Re: Hyper-Lorentzian effect on quantitative analysis

2021-03-04 Thread Florentino Sanchez Bajo 
Dear François, 

only a minor comment, that I don't know if it can be applied to your sample. 
Years ago (1988), a published paper indicated the possible relation between the 
super-Lorentzian shape of the peaks and the presence of a bimodal crystallite 
size distribution. Best regards, 

Florentino Sánchez 


De: "François Goutenoire"  
Para: "rietveld l"  
Enviados: Jueves, 4 de Marzo 2021 10:41:05 
Asunto: Re: Hyper-Lorentzian effect on quantitative analysis 

Dear Rietveld users, 

Thank you very much for all your responses, it will help us move forward on the 
subject. 
Unfortunately, I cannot say more because of an NDA. 
But it still looks very interesting from a fundamental point of view. 

Best whishes, françois Goutenoire 
Le 03/03/2021 à 18:47, Mendenhall, Marcus H. (Fed) a écrit : 



Is it really amorphous content, or is there a whole bunch of very fine 
nanocrystalline stuff or material with a very high defect density that is 
widening the peak?  If the fitter is having trouble matching the peak shape, it 
may be ascribing a fairly arbitrary portion between amorphous and crystalline.

Marcus Mendenhall

Materials Measurement Science Division
National Institute of Science and Technology
100 Bureau Dr. stop 8370 (217/B115)
Gaithersburg, MD 20899 USA
Phone: +1-301-975-8631
during COVID-19 response period:
Home phone: 301-916-5486
Cell: 615-293-3120 

BQ_BEGIN

On Mar 3, 2021, at 7:34 AM, François Goutenoire [ 
mailto:francois.gouteno...@univ-lemans.fr | 
 ] wrote:

Dear Rietveld users,

I have some industrial compound presenting a strong hyper-Lorentzian peak shape 
(eta=1.1 with HighScore). When we calculate the amorphous content after an 
internal standard addition, the result is 40%. The micro-absorption effect has 
been minimized (mu of the internal standard is closed to the compound).

But with some electronic transmission analysis no amorphous is observed.

The question is : Does a strong hyper-Lorentzian peak shape could influence 
quantitative analysis ?

François

-- 
*
Pr. Francois GOUTENOIRE
e-mail: [ mailto:francois.gouteno...@univ-lemans.fr | 
francois.gouteno...@univ-lemans.fr ] Tel: 02.43.83.33.54
FAX: 02.43.83.35.06
Skype Entreprise visio conférence
Département des Oxydes et Fluorures
Institut des Molécules et des Matériaux du Mans
IMMM - UMR CNRS 6283
Université du Maine - Avenue Olivier Messiaen
F-72085 Le Mans Cedex 9
FRANCE
*
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Re: Hyper-Lorentzian effect on quantitative analysis

2021-03-04 Thread François Goutenoire 

 Dear Rietveld users,

Thank you very much for all your responses, it will help us move forward 
on the subject.

Unfortunately, I cannot say more because of an NDA.
But it still looks very interesting from a fundamental point of view.

Best whishes, françois Goutenoire

Le 03/03/2021 à 18:47, Mendenhall, Marcus H. (Fed) a écrit :

Is it really amorphous content, or is there a whole bunch of very fine 
nanocrystalline stuff or material with a very high defect density that is 
widening the peak?  If the fitter is having trouble matching the peak shape, it 
may be ascribing a fairly arbitrary portion between amorphous and crystalline.

Marcus Mendenhall

Materials Measurement Science Division
National Institute of Science and Technology
100 Bureau Dr. stop 8370 (217/B115)
Gaithersburg, MD 20899 USA
Phone: +1-301-975-8631
during COVID-19 response period:
Home phone: 301-916-5486
Cell: 615-293-3120


On Mar 3, 2021, at 7:34 AM, François Goutenoire 
 wrote:

Dear Rietveld users,

I have some industrial compound presenting a strong hyper-Lorentzian peak shape 
(eta=1.1 with HighScore). When we calculate the amorphous content after an 
internal standard addition, the result is 40%. The micro-absorption effect has 
been minimized (mu of the internal standard is closed to the compound).

But with some electronic transmission analysis no amorphous is observed.

The question is : Does a strong hyper-Lorentzian peak shape could influence 
quantitative analysis ?

