
Unfortunately my d-spacing PfE updating saga continues  >:(

I've attached the a snipit showing the log output from (yet another) brand new mdb and the crystals.dat file saved immediately before creating the new mdb....  I remain very puzzled (the polite way of saying getting very p****d off with all this now!) to know why PfE is STILL seeing the legacy d-spacings while the crystals.dat file has different (more appropriate) d values stored and saved in it.

In addition, before modifying the crystals.dat file I deliberately closed the PfE application, then editted the crystals.dat file, then restarted the PfE application, then created the brand new mdb. Then created Un 1 as the initial setup, then the first wavescan sample (WA 1).  With the incorrect d-spacings (CRY2D) seemingly in place viz the log window output I haven't progressed any further.

"All" I want to do is rescan a few samples with the new d-spacings to check the KLM markers are much closer to the measured peaks than when using the default d-spacings  :'(

Hi David,
Well first of all, this works fine as I just tested it.

Here is the sample with the original 2d spacing:

Wa    1 wavescan sample
TakeOff = 40.0  KiloVolt = 15.0  Beam Current = 30.0  Beam Size =    0
(Magnification (analytical) =   4000),        Beam Mode = Analog  Spot
(Magnification (default) =      200, Magnification (imaging) =    100)
Image Shift (X,Y):                                        -2.00,  3.00

Normal Wavescan: Step/Count Scan
Number of Data Lines:   0             Number of 'Good' Data Lines:   0

ELEM:  Spectro    o ka   BEAM
BRAGG:               1
SPEC:                3
CRYST:           WSI60
CRY2D:         61.0000
CRYK :         .014830

And after editing the Crystals.dat file and creating a new probe run database, here is my sample with the newly edited 2d spacing in the crystals.dat file:

Wa    1 wavescan sample
TakeOff = 40.0  KiloVolt = 15.0  Beam Current = 30.0  Beam Size =    0
(Magnification (analytical) =   4000),        Beam Mode = Analog  Spot
(Magnification (default) =      200, Magnification (imaging) =    100)
Image Shift (X,Y):                                        -2.00,  3.00

Normal Wavescan: Step/Count Scan
Number of Data Lines:   0             Number of 'Good' Data Lines:   0

ELEM:  Spectro    o ka   BEAM
BRAGG:               1
SPEC:                3
CRYST:           WSI60
CRY2D:         60.5000
CRYK :         .014830


One problem I can see is that you are editing the Crystals.dat.txt file, not the Crystals.dat file!   ???
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David Steele

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Re: Light Element Crystal Refractive Index Values
« Reply #21 on: December 04, 2014, 04:30:42 PM »
OK, how do I edit the crystals.dat file without using a text editor?

In my very last attempt, I editted the crystals.dat file using Notepad++, it was saved as crystals.dat.txt (as you point out) BUT I then renamed it crystals.dat.  That is the file (name) stored in the ProbeSoftware directory.

David

John Donovan

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Re: Light Element Crystal Refractive Index Values
« Reply #22 on: December 04, 2014, 04:36:32 PM »
OK, how do I edit the crystals.dat file without using a text editor?

Any text editor will work. I use TextPad, but NotePad works fine too. Just be sure to save it as crystals.dat not crystals.dat.txt!

In my very last attempt, I editted [sic] the crystals.dat file using Notepad++, it was saved as crystals.dat.txt (as you point out) BUT I then renamed it crystals.dat.  That is the file (name) stored in the ProbeSoftware directory.

Also it needs to be in the Probe Software\Probe for EPMA folder, not the Probe Software folder!

Well, you might want to double check your work because it looks like "who-man" error to me... I should know, I've made more than my share of "who-man" errors!
« Last Edit: December 04, 2014, 04:43:21 PM by John Donovan »
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David Steele

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Re: Light Element Crystal Refractive Index Values
« Reply #23 on: December 04, 2014, 11:52:57 PM »
John is correct....  "who-man" error, or "the nut on the keyboard" if you have a more computer-oriented inclination!  :-[

All working now with the appropriate d-spacings.

I have to be much more careful with Notepad+++ and how the files are saved.  I suspect I've done a "Save As" and Notepad++ has added the .txt suffix.  What I should do is update (any) .dat file in Notepad++ but simply "Save" it.  Any additional copies (i.e. for off-probe users of PfE) should be simple copies of the file in the ProbeSoftware directory rather than saved from Notepad++....

Live and learn, and hopefully remember all these issues :)

Unfortunately my Memory seems to be increasingly more "Random" and less "Access" as time goes by....

Cheers,
David
 
« Last Edit: December 06, 2014, 12:12:04 PM by John Donovan »

David Steele

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Re: Light Element Crystal Refractive Index Values
« Reply #24 on: December 14, 2014, 03:58:20 PM »
My contributions to the crowd source:

LDE1 (nom. 60A): dcalc = 61.05 A, k = 0.013  (The JEOL inspection certificate I received gives 60.1 A, and no value for k)

LDE2 (nom. 100A): dcalc = 101.66 A, k = 0.034  (The JEOL inspection certificate I received gives 98.6 A, no value for k)

LDEB (nom. 145A): dcalc = 148.11 A, k = 0.034  (The JEOL inspection certificate I received gives 144.0A, and no value for k)

These values were determined iteratively using Excel (but not using Julien's macro, which I've only just seen - today (Dec 15th...)).  I'll give Julien's macro a run sometime "soon" (i.e. before AMAS-XIII in Feb next year) and see how the sets of d and k actually compare!  I presume the macro is multi-lingual, i.e. conversant with JEOL-speak L (mm) values and not just CAMECA-speak sinthetas??

