Re: FPSM : (was Re: [EXT] [External] Re: Step-like basline)

[Luca Lutterotti]

.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 >> <mailto: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/ <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 
>>>>> 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 
>>>>> 
>>>>> 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 
>>>

Re: FPSM : (was Re: [EXT] [External] Re: Step-like basline)

[Luca Lutterotti]

No they did not, I think the reviewer was American, in fact he was also wining 
about unfair competition by the EU that provides funds to develop technologies 
directly competing against US companies…..
The FPSM was originally developed in 2013-2014 inside one EU project. I would 
have not developed it without in reality ;-)

Thanks Reinhard for the explanation of WPF related to Search-match. I can only 
see the advertisement/brochure and I didn’t know what exactly they do or mean 
with it.

Best regards,

Luca


 

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 


> On 7 Sep 2023, at 10:13, Jonathan WRIGHT  wrote:
> 
> 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).

++
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Send commands to  eg: HELP as the subject with no body text
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++

RE: [EXT] Re: [External] Re: Step-like basline

[Scott Speakman]

Unrestricted Document

Modeling of the absorption edge is also available in HighScore Plus v5.x

However, as some have said, it is much better to avoid this artifact 
altogether.  The energy discriminating linear detectors are good at filtering 
spectral contamination without introducing these artifacts, but with two 
caveats: 1) none of them completely remove the K-beta (even though they claim 
to); and  2) there is a residual spectral hump under the peaks from 
Bremsstrahlung with wavelengths close to K-alpha which needs to be modelled 
(HighScore and Topas can model this; I assume GSAS-II can too).

The best data quality that I have seen, without sacrificing the speed from the 
linear PSD, comes by combining an incident beam monochromator with the energy 
discriminating linear detector.  The most common incident-beam monochromator 
now seems to be the flat Gobel mirror, which removes quite a lot of the 
spectral contamination while preserving the divergent beam for parafocusing 
geometry.  The detector then removes what remains, plus fluoresced noise from 
the specimen.   This can match the data collection speed of a system using just 
a foil beta filter, but with much better spectral purity and therefore data 
quality.

It does make me wonder what happened to the humble incident-beam graphite 
monochromator?  I know it was not as popular as the diffracted-beam 
monochromator, but it seems that it would also be a good complement to the 
energy discriminating linear detector and would be more flexible than a mirror 
for accommodating different X-ray tubes.

Best Regards,

Scott A Speakman, PhD
XRD Principal Scientist

Tel: +1 800 279-7297
Mob: +1 508 361-8121

Malvern Panalytical Inc.
2400 Computer Drive, Ste. 2100
Westborough MA 01581
United States

scott.speak...@malvernpanalytical.com
www.malvernpanalytical.com

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Unrestricted Document
-Original Message-
From: rietveld_l-requ...@ill.fr  On Behalf Of 
Reinhard Kleeberg
Sent: Monday, September 4, 2023 2:19 AM
To: rietveld_l@ill.fr
Subject: Re: [EXT] Re: [External] Re: Step-like basline

CAUTION: This email originated from outside of the organization. Do not click 
links or open attachments unless you recognize the sender and know the content 
is safe.

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 :

> Topas can model them quite well. The functionality was introduced in
> version 5.
>
> On Mon, 4 Sep 2023, 00:54 Kurt Leinenweber,  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  *On
>> Behalf Of *Thomas Gegan
>> *Sent:* Sunday, September 3, 2023 9:16 AM
>> *To:* Bish, David L ; Shay Tirosh
>> ; Fernando Igoa 
>> *Cc:* Rietveld List (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 Postal Address:
>> BASF Corporation, , 25 Middlesex Essex Turnpike, 08830 Iselin, United
>> States
>>
>>
>>
>> *From

Re: FPSM : (was Re: [EXT] [External] Re: Step-like basline)

[Reinhard Kleeberg]

he 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  
 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 <mailto: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/ <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 
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 

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 suc

Re: Step-like basline

[Matthew Rowles]

Bad quality mono is always possible. I've got kb coming through with a
current instrument.

On Thu, 7 Sep 2023, 18:56 Reinhard Kleeberg, <
kleeb...@mineral.tu-freiberg.de> wrote:

> Hm, as Philips systems at this time always had combined a
> scintillation counter with a diffracted beam graphite 002 bent
> monochromator, the question arises how the W L series and Cu Kbeta
> lines could reach the detector... Bad quality of the graphite mosaic
> crystal?
>
> Reinhard
>
> Zitat von Le Bail Armel :
>
> > The muscovite data is dated 1996 from an old Philips 1710 diffractometer,
> >
> > vertical sample holder, scintillation counter, not much used because we
> >
> > had better instruments, hence this stupid test ;-)
> >
> > Armel
> >
> >> envoyé : 7 septembre 2023 à 10:57
> >> de : Reinhard Kleeberg 
> >> à : rietveld_l@ill.fr
> >> objet : Re: Step-like basline
> >>
> >> Dear Luca,
> >> sorry, I don't understand the "mosaic crystal" eplanation, especially
> >> not the "non-centre position" issue. IMHO, when the pattern was
> >> measured at a "powder" Bragg-Brentano configuration, in reflection
> >> mode, axial and equatorial divergence maximum ~ 2 degree, the 00l
> >> series of all misoriented crystal blocks can fulfill the diffraction
> >> condition only within the range of the instruments divergence, and the
> >> parafocusing arrangement would reflect such blocks back very close to
> >> the nominal angular position (as it is the case for a powder as well).
> >> So single crystal reflection of big blocks should only be observable
> >> within the total profile of a "normal" ideal powder peak (the
> >> "instrumental" profile"). This is indeed what we see if coarsely
> >> crystalline materials (e.g. quartz sand) are measured on a typical
> >> powder diffractometer: Such peaks are extremely sharp, sometimes split
> >> or doubled, sometimes with "wrong" alpha1/2 intensity ratio, or may
> >> have small additional maxima and may be "edges" in their slopes,
> >> depending on the number or size of crystals, but all these effects are
> >> very close to the correct maximum position (+- <1 degree). So I can't
> >> imagine that the unknown satellites in the mica pattern are
> >> "misoriented-displaced" Cu Kalpha 00l peaks?
> >>
> >> Armel, what type of detector was used for this measurement? If the W L
> >> series was detected, probably no diffracted beam monochromator, and no
> >> Peltier cooled Si drift detector? If so, even more spectral
> >> contamination may come into account. For example, I remember to have
> >> complained about a new Co tube (no company names here) showing
> >> systematic satellites ~ 1 % intensity from standard Si and LaB6 powder
> >> measurements. The wavelength recalculated by Bragg's law was Zn Kalpha
> >> (!!!), confirmed by spectral analysis, the tube Co target was
> >> obviously contaminated. As the satellites in your example in the < 0.x
> >> % magnitude of the Cu K alpha1 intensity, even quite low contamination
> >> of other elements than W may be the source. So it could be
> >> interesting to calculate wavelengths from all positions of the unknown
> >> satellites for the d-spacings of the mica 00l series and see if any
> >> calculated wavelengths do repeat.
> >>
> >> Another thought:
> >> Here we have a single crystal of muscovite. As some of the unexplained
> >> peaks appear to be extremely sharp, what about Renninger (multiple
> >> diffraction) hkl peaks? Maybe there are enough lattice planes in the
> >> monoclinic mica structure to give a chance for multiple diffraction to
> >> get registered by a divergent beam (Bragg-Brentano) configuration?
> >> Such peak positions appear to be unsystematic, with no relatiion to
> >> the Cu Kalpha 00l.
> >>
> >> However, a take-home message of your example should be: Do never
> >> measure single crystals in parafocusing geometry without safely
> >> monochromatic radiation ;-)
> >>
> >> Best regards
> >>
> >> Reinhard
> >>
> >> Zitat von Luca Lutterotti :
> >>
> >>> It is call graininess, as Miguel said before, these are mosaic
> >>> single crystals and depending on your source (divergence, spot
> >>> dimension at different angles etc.) you get each mosaic crystal to
> >>> create a di

Re: Step-like basline

[Reinhard Kleeberg]

Hm, as Philips systems at this time always had combined a  
scintillation counter with a diffracted beam graphite 002 bent  
monochromator, the question arises how the W L series and Cu Kbeta  
lines could reach the detector... Bad quality of the graphite mosaic  
crystal?


Reinhard

Zitat von Le Bail Armel :


The muscovite data is dated 1996 from an old Philips 1710 diffractometer,

vertical sample holder, scintillation counter, not much used because we

had better instruments, hence this stupid test ;-)

Armel


envoyé : 7 septembre 2023 à 10:57
de : Reinhard Kleeberg 
à : rietveld_l@ill.fr
objet : Re: Step-like basline

Dear Luca,
sorry, I don't understand the "mosaic crystal" eplanation, especially
not the "non-centre position" issue. IMHO, when the pattern was
measured at a "powder" Bragg-Brentano configuration, in reflection
mode, axial and equatorial divergence maximum ~ 2 degree, the 00l
series of all misoriented crystal blocks can fulfill the diffraction
condition only within the range of the instruments divergence, and the
parafocusing arrangement would reflect such blocks back very close to
the nominal angular position (as it is the case for a powder as well).
So single crystal reflection of big blocks should only be observable
within the total profile of a "normal" ideal powder peak (the
"instrumental" profile"). This is indeed what we see if coarsely
crystalline materials (e.g. quartz sand) are measured on a typical
powder diffractometer: Such peaks are extremely sharp, sometimes split
or doubled, sometimes with "wrong" alpha1/2 intensity ratio, or may
have small additional maxima and may be "edges" in their slopes,
depending on the number or size of crystals, but all these effects are
very close to the correct maximum position (+- <1 degree). So I can't
imagine that the unknown satellites in the mica pattern are
"misoriented-displaced" Cu Kalpha 00l peaks?

Armel, what type of detector was used for this measurement? If the W L
series was detected, probably no diffracted beam monochromator, and no
Peltier cooled Si drift detector? If so, even more spectral
contamination may come into account. For example, I remember to have
complained about a new Co tube (no company names here) showing
systematic satellites ~ 1 % intensity from standard Si and LaB6 powder
measurements. The wavelength recalculated by Bragg's law was Zn Kalpha
(!!!), confirmed by spectral analysis, the tube Co target was
obviously contaminated. As the satellites in your example in the < 0.x
% magnitude of the Cu K alpha1 intensity, even quite low contamination
of other elements than W may be the source. So it could be
interesting to calculate wavelengths from all positions of the unknown
satellites for the d-spacings of the mica 00l series and see if any
calculated wavelengths do repeat.

Another thought:
Here we have a single crystal of muscovite. As some of the unexplained
peaks appear to be extremely sharp, what about Renninger (multiple
diffraction) hkl peaks? Maybe there are enough lattice planes in the
monoclinic mica structure to give a chance for multiple diffraction to
get registered by a divergent beam (Bragg-Brentano) configuration?
Such peak positions appear to be unsystematic, with no relatiion to
the Cu Kalpha 00l.