François

--
*
Pr. Francois GOUTENOIRE
e-mail: francois.gouteno...@univ-lemans.fr
Tel: 02.43.83.33.54
FAX: 02.43.83.35.06
Skype Entreprise visio conférence
Département des Oxydes et Fluorures
Institut des Molécules et des Matériaux du Mans
IMMM - UMR CNRS 6283
Université du Maine - Avenue Olivier Messiaen
F-72085 Le Mans Cedex 9
FRANCE
*
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Re: Hyper-Lorentzian effect on quantitative analysis

2021-03-03 Thread kleeberg 
Julian has pointed to an important issue, the particle size in the 
mixtures. Even when mue of the standard and sample material are in the 
same magnitude, and even when the particles sizes of both powders 
powders are known and acceptable small with respect to microabsorbtion, 
absorbtion contrast may result by insufficient homogenization. Powdered 
materials having sticky or magnetic properties are hard to mix 
homogeneously by stirring or shaking, so maybe additional milling of the 
mixture is necessary to destroy aggregates. In our practice we add the 
standard (corundum powder 0.4 µm) to the < 0.4 mm precrushed sample 
materials and mill the mixture together with ethanol in the McCrone mill 
with VHD Y stabilized ZrO2 grinding elements. But even by this method 
the sample and standard material may segregate when drying the milled 
slurry, and additional dry homogenization (by hand or in a low energy 
ball mill) is recommended.


Reinhard

Am 03/03/2021 um 17:16 schrieb Julian Richard Tolchard:

Thinking a little outside of the crystallographic aspects, do you have element 
analysis data? Either XRF or ICP-MS would give a good guide to the sample 
composition, and it should match to the composition you are using in the 
structure model.

I find it is worth drying both the sample and spike before weighing them, as 
you can introduce some errors if one component likes to adsorb a lot of water 
from the air. And are you sure your spike is fully crystalline (95% or more), 
is intimately mixed with the sample and doesn't have massively different 
particle size to the sample?


Jools


-Original Message-
From: rietveld_l-requ...@ill.fr  On Behalf Of 
François Goutenoire
Sent: onsdag 3. mars 2021 13.34
To: rietveld_l@ill.fr
Subject: Hyper-Lorentzian effect on quantitative analysis

Dear Rietveld users,

I have some industrial compound presenting a strong hyper-Lorentzian peak shape 
(eta=1.1 with HighScore). When we calculate the amorphous content after an 
internal standard addition, the result is 40%. The micro-absorption effect has 
been minimized (mu of the internal standard is closed to the compound).

But with some electronic transmission analysis no amorphous is observed.

The question is : Does a strong hyper-Lorentzian peak shape could influence 
quantitative analysis ?

François

--
*
Pr. Francois GOUTENOIRE
e-mail: francois.gouteno...@univ-lemans.fr
Tel: 02.43.83.33.54
FAX: 02.43.83.35.06
Skype Entreprise visio conférence
Département des Oxydes et Fluorures
Institut des Molécules et des Matériaux du Mans IMMM - UMR CNRS 6283 Université 
du Maine - Avenue Olivier Messiaen
F-72085 Le Mans Cedex 9
FRANCE
*
Formation Rietveld CNRS 2020
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Re: Hyper-Lorentzian effect on quantitative analysis

2021-03-03 Thread Mendenhall, Marcus H. (Fed) 
Is it really amorphous content, or is there a whole bunch of very fine 
nanocrystalline stuff or material with a very high defect density that is 
widening the peak?  If the fitter is having trouble matching the peak shape, it 
may be ascribing a fairly arbitrary portion between amorphous and crystalline.

Marcus Mendenhall

Materials Measurement Science Division
National Institute of Science and Technology
100 Bureau Dr. stop 8370 (217/B115)
Gaithersburg, MD 20899 USA
Phone: +1-301-975-8631
during COVID-19 response period:
Home phone: 301-916-5486
Cell: 615-293-3120

