[Ifeffit] Stoichiometry from EXAFS data
Peter Zalden
zalden at physik.rwth-aachen.de
Mon Aug 2 07:51:57 CDT 2010
Hi Scott,
thanks a lot for your quick response! I found your suggestion very
helpful and tried to change the edge step to both extremes by tuning the
fitting range for the pre- and post-edge lines in Athena. Due to the
very flat structure in the XANES range (cf. attachement), I could modify
the value for the edge step by 3% total, which corresponds to an error
of +/-2%. One could possibly discuss if this value represents the
one-sigma or maybe the two-sigma interval, but the error is nicely small
anyway.
In the last campaign, we measured a sample of Sb_2Te_1 in two different
annealing conditions and from those different data sets (as concerns the
EXAFS range), I determined the stoichiometries: Sb_2.06Te_0.94 and
exactly the same for the second sample. Therefore, a sub-5% error seems
reasonable to assume for these semi-metallic systems.
Concerning the influence of higher harmonics: The beam was usually
detuned to 70% intensity of the main reflection so that this should not
have a strong influence, since the amount of detuning was not changed
for both edges.
Best regards,
Peter
Am 02.08.2010 12:52, schrieb Scott Calvin:
> Hi Peter,
>
> I've done this as well, and compared to reliable methods (e.g. ICP).
> I'd be skeptical of 1%. It's generally quite difficult to determine
> edge steps to that accuracy. Assuming you're using Athena to determine
> the edge step, find the most extreme pre- and post-edge lines that
> seem acceptable and note the range of edge steps. That will yield an
> uncertainty range.
>
> If you have strong features at the white line and just past it, I'd be
> surprised if you can do much better than 10%. If features in that
> region are small, such as you might have in an intermetallic alloy,
> then you might get down to the sub-5% range.
>
> While I think that determining the edge step is likely the major
> source of error, you also have to be aware of the usual suspects in
> XANES analysis, such as the presence of harmonics in transmission or
> self-absorption in fluorescence. Testing for linearity with tricks
> like putting sheets of aluminum foil before I0 can help detect some
> (but not all) of those kinds of issues.
>
> --Scott Calvin
> Sarah Lawrence College
>
> On Aug 2, 2010, at 4:03 AM, Peter Zalden wrote:
>
>> Dear Feff users,
>>
>> lately, we measured a sample containing Sb and Te at EXAFS beamline
>> CEMO, Hasylab and are wondering whether one can determine the
>> stoichiometry from the height of the different K edges´ steps, if one
>> normalizes the values on the edge steps of the elements (cf.
>> http://physics.nist.gov/PhysRefData/XrayMassCoef/tab3.html). The
>> absorption gases and the specimen were not changed for the different
>> K edges.
>> Of course, I have already tried doing so and from statistical
>> reproducibility and from the resulting values compared to the
>> expected ones I would estimate an error of this method of about 1%. A
>> source of error that I could imagine originates from the different
>> beam position at different energies combined with a slight
>> inhomogenity in the pressed sample powder. Now my question is: Are
>> there any other sources of error that I should take into accout? Is
>> there any reference on this method from a more experienced user that
>> I could cite?
>>
>> Kind regards,
>> Peter
>
> _______________________________________________
> Ifeffit mailing list
> Ifeffit at millenia.cars.aps.anl.gov
> http://millenia.cars.aps.anl.gov/mailman/listinfo/ifeffit
>
-------------- next part --------------
A non-text attachment was scrubbed...
Name: sb_sb2te_c_edge_step.png
Type: image/png
Size: 12934 bytes
Desc: not available
URL: <http://millenia.cars.aps.anl.gov/pipermail/ifeffit/attachments/20100802/fc935a4b/attachment.png>
-------------- next part --------------
A non-text attachment was scrubbed...
Name: te_sb2te_c_edge_step.png
Type: image/png
Size: 16922 bytes
Desc: not available
URL: <http://millenia.cars.aps.anl.gov/pipermail/ifeffit/attachments/20100802/fc935a4b/attachment-0001.png>
More information about the Ifeffit
mailing list