However, a take-home message of your example should be: Do never
measure single crystals in parafocusing geometry without safely
monochromatic radiation ;-)

Best regards

Reinhard

Zitat von Luca Lutterotti :


It is call graininess, as Miguel said before, these are mosaic
single crystals and depending on your source (divergence, spot
dimension at different angles etc.) you get each mosaic crystal to
create a diffraction peak that especially at low two-theta angle may
be displaced a lot from its theoretical position because it is
diffracting from a non center position. This is what you get also
when you analyse samples with extremely large grains. If you use a
2D detector instead of scanning with a point or small psd, you will
see all these individual grain or mosaic crystals diffracting around
their ideal spot or if it is a sample with just large grains,
distributed around the Laue circle. More the grain is on a lateral
position respect to the center of the beam, more it is displaced in
two-theta. At higher angle your beam size on the sample is smaller
and there is less displacement for geometrical reasons.
I like to work with 2D detectors (texture, stresses) because it is
easy to see these “figures”.
In addition you have the spectral impurities identified by Frank and
you may get some small grains with different orientation and twins
that will create some of the non 00l peaks.
Analysing these kind of patterns would require a sophisticated
simulation of the grains-crystals distribution and computing like
ray-tracing for the geometrical effects. Not worth it. Single
crystals and sharp t

Re: Step-like basline

[Le Bail Armel]

;>>> Dear Frank,>>>> Same as you. I have not a complete solution.>>>> Best>>>> Armel>>>>> envoyé : 6 septembre 2023 à 16:57>>> de : Frank Girgsdies >>> >>>> à : Le Bail Armel >>> >>>> Cc: Rietveld_L >>>> objet : Re: Step-like basline>>>>>>>>> Dear Armel,>>>>>> Thanks for this nice quiz!>>>>>> However, after identifying the following spectral impurities:>>> Cu K_beta,>>> W L_alpha1,2>>> W L_beta1,2,3,4 and>>> W L_gamma1,>>> I am stuck now, leaving bout 1/2 to 1/3 of the tiny extra peaks>>> unexplained.>>>>>> Some of them look suspiciously like Cu K_alpha1+2 doublets and might>>> thus belong to an impurity phase, or differently oriented crystallites>>> of the main phase, which could lie as dust on the single crystal>>> surface, but I had no luck trying to identify them.>>>>>> Furthermore, the irregular high angle tailing of the 00l series (maybe>>> stacking faults?) makes peak fitting difficult.>>>>>> Thus, I give up (at least for now), hoping that you might disclose the>>> solution to the riddle, as far as it is known, for us after a while.>>>>>> Best wishes,>>> Frank>>>>>>>>>>>> On 06.09.2023 10:47, Le Bail Armel wrote:>>>>>>> Hi,>>>>>>>> In the same subject.>>>>>>>> A special "powder pattern" to play with (try to explain all peaks) :>>>>>>>> http://cristal.org/muscovite.pdf >>>>>>>> Best>>>>>>>> Armel>>>>>>>>>>>> ++>>>> Please do NOT attach files to the whole list >>>> >>>> Send commands to  eg: HELP as the subject with >>>> no body text>>>> The Rietveld_L list archive is on >>>> http://www.mail-archive.com/rietveld_l@ill.fr/>>>> ++>>>>>>> >>>>>> ++>> Please do NOT attach files to the whole list >> >>> Send commands to > eg: >> HELP as the subject with no body text>> The Rietveld_L list archive is on >> http://www.mail-archive.com/rietveld_l@ill.fr/>> ++-- TU Bergakademie FreibergDr. R. KleebergMineralogisches LaborBrennhausgasse 14D-09596 FreibergTel. ++49 (0) 3731-39-3244Fax. ++49 (0) 3731-39-3129++Please do NOT attach files to the whole list Send commands to  eg: HELP as the subject with no body textThe Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/++
++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

Re: Step-like basline

[Reinhard Kleeberg]

 septembre 2023 à 16:57
de : Frank Girgsdies <mailto:girgs...@fhi-berlin.mpg.de>>
à : Le Bail Armel <mailto:le-bail.ar...@orange.fr>>

Cc: Rietveld_L mailto:Rietveld_L@ill.fr>>
objet : Re: Step-like basline


Dear Armel,

Thanks for this nice quiz!

However, after identifying the following spectral impurities:
Cu K_beta,
W L_alpha1,2
W L_beta1,2,3,4 and
W L_gamma1,
I am stuck now, leaving bout 1/2 to 1/3 of the tiny extra peaks
unexplained.

Some of them look suspiciously like Cu K_alpha1+2 doublets and might
thus belong to an impurity phase, or differently oriented crystallites
of the main phase, which could lie as dust on the single crystal
surface, but I had no luck trying to identify them.

Furthermore, the irregular high angle tailing of the 00l series (maybe
stacking faults?) makes peak fitting difficult.

Thus, I give up (at least for now), hoping that you might disclose the
solution to the riddle, as far as it is known, for us after a while.

Best wishes,
Frank



On 06.09.2023 10:47, Le Bail Armel wrote:


Hi,

In the same subject.

A special "powder pattern" to play with (try to explain all peaks) :

http://cristal.org/muscovite.pdf <http://cristal.org/muscovite.pdf>

Best

Armel


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FPSM : (was Re: [EXT] [External] Re: Step-like basline)

[Jonathan WRIGHT]

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 
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 

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 :


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  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 rig

Re: [EXTERNAL] Re: [EXT] [External] Re: Step-like basline

[Matthew Rowles]

Not only is it a possible explanation, it is the explanation.

It represents the tube bremsstralum truncated by the Ni absorption edge.

As long as you're careful, removing it shouldn't be an issue, although it
is always better to either model it properly, or to not collect such data
on the first place.

Matthew


On Wed, 6 Sep 2023, 16:35 Shay Tirosh,  wrote:

> Dear Reitvelders
>
> I am overwhelmed with your insightful responses. I am grateful for that.
>
> Indeed I have Ni filter and the adsorption added is indeed a good possible
> explanation since we get similar step-like profiles with completely
> different materials and samples.
>
> With the understanding that this step contains no special information that
> I might lose by using Spilne as the baseline subtraction. I just need to
> make sure I am not affecting peak positions and creating artificial peaks
> and humps
>
> Any comments?
>
> Thanks
>
> Shay
>
>
> <https://www.avast.com/sig-email?utm_medium=email&utm_source=link&utm_campaign=sig-email&utm_content=webmail>
> Virus-free.www.avast.com
> <https://www.avast.com/sig-email?utm_medium=email&utm_source=link&utm_campaign=sig-email&utm_content=webmail>
> <#m_-4699204290736215942_DAB4FAD8-2DD7-40BB-A1B8-4E2AA1F9FDF2>
>
> On Wed, Sep 6, 2023 at 9:35 AM Reinhard Kleeberg <
> kleeb...@mineral.tu-freiberg.de> wrote:
>
>> 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 :
>>
>> > 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  on
>> > behalf of Reinhard Kleeberg 
>> > Sent: Tuesday, September 5, 2023 1:49:57 PM
>> > To: 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 :
>> >
>> >> 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 on

Re: [EXT] [External] Re: Step-like basline

[Luca Lutterotti]

roblem. 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.com/> 
>> <http://maud.radiographema/>
>> 
>> 
>>> Begin forwarded message:
>>> 
>>> From: Reinhard Kleeberg 
>>> 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 
>>> 
>>> 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 :
>>> 
>>>> 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 

Re: Step-like basline

[Luca Lutterotti]

It is call graininess, as Miguel said before, these are mosaic single crystals 
and depending on your source (divergence, spot dimension at different angles 
etc.) you get each mosaic crystal to create a diffraction peak that especially 
at low two-theta angle may be displaced a lot from its theoretical position 
because it is diffracting from a non center position. This is what you get also 
when you analyse samples with extremely large grains. If you use a 2D detector 
instead of scanning with a point or small psd, you will see all these 
individual grain or mosaic crystals diffracting around their ideal spot or if 
it is a sample with just large grains, distributed around the Laue circle. More 
the grain is on a lateral position respect to the center of the beam, more it 
is displaced in two-theta. At higher angle your beam size on the sample is 
smaller and there is less displacement for geometrical reasons.
I like to work with 2D detectors (texture, stresses) because it is easy to see 
these “figures”.
In addition you have the spectral impurities identified by Frank and you may 
get some small grains with different orientation and twins that will create 
some of the non 00l peaks.
Analysing these kind of patterns would require a sophisticated simulation of 
the grains-crystals distribution and computing like ray-tracing for the 
geometrical effects. Not worth it. Single crystals and sharp textures requires 
a point beam to avoid these effects. And a monochromatic one.

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 6 Sep 2023, at 17:43, Le Bail Armel  wrote:
> 
> Dear Frank,
> 
> Same as you. I have not a complete solution.
> 
> Best
> 
> Armel
> 
>> envoyé : 6 septembre 2023 à 16:57
>> de : Frank Girgsdies > <mailto:girgs...@fhi-berlin.mpg.de>>
>> à : Le Bail Armel mailto:le-bail.ar...@orange.fr>>
>> Cc: Rietveld_L mailto:Rietveld_L@ill.fr>>
>> objet : Re: Step-like basline
>> 
>> 
>> Dear Armel,
>> 
>> Thanks for this nice quiz!
>> 
>> However, after identifying the following spectral impurities:
>> Cu K_beta,
>> W L_alpha1,2
>> W L_beta1,2,3,4 and
>> W L_gamma1,
>> I am stuck now, leaving bout 1/2 to 1/3 of the tiny extra peaks 
>> unexplained.
>> 
>> Some of them look suspiciously like Cu K_alpha1+2 doublets and might 
>> thus belong to an impurity phase, or differently oriented crystallites 
>> of the main phase, which could lie as dust on the single crystal 
>> surface, but I had no luck trying to identify them.
>> 
>> Furthermore, the irregular high angle tailing of the 00l series (maybe 
>> stacking faults?) makes peak fitting difficult.
>> 
>> Thus, I give up (at least for now), hoping that you might disclose the 
>> solution to the riddle, as far as it is known, for us after a while.
>> 
>> Best wishes,
>> Frank
>> 
>> 
>> 
>> On 06.09.2023 10:47, Le Bail Armel wrote:
>> 
>>> Hi,
>>> 
>>> In the same subject.
>>> 
>>> A special "powder pattern" to play with (try to explain all peaks) :
>>> 
>>> http://cristal.org/muscovite.pdf <http://cristal.org/muscovite.pdf>
>>> 
>>> Best
>>> 
>>> Armel
>>> 
>>> 
>>> ++
>>> Please do NOT attach files to the whole list 
>>> Send commands to  eg: HELP as the subject with no body text
>>> The Rietveld_L list archive is on 
>>> http://www.mail-archive.com/rietveld_l@ill.fr/
>>> ++
>>> 
>> >
>> 
> ++
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> Send commands to mailto:lists...@ill.fr>> eg: HELP as the 
> subject with no body text
> The Rietveld_L list archive is on 
> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++