> On Mar 3, 2021, at 7:34 AM, François Goutenoire 
>  wrote:
> 
> Dear Rietveld users,
> 
> I have some industrial compound presenting a strong hyper-Lorentzian peak 
> shape (eta=1.1 with HighScore). When we calculate the amorphous content after 
> an internal standard addition, the result is 40%. The micro-absorption effect 
> has been minimized (mu of the internal standard is closed to the compound).
> 
> But with some electronic transmission analysis no amorphous is observed.
> 
> The question is : Does a strong hyper-Lorentzian peak shape could influence 
> quantitative analysis ?
> 
> François
> 
> -- 
> *
> Pr. Francois GOUTENOIRE
> e-mail: francois.gouteno...@univ-lemans.fr
> Tel: 02.43.83.33.54
> FAX: 02.43.83.35.06
> Skype Entreprise visio conférence
> Département des Oxydes et Fluorures
> Institut des Molécules et des Matériaux du Mans
> IMMM - UMR CNRS 6283
> Université du Maine - Avenue Olivier Messiaen
> F-72085 Le Mans Cedex 9
> FRANCE
> *
> Formation Rietveld CNRS 2020
> https://gcc02.safelinks.protection.outlook.com/?url=https%3A%2F%2Fcnrsformation.cnrs.fr%2Fdiffraction-des-rayons-x-sur-materiaux-polycristallins%3Faxe%3D135data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543667809%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000sdata=9gZI92veVdDCLrWYKl0yrXubDMwEUmE25mlMINC6DYo%3Dreserved=0
> Formation EDX CNRS 2020
> https://gcc02.safelinks.protection.outlook.com/?url=https%3A%2F%2Fcnrsformation.cnrs.fr%2Ffluorescence-x-edx%3Faxe%3D135data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543672776%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000sdata=x8bUNVf2BOq7ieMi4rxcGiyMaf8urlMcL9mdS96lmQI%3Dreserved=0
> Formation SAXS et Réflectivités pour couches minces et matériaux 
> nanostructurés.
> https://gcc02.safelinks.protection.outlook.com/?url=https%3A%2F%2Fcnrsformation.cnrs.fr%2Fcaracterisation-des-materiaux-nanostructures-par-diffusion-des-rayons-x%3Faxe%3D135data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543672776%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000sdata=poVfPX20d0oyP2hPSijvyNFCrmqKXlQIIX0FPr%2FbnQ0%3Dreserved=0
> Bibliographie
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RE: Hyper-Lorentzian effect on quantitative analysis

2021-03-03 Thread Julian Richard Tolchard 
Thinking a little outside of the crystallographic aspects, do you have element 
analysis data? Either XRF or ICP-MS would give a good guide to the sample 
composition, and it should match to the composition you are using in the 
structure model.

I find it is worth drying both the sample and spike before weighing them, as 
you can introduce some errors if one component likes to adsorb a lot of water 
from the air. And are you sure your spike is fully crystalline (95% or more), 
is intimately mixed with the sample and doesn't have massively different 
particle size to the sample?


Jools


-Original Message-
From: rietveld_l-requ...@ill.fr  On Behalf Of 
François Goutenoire
Sent: onsdag 3. mars 2021 13.34
To: rietveld_l@ill.fr
Subject: Hyper-Lorentzian effect on quantitative analysis

Dear Rietveld users,

I have some industrial compound presenting a strong hyper-Lorentzian peak shape 
(eta=1.1 with HighScore). When we calculate the amorphous content after an 
internal standard addition, the result is 40%. The micro-absorption effect has 
been minimized (mu of the internal standard is closed to the compound).

But with some electronic transmission analysis no amorphous is observed.

The question is : Does a strong hyper-Lorentzian peak shape could influence 
quantitative analysis ?

François

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Re: Hyper-Lorentzian effect on quantitative analysis

2021-03-03 Thread Jeff Nicolich 
It would be useful to have more details. Certain types of materials may be
tricky to refine if your measurement range extends beyond where you can
visibly see distinct peaks. At higher angles you might have a majority of
low intensity overlapping peaks (exacerbated by the addition of an internal
standard). This can lead to high eta values if you are not careful. Proper
fitting of all peak shape parameters requires good data at higher angles.
If this is the case I would try trimming your data range and/or setting
some of your peak parameters to "reasonable" values (what is "reasonable"
???). Maybe only refine u and keep v and w at zero (if you are using that
kind of profile function).
Conversely, the choice of internal standard is important too. Is the lowest
angle peak of the standard underfitted while higher angle peaks are
overfitted? This would point to a problem with either the measurement setup
or the standard material.

Some simple ideas to verify the results: Try the spiking method (vary the
proportion of standard and sample and see if results are the same) or the
external standard method (if you know the composition of both sample and
standard).

