[Ifeffit] Reported W L3-edge and L2-edge energy

Tue May 5 22:55:36 CDT 2020

On a tangentially related topic, I find that phosphorus K-edge XAS energy calibration conventions are still in a bit of a "Wild West" state, with a wide variety of materials and values in use for energy calibration. As an extreme example, one or two frequently cited papers in my field from the 2000s don't even report the material or value used for energy calibration, and only show portions of the spectra on an energy axis with values relative to an unknown E0.

I too have picked my own material and value, and will be the first to acknowledge that I did so out of necessity and ease of comparison to other available data, rather than because I thought it was correct.

The issue of calibration conventions and values definitely seems to be one that merits continued discussion. It has been interesting to watch things evolve over time in the case of iron, for example (it's good to know that 7110.75 is a candidate calibration value...) I appreciate Matt's detailed thoughts, and the data that he's been working with. Thanks Matt!

Cheers,

Mike

> On May 6, 2020, at 3:32 PM, Matt Newville <newville at cars.uchicago.edu> wrote:
> 
> 
> Hi Simon,
> 
> This is definitely a timely discussion for me, as I've been spending part of the quartine working on collating data and expanding datasets for an XAFS spectral database.  I'm hoping to have something ready for public comment and to start asking for contributions of data in a few weeks, but I'll be happy to have more discussion about that sooner too. 
> 
> I generally believe that the monochromator I use at GSECARS is both well-calibrated and reasonably accurate.  That is, with 2 angular encoders with a resolution of >130,000 lines per degree and an air-bearing, I believe the angular accuracy and repeatability are very good.  I believe there are equally good moons in existence.   As Matthew Marcus pointed to the Kraft paper (which used an older source but 4-bounce mono to improve resolution), we find that Fe foil is definitely better defined as 7110.75 and Cu foil is between 8980.0 and 8980.5 eV.  That is, we've measured multiple foils, found their first derivatives, and refined the d-spacing and angular offset.  We do this about once per run, and the offsets tend to be very consistent.   For sure, there is some question about whether the Kraft numbers are perfect.   For sure, putting Fe foil at 7110.75 +/- 0.25 eV appears to be "most right" to us.
> 
> I also believe that we should probably re-measure these metal foils (and other compounds) with a single calibration set for both Si(111) and Si(311).  We will probably have time to do that this summer in the time between "beamline staff can get back to the beamline" and "open for outside users".
> 
> What I can tell you now is:  I have some data on W metal, WO2, and WO3 measured all at the same time on our bending magnet line, with Si(111).  An Athena project for this is attached (W.prj).   I cannot vouch for the absolute calibration. 
> 
> I also attach a set of foils (V, Fe, Cu, Mo) measured with the same calibration (and Si(111) on our ID line), after adjusting d-space and offset to be close to the Kraft values (CalibratedFoils2013.prj). 
> 
> I also attach a set of foils (Fe, Cu, Au L3, Au L2, Au L1, Pb L3, Pb L2, Pb L1 edges) measured in 2016 (again, using Si(111) on our ID line), also with the same calibration values (FeCu_Au_Pb.prj).  I'm pretty certain these use the same d-spacing as the 2013 Foils to at least 5 digits.   For completeness, all of the raw data files are also under https://github.com/XraySpectroscopy/XASDataLibrary/tree/master/data
> 
> In my experience, the Pb L3 edge value has the biggest variation in the literature, with values ranging from 13035 to 13055 eV (possibly a typo somewhere along the line).  Fortunately, the Kraft-based calibration splits the difference and puts the value at 13040 eV.
> 
> For W in particular, I will look if I have measured this recently on our ID line.  I can tell you that I use CdWO4 as a phosphor and use that to focus our X-ray beam.   I use this trick all the time: any tail from the beam penetrating the phosphor is shortest at the peak of the white-line and for CdWO4 that is always between 10210 and 10215 eV.
> 
> I hope that helps.  I am interested in trying to get all these values as accurately as possible, so any comments or suggestions would be most welcome.
> 
> --Matt
> 
> 
> 
> 
> 
> 
> 
> 
> 
>> On Tue, May 5, 2020 at 5:14 PM Bare, Simon R <srbare at slac.stanford.edu> wrote:
>> All:
>> 
>>  
>> 
>> We are wondering if others agree that the reported values for the W L3 and W L2 edges are incorrect. We recently noticed the following:
>> 
>>  
>> 
>> The “Edge” – defined by the inflection point of the absorption edge step
>> 
>>  
>> 
>> When using the Ir L3 edge (11215.0 eV) as a calibration, the W L3- and L2-edges are 10203.4 eV and 11542.4 eV, respectively.  
>> 
>>  
>> 
>> When using the Pt L3 edge (11564.0 eV) as a calibration, the W L3- and L2-edges are 10203.3 eV and 11542.4 eV, respectively.
>> 
>>  
>> 
>> These observations are thus different than the reported values of 10207.0 eV and 11544.0 eV for the L3 and L2 edges, respectively.
>> 
>>  
>> 
>> Thanks in advance for the discussion and feedback.
>> 
>>  
>> 
>>  
>> 
>> Simon R Bare
>> 
>> Distinguished Scientist
>> 
>> SSRL, MS69
>> 
>> SLAC National Accelerator Lab
>> 
>> 2575 Sand Hill Road
>> 
>> Menlo Park CA 94025
>> 
>>  
>> 
>> simon.bare at slac.stanford.edu
>> 
>> Ph: 650-926-2629
>> 
>>  
>> 
>> <image001.png>
>> 
>>  
>> 
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> 
> 
> -- 
> --Matt Newville <newville at cars.uchicago.edu> 630-252-0431
> <W.prj>
> <CalibratedFoils2013.prj>
> <FeCu_AuPb.prj>
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