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++

Re: Step-like basline

[Le Bail Armel]

Dear Frank,Same as you. I have not a complete solution.BestArmelenvoyé : 6 septembre 2023 à 16:57de : Frank Girgsdies à : Le Bail Armel Cc: Rietveld_L objet : Re: Step-like baslineDear Armel,Thanks for this nice quiz!However, after identifying the following spectral impurities: Cu K_beta, W L_alpha1,2 W L_beta1,2,3,4 and W L_gamma1,I am stuck now, leaving bout 1/2 to 1/3 of the tiny extra peaks unexplained.Some of them look suspiciously like Cu K_alpha1+2 doublets and might thus belong to an impurity phase, or differently oriented crystallites of the main phase, which could lie as dust on the single crystal surface, but I had no luck trying to identify them.Furthermore, the irregular high angle tailing of the 00l series (maybe stacking faults?) makes peak fitting difficult.Thus, I give up (at least for now), hoping that you might disclose the solution to the riddle, as far as it is known, for us after a while.Best wishes,FrankOn 06.09.2023 10:47, Le Bail Armel wrote:Hi,In the same subject.A special "powder pattern" to play with (try to explain all peaks) :http://cristal.org/muscovite.pdf BestArmel++Please do NOT attach files to the whole list Send commands to  eg: HELP as the subject with no body textThe Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/++>
++
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++

Re: Step-like basline

[Frank Girgsdies]

Dear Armel,

Thanks for this nice quiz!

However, after identifying the following spectral impurities:
 Cu K_beta,
 W L_alpha1,2
 W L_beta1,2,3,4 and
 W L_gamma1,
I am stuck now, leaving bout 1/2 to 1/3 of the tiny extra peaks 
unexplained.


Some of them look suspiciously like Cu K_alpha1+2 doublets and might 
thus belong to an impurity phase, or differently oriented crystallites 
of the main phase, which could lie as dust on the single crystal 
surface, but I had no luck trying to identify them.


Furthermore, the irregular high angle tailing of the 00l series (maybe 
stacking faults?) makes peak fitting difficult.


Thus, I give up (at least for now), hoping that you might disclose the 
solution to the riddle, as far as it is known, for us after a while.


Best wishes,
Frank



On 06.09.2023 10:47, Le Bail Armel wrote:

Hi,

In the same subject.

A special "powder pattern" to play with (try to explain all peaks) :

http://cristal.org/muscovite.pdf 

Best

Armel


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Re: [EXTERNAL] Re: Step-like basline

[Alan W Hewat]

You are right Radovan. The sample mail-in system is one way of improving SR
and N access times. "Discretionary time" reserved for people who have a hot
experiment and can come at short notice, is another, together with speeding
up the usual proposal system. These mechanisms already apply at ILL, but
on-site manpower is a limiting factor. And yes, a SR pattern will almost
always be superior to a lab pattern, because you can afford an instrument
to produce a cleaner pattern, and it is also easier with a monochromated
white beam.

Dr Alan Hewat, NeutronOptics
Grenoble, FRANCE (from phone)
alan.he...@neutronoptics.com
+33.476984168 VAT:FR79499450856
http://NeutronOptics.com/hewat
___


On Wed, 6 Sept 2023, 11:31 Radovan Cerny,  wrote:

> No, you are not provocative Alan. You are right. I have reacted only to
> the X-ray discussion (no neutrons in the labs).
> It is a pity that the procedure for getting the beamtime at the
> synchrotron and neutron sources is still so time-consuming. At least at the
> synchrotron, there is an activity to introduce or improve already existing
> mail-in system. I have a feeling that there is enough synchrotron beamtime
> for everybody to collect standard powder patterns. 20-60 sec / pattern with
> 2D detector + few min. for sample mounting is not so much.
> Who has analyzed powder patterns from synchrotron will never come back to
> the lab (this is provocative 🙂)
>
> Radovan
>
>
> Radovan Cerny
> DQMP
> Université de Genève
> 24, quai Ernest-Ansermet
> CH-1211 Geneva 4, Switzerland
> mailto : radovan.ce...@unige.ch
> URL: http://www.unige.ch/sciences/crystal/cerny/rcerny.htm
> --
> *De :* rietveld_l-requ...@ill.fr  de la part
> de Alan W Hewat 
> *Envoyé :* mercredi 6 septembre 2023 11:17
> *À :* Le Bail Armel 
> *Cc :* Rietveld_L 
> *Objet :* [EXTERNAL] Re: Step-like basline
>
> "*The biggest improvement was synchrotron radiation*".
> No. The biggest improvement for the profile refinement of atomic and
> magnetic structures (Rietveld refinement in the strict sense) was high
> resolution neutron powder diffractometers with large area detectors :-)
> Even SR gives undue weight to heavy atoms, can suffer from systematic
> errors due to small samples, and of course is "not ideal" for magnetism,
> important for the properties of many materials. SR has some advantages to
> counter these disadvantages, but not for most new materials. Lab x-rays can
> do some structural work, but have most application for materials
> characterisation by multi-component profile refinement, when you need a
> result now, and not in 6 months time.
>
> But Radovan, is just being provocative (like me).
>
> Alan
>
>
> 
> Dr Alan Hewat, NeutronOptics
> Grenoble, FRANCE (from phone)
> alan.he...@neutronoptics.com
> +33.476984168 VAT:FR79499450856
> http://NeutronOptics.com/hewat
> ___
>
>
> On Wed, 6 Sept 2023, 10:48 Le Bail Armel,  wrote:
>
> Hi,
>
> In the same subject.
>
> A special "powder pattern" to play with (try to explain all peaks) :
>
> http://cristal.org/muscovite.pdf
>
> Best
>
> Armel
> ++
> Please do NOT attach files to the whole list  >
> Send commands to  eg: HELP as the subject with no body
> text
> The Rietveld_L list archive is on
> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++
>
>
++
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The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

RE: [EXTERNAL] Re: Step-like basline

[Radovan Cerny]

No, you are not provocative Alan. You are right. I have reacted only to the 
X-ray discussion (no neutrons in the labs).
It is a pity that the procedure for getting the beamtime at the synchrotron and 
neutron sources is still so time-consuming. At least at the synchrotron, there 
is an activity to introduce or improve already existing mail-in system. I have 
a feeling that there is enough synchrotron beamtime for everybody to collect 
standard powder patterns. 20-60 sec / pattern with 2D detector + few min. for 
sample mounting is not so much.
Who has analyzed powder patterns from synchrotron will never come back to the 
lab (this is provocative 🙂)

Radovan


Radovan Cerny
DQMP
Université de Genève
24, quai Ernest-Ansermet
CH-1211 Geneva 4, Switzerland
mailto : radovan.ce...@unige.ch<mailto:radovan.ce...@unige.ch>
URL: http://www.unige.ch/sciences/crystal/cerny/rcerny.htm

De : rietveld_l-requ...@ill.fr  de la part de Alan W 
Hewat 
Envoyé : mercredi 6 septembre 2023 11:17
À : Le Bail Armel 
Cc : Rietveld_L 
Objet : [EXTERNAL] Re: Step-like basline

"The biggest improvement was synchrotron radiation".
No. The biggest improvement for the profile refinement of atomic and magnetic 
structures (Rietveld refinement in the strict sense) was high resolution 
neutron powder diffractometers with large area detectors :-) Even SR gives 
undue weight to heavy atoms, can suffer from systematic errors due to small 
samples, and of course is "not ideal" for magnetism, important for the 
properties of many materials. SR has some advantages to counter these 
disadvantages, but not for most new materials. Lab x-rays can do some 
structural work, but have most application for materials characterisation by 
multi-component profile refinement, when you need a result now, and not in 6 
months time.

But Radovan, is just being provocative (like me).

Alan



Dr Alan Hewat, NeutronOptics
Grenoble, FRANCE (from phone)
alan.he...@neutronoptics.com
+33.476984168 VAT:FR79499450856
http://NeutronOptics.com/hewat
___


On Wed, 6 Sept 2023, 10:48 Le Bail Armel, 
mailto:le-bail.ar...@orange.fr>> wrote:

Hi,

In the same subject.

A special "powder pattern" to play with (try to explain all peaks) :

http://cristal.org/muscovite.pdf

Best

Armel

++
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++

++
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++

Re: Step-like basline

[miguel gregorkiewitz]

Nice example for real world, Armel!

These huge flakes are by no means single crystals, so I tend to interpret
the small peaks in the feet of the maxima as stemming from slightly
misaligned regions, sort of graininess.

Did you try under the polarizing microscope?

Best

Miguel


El mié, 6 sep. 2023 10:48, Le Bail Armel  escribió:

> Hi,
>
> In the same subject.
>
> A special "powder pattern" to play with (try to explain all peaks) :
>
> http://cristal.org/muscovite.pdf
>
> Best
>
> Armel
> ++
> Please do NOT attach files to the whole list  >
> Send commands to  eg: HELP as the subject with no body
> text
> The Rietveld_L list archive is on
> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++
>
>
++
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Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

Re: Step-like basline

[Alan W Hewat]

"*The biggest improvement was synchrotron radiation*".
No. The biggest improvement for the profile refinement of atomic and
magnetic structures (Rietveld refinement in the strict sense) was high
resolution neutron powder diffractometers with large area detectors :-)
Even SR gives undue weight to heavy atoms, can suffer from systematic
errors due to small samples, and of course is "not ideal" for magnetism,
important for the properties of many materials. SR has some advantages to
counter these disadvantages, but not for most new materials. Lab x-rays can
do some structural work, but have most application for materials
characterisation by multi-component profile refinement, when you need a
result now, and not in 6 months time.

But Radovan, is just being provocative (like me).

Alan



Dr Alan Hewat, NeutronOptics
Grenoble, FRANCE (from phone)
alan.he...@neutronoptics.com
+33.476984168 VAT:FR79499450856
http://NeutronOptics.com/hewat
___


On Wed, 6 Sept 2023, 10:48 Le Bail Armel,  wrote:

> Hi,
>
> In the same subject.
>
> A special "powder pattern" to play with (try to explain all peaks) :
>
> http://cristal.org/muscovite.pdf
>
> Best
>
> Armel
> ++
> Please do NOT attach files to the whole list  >
> Send commands to  eg: HELP as the subject with no body
> text
> The Rietveld_L list archive is on
> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++
>
>
++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

Re: Step-like basline

[Le Bail Armel]

Hi,In the same subject.A special "powder pattern" to play with (try to explain all peaks) :http://cristal.org/muscovite.pdfBestArmel
++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

Re: [EXTERNAL] Re: [EXT] [External] Re: Step-like basline

[Shay Tirosh]

Dear Reitvelders

I am overwhelmed with your insightful responses. I am grateful for that.

