Dear Luca,
the respect to your method was correctly referenced by Nicola in the
Profex user manual, p. 8, since this method was (partially) implemented:
https://www.profex-xrd.org/wp-content/uploads/2022/04/Profex-BGMN-Part-2-Application-EN.pdf
In fact Joerg Bergmann and me have also tried similar "FPSM" workflows
with BGMN/AUTOQUAN in the past, but without convincing results.
2020/2021 I discussed this issue and some experiences with Nicola. He
found your paper and decided to try the first step, the sequential
limited "Rietveld" fitting (restricted in parameter space of lattice
parameters and line broadening) within the BGMN algorithm and tools.
As you wrote, the primary limiting factor is computing time. So your
ultrafast algorithm is a real breakthrough!
However, in my experience the sorting of candidates according the FoM
criterion stays (as in traditional Search-Match procedures based on
peak positions) a source of wrong or suboptimal identification,
especially when disordered phases come into play or complicated real
rock samples showing hundreds of peaks must be analyzed. In the latter
case, simple cubic phases can be misidentified by chance, and
low-symmetry phases like feldspars are sometimes not listed in the
optimal order. When clay mineral models with extreme disorder are
tried to fit together with any complicated background models, the clay
phases always tend to get high FoM, even when not present at all.
Therefore I do exclude clay minerals from the Search-Match in the
daily practice. You can imagine that I'm very interested in your new
approach!
Regarding the term "WPF" search match procedures, I remember several
early publications based on a set of experimental reference patterns
(QUAX, automated RockJock, more recently Steve Hillier and
coworkers...). They can (and have) include structure-based calculated
patterns in their libraries as well, and such "pattern summation"
methods do work quite nicely as Steve has shown. Of course there is no
real refinement of structure parameters, but there is not much
difference to the use of any Rietveld code with strictly limited
parameter space for lattice parameters and line broadening and fixed
structure. So the label "WPF" used for any commercial software may
mean anything (or nothing).
Your approach and workflow is much more sophisticated and original, as
it combines the simple sequential "Rietveld" search-match with
following more detailed refinement, and as it enables the use of
bigger structure database. Congrats!
Best regards
Reinhard
Zitat von Jonathan WRIGHT <[email protected]>:
Hi Luca,
Thanks for sharing the links to your method - I hope we can try it
the next time we get stuck on identification.
It is a shame to hear you were delayed for so long by J.Appl.Cryst.
Did they ask you to cite some work from the Glasgow group as the
commercial competitor? I have in mind that they were looking at
measured profiles too (https://doi.org/10.1107/S002188980400038X,
https://doi.org/10.1107/S0021889804011847).
Indeed I had overlooked your paper, so perhaps this list is still
one of the better ways to reach some parts of the powder diffraction
community!
With best regards,
Jon
On 06/09/2023 18:52, Luca Lutterotti wrote:
I am glad you find FPSM an inspiring idea, me and my co-workers
will be quite happy if this will results in some citations. The
FPSM publication back in 2019 was a troubled submission. It took us
more than 3 years as initially was just rejected (for economical
reasons, as it would be unfair against the traditional search-match
software developed by companies; you read it right, that was the
reason for rejection by the reviewer and the editor accepted it
even if the other reviewer was for accepting it as it is). We had
some discussion, but no way. Then we tried to change journal (www
were hesitant as it would have had much less visibility on the
powder diffraction community) but finally Daniel discussed with
another editor of the same journal and we re-submitted and got some
fair reviewers. But it was long and the first rejection a bit
shocking. I thought before you have to reject for scientific
reasons…….
Now I am learning that not only at the academic level, but also
some companies selling search-match software are including what
they call WPF search-match, but no one cite the origin of the idea.
I hope I don’t get a second Loopstra-Rietveld case….. ;-) Well in
my case I wrote the software before publishing the idea.
That software was re-written from scratch to optimise for the speed
and the method. That’s why we can work with several thousand
structures at the same speed the other softwares work on less than
hundreds. I did not use Maud for that in fact.
But I want you to know that the last version I developed on a
recent EU project (not the one online), works also with
turbostratic and modulated clay structures using your model (the
Ufer et al.) to simulate them in the Rietveld. It is a fantastic
trick that I use for texture analysis but also quantification and
now in FPSM. Having a quick Rietveld help to search-match samples
containing clays using data even at high angles (more than 60
degs). I indeed don’t pre-calculate and store structures because
when you work with many of them it takes more time to load all the
precalculations from a database (even the speedy ones) than to
re-calculate everything.
So I am glad we both made use of each other models/ideas!
