Re: Hyper-Lorentzian effect on quantitative analysis
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 * 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%3D135&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543667809%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=9gZI92veVdDCLrWYKl0yrXubDMwEUmE25mlMINC6DYo%3D&reserved=0 | https://gcc02.safelinks.protection.outlook.com/?url=https%3A%2F%2Fcnrsformation.cnrs.fr%2Fdiffraction-des-rayons-x-sur-materiaux-polycristallins%3Faxe%3D135&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543667809%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=9gZI92veVdDCLrWYKl0yrXubDMwEUmE25mlMINC6DYo%3D&reserved=0 ] Formation EDX CNRS 2020 [ https://gcc02.safelinks.protection.outlook.com/?url=https%3A%2F%2Fcnrsformation.cnrs.fr%2Ffluorescence-x-edx%3Faxe%3D135&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543672776%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=x8bUNVf2BOq7ieMi4rxcGiyMaf8urlMcL9mdS96lmQI%3D&reserved=0 | https://gcc02.safelinks.protection.outlook.com/?url=https%3A%2F%2Fcnrsformation.cnrs.fr%2Ffluorescence-x-edx%3Faxe%3D135&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543672776%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=x8bUNVf2BOq7ieMi4rxcGiyMaf8urlMcL9mdS96lmQI%3D&reserved=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%3D135&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543672776%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn
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 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%3D135&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543667809%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=9gZI92veVdDCLrWYKl0yrXubDMwEUmE25mlMINC6DYo%3D&reserved=0 Formation EDX CNRS 2020 https://gcc02.safelinks.protection.outlook.com/?url=https%3A%2F%2Fcnrsformation.cnrs.fr%2Ffluorescence-x-edx%3Faxe%3D135&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543672776%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=x8bUNVf2BOq7ieMi4rxcGiyMaf8urlMcL9mdS96lmQI%3D&reserved=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%3D135&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543672776%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=poVfPX20d0oyP2hPSijvyNFCrmqKXlQIIX0FPr%2FbnQ0%3D&reserved=0 Bibliographie https://gcc02.safelinks.protection.outlook.com/?url=https%3A%2F%2Fscholar.google.fr%2Fcitations%3Fhl%3Dfr%26user%3DqC-lmN4J%26view_op%3Dlist_works%26authuser%3D1%26sortby%3Dtitle&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543672776%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=RtgAB7fNy3VIqLDR1hoNyexqtir8Z1mHXSbG2Q%2B0a%2BQ%3D&reserved=0 https://gcc02.safelinks.protection.outlook.com/?url=https%3A%2F%2Forcid.org%2F-0001-5339-3002&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543672776%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=5PnfX1KDGdijLrs4taQu%2Bi0lfu87dfh4%2BhGvChowCmE%3D&reserved=0 ++ 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
Re: Hyper-Lorentzian effect on quantitative analysis
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 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-lmN4J%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=ht
Re: Hyper-Lorentzian effect on quantitative analysis
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%3D135&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543667809%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=9gZI92veVdDCLrWYKl0yrXubDMwEUmE25mlMINC6DYo%3D&reserved=0 > Formation EDX CNRS 2020 > https://gcc02.safelinks.protection.outlook.com/?url=https%3A%2F%2Fcnrsformation.cnrs.fr%2Ffluorescence-x-edx%3Faxe%3D135&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543672776%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=x8bUNVf2BOq7ieMi4rxcGiyMaf8urlMcL9mdS96lmQI%3D&reserved=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%3D135&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543672776%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=poVfPX20d0oyP2hPSijvyNFCrmqKXlQIIX0FPr%2FbnQ0%3D&reserved=0 > Bibliographie > https://gcc02.safelinks.protection.outlook.com/?url=https%3A%2F%2Fscholar.google.fr%2Fcitations%3Fhl%3Dfr%26user%3DqC-lmN4J%26view_op%3Dlist_works%26authuser%3D1%26sortby%3Dtitle&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543672776%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=RtgAB7fNy3VIqLDR1hoNyexqtir8Z1mHXSbG2Q%2B0a%2BQ%3D&reserved=0 > https://gcc02.safelinks.protection.outlook.com/?url=https%3A%2F%2Forcid.org%2F-0001-5339-3002&data=04%7C01%7Cmarcus.mendenhall%40nist.gov%7C6e1cde8aec7f4b0a22f908d8de40e15f%7C2ab5d82fd8fa4797a93e054655c61dec%7C1%7C0%7C637503717543672776%7CUnknown%7CTWFpbGZsb3d8eyJWIjoiMC4wLjAwMDAiLCJQIjoiV2luMzIiLCJBTiI6Ik1haWwiLCJXVCI6Mn0%3D%7C3000&sdata=5PnfX1KDGdijLrs4taQu%2Bi0lfu87dfh4%2BhGvChowCmE%3D&reserved=0 > > ++ > 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: Hyper-Lorentzian effect on quantitative analysis
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 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-lmN4J%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%2F-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 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/ ++
AW: Hyper-Lorentzian effect on quantitative analysis
> But with some electronic transmission analysis no amorphous is observed. Could the TEM investigation have led to recrystallisation? Have you tried polarised-light microscopy to check the character of the amorphous phase? Cheers, Uwe -Ursprüngliche Nachricht- Von: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] Im Auftrag von Wörle Michael Gesendet: Mittwoch, 03. März 2021 15:32 An: rietveld_l@ill.fr Betreff: AW: Hyper-Lorentzian effect on quantitative analysis Dear François, Maybe you have a strongly disordered system. Depending on the type of disorder and the distribution of diffuse intensity, it can also have an influence on the reflection profile (thermal diffuse scattering). Michael Dr. Michael Wörle Head Small Molecule Crystallography Center Laboratorium für Anorganische Chemie ETH Zürich HCI H103 Vladimir-Prelog-Weg 1 CH-8093 Zürich Tel.: +41 44 632 5684 FAX: +41 44 632 1149 email: woe...@inorg.chem.ethz.ch http://www.smocc.ethz.ch --- The Zurich School of Crystallography, University of Zurich, June 6-17, 2021 http://www.chem.uzh.ch/linden/zsc --- -Ursprüngliche Nachricht- Von: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] Im Auftrag von François Goutenoire Gesendet: Wednesday, 3 March 2021 13:34 An: rietveld_l@ill.fr Betreff: 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://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&user=qC-lmN4J&view_op=list_works&authuser=1&sortby=title https://orcid.org/-0001-5339-3002 ++ 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/ ++
AW: Hyper-Lorentzian effect on quantitative analysis
Dear François, Maybe you have a strongly disordered system. Depending on the type of disorder and the distribution of diffuse intensity, it can also have an influence on the reflection profile (thermal diffuse scattering). Michael Dr. Michael Wörle Head Small Molecule Crystallography Center Laboratorium für Anorganische Chemie ETH Zürich HCI H103 Vladimir-Prelog-Weg 1 CH-8093 Zürich Tel.: +41 44 632 5684 FAX: +41 44 632 1149 email: woe...@inorg.chem.ethz.ch http://www.smocc.ethz.ch --- The Zurich School of Crystallography, University of Zurich, June 6-17, 2021 http://www.chem.uzh.ch/linden/zsc --- -Ursprüngliche Nachricht- Von: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] Im Auftrag von François Goutenoire Gesendet: Wednesday, 3 March 2021 13:34 An: rietveld_l@ill.fr Betreff: 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://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&user=qC-lmN4J&view_op=list_works&authuser=1&sortby=title https://orcid.org/-0001-5339-3002 ++ 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: Hyper-Lorentzian effect on quantitative analysis
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&user=qC-lmN4J&view_op=list_works&authuser=1&sortby=title > https://orcid.org/-0001-5339-3002 > > ++ > 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: Hyper-Lorentzian effect on quantitative analysis
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 ++ 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/ ++ -- David L. Bish Indiana University Molecular Structure Center Chemistry Building, A421 800 E. Kirkwood Ave. Bloomington IN 47405-7102 812-855-2039 ++ 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: Hyper-Lorentzian effect on quantitative analysis