Indeed I have Ni filter and the adsorption added is indeed a good possible
explanation since we get similar step-like profiles with completely
different materials and samples.

With the understanding that this step contains no special information that
I might lose by using Spilne as the baseline subtraction. I just need to
make sure I am not affecting peak positions and creating artificial peaks
and humps

Any comments?

Thanks

Shay

<https://www.avast.com/sig-email?utm_medium=email&utm_source=link&utm_campaign=sig-email&utm_content=webmail>
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On Wed, Sep 6, 2023 at 9:35 AM Reinhard Kleeberg <
kleeb...@mineral.tu-freiberg.de> wrote:

> 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 :
>
> > 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  on
> > behalf of Reinhard Kleeberg 
> > Sent: Tuesday, September 5, 2023 1:49:57 PM
> > To: 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 :
> >
> >> 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,
> >>
&

Re: [EXTERNAL] Re: [EXT] [External] Re: Step-like basline

[Reinhard Kleeberg]

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 :


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  on  
behalf of Reinhard Kleeberg 

Sent: Tuesday, September 5, 2023 1:49:57 PM
To: 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 :


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 
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 

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
(mor

Re: [EXTERNAL] Re: [EXT] [External] Re: Step-like basline

[Radovan Cerny]

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  on behalf of 
Reinhard Kleeberg 
Sent: Tuesday, September 5, 2023 1:49:57 PM
To: 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 :

> 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 
>> 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 
>>
>> 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 ou

Re: [EXT] [External] Re: Step-like basline

[Reinhard Kleeberg]

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 :


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 
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 

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 i

Fwd: [EXT] [External] Re: Step-like basline

[Luca Lutterotti]

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 
> 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 
> 
> 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 :
> 
>> 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 Ingegn

Re: [EXT] [External] Re: Step-like basline

[Reinhard Kleeberg]

er 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  
 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" <mailto:kleeb...@mineral.tu-freiberg.de>>

À "Habib Boughzala" 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 <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" <mailto:alan.he...@neutronoptics.com>>
À "Reinhard Kleeberg" <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  
<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 complica

Re: [EXT] [External] Re: Step-like basline

[francois Goutenoire]

Dear everyone,

A very nice discussion to help young people in the field of powder 
diffraction.
In our case we are the happy user of two "quick and dirty" 
diffractometers (no brand of course !)
but with two different radiations : copper and cobalt with respectively 
Nickel and Iron K filter + Modern strip detector
Then in order to check for chemical or spectral pollution ?  we combine 
the both set of data in order to check and explain all the peaks.

Otherwise, we use Topas V5 to calculate all the tungstene pollution.
Sometimes many with some old X-ray tube (4 years !)
To help you few documents ( sorry some are in french).
https://perso.univ-lemans.fr/~fgouten/Spectral_Pollution

Best wishes François

Le 05/09/2023 à 08:56, Reinhard Kleeberg a écrit :

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 :


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 
 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" <mailto:kleeb...@mineral.tu-freiberg.de>>

À "Habib Boughzala" 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 an

Re: [EXT] [External] Re: Step-like basline

[Reinhard Kleeberg]

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 :


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  
 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" <mailto:kleeb...@mineral.tu-freiberg.de>>

À "Habib Boughzala" 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 <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 vis

RE: [EXT] [External] Re: Step-like basline

[Cline, James P. Dr. (Fed)]

Our favored configuration is a Johansson incident beam monochromator and a 
naked PSD.


James P. Cline
Materials Measurement Science Division
National Institute of Standards and Technology
100 Bureau Dr. stop 8370 [ B113 / Bldg 217 ]
Gaithersburg, MD 20899-8523USA
james.cl...@nist.gov<mailto:james.cl...@nist.gov>
https://www.nist.gov/people/james-p-cline
(301) 975 5793

From: rietveld_l-requ...@ill.fr  On Behalf Of Luca 
Lutterotti
Sent: Monday, September 4, 2023 1:08 PM
To: rietveld_l@ill.fr
Cc: Habib Boughzala 
Subject: Re: [EXT] [External] Re: Step-like basline

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

[cid:image001.png@01D9DF3B.30AEB200]

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)

[cid:image002.png@01D9DF3B.30AEB200][cid:image003.png@01D9DF3B.30AEB200][cid:image004.png@01D9DF3B.30AEB200][cid:image005.png@01D9DF3B.30AEB200][cid:image006.png@01D9DF3B.30AEB200]

Maud: http://maud.radiographema.com<http://maud.radiographema/>




On 4 Sep 2023, at 12:20, Habib Boughzala 
mailto: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" 
mailto:kleeb...@mineral.tu-freiberg.de>>
À "Habib Boughzala" 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 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" 
mailto:alan.he...@neutronoptics.com>>
À "Reinhard Kleeberg" 
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

Re: Re[4]: [EXT] Re: [External] Re: Step-like basline

[Alan W Hewat]

It's Shay who has the problem, not Habib, and we have heard nothing more
from him following his initial enquiry and all this expert advice.

Dr Alan Hewat, NeutronOptics
Grenoble, FRANCE (from phone)
alan.he...@neutronoptics.com
+33.476984168 VAT:FR79499450856
http://NeutronOptics.com/hewat
___


On Mon, 4 Sept 2023, 19:39 Roberto de Avillez,  wrote:

> Dear Habib,
>
> Run the silicon crystal diffraction without the Ni filter, you will
> confirm Kleeberg's explanation.
>
> Best regards,
> Roberto de Avillez
>
> Em seg., 4 de set. de 2023 às 07:20, Habib Boughzala <
> habib.boughz...@ipein.rnu.tn> escreveu:
>
>> 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" 
>> À "Habib Boughzala" 
>> Cc 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 :
>>
>>
>> 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" 
>> À "Reinhard Kleeberg" 
>> Cc 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> 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 "e

Re: Re[4]: [EXT] Re: [External] Re: Step-like basline

[Roberto de Avillez]

Dear Habib,

Run the silicon crystal diffraction without the Ni filter, you will confirm
Kleeberg's explanation.

Best regards,
Roberto de Avillez

Em seg., 4 de set. de 2023 às 07:20, Habib Boughzala <
habib.boughz...@ipein.rnu.tn> escreveu:

> 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" 
> À "Habib Boughzala" 
> Cc 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 :
>
>
> 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" 
> À "Reinhard Kleeberg" 
> Cc 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> 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 :
>
>
> Topas can model them quite well. The functionality was introduced in
> version 5.
>
> On Mon, 4 Sep 2023, 00:54 Kurt Leinenweber,  wrote:
>
>
> Hi, Are these things modeled in Rietveld programs, by chance? It seems
> like a lot of

Re: [EXT] [External] Re: Step-like basline

[Luca Lutterotti]

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  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"  <mailto:kleeb...@mineral.tu-freiberg.de>>
> À "Habib Boughzala" 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 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" >> <mailto:alan.he...@neutronoptics.com>>
>>> À "Reinhard Kleeberg" >> <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 
>>>&

Re[4]: [EXT] Re: [External] Re: Step-like basline

[Habib Boughzala]

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" 
À "Habib Boughzala" 
Cc 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 :


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" 
À "Reinhard Kleeberg" 
Cc 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  
 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 :


Topas can model them quite well. The functionality was introduced in
version 5.

On Mon, 4 Sep 2023, 00:54 Kurt Leinenweber,  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  *On Behalf
Of *Thomas Gegan
*Sent:* Sunday, September 3, 2023 9:16 AM
*To:* Bish, David L ; Shay Tirosh ;
Fernando Igoa 
*Cc:* Rietveld List (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
Postal Address: BASF Corporation, , 25 Middlesex Essex Turnpike, 08830
Iselin, United States



*From:* rietveld_l-requ...@ill.fr  *On Behalf
Of *Bish, David L
*Sent:* Sunday, September 3, 2023 7:08 AM
*To:* Shay Tirosh ; Fernando Igoa <
fer.igoa.1...@gmail.com

Re: [EXTERNAL] Re: Step-like basline

[Payzant, Andrew]

Habib,

Reinhard has nailed it – no need for a larger discussion as these artifacts are 
well understood. The late William Parrish published a paper describing these 
sort of artifacts ages ago (maybe 1950’s?).

Andrew
---
Dr. E. Andrew Payzant, FASM
Distinguished R&D Staff Member
Leader, Materials Engineering Group
Neutron Scattering Division

Mailing Address:
Oak Ridge National Laboratory
P.O. Box 2008
Building 8600, MS 6475
Oak Ridge, TN, 37831

Cell: (865) 235-4981
Email: payza...@ornl.gov<mailto:payza...@ornl.gov>
https://www.ornl.gov/staff-profile/e-andrew-payzant



From: rietveld_l-requ...@ill.fr  on behalf of 
Reinhard Kleeberg 
Date: Monday, September 4, 2023 at 10:47 AM
To: Habib Boughzala 
Cc: rietveld_l-requ...@ill.fr , rietveld_l@ill.fr 

Subject: [EXTERNAL] Re: Step-like basline
Habib,
obviously your instrument is equipped with a not cooled solid state 1D
detector (maybe Bruker Lynxeye?) and a Ni filter what is used for
"selective" absorbtion of the Cu K beta radiation.
What you see in the pattern is mainly a significant part of the tube
emission spectrum, diffracted at the Si 111 plane, and modified by the
Ni K absorption edge.
The peak at ~ 25.8 ° is the remnant Si 111 diffracting the Cu Kbeta1
wavelength 1.39223 A.
The edge is the Ni K absorbtion edge (I don't know the wavelength of
the edge exactly, ~ 1.49 A), and the doublet at ~ 28.4 ° is the Si 111
diffracting the Cu K alpha1 and alpha2, 1.54059 and 1.54443 A,
respectively.
The asymmetric slope of the background on the rigth side of the peak
is the unfiltered part of the Bremsstrahlung, their low energy part
what is not more cut by the Ni absorbtion.
As your wafer is a perfect Si 111 plane you get extreme intensity and
< 1 % intensity effects become clearly visible. Maybe you have seen a
Si powder pattern what appeared to be "clean", but if you would have
measured the powder pattern with better counting statistics, your Si
111 region would look quite similar.
Greetings

Reinhard

Zitat von Habib Boughzala :

> 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


--
TU Bergakademie Freiberg
Dr. R. Kleeberg
Mineralogisches Labor
Brennhausgasse 14
D-09596 Freiberg

Tel. ++49 (0) 3731-39-3244
Fax. ++49 (0) 3731-39-3129
++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

Re: Step-like basline

[Reinhard Kleeberg]

Habib,
obviously your instrument is equipped with a not cooled solid state 1D  
detector (maybe Bruker Lynxeye?) and a Ni filter what is used for  
"selective" absorbtion of the Cu K beta radiation.
What you see in the pattern is mainly a significant part of the tube  
emission spectrum, diffracted at the Si 111 plane, and modified by the  
Ni K absorption edge.
The peak at ~ 25.8 ° is the remnant Si 111 diffracting the Cu Kbeta1  
wavelength 1.39223 A.
The edge is the Ni K absorbtion edge (I don't know the wavelength of  
the edge exactly, ~ 1.49 A), and the doublet at ~ 28.4 ° is the Si 111  
diffracting the Cu K alpha1 and alpha2, 1.54059 and 1.54443 A,  
respectively.
The asymmetric slope of the background on the rigth side of the peak  
is the unfiltered part of the Bremsstrahlung, their low energy part  
what is not more cut by the Ni absorbtion.
As your wafer is a perfect Si 111 plane you get extreme intensity and  
< 1 % intensity effects become clearly visible. Maybe you have seen a  
Si powder pattern what appeared to be "clean", but if you would have  
measured the powder pattern with better counting statistics, your Si  
111 region would look quite similar.