Best regards,
Luca
<http://www.unitn.it/>
logo_unitrento_firma.png
*
Luca Lutterotti*
Dipartimento di Ingegneria Industriale
Università di Trento
via Sommarive, 9 - 38123 Trento (Italy)
tel. +39 0461 2824-14 (Office), -34 (X-Ray lab)
ico_fb_32x32.pngico_twitter_32x32.pngico_insta_32x32.pngico_linkedin_32x32.pngico_youtube_32x32.png
Maud: http://maud.radiographema.com <http://maud.radiographema>
On 5 Sep 2023, at 13:49, Reinhard Kleeberg
<[email protected]> wrote:
Dear Luca,
I completely agree and will be very happy to have a 1D detector
with sufficient energy resolution to resolve a "pure" Cu Kalpha1/2
doublet from W Lalpha1. This would make routine work much easier.
IMHO, the biggest improvements in XRPD instrumentation within the
last decades came solely from the detector side, should be
continued.
Regarding search-match by Rietveld: Your FSPM method is a very
inspiring idea. Nicola Doebelin has incorporated a simplified
approach in PROFEX, too:
https://www.youtube.com/watch?v=Oqj71TiifeI
<https://www.youtube.com/watch?v=Oqj71TiifeI>
I'm routinely applying a run of ~500 structures/minerals what we
are commonly using (+- the former QPA database of Seifert AUTOQUAN
or from the BGMN webpage) for a phase screening of unknown
samples, needs ~ 5 min without interaction. Than running QPA
refinement with the best matching structures, clicking on
remaining peaks in the difference plot for getting a proposal of
best matching main line positions in the database, and adding
these structure(s) to the refinement, running again... This is a
typical workflow in our lab, no need for peak search, background
treatment, thinking about artifact peaks...
Best regards
Reinhard
Zitat von Luca Lutterotti <[email protected]
<mailto:[email protected]>>:
Dear Reinhard and Rietvelders,
It is always a compromise. Ideally we would like the fastest
instrument with a lot of intensity (so, 1D or 2D detectors) but
no lines outside the Kalpha or even just the Kapha1 like the one
of James Cline. But this means a monochromator on the incident
beam and you get fluorescence background. Now I like your
solution of the Si Drift detector, so you just cut the
fluorescence and you don’t need the monochromator in the first
place.
So we are working and we are testing some lab prototypes of a 1D
Si Drift like detector to get the best of both world. It is only
a lot of electronic, but one day we will have wonderful
instrument with only the lines we need and no fluorescence for
the background. Actually we use fluorescence for the chemical
analysis (quantitative).
About the search-match problem. Have a look on our FPSM method (
http://fpsm.radiographema.com/ <http://fpsm.radiographema.com/>)
where we don’t care about extra lines as it is a Rietveld
search-match. We don’t need to identify or search peaks. We don’t
use peak positions, we just fit with the Rietveld. It is slower
indeed, but every day is becoming faster and in a few years it
will run quickly on our cellphones (I have a prototype running
there).
Best regards,
Luca
<http://www.unitn.it/ <http://www.unitn.it/>>
Luca Lutterotti
Dipartimento di Ingegneria Industriale
Università di Trento
via Sommarive, 9 - 38123 Trento (Italy)
tel. +39 0461 2824-14 (Office), -34 (X-Ray lab)

Maud:http://maud.radiographema.com
<http://maud.radiographema.com/><http://maud.radiographema/
<http://maud.radiographema/>>
Begin forwarded message:
From: Reinhard Kleeberg <[email protected]>
Subject: Re: [EXT] [External] Re: Step-like basline
Date: 5 September 2023 at 08:56:15 CEST
To: [email protected]
Reply-To: Reinhard Kleeberg <[email protected]>
Dear Luca,
I completely agree with your opinion, and want to add that even
for "trivial" tasks in XRPD like phase analysis and standard
Rietveld refinements the satellites/spectral impurities do cause
significant trouble:
- The K beta and W L satellites of strong peaks of major phases
like quartz, carbonates or cubic structures in geomaterials are
typically not automatically recognized in the standard peak
search procedures and therefore misinterpreted to be K alpha
peaks and added to the peak list. I can't tell you how often I
was asked from colleagues for explanation of such "unidentified
peaks", and how much time people have spent for searching for
explanation of such artefact lines.