Jeff Nicolich


On Wed, Mar 3, 2021 at 12:36 PM François Goutenoire <
francois.gouteno...@univ-lemans.fr> wrote:

> Dear Rietveld users,
>
> I have some industrial compound presenting a strong hyper-Lorentzian peak
> shape (eta=1.1 with HighScore). When we calculate the amorphous content
> after an internal standard addition, the result is 40%. The
> micro-absorption effect has been minimized (mu of the internal standard is
> closed to the compound).
>
> But with some electronic transmission analysis no amorphous is observed.
>
> The question is : Does a strong hyper-Lorentzian peak shape could
> influence quantitative analysis ?
>
> François
>
> --
>
> *
> Pr. Francois GOUTENOIRE
> e-mail: francois.gouteno...@univ-lemans.fr
> Tel: 02.43.83.33.54
> FAX: 02.43.83.35.06
> Skype Entreprise visio conférence
> Département des Oxydes et Fluorures
> Institut des Molécules et des Matériaux du Mans
> IMMM - UMR CNRS 6283
> Université du Maine - Avenue Olivier Messiaen
> F-72085 Le Mans Cedex 9
> FRANCE
>
> *
> Formation Rietveld CNRS 2020
>
> https://cnrsformation.cnrs.fr/diffraction-des-rayons-x-sur-materiaux-polycristallins?axe=135
> Formation EDX CNRS 2020
> https://cnrsformation.cnrs.fr/fluorescence-x-edx?axe=135
> Formation SAXS et Réflectivités pour couches minces et matériaux
> nanostructurés.
>
> https://cnrsformation.cnrs.fr/caracterisation-des-materiaux-nanostructures-par-diffusion-des-rayons-x?axe=135
> Bibliographie
>
> https://scholar.google.fr/citations?hl=fr=qC-lmN4J_op=list_works=1=title
> https://orcid.org/-0001-5339-3002
>
> ++
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> text
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>
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Re: Hyper-Lorentzian effect on quantitative analysis

2021-03-03 Thread Bish, David L 
Dear François,

I can think of no reason for a correlation between your peak shape and your 
resultant amorphous content, unless somehow the super-Lorentzian peak shape is 
not providing accurate intensities. Have you tried your fit with another peak 
shape or a fundamental parameters approach? I assume that you used an 
"infinitely thick" specimen and modeled the internal standard well.

I agree with Reinhard, generally 40% amorphous will be visible, although if you 
are unfamiliar with the scattering from partially to completely disordered or 
amorphous materials, it could be possible to miss this much. I will send you 
separately a reprint with some example patterns with increasing amounts of 
added amorphous material, wherein you will see that even 50% amorphous is not 
"extremely" obvious.

Best of luck,

David

On 3/3/2021 7:34 AM, François Goutenoire wrote:
This message was sent from a non-IU address. Please exercise caution when 
clicking links or opening attachments from external sources.
---

Dear Rietveld users,

I have some industrial compound presenting a strong hyper-Lorentzian peak shape 
(eta=1.1 with HighScore). When we calculate the amorphous content after an 
internal standard addition, the result is 40%. The micro-absorption effect has 
been minimized (mu of the internal standard is closed to the compound).

But with some electronic transmission analysis no amorphous is observed.

The question is : Does a strong hyper-Lorentzian peak shape could influence 
quantitative analysis ?

François




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Re: Hyper-Lorentzian effect on quantitative analysis

2021-03-03 Thread Reinhard Neder 

Dear François,

I've to admit that I am no expert on the quantitative phase analysis. If 
the analysis suggest 40% amorphous compound, I'd expect that should be 
clearly visible in the diffraction pattern as a fairly strong, broad 
maximum with a FWHM of some 7 to 10° (CuKalpha). If you do not see that, 
then the quantitative analysis is certainly misleading.


Best

Reinhard Neder

Am 03.03.21 um 13:34 schrieb François Goutenoire:


Dear Rietveld users,

I have some industrial compound presenting a strong hyper-Lorentzian 
peak shape (eta=1.1 with HighScore). When we calculate the amorphous 
content after an internal standard addition, the result is 40%. The 
micro-absorption effect has been minimized (mu of the internal 
standard is closed to the compound).


But with some electronic transmission analysis no amorphous is observed.

The question is : Does a strong hyper-Lorentzian peak shape could 
influence quantitative analysis ?


François


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Kristallographie und Strukturphysik
Universität Erlangen
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tel. +49-9131-8525191
fax  +49-9131-8525182

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