Greetings

Reinhard

Zitat von Habib Boughzala :


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



--
TU Bergakademie Freiberg
Dr. R. Kleeberg
Mineralogisches Labor
Brennhausgasse 14
D-09596 Freiberg

Tel. ++49 (0) 3731-39-3244
Fax. ++49 (0) 3731-39-3129

++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

Re: Step-like basline

[Habib Boughzala]

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++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

Re: Re[2]: [EXT] Re: [External] Re: Step-like basline

[Reinhard Kleeberg]

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 :


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" 
À "Reinhard Kleeberg" 
Cc 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  
 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 :


Topas can model them quite well. The functionality was introduced in
version 5.

On Mon, 4 Sep 2023, 00:54 Kurt Leinenweber,  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  *On Behalf
Of *Thomas Gegan
*Sent:* Sunday, September 3, 2023 9:16 AM
*To:* Bish, David L ; Shay Tirosh ;
Fernando Igoa 
*Cc:* Rietveld List (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
Postal Address: BASF Corporation, , 25 Middlesex Essex Turnpike, 08830
Iselin, United States



*From:* rietveld_l-requ...@ill.fr  *On Behalf
Of *Bish, David L
*Sent:* Sunday, September 3, 2023 7:08 AM
*To:* Shay Tirosh ; Fernando Igoa <
fer.igoa.1...@gmail.com>
*Cc:* Rietveld List (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. 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

Re: [EXT] Re: [External] Re: Step-like basline

[Reinhard Kleeberg]

Alan, I'm quite sure that Shay's pattern shows the typical profile for  
a profile standard or any "highly crystalline" material measured with  
a standard configuration of his instrument. No problem with sample  
prep, no chance for improvement by modified instrumental setting  
(thicker filter would reduce K beta but make the Ni absorbtion edge  
more prominent). Unfortunately, lab instruments with "fast" 1D  
detectors with high intensity efficiency but bad energy resolution  
demanding for K beta filtering seem to be now the "quasi standard" on  
the market. Low noise patterns can be measured in short time, but the  
distorted profiles are hard to fit by simple standard profiles in a  
similar quality. From this point of view it makes sense to find a  
working approach for fitting the data of such machines, too.


However, I got several measurements showing Co or Cu K beta remnants  
from users despite the manufacturer has claimed that the good energy  
resolution of their detector (no names here!) alone would remove K  
beta "completely". Sometimes the customers were adviced by the company  
cases to insert an additional filter, and the "edge problem" is back...


Btw, I learned that even traditional secondary-beam curved graphite  
002 monochromators are not always able to resolve a completely "clean"  
Cu K alpha1/2 doublet: As the W L alpha wavelength is close to Cu K  
alpha, in unfortunate cases (crystal quality or alignment) even such  
machines may produce measurable/visible W L satellites when old tubes  
are in use. For economic reasons, some people prefer to add a scalable  
W L satellite peak in the BGMN wavelength model instead of buying a  
new tube...


Personally, I love my Peltier cooled 0D Si drift detectors. They  
really can completely suppress K beta and even remove any W L from Cu  
K alpha, no need for scalable satellite peaks in the profile model.  
Just some minor "wavelength feets" must be added to approximate the  
ROI window. Practically, the profiles are comparable with the ones  
obtained by a classical well aligned graphite monochromator plus  
szintillation counter, but with 5 times more intensity. And the  
detector may be used for some qualitative XRF (of course elements from  
K- only, as in air).


Reinhard

Zitat von Alan W Hewat :


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> 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 :

> Topas can model them quite well. The functionality was introduced in
> version 5.
>
> On Mon, 4 Sep 2023, 00:54 Kurt Leinenweber,  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  *On
Behalf
>> Of *Thomas Gegan
>> *Sent:* Sunday, September 3, 2023 9:16 AM
>> *To:* Bish, David L ; Shay Tirosh ;
>> Fernando Igoa 
>> *Cc:* Rietveld List (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 

RE: [EXT] Re: [External] Re: Step-like basline

[alancoelho]

Yes Frank, the macro is working with V5 of TOPAS-Academic; TOPAS should be the 
same.

Cheers

Alan

 

-Original Message-
From: Frank Girgsdies  
Sent: Monday, September 4, 2023 7:09 PM
To: alancoe...@bigpond.com
Cc: rietveld_l@ill.fr
Subject: Re: [EXT] Re: [External] Re: Step-like basline

 

Dear Alan,

 

Is this updated macro downward compatible with TOPAS version 5?

 

If yes, I would edit my topas.inc and try it.

 

Thanks and cheers,

Frank

 

On 04.09.2023 10:44,  <mailto:alancoe...@bigpond.com> alancoe...@bigpond.com 
wrote:

> Hi Kurt

> 

> TOPAS models absorption edges well. Page 158 of the Technical 

> Reference at  <http://www.topas-academic.net/Technical_Reference.pdf> 
> http://www.topas-academic.net/Technical_Reference.pdf

> < <http://www.topas-academic.net/Technical_Reference.pdf> 
> http://www.topas-academic.net/Technical_Reference.pdf> shows the result.

> 

> The macro in question is modifies the emission profile which is how I 

> think it should be modelled:

> 

> macro Absorption_Edge_Correction_Eqn(& edge, & a_white, & b_white, & 

> a_erf, & edge_extra)

> 

> {

> 

>modify_peak_eqn =

> 

>   (

> 

>  Get(current_peak) +

> 

>  a_white Exp(- b_white (Get(current_peak_x) - edge)^2) / 

> Tan(Th)

> 

>  ' Not necessary

> 

>  ' If(Get(current_peak_x) < edge, 1/Get(current_peak_x)^3, 

> 1 )

> 

>   )

> 

>   (edge_extra + 0.5 (1 + Erf_Approx( a_erf 

> (Get(current_peak_x)

> - edge))) );

> 

> }

> 

> If someone spots a problem then I would be happy to know. The line 

> commented out is due to the fact it makes little difference to the result.

> 

> Cheers

> 

> Alan

> 

> *From:*rietveld_l-requ...@ill.fr < <mailto:rietveld_l-requ...@ill.fr> 
> rietveld_l-requ...@ill.fr> *On 

> Behalf Of *Kurt Leinenweber

> *Sent:* Monday, September 4, 2023 2:53 AM

> *To:* Thomas Gegan < <mailto:tom.ge...@basf.com> tom.ge...@basf.com>; Bish, 
> David L 

> < <mailto:b...@indiana.edu> b...@indiana.edu>; Shay Tirosh < 
> <mailto:stiro...@gmail.com> stiro...@gmail.com>; Fernando Igoa 

> < <mailto:fer.igoa.1...@gmail.com> fer.igoa.1...@gmail.com>

> *Cc:* Rietveld List ( <mailto:rietveld_l@ill.fr> rietveld_l@ill.fr) < 
> <mailto:rietveld_l@ill.fr> rietveld_l@ill.fr>

> *Subject:* RE: [EXT] Re: [External] Re: Step-like basline

> 

> 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> 
> mailto:rietveld_l-requ...@ill.fr>

> < <mailto:rietveld_l-requ...@ill.fr%20%3cmailto: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 < <mailto:b...@indiana.edu%20%3cmailto:b...@indiana.edu> 
> b...@indiana.edu <mailto:b...@indiana.edu>>; Shay 

> Tirosh < <mailto:stiro...@gmail.com%20%3cmailto:stiro...@gmail.com> 
> stiro...@gmail.com <mailto:stiro...@gmail.com>>; Fernando Igoa 

> < <mailto:fer.igoa.1...@gmail.com%20%3cmailto:fer.igoa.1...@gmail.com> 
> fer.igoa.1...@gmail.com <mailto:fer.igoa.1...@gmail.com>>

> *Cc:* Rietveld List ( <mailto:rietveld_l@ill.fr> rietveld_l@ill.fr < 
> <mailto:rietveld_l@ill.fr> mailto:rietveld_l@ill.fr>) 

> < <mailto:rietveld_l@ill.fr%20%3cmailto: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:  <mailto:tom.ge...@basf.com> 
> tom.ge...@basf.com 

> < <mailto: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> 
> mailto:rietveld_l-requ...@ill.fr>

> < <mailto:rietveld_l-requ...@ill.fr%20%3cmailto: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 < 
> <mailto:stiro...@gmail.com%20%3cmai

Re: [EXT] Re: [External] Re: Step-like basline

[Frank Girgsdies]

Dear Alan,

Is this updated macro downward compatible with TOPAS version 5?

If yes, I would edit my topas.inc and try it.

Thanks and cheers,
Frank

On 04.09.2023 10:44, alancoe...@bigpond.com wrote:

Hi Kurt

TOPAS models absorption edges well. Page 158 of the Technical Reference 
at http://www.topas-academic.net/Technical_Reference.pdf 
<http://www.topas-academic.net/Technical_Reference.pdf> shows the result.


The macro in question is modifies the emission profile which is how I 
think it should be modelled:


macro Absorption_Edge_Correction_Eqn(& edge, & a_white, & b_white, & 
a_erf, & edge_extra)


    {

   modify_peak_eqn =

  (

     Get(current_peak) +

     a_white Exp(- b_white (Get(current_peak_x) - edge)^2) / Tan(Th)

     ' Not necessary

     ' If(Get(current_peak_x) < edge, 1/Get(current_peak_x)^3, 1 )

  )

  (edge_extra + 0.5 (1 + Erf_Approx( a_erf (Get(current_peak_x) 
- edge))) );


    }

If someone spots a problem then I would be happy to know. The line 
commented out is due to the fact it makes little difference to the result.