- In Rietveld analysis our software must generate the peaks at
least for the measured angular range. Depending on the method
how the software is doing this, we run into problems with the
satellites. If the software generates the reflections from the
positions of K alpha peaks from the start lattice parameters and
the (extended) upper measured angle, K beta satellites of K
alpha peaks outside this angular range will maybe not generated
and remain unfitted in the pattern. If the software generates
the peaks depending on the shortest wavelength in the wavelength
profile (more intelligent approach), the software must generate
much more reflections (with maxima outside the measured angular
range) and all these peaks must be calculated over an extremely
broad angular range. In the case of low symmetry structures with
big cells or disordered structures described by partial
structure factors and the resulting extreme high numbers of
peaks, the "extension effect" will cause significantly prolonged
time for calculations, without any positive effect.
That's why I prefer to use instrumentation with better
monochromatic radiation (monochromators, high energy resolution
detectors) even in the daily business of phase analysis. We do
use our 1D detector Mythen2 with Fe filter (Co radiation) only
for "quick and dirty" measurements.
Best regards
Reinhard
Zitat von Luca Lutterotti <[email protected]>:
Dear Habib,
Reinhard is right, and what he explained is exactly what you
observed. Now I would add that I may not define your Bruker
clean and optimised, because for this kind of samples, wafers
and extremely textured thin films, it would be better to have a
monochromator in the incident beam and not a Ni filtered (I
would more say it is a requirement). It was already showed many
times in the past as a monochromator in the incident beam is a
necessity for this materials to avoid all the "physical
artifacts" created by the strong intensity and not clean Kalpha
radiation.
Best regards,
Luca
<http://www.unitn.it/>
Luca Lutterotti
Dipartimento di Ingegneria Industriale
Università di Trento
via Sommarive, 9 - 38123 Trento (Italy)
tel. +39 0461 2824-14 (Office), -34 (X-Ray lab)

Maud: http://maud.radiographema.com <http://maud.radiographema/>
On 4 Sep 2023, at 12:20, Habib Boughzala
<[email protected]> wrote:
Many thanks Reinhard,
That's exactly what I wanted to say by "I can assure that our
Bruker D8 is clean and optimized!"
Otherwise, in some other cases of well conditioned thin film
no similar phenomenon is observed!
So, yes, it's obviously possible that your point of view is right.
Regards
Habib
------ Message d'origine ------
De "Reinhard Kleeberg" <[email protected]
<mailto:[email protected]>>
À "Habib Boughzala" <[email protected] <mailto:[email protected]>>
Cc [email protected] <mailto:[email protected]>
Date 04/09/2023 11:07:50
Objet Re: Re[2]: [EXT] Re: [External] Re: Step-like basline
Dear Habib,
the phenomenom "satellites or edges" originates from the
diffraction process. The critical parameters are:
- spectral pureness of the primary beam (primary beam
monochromator, tube spectral contamination like W...)
- the use of K beta absorbtion filter (and its thickness)
- the energy resolution ("window") of the detector system.
Even a D8 system may be equipped with different types of
detectors, slits and energy limits can be set differently for
an identical configuration, and quite often satellite peaks
may appear later in the time of use (aging of the tube
produces more W L, Fe filters may corrode and get
perforated...). So it is strictly recommended to check the
instrument peridically, by measuring a full pattern of a
profile standard (LaB6 or Si or similar).
Greetings
Reinhard
Zitat von Habib Boughzala <[email protected]
<mailto:[email protected]>>:
Dear all,
I would like to send you my witness related to this kind of
observation.
I can assure that our Bruker D8 is clean and optimized!
In many cases of well conditioned thin film (spin coating or
controlled diffusion) material this kind of phenomenon is
visible around the highest reflection, especially when the
preferred orientation is drastically present.
So, in my opinion, Reinhard and Alan are right, and what is
observed is just like reflections broadening, asymmetry,
shifting ...etc ... and can be related to the material
behavior.
Now, what is the physical (crystallographic!) property
responsible of this phenomenon? let's open the floor for a
large discussion.
Habib
------ Message d'origine ------
De "Alan W Hewat" <[email protected]
<mailto:[email protected]>>
À "Reinhard Kleeberg" <[email protected]
<mailto:[email protected]>>
Cc [email protected] <mailto:[email protected]>
Date 04/09/2023 09:29:08
Objet Re: [EXT] Re: [External] Re: Step-like basline
Reinhard is right that it is best to improve the instrument
to produce cleaner data. I'm concerned about the advice to
model all kinds of features whose origin is not fully
understood, simply to obtain a better fit. Shay has told us
nothing about his instrument or his conditions of data
collection. He asks "Is it a sample preparation problem",
to which the obvious reply is "Do you see this with other
samples or different materials" ? Only he can answer that.
