Dear Radovan,
may be you are right, but this great development will unfortunately
not help the big number of lab diffractionists to puzzle the patterns
to be analyzed in their daily business ;-)
Best regards
Reinhard
Zitat von Radovan Cerny <radovan.ce...@unige.ch>:
Dear Reinhard,
I wouldn't say "solely from the detector side". The biggest
improvement is synchrotron radiation (+2D detectors🤓).
Best greetings from Lac Leman
Radovan Cerny
Envoyé à partir de Outlook pour Android<https://aka.ms/AAb9ysg>
________________________________
From: rietveld_l-requ...@ill.fr <rietveld_l-requ...@ill.fr> on
behalf of Reinhard Kleeberg <kleeb...@mineral.tu-freiberg.de>
Sent: Tuesday, September 5, 2023 1:49:57 PM
To: rietveld_l@ill.fr <rietveld_l@ill.fr>
Subject: [EXTERNAL] Re: [EXT] [External] Re: Step-like basline
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
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 <luca.luttero...@unitn.it>:
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/) 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/>
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/>
Begin forwarded message:
From: Reinhard Kleeberg <kleeb...@mineral.tu-freiberg.de>
Subject: Re: [EXT] [External] Re: Step-like basline
Date: 5 September 2023 at 08:56:15 CEST
To: rietveld_l@ill.fr
Reply-To: Reinhard Kleeberg <kleeb...@mineral.tu-freiberg.de>
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 <luca.luttero...@unitn.it>:
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
<habib.boughz...@ipein.rnu.tn> 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" <kleeb...@mineral.tu-freiberg.de
<mailto:kleeb...@mineral.tu-freiberg.de>>
À "Habib Boughzala" <boughz...@yahoo.com <mailto:boughz...@yahoo.com>>
Cc rietveld_l@ill.fr <mailto:rietveld_l@ill.fr>
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 <boughz...@yahoo.com
<mailto:boughz...@yahoo.com>>:
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" <alan.he...@neutronoptics.com
<mailto:alan.he...@neutronoptics.com>>
À "Reinhard Kleeberg" <kleeb...@mineral.tu-freiberg.de
<mailto:kleeb...@mineral.tu-freiberg.de>>
Cc rietveld_l@ill.fr <mailto:rietveld_l@ill.fr>
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
<kleeb...@mineral.tu-freiberg.de
<mailto:kleeb...@mineral.tu-freiberg.de>> 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 <rowle...@gmail.com
<mailto:rowle...@gmail.com>>:
Topas can model them quite well. The functionality was introduced in
version 5.
On Mon, 4 Sep 2023, 00:54 Kurt Leinenweber, <ku...@asu.edu
<mailto:ku...@asu.edu>> 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:* rietveld_l-requ...@ill.fr
<mailto:rietveld_l-requ...@ill.fr>
<rietveld_l-requ...@ill.fr
<mailto:rietveld_l-requ...@ill.fr>> *On Behalf
Of *Thomas Gegan
*Sent:* Sunday, September 3, 2023 9:16 AM
*To:* Bish, David L <b...@indiana.edu
<mailto:b...@indiana.edu>>; Shay Tirosh <stiro...@gmail.com
<mailto:stiro...@gmail.com>>;
Fernando Igoa <fer.igoa.1...@gmail.com
<mailto:fer.igoa.1...@gmail.com>>
*Cc:* Rietveld List (rietveld_l@ill.fr
<mailto:rietveld_l@ill.fr>) <rietveld_l@ill.fr
<mailto:rietveld_l@ill.fr>>
*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: tom.ge...@basf.com
<mailto:tom.ge...@basf.com>
Postal Address: BASF Corporation, , 25 Middlesex Essex
Turnpike, 08830
Iselin, United States
*From:* rietveld_l-requ...@ill.fr
<mailto:rietveld_l-requ...@ill.fr>
<rietveld_l-requ...@ill.fr
<mailto:rietveld_l-requ...@ill.fr>> *On Behalf
Of *Bish, David L
*Sent:* Sunday, September 3, 2023 7:08 AM
*To:* Shay Tirosh <stiro...@gmail.com
<mailto:stiro...@gmail.com>>; Fernando Igoa <
fer.igoa.1...@gmail.com <mailto:fer.igoa.1...@gmail.com>>
*Cc:* Rietveld List (rietveld_l@ill.fr
<mailto:rietveld_l@ill.fr>) <rietveld_l@ill.fr
<mailto:rietveld_l@ill.fr>>
*Subject:* [EXT] Re: [External] Re: Step-like basline
Some people who received this message don't often get email from
b...@indiana.edu <mailto:b...@indiana.edu>. Learn why this
is important
<https://urldefense.com/v3/__https:/aka.ms/LearnAboutSenderIdentification__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjKqH-aqqA$>
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:* rietveld_l-requ...@ill.fr
<mailto:rietveld_l-requ...@ill.fr>
<rietveld_l-requ...@ill.fr
<mailto:rietveld_l-requ...@ill.fr>> on behalf
of Fernando Igoa <fer.igoa.1...@gmail.com
<mailto:fer.igoa.1...@gmail.com>>
*Sent:* Sunday, September 3, 2023 3:06 AM
*To:* Shay Tirosh <stiro...@gmail.com <mailto:stiro...@gmail.com>>
*Cc:* Rietveld List (rietveld_l@ill.fr
<mailto:rietveld_l@ill.fr>) <rietveld_l@ill.fr
<mailto:rietveld_l@ill.fr>>
*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
<stiro...@gmail.com <mailto:stiro...@gmail.com>> 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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