Cheers

Alan

*From:*rietveld_l-requ...@ill.fr  *On Behalf 
Of *Kurt Leinenweber

*Sent:* Monday, September 4, 2023 2:53 AM
*To:* Thomas Gegan ; Bish, David L 
; Shay Tirosh ; Fernando Igoa 


*Cc:* Rietveld List (rietveld_l@ill.fr) 
*Subject:* RE: [EXT] Re: [External] Re: Step-like basline

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> 
mailto:rietveld_l-requ...@ill.fr>> *On 
Behalf Of *Thomas Gegan

*Sent:* Sunday, September 3, 2023 9:16 AM
*To:* Bish, David L mailto:b...@indiana.edu>>; Shay 
Tirosh mailto:stiro...@gmail.com>>; Fernando Igoa 
mailto:fer.igoa.1...@gmail.com>>
*Cc:* Rietveld List (rietveld_l@ill.fr <mailto: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> 
mailto:rietveld_l-requ...@ill.fr>> *On 
Behalf Of *Bish, David L

*Sent:* Sunday, September 3, 2023 7:08 AM
*To:* Shay Tirosh mailto:stiro...@gmail.com>>; 
Fernando Igoa mailto:fer.igoa.1...@gmail.com>>
*Cc:* Rietveld List (rietveld_l@ill.fr <mailto: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> 
mailto:rietveld_l-requ...@ill.fr>> on behalf 
of Fernando Igoa mailto:fer.igoa.1...@gmail.com>>

*Sent:* Sunday, September 3, 2023 3:06 AM
*To:* Shay Tirosh mailto:stiro...@gmail.com>>
*Cc:* Rietveld List (rietveld_l@ill.fr <mailto: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 <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

-- 


++
Please do NOT attach files to the whole list
mailto:alan.he...@neutronoptics.com>>
Send commands to mailto:lists..

RE: [EXT] Re: [External] Re: Step-like basline

[alancoelho]

Hi Kurt

 

TOPAS models absorption edges well. Page 158 of the Technical Reference at
http://www.topas-academic.net/Technical_Reference.pdf shows the result. 

 

The macro in question is modifies the emission profile which is how I think
it should be modelled:

 

macro Absorption_Edge_Correction_Eqn(& edge, & a_white, & b_white, & a_erf,
& edge_extra)

   {

  modify_peak_eqn =

 (

Get(current_peak) +

a_white Exp(- b_white (Get(current_peak_x) - edge)^2) / Tan(Th)

' Not necessary

' If(Get(current_peak_x) < edge, 1/Get(current_peak_x)^3, 1 )

 )

 (edge_extra + 0.5 (1 + Erf_Approx( a_erf (Get(current_peak_x) -
edge))) );

   }

 

If someone spots a problem then I would be happy to know. The line commented
out is due to the fact it makes little difference to the result. 

 

Cheers

Alan

 

From: rietveld_l-requ...@ill.fr  On Behalf Of
Kurt Leinenweber
Sent: Monday, September 4, 2023 2:53 AM
To: Thomas Gegan ; Bish, David L ;
Shay Tirosh ; Fernando Igoa 
Cc: Rietveld List (rietveld_l@ill.fr) 
Subject: RE: [EXT] Re: [External] Re: Step-like basline

 

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>
mailto:rietveld_l-requ...@ill.fr> > On Behalf Of
Thomas Gegan
Sent: Sunday, September 3, 2023 9:16 AM
To: Bish, David L mailto:b...@indiana.edu> >; Shay Tirosh
mailto:stiro...@gmail.com> >; Fernando Igoa
mailto:fer.igoa.1...@gmail.com> >
Cc: Rietveld List (rietveld_l@ill.fr <mailto: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:  <mailto:tom.ge...@basf.com>
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>
mailto:rietveld_l-requ...@ill.fr> > On Behalf Of
Bish, David L
Sent: Sunday, September 3, 2023 7:08 AM
To: Shay Tirosh mailto:stiro...@gmail.com> >; Fernando
Igoa mailto:fer.igoa.1...@gmail.com> >
Cc: Rietveld List (rietveld_l@ill.fr <mailto: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_2SKhRniGa71nxuOL3GcxiyD83i2mnNN
0Z48HPkn4zjKqH-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>
mailto:rietveld_l-requ...@ill.fr> > on behalf of
Fernando Igoa mailto:fer.igoa.1...@gmail.com> >
Sent: Sunday, September 3, 2023 3:06 AM
To: Shay Tirosh mailto:stiro...@gmail.com> >
Cc: Rietveld List (rietveld_l@ill.fr <mailto: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 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

-- 

 

 

 

 

 

++
Please do NOT attach files to the whole list mailto:alan.he...@neutronoptics.com> >
Send commands to mailto:lists...@ill.fr> > eg: HELP as the
subject with no body text
The Rietveld_L list archive is on
http://www.mail-archive.com/rietveld_l@ill.fr/
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N0Z48HPkn4zjJTf8rNHg$> 
+

Re: [EXT] Re: [External] Re: Step-like basline

[Alan W Hewat]

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> 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 :
>
> > Topas can model them quite well. The functionality was introduced in
> > version 5.
> >
> > On Mon, 4 Sep 2023, 00:54 Kurt Leinenweber,  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  *On
> Behalf
> >> Of *Thomas Gegan
> >> *Sent:* Sunday, September 3, 2023 9:16 AM
> >> *To:* Bish, David L ; Shay Tirosh  >;
> >> Fernando Igoa 
> >> *Cc:* Rietveld List (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
> >> Postal Address: BASF Corporation, , 25 Middlesex Essex Turnpike, 08830
> >> Iselin, United States
> >>
> >>
> >>
> >> *From:* rietveld_l-requ...@ill.fr  *On
> Behalf
> >> Of *Bish, David L
> >> *Sent:* Sunday, September 3, 2023 7:08 AM
> >> *To:* Shay Tirosh ; Fernando Igoa <
> >> fer.igoa.1...@gmail.com>
> >> *Cc:* Rietveld List (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. 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  on behalf
> >> of Fernando Igoa 
> >> *Sent:* Sunday, September 3, 2023 3:06 AM
> >> *To:* Shay Tirosh 
> >> *Cc:* Rietveld List (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.
> >>
> >>

Re: [EXT] Re: [External] Re: Step-like basline

[Frank Girgsdies]

-

*From:*rietveld_l-requ...@ill.fr <mailto:rietveld_l-requ...@ill.fr>
mailto:rietveld_l-requ...@ill.fr>> on
behalf of Fernando Igoa mailto:fer.igoa.1...@gmail.com>>
*Sent:* Sunday, September 3, 2023 3:06 AM
    *To:* Shay Tirosh mailto:stiro...@gmail.com>>
*Cc:* Rietveld List (rietveld_l@ill.fr <mailto: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 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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Re: [EXT] Re: [External] Re: Step-like basline

[Reinhard Kleeberg]

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 :


Topas can model them quite well. The functionality was introduced in
version 5.

On Mon, 4 Sep 2023, 00:54 Kurt Leinenweber,  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  *On Behalf
Of *Thomas Gegan
*Sent:* Sunday, September 3, 2023 9:16 AM
*To:* Bish, David L ; Shay Tirosh ;
Fernando Igoa 
*Cc:* Rietveld List (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
Postal Address: BASF Corporation, , 25 Middlesex Essex Turnpike, 08830
Iselin, United States



*From:* rietveld_l-requ...@ill.fr  *On Behalf
Of *Bish, David L
*Sent:* Sunday, September 3, 2023 7:08 AM
*To:* Shay Tirosh ; Fernando Igoa <
fer.igoa.1...@gmail.com>
*Cc:* Rietveld List (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. 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:* rietveld_l-requ...@ill.fr  on behalf
of Fernando Igoa 
*Sent:* Sunday, September 3, 2023 3:06 AM
*To:* Shay Tirosh 
*Cc:* Rietveld List (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  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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++

Re: [EXT] Re: [External] Re: Step-like basline

[Matthew Rowles]

Topas can model them quite well. The functionality was introduced in
version 5.

On Mon, 4 Sep 2023, 00:54 Kurt Leinenweber,  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  *On Behalf
> Of *Thomas Gegan
> *Sent:* Sunday, September 3, 2023 9:16 AM
> *To:* Bish, David L ; Shay Tirosh ;
> Fernando Igoa 
> *Cc:* Rietveld List (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
> Postal Address: BASF Corporation, , 25 Middlesex Essex Turnpike, 08830
> Iselin, United States
>
>
>
> *From:* rietveld_l-requ...@ill.fr  *On Behalf
> Of *Bish, David L
> *Sent:* Sunday, September 3, 2023 7:08 AM
> *To:* Shay Tirosh ; Fernando Igoa <
> fer.igoa.1...@gmail.com>
> *Cc:* Rietveld List (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. Learn why this is important
> <https://urldefense.com/v3/__https:/aka.ms/LearnAboutSenderIdentification__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjKqH-aqqA$>
>
> Hello Shay,
>
> I think it is probably related to "tube tails". You can read about this in
> the literature (e.g., on the BGMN web site) and you can model it in some
> Rietveld software such as Topas. You don't normally notice this but it
> becomes apparent with higher-intensity peaks.
>
>
>
> Regards,
>
> Dave
> ----------
>
> *From:* rietveld_l-requ...@ill.fr  on behalf
> of Fernando Igoa 
> *Sent:* Sunday, September 3, 2023 3:06 AM
> *To:* Shay Tirosh 
> *Cc:* Rietveld List (rietveld_l@ill.fr) 
> *Subject:* [External] Re: Step-like basline
>
>
>
> This message was sent from a non-IU address. Please exercise caution when
> clicking links or opening attachments from external sources.
>
>
>
> Hey Shay,
>
>
>
> Are you using a motorized slit during the measurement? These may open up
> abruptly to compensate for the angular dependence of the footprint and thus
> generate an abrupt increase in the intensity.
>
>
>
> Hope it helps :)
>
>
>
> On Sun, Sep 3, 2023, 8:50 AM Shay Tirosh  wrote:
>
> Dear Rietvelders
>
> I am attaching a zoom-in on a diffraction profile.
>
> My question is what is the origin of the step-like profile next to a very
> large reflection peak?
>
> Is it a sample preparation problem?
>
> Is it part of the baseline?
>
> Thanks
>
> Shay
>
> --
>
>
>
>
>
>
>
>
>
>
>
> ++
> Please do NOT attach files to the whole list  >
> Send commands to  eg: HELP as the subject with no body
> text
> The Rietveld_L list archive is on
> http://www.mail-archive.com/rietveld_l@ill.fr/
> <https://urldefense.com/v3/__http:/www.mail-archive.com/rietveld_l@ill.fr/__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjJTf8rNHg$>
> ++
>
> ++
> Please do NOT attach files to the whole list  >
> Send commands to  eg: HELP as the subject with no body
> text
> The Rietveld_L list archive is on
> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++
>
>
++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

Re: [EXT] Re: [External] Re: Step-like basline

[Bish, David L]

I agree, it does look more like an absorption edge than tube tails (not enough 
coffee yet at 7AM). But tube tails will be there in addition. I do not have the 
absorption edge problem on my primary instrument as we do not use a PSD or a 
beta filter, but we easily see tube tail effects on very intense reflections.