Rescans in a new MDB using the above info in the crystals.dat file gives Plot! KLM markers that fit very well on the LDE1 and LDE2 crystals, but the KLMs on the LDEB using 148.11 are still a little "off".  One thing I noted was a huge (2.6mm!) peak shift between BKa measured on B metal and BKa measured on BN.  The B metal gives a calculated d of 150.7, whereas the BN gives a calculated d of 148.72.  The latter is much closer to the values calculated from the higher order Ka peaks from Si, Al, Mg and O (using SiO2, Al2O3 and MgO), supplemented by various fluorides and pure metals (L lines....).

PS: Haven't got close to using CalcZAF, which was why I was puzzled where the peak position calculator was hiding.....

PPS: Yes curious the JEOL 100mm RC spectros use the same L mm value as the 140mm RCs!  Some behind the scenes jiggery-pokery from JEOL...

Cheers,
DAvid
QUT 

Mike Matthews

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Re: Light Element Crystal Refractive Index Values
« Reply #25 on: December 03, 2015, 01:28:02 PM »
Does anyone have the nominal 2d spacing value for the LDE6 multilayer crystal? Also, if anyone can tell me what the PC/LDE crystals are each made of it'd be interesting to know. The only one I have info so far is PC1/LDE1 (W/Si). I'm looking for PC3/LDE3, PC2.5/LDEB, PC2/LDE2, and PC0/LDE45.

P.S. I understand the reason JEOL use a Roland circle value of 140 rather than 100 to calculate the 'mm' values is so that they are consistent for a given element across all three spectrometer types.

Probeman

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Re: Light Element Crystal Refractive Index Values
« Reply #26 on: December 03, 2015, 02:05:12 PM »
Does anyone have the nominal 2d spacing value for the LDE6 multilayer crystal? Also, if anyone can tell me what the PC/LDE crystals are each made of it'd be interesting to know. The only one I have info so far is PC1/LDE1 (W/Si). I'm looking for PC3/LDE3, PC2.5/LDEB, PC2/LDE2, and PC0/LDE45.

P.S. I understand the reason JEOL use a Roland circle value of 140 rather than 100 to calculate the 'mm' values is so that they are consistent for a given element across all three spectrometer types.

I quote this from a preprint by Owen Neill:



http://www.minsocam.org/msa/ammin/AM_Preprints/5370McCloyPreprintFeb.pdf
The only stupid question is the one not asked!

Probeman

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Re: Light Element Crystal Refractive Index Values
« Reply #27 on: December 03, 2015, 02:44:12 PM »
And yes, L-values are consistent between 140 and 100m JEOL spectros, so (for example) Fe Ka is at ~134.7mm on both types of spectros.

There is a cute little dialog in CalcZAF for calculating nominal spectrometer positions for both Cameca and JEOL (all three spectrometer types) that is accessed from the X-Ray menu as described here:

http://probesoftware.com/smf/index.php?topic=375.msg1990#msg1990

You can try different refractive indices to see the effect, or not use any refractive index correction...
The only stupid question is the one not asked!

Probeman

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Re: Light Element Crystal Refractive Index Values
« Reply #28 on: December 03, 2015, 03:05:48 PM »
According to a sheet I found in a drawer:

LDE1 = W/Si, 60A
LDE2 = Ni/C, 100A
LDEN = W/Si, 80A
LDE3 = Mo/B4C, 200A
LDEB = Mo/B4C, 145A
LDE5 = Cr/Sc, 80A
LDE6 = Cr/C, 120A

This is a most excellent table for the 2D spacing and compositions of these JEOL analyzing crystals!

Does anyone have a similar table for Cameca instruments PC analyzing crystals?  I only have the nominal 2D spacings and refractive index values for these crystals:

"PC0"       45.0           0.006     
"PC1"       60.6           0.00832     
"PC2"       95.0           0.021     
"PC25"      147.66         0.02     
"PC3"       200.5          0.02       


For the PC25 crystal I "tuned" the 2D per John Fournelle's procedure here:

http://probesoftware.com/smf/index.php?topic=197.msg1732#msg1732

It's in the attachment at the bottom of the post.
« Last Edit: December 03, 2015, 03:13:17 PM by Probeman »
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Mike Matthews

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Re: Light Element Crystal Refractive Index Values
« Reply #29 on: December 04, 2015, 10:03:49 AM »
Thanks for the summary Owen, that's excellent.

John, my understanding is that both the JEOL and Cameca crystals come from the same supplier, they just name them differently, so the following are direct equivalents:

PC3 = LDE3
PC25 = LDEB
PC2 = LDE2
PC1 = LDE1
PC0 = LDE45

I'm not sure which PC, if any, is equivalent to LDE6 though.