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 ++ 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/ ++ -- Prof. Dr. Reinhard Neder Kristallographie und Strukturphysik Universität Erlangen Staudtststr. 3; 91058 Erlangen tel. +49-9131-8525191 fax +49-9131-8525182 ++ 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/ ++
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://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&user=qC-lmN4J&view_op=list_works&authuser=1&sortby=title https://orcid.org/-0001-5339-3002 ++ 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: Alumina standard for quantitative analysis
Dear Davide, We often purchase 1 micrometer alumina from the following: Metallurgical Supply Company 713-827-0700 sa...@metsuco.com Item # ME-300-C 1.0um Al2O3 powder ~$240/5 pounds www.metsuco.com It is sufficient for routine internal-standard quantitative analyses (and it is quite inexpensive), but you can evaluate it yourself. Regards, David On 1/23/2018 1:05 AM, Davide Levy wrote: Hi I would like to buy alumina standard to use for XRD quantitative analysis. I looked in NIST website and it finished. Sigma-aldrich sells it but is too expensive. do you know other suppliers? Or other quantitative analysis standards? Thanks *Dr. Davide Levy, Ph.D.* * Director of XRD laboratory Wolfson Applied Materials Research Centre* *Tel Aviv University,* *Ramat Aviv, Tel Aviv 69978, Israel* *Phone: +972-3-6407815 * *Fax: +972-3-6407819 * *http://www3.tau.ac.il/wamrc/ * ++ 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/ ++ -- David L. Bish Department of Earth & Atmospheric Sciences Indiana University 1001 E. 10th St. Bloomington, IN 47405 812-855-2039 ++ 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: Alumina standard for quantitative analysis
Davide Hi, Welcome and nice to meet you. I can borrow you some Lab6 NIST 660c standard reference. Best regards, Gili [cid:image003.png@01C98092.6937E0A0] --- Dr. Gili Cohen Taguri Head of XRD Lab Bar Ilan Institute of Nanotechnology and Advanced Materials Bar Ilan University Ramat Gan 52900 Israel lab: +972-3-7384291 cell: +972-54-3322142 www.nano.biu.ac.il<http://www.nano.biu.ac.il/> [Looking for]<http://nano.biu.ac.il/equipment-facilities> From: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] On Behalf Of Davide Levy Sent: Tuesday, January 23, 2018 8:06 AM To: 'RIETVELD_L Distribution List' Subject: Alumina standard for quantitative analysis Hi I would like to buy alumina standard to use for XRD quantitative analysis. I looked in NIST website and it finished. Sigma-aldrich sells it but is too expensive. do you know other suppliers? Or other quantitative analysis standards? Thanks Dr. Davide Levy, Ph.D. Director of XRD laboratory Wolfson Applied Materials Research Centre Tel Aviv University, Ramat Aviv, Tel Aviv 69978, Israel Phone: +972-3-6407815 Fax: +972-3-6407819 http://www3.tau.ac.il/wamrc/ ++ 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/ ++
R: Alumina standard for quantitative analysis
Another option could be to prepare the standard in-house. This paper: J. Appl. Cryst. (2014). 47, 136–145 describes an annealing procedure to produce Al2O3 with a very low amorphous content (even lower than the NIST standard). Marco Da: rietveld_l-requ...@ill.fr per conto di Fabrizio Guzzetta Inviato: martedì 23 gennaio 2018 13:25 A: Davide Levy; rietveld_l@ill.fr Oggetto: Re: Alumina standard for quantitative analysis davide, you can look the same dealers for neutron diffraction as well, or maybe some colleague can borrow some. (First guess) The other thing, if you are trying to reproduce data is to ask the people who performed it (and published in journal) to send you some quantity (second guess). Ask NIST if they can direct you to some other dealer (Third guess). I would ask X - Ray diffraction instrument builders as they normally have it to calibrate their instruments. (Fourth guess). I hope some of these can be of help El 23/01/2018 07:07, "Davide Levy" mailto:davide.lev...@gmail.com>> escribió: Hi I would like to buy alumina standard to use for XRD quantitative analysis. I looked in NIST website and it finished. Sigma-aldrich sells it but is too expensive. do you know other suppliers? Or