We do not yet know Shay's instrumental configuration, but I assume he is using 
a PSD with a K-beta filter.  How important the effects are in his pattern is 
open to discussion/argument. If tube tails are modeled, then the absorption 
edge effect is minor and is probably sufficiently removed from peak centroids 
that it will not significantly affect profile parameters; a test would be easy. 
I imagine that the effects in question would not be very noticeable on a linear 
plot with the intense peak on scale. But, as Jim said, these effects can also 
be modeled.

The contribution from K-beta (and any other "extra" radiations, e.g., W) can 
and should always be modeled.

Dave

From: miguel gregorkiewitz 
Sent: Sunday, September 3, 2023 3:02 PM
To: Kurt Leinenweber 
Cc: Thomas Gegan ; Bish, David L ; Shay 
Tirosh ; Fernando Igoa ; Rietveld 
List (rietveld_l@ill.fr) 
Subject: Re: [EXT] Re: [External] Re: Step-like basline

Forgot to say that the problem is absent in diffractometers with monochromator. 
I observed it first in a bragg-brentano diffractometer with accelrys linear 
position sensitive detector (panalytical) which had no monochromator


El dom, 3 sep. 2023 20:47, miguel gregorkiewitz 
mailto:gregorm...@gmail.com>> escribió:
Kbeta can always be added, but for the absorption edge there seems to be no 
remedy, and as seen in the graph, it is far more important


El dom, 3 sep. 2023 18:54, Kurt Leinenweber 
mailto:ku...@asu.edu>> escribió:

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> 
mailto:rietveld_l-requ...@ill.fr>> On Behalf Of 
Thomas Gegan
Sent: Sunday, September 3, 2023 9:16 AM
To: Bish, David L mailto:b...@indiana.edu>>; Shay Tirosh 
mailto:stiro...@gmail.com>>; Fernando Igoa 
mailto:fer.igoa.1...@gmail.com>>
Cc: Rietveld List (rietveld_l@ill.fr<mailto: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

[X]



From: rietveld_l-requ...@ill.fr<mailto: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 mailto:stiro...@gmail.com>>; Fernando Igoa 
mailto:fer.igoa.1...@gmail.com>>
Cc: Rietveld List (rietveld_l@ill.fr<mailto: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> 
mailto:rietveld_l-requ...@ill.fr>> on behalf of 
Fernando Igoa mailto:fer.igoa.1...@gmail.com>>
Sent: Sunday, September 3, 2023 3:06 AM
To: Shay Tirosh mailto:stiro...@gmail.com>>
Cc: Rietveld List (rietveld_l@ill.fr<mailto: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 
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 prepar

Re: [EXT] Re: [External] Re: Step-like basline

[miguel gregorkiewitz]

Sorry for the error in my previous mail: the detector was of course an
X'celerator, not Accelrys. Apologies


El dom, 3 sep. 2023 21:02, miguel gregorkiewitz 
escribió:

> Forgot to say that the problem is absent in diffractometers with
> monochromator. I observed it first in a bragg-brentano diffractometer with
> accelrys linear position sensitive detector (panalytical) which had no
> monochromator
>
>
> El dom, 3 sep. 2023 20:47, miguel gregorkiewitz 
> escribió:
>
>> Kbeta can always be added, but for the absorption edge there seems to be
>> no remedy, and as seen in the graph, it is far more important
>>
>>
>> El dom, 3 sep. 2023 18:54, Kurt Leinenweber  escribió:
>>
>>> 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  *On
>>> Behalf Of *Thomas Gegan
>>> *Sent:* Sunday, September 3, 2023 9:16 AM
>>> *To:* Bish, David L ; Shay Tirosh ;
>>> Fernando Igoa 
>>> *Cc:* Rietveld List (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
>>> Postal Address: BASF Corporation, , 25 Middlesex Essex Turnpike, 08830
>>> Iselin, United States
>>>
>>>
>>>
>>> *From:* rietveld_l-requ...@ill.fr  *On
>>> Behalf Of *Bish, David L
>>> *Sent:* Sunday, September 3, 2023 7:08 AM
>>> *To:* Shay Tirosh ; Fernando Igoa <
>>> fer.igoa.1...@gmail.com>
>>> *Cc:* Rietveld List (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. Learn why this is important
>>> <https://urldefense.com/v3/__https:/aka.ms/LearnAboutSenderIdentification__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjKqH-aqqA$>
>>>
>>> Hello Shay,
>>>
>>> I think it is probably related to "tube tails". You can read about this
>>> in the literature (e.g., on the BGMN web site) and you can model it in some
>>> Rietveld software such as Topas. You don't normally notice this but it
>>> becomes apparent with higher-intensity peaks.
>>>
>>>
>>>
>>> Regards,
>>>
>>> Dave
>>> --
>>>
>>> *From:* rietveld_l-requ...@ill.fr  on behalf
>>> of Fernando Igoa 
>>> *Sent:* Sunday, September 3, 2023 3:06 AM
>>> *To:* Shay Tirosh 
>>> *Cc:* Rietveld List (rietveld_l@ill.fr) 
>>> *Subject:* [External] Re: Step-like basline
>>>
>>>
>>>
>>> This message was sent from a non-IU address. Please exercise caution
>>> when clicking links or opening attachments from external sources.
>>>
>>>
>>>
>>> Hey Shay,
>>>
>>>
>>>
>>> Are you using a motorized slit during the measurement? These may open up
>>> abruptly to compensate for the angular dependence of the footprint and thus
>>> generate an abrupt increase in the intensity.
>>>
>>>
>>>
>>> Hope it helps :)
>>>
>>>
>>>
>>> On Sun, Sep 3, 2023, 8:50 AM Shay Tirosh  wrote:
>>>
>>> Dear Rietvelders
>>>
>>> I am attaching a zoom-in on a diffraction profile.
>>>
>>> My question is what is the origin of the step-like profile next to a
>>> very large reflection peak?
>>>
>>> Is it a sample preparation problem?
>>>
>>> Is it part of the baseline?
>>>
>>> Thanks
>>>
>>> Shay
>>>
>>> --
>>>
>>>
>>>
>>>
>>>
>>>
>>>
>>>
>>>
>>>
>>>
>>> ++
>>> Please do NOT attach files to the whole list <
>>> alan.he...@neutronoptics.com>
>>> Send commands to  eg: HELP as the subject with no body
>>> text
>>> The Rietveld_L list archive is on
>>> http://www.mail-archive.com/rietveld_l@ill.fr/
>>> <https://urldefense.com/v3/__http:/www.mail-archive.com/rietveld_l@ill.fr/__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjJTf8rNHg$>
>>> ++
>>>
>>> ++
>>> Please do NOT attach files to the whole list
>>> 
>>> Send commands to  eg: HELP as the subject with no body
>>> text
>>> The Rietveld_L list archive is on
>>> http://www.mail-archive.com/rietveld_l@ill.fr/
>>> ++
>>>
>>>
++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

RE: [EXT] Re: [External] Re: Step-like basline

[Cline, James P. Dr. (Fed)]

It can be modeled in Topas


James P. Cline
Materials Measurement Science Division
National Institute of Standards and Technology
100 Bureau Dr. stop 8370 [ B113 / Bldg 217 ]
Gaithersburg, MD 20899-8523USA
james.cl...@nist.gov<mailto:james.cl...@nist.gov>
https://www.nist.gov/people/james-p-cline
(301) 975 5793

From: rietveld_l-requ...@ill.fr  On Behalf Of Kurt 
Leinenweber
Sent: Sunday, September 3, 2023 12:53 PM
To: Thomas Gegan ; Bish, David L ; Shay 
Tirosh ; Fernando Igoa 
Cc: Rietveld List (rietveld_l@ill.fr) 
Subject: RE: [EXT] Re: [External] Re: Step-like basline

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> 
mailto:rietveld_l-requ...@ill.fr>> On Behalf Of 
Thomas Gegan
Sent: Sunday, September 3, 2023 9:16 AM
To: Bish, David L mailto:b...@indiana.edu>>; Shay Tirosh 
mailto:stiro...@gmail.com>>; Fernando Igoa 
mailto:fer.igoa.1...@gmail.com>>
Cc: Rietveld List (rietveld_l@ill.fr<mailto: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
[cid:image001.png@01D9DE7A.0C97ED80]

From: rietveld_l-requ...@ill.fr<mailto: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 mailto:stiro...@gmail.com>>; Fernando Igoa 
mailto:fer.igoa.1...@gmail.com>>
Cc: Rietveld List (rietveld_l@ill.fr<mailto: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> 
mailto:rietveld_l-requ...@ill.fr>> on behalf of 
Fernando Igoa mailto:fer.igoa.1...@gmail.com>>
Sent: Sunday, September 3, 2023 3:06 AM
To: Shay Tirosh mailto:stiro...@gmail.com>>
Cc: Rietveld List (rietveld_l@ill.fr<mailto: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 
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?
[cid:image002.png@01D9DE7A.0C97ED80]
Thanks
Shay
--









++
Please do NOT attach files to the whole list 
mailto:alan.he...@neutronoptics.com>>
Send commands to mailto:lists...@ill.fr>> eg: HELP as the 
subject with no body text
The Rietveld_L list archive is on 
http://www.mail-archive.com/rietveld_l@ill.fr/<https://urldefense.com/v3/__http:/www.mail-archive.com/rietveld_l@ill.fr/__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjJTf8rNHg$>
++
++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
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++

Re: [EXT] Re: [External] Re: Step-like basline

[miguel gregorkiewitz]

Forgot to say that the problem is absent in diffractometers with
monochromator. I observed it first in a bragg-brentano diffractometer with
accelrys linear position sensitive detector (panalytical) which had no
monochromator


El dom, 3 sep. 2023 20:47, miguel gregorkiewitz 
escribió:

