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 <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
https://eur03.safelinks.protection.outlook.com/?url=https%3A%2F%2Fcnrsformation.cnrs.fr%2Fdiffraction-des-rayons-x-sur-materiaux-polycristallins%3Faxe%3D135&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7C0d9a81efc5fb4c83e5b808d8de40fb8e%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C1%7C637503717984009944%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=A583rGrlzvqcO4eaEFccihRE1u1rUYmhqUO12DKRv28%3D&reserved=0
Formation EDX CNRS 2020
https://eur03.safelinks.protection.outlook.com/?url=https%3A%2F%2Fcnrsformation.cnrs.fr%2Ffluorescence-x-edx%3Faxe%3D135&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7C0d9a81efc5fb4c83e5b808d8de40fb8e%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C1%7C637503717984019908%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=JzG1Vfz1vqnmeFy2b2uwI%2BDW9qFwy78H7vSTkHSXaYA%3D&reserved=0
Formation SAXS et Réflectivités pour couches minces et matériaux nanostructurés.
https://eur03.safelinks.protection.outlook.com/?url=https%3A%2F%2Fcnrsformation.cnrs.fr%2Fcaracterisation-des-materiaux-nanostructures-par-diffusion-des-rayons-x%3Faxe%3D135&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7C0d9a81efc5fb4c83e5b808d8de40fb8e%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C1%7C637503717984019908%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=SR75omVvQuf%2BGEHPKqiRhturUjHHKPZ7jjwpO%2F1%2FRFc%3D&reserved=0
Bibliographie
https://eur03.safelinks.protection.outlook.com/?url=https%3A%2F%2Fscholar.google.fr%2Fcitations%3Fhl%3Dfr%26user%3DqC-lmN4AAAAJ%26view_op%3Dlist_works%26authuser%3D1%26sortby%3Dtitle&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7C0d9a81efc5fb4c83e5b808d8de40fb8e%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C1%7C637503717984019908%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=FUvhYq9in61L2d1leC91oIo8UwxlaGfN78my%2F6VvHFc%3D&reserved=0
https://eur03.safelinks.protection.outlook.com/?url=https%3A%2F%2Forcid.org%2F0000-0001-5339-3002&data=04%7C01%7Cjulianrichard.tolchard%40sintef.no%7C0d9a81efc5fb4c83e5b808d8de40fb8e%7Ce1f00f39604145b0b309e0210d8b32af%7C1%7C1%7C637503717984019908%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=9%2BqjLOomkLsLIJHYxFfW1GQ0ZKuJO9x4lO1N58RSSxk%3D&reserved=0
++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
Please do NOT attach files to the whole list <alan.he...@neutronoptics.com>
Send commands to <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/
++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
--
Dr. Reinhard Kleeberg
TU Bergakademie Freiberg
Institut für Mineralogie
Brennhausgasse 14
D-09596 Freiberg
Tel.: +49(0)3731 393244
Fax: +49(0)3731 393129
++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
Please do NOT attach files to the whole list <alan.he...@neutronoptics.com>
Send commands to <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/
++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