If the answer is yes, he might try modifying his instrument
(remove filters etc) to see what effect that has on the
pattern from a simple well characterised material. Again
only he can do that. Data collection is an experimental
science, and data refinement should not be reduced to a
"black box" computer program where extra parameters can be
added to reduce the R-factor.
Alan.
On Mon, 4 Sept 2023 at 08:18, Reinhard Kleeberg
<[email protected]
<mailto:[email protected]>> wrote:
Can be modeled in the BGMN peak profile model as well, by modifying
the *.lam file by a series of additional Lorentzians on
the 1/lambda
scale, see figure.
The same can be done for other spectral impurities, e.g. W L
satellites. Also "electronic effects" on the wavelength
distribution
profile like the "edges" from the ROI settings of Si drift
detectors
can be modelled in such a convolution based approach.
However, better to have a pure/simple wavelength
distribution (clear
alpha1/2 doublet) by a monochromator or high energy resolution
detector, as any satellites make trouble in trace phase
analysis and
do cause prolonged calculation time in complicated
Rietveld refinements.
Reinhard
Zitat von Matthew Rowles <[email protected]
<mailto:[email protected]>>:
Topas can model them quite well. The functionality was
introduced in
version 5.
On Mon, 4 Sep 2023, 00:54 Kurt Leinenweber,
<[email protected] <mailto:[email protected]>> wrote:
Hi, Are these things modeled in Rietveld programs, by
chance? It seems
like a lot of baggage to put in a refinement but if it
makes the results
better…
- Kurt
*From:* [email protected]
<mailto:[email protected]>
<[email protected]
<mailto:[email protected]>> *On Behalf
Of *Thomas Gegan
*Sent:* Sunday, September 3, 2023 9:16 AM
*To:* Bish, David L <[email protected]
<mailto:[email protected]>>; Shay Tirosh
<[email protected] <mailto:[email protected]>>;
Fernando Igoa <[email protected]
<mailto:[email protected]>>
*Cc:* Rietveld List ([email protected]
<mailto:[email protected]>) <[email protected]
<mailto:[email protected]>>
*Subject:* RE: [EXT] Re: [External] Re: Step-like basline
I agree with a Ni absorption edge, possibly with a Kβ
peak around 38° 2θ.
*Tom Gegan*
Chemist III
Phone: +1 732 205-5111, Email: [email protected]
<mailto:[email protected]>
Postal Address: BASF Corporation, , 25 Middlesex Essex
Turnpike, 08830
Iselin, United States
*From:* [email protected]
<mailto:[email protected]>
<[email protected]
<mailto:[email protected]>> *On Behalf
Of *Bish, David L
*Sent:* Sunday, September 3, 2023 7:08 AM
*To:* Shay Tirosh <[email protected]
<mailto:[email protected]>>; Fernando Igoa <
[email protected] <mailto:[email protected]>>
*Cc:* Rietveld List ([email protected]
<mailto:[email protected]>) <[email protected]
<mailto:[email protected]>>
*Subject:* [EXT] Re: [External] Re: Step-like basline
Some people who received this message don't often get email from
[email protected] <mailto:[email protected]>. Learn why
this is important
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Hello Shay,
I think it is probably related to "tube tails". You can
read about this in
the literature (e.g., on the BGMN web site) and you can
model it in some
Rietveld software such as Topas. You don't normally
notice this but it
becomes apparent with higher-intensity peaks.
Regards,
Dave
------------------------------
*From:* [email protected]
<mailto:[email protected]>
<[email protected]
<mailto:[email protected]>> on behalf
of Fernando Igoa <[email protected]
<mailto:[email protected]>>
*Sent:* Sunday, September 3, 2023 3:06 AM
*To:* Shay Tirosh <[email protected]
<mailto:[email protected]>>
*Cc:* Rietveld List ([email protected]
<mailto:[email protected]>) <[email protected]
<mailto:[email protected]>>
*Subject:* [External] Re: Step-like basline
This message was sent from a non-IU address. Please
exercise caution when
clicking links or opening attachments from external sources.
Hey Shay,
Are you using a motorized slit during the measurement?
These may open up
abruptly to compensate for the angular dependence of the
footprint and thus
generate an abrupt increase in the intensity.
Hope it helps :)
On Sun, Sep 3, 2023, 8:50 AM Shay Tirosh
<[email protected] <mailto:[email protected]>> wrote:
Dear Rietvelders
I am attaching a zoom-in on a diffraction profile.
My question is what is the origin of the step-like
profile next to a very
large reflection peak?
Is it a sample preparation problem?
Is it part of the baseline?
Thanks
Shay
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<http://www.neutronoptics.com/hewat>
<http://www.neutronoptics.com/hewat>
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