> Kbeta can always be added, but for the absorption edge there seems to be
> no remedy, and as seen in the graph, it is far more important
>
>
> El dom, 3 sep. 2023 18:54, Kurt Leinenweber  escribió:
>
>> 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  *On Behalf
>> Of *Thomas Gegan
>> *Sent:* Sunday, September 3, 2023 9:16 AM
>> *To:* Bish, David L ; Shay Tirosh ;
>> Fernando Igoa 
>> *Cc:* Rietveld List (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
>> Postal Address: BASF Corporation, , 25 Middlesex Essex Turnpike, 08830
>> Iselin, United States
>>
>>
>>
>> *From:* rietveld_l-requ...@ill.fr  *On Behalf
>> Of *Bish, David L
>> *Sent:* Sunday, September 3, 2023 7:08 AM
>> *To:* Shay Tirosh ; Fernando Igoa <
>> fer.igoa.1...@gmail.com>
>> *Cc:* Rietveld List (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. Learn why this is important
>> <https://urldefense.com/v3/__https:/aka.ms/LearnAboutSenderIdentification__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjKqH-aqqA$>
>>
>> Hello Shay,
>>
>> I think it is probably related to "tube tails". You can read about this
>> in the literature (e.g., on the BGMN web site) and you can model it in some
>> Rietveld software such as Topas. You don't normally notice this but it
>> becomes apparent with higher-intensity peaks.
>>
>>
>>
>> Regards,
>>
>> Dave
>> --
>>
>> *From:* rietveld_l-requ...@ill.fr  on behalf
>> of Fernando Igoa 
>> *Sent:* Sunday, September 3, 2023 3:06 AM
>> *To:* Shay Tirosh 
>> *Cc:* Rietveld List (rietveld_l@ill.fr) 
>> *Subject:* [External] Re: Step-like basline
>>
>>
>>
>> This message was sent from a non-IU address. Please exercise caution when
>> clicking links or opening attachments from external sources.
>>
>>
>>
>> Hey Shay,
>>
>>
>>
>> Are you using a motorized slit during the measurement? These may open up
>> abruptly to compensate for the angular dependence of the footprint and thus
>> generate an abrupt increase in the intensity.
>>
>>
>>
>> Hope it helps :)
>>
>>
>>
>> On Sun, Sep 3, 2023, 8:50 AM Shay Tirosh  wrote:
>>
>> Dear Rietvelders
>>
>> I am attaching a zoom-in on a diffraction profile.
>>
>> My question is what is the origin of the step-like profile next to a very
>> large reflection peak?
>>
>> Is it a sample preparation problem?
>>
>> Is it part of the baseline?
>>
>> Thanks
>>
>> Shay
>>
>> --
>>
>>
>>
>>
>>
>>
>>
>>
>>
>>
>>
>> ++
>> Please do NOT attach files to the whole list <
>> alan.he...@neutronoptics.com>
>> Send commands to  eg: HELP as the subject with no body
>> text
>> The Rietveld_L list archive is on
>> http://www.mail-archive.com/rietveld_l@ill.fr/
>> <https://urldefense.com/v3/__http:/www.mail-archive.com/rietveld_l@ill.fr/__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjJTf8rNHg$>
>> ++
>>
>> ++
>> Please do NOT attach files to the whole list > >
>> Send commands to  eg: HELP as the subject with no body
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>> ++
>>
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Re: [EXT] Re: [External] Re: Step-like basline

[miguel gregorkiewitz]

Kbeta can always be added, but for the absorption edge there seems to be no
remedy, and as seen in the graph, it is far more important


El dom, 3 sep. 2023 18:54, Kurt Leinenweber  escribió:

> 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  *On Behalf
> Of *Thomas Gegan
> *Sent:* Sunday, September 3, 2023 9:16 AM
> *To:* Bish, David L ; Shay Tirosh ;
> Fernando Igoa 
> *Cc:* Rietveld List (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
> Postal Address: BASF Corporation, , 25 Middlesex Essex Turnpike, 08830
> Iselin, United States
>
>
>
> *From:* rietveld_l-requ...@ill.fr  *On Behalf
> Of *Bish, David L
> *Sent:* Sunday, September 3, 2023 7:08 AM
> *To:* Shay Tirosh ; Fernando Igoa <
> fer.igoa.1...@gmail.com>
> *Cc:* Rietveld List (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. Learn why this is important
> <https://urldefense.com/v3/__https:/aka.ms/LearnAboutSenderIdentification__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjKqH-aqqA$>
>
> Hello Shay,
>
> I think it is probably related to "tube tails". You can read about this in
> the literature (e.g., on the BGMN web site) and you can model it in some
> Rietveld software such as Topas. You don't normally notice this but it
> becomes apparent with higher-intensity peaks.
>
>
>
> Regards,
>
> Dave
> ----------
>
> *From:* rietveld_l-requ...@ill.fr  on behalf
> of Fernando Igoa 
> *Sent:* Sunday, September 3, 2023 3:06 AM
> *To:* Shay Tirosh 
> *Cc:* Rietveld List (rietveld_l@ill.fr) 
> *Subject:* [External] Re: Step-like basline
>
>
>
> This message was sent from a non-IU address. Please exercise caution when
> clicking links or opening attachments from external sources.
>
>
>
> Hey Shay,
>
>
>
> Are you using a motorized slit during the measurement? These may open up
> abruptly to compensate for the angular dependence of the footprint and thus
> generate an abrupt increase in the intensity.
>
>
>
> Hope it helps :)
>
>
>
> On Sun, Sep 3, 2023, 8:50 AM Shay Tirosh  wrote:
>
> Dear Rietvelders
>
> I am attaching a zoom-in on a diffraction profile.
>
> My question is what is the origin of the step-like profile next to a very
> large reflection peak?
>
> Is it a sample preparation problem?
>
> Is it part of the baseline?
>
> Thanks
>
> Shay
>
> --
>
>
>
>
>
>
>
>
>
>
>
> ++
> Please do NOT attach files to the whole list  >
> Send commands to  eg: HELP as the subject with no body
> text
> The Rietveld_L list archive is on
> http://www.mail-archive.com/rietveld_l@ill.fr/
> <https://urldefense.com/v3/__http:/www.mail-archive.com/rietveld_l@ill.fr/__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjJTf8rNHg$>
> ++
>
> ++
> Please do NOT attach files to the whole list  >
> Send commands to  eg: HELP as the subject with no body
> text
> The Rietveld_L list archive is on
> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++
>
>
++
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The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

RE: [EXT] Re: [External] Re: Step-like basline

[Kurt Leinenweber]

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  On Behalf Of Thomas 
Gegan
Sent: Sunday, September 3, 2023 9:16 AM
To: Bish, David L ; Shay Tirosh ; 
Fernando Igoa 
Cc: Rietveld List (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
[cid:image001.png@01D9DE4C.79FBB4C0]

From: rietveld_l-requ...@ill.fr<mailto: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 mailto:stiro...@gmail.com>>; Fernando Igoa 
mailto:fer.igoa.1...@gmail.com>>
Cc: Rietveld List (rietveld_l@ill.fr<mailto: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> 
mailto:rietveld_l-requ...@ill.fr>> on behalf of 
Fernando Igoa mailto:fer.igoa.1...@gmail.com>>
Sent: Sunday, September 3, 2023 3:06 AM
To: Shay Tirosh mailto:stiro...@gmail.com>>
Cc: Rietveld List (rietveld_l@ill.fr<mailto: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 
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?
[cid:image003.png@01D9DE4C.79FBB4C0]
Thanks
Shay
--









++
Please do NOT attach files to the whole list 
mailto:alan.he...@neutronoptics.com>>
Send commands to mailto:lists...@ill.fr>> eg: HELP as the 
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The Rietveld_L list archive is on 
http://www.mail-archive.com/rietveld_l@ill.fr/<https://urldefense.com/v3/__http:/www.mail-archive.com/rietveld_l@ill.fr/__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjJTf8rNHg$>
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++

RE: [EXT] Re: [External] Re: Step-like basline

[Thomas Gegan]

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
[cid:image001.png@01D9DE60.71BF4F10]

From: rietveld_l-requ...@ill.fr  On Behalf Of Bish, 
David L
Sent: Sunday, September 3, 2023 7:08 AM
To: Shay Tirosh ; Fernando Igoa 
Cc: Rietveld List (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://aka.ms/LearnAboutSenderIdentification>
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> 
mailto:rietveld_l-requ...@ill.fr>> on behalf of 
Fernando Igoa mailto:fer.igoa.1...@gmail.com>>
Sent: Sunday, September 3, 2023 3:06 AM
To: Shay Tirosh mailto:stiro...@gmail.com>>
Cc: Rietveld List (rietveld_l@ill.fr<mailto: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 
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?
[cid:image002.png@01D9DE60.71BF4F10]
Thanks
Shay
--









++
Please do NOT attach files to the whole list 
mailto:alan.he...@neutronoptics.com>>
Send commands to mailto:lists...@ill.fr>> eg: HELP as the 
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The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++
++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

RE: Step-like basline

[Cline, James P. Dr. (Fed)]

Yes; not the tube tails, however.


James P. Cline
Materials Measurement Science Division
National Institute of Standards and Technology
100 Bureau Dr. stop 8370 [ B113 / Bldg 217 ]
Gaithersburg, MD 20899-8523USA
james.cl...@nist.gov<mailto:james.cl...@nist.gov>
https://www.nist.gov/people/james-p-cline
(301) 975 5793

From: rietveld_l-requ...@ill.fr  On Behalf Of 
Matthew Rowles
Sent: Sunday, September 3, 2023 7:39 AM
To: Shay Tirosh 
Cc: RIETVELD_L Distribution List 
Subject: Re: Step-like basline

That's a k beta peak followed by a metal foil absorption edge followed by the K 
alpga peak.

On Sun, 3 Sep 2023, 14:50 Shay Tirosh, 
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?
[cid:image001.png@01D9DE43.8A7440F0]
Thanks
Shay
--





++
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mailto:alan.he...@neutronoptics.com>>
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++
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++

Re: Step-like basline

[Matthew Rowles]

That's a k beta peak followed by a metal foil absorption edge followed by
the K alpga peak.

On Sun, 3 Sep 2023, 14:50 Shay Tirosh,  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?
> [image: image.png]
> Thanks
> Shay
> --
>
>
>
>
>
>
>
>
> ++
> Please do NOT attach files to the whole list  >
> Send commands to  eg: HELP as the subject with no body
> text
> The Rietveld_L list archive is on
> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++
>
>
++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

Re: [External] Re: Step-like basline

[Bish, David L]

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  on behalf of 
Fernando Igoa 
Sent: Sunday, September 3, 2023 3:06 AM
To: Shay Tirosh 
Cc: Rietveld List (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 
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?
[image.png]
Thanks
Shay
--








++
Please do NOT attach files to the whole list 
Send commands to mailto:lists...@ill.fr>> eg: HELP as the 
subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++

Re: Step-like basline

[Fernando Igoa]

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  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?
> [image: image.png]
> Thanks
> Shay
> --
>
>
>
>
>
>
>
>
> ++
> Please do NOT attach files to the whole list  >
> Send commands to  eg: HELP as the subject with no body
> text
> The Rietveld_L list archive is on
> http://www.mail-archive.com/rietveld_l@ill.fr/
> ++
>
>
++
Please do NOT attach files to the whole list 
Send commands to  eg: HELP as the subject with no body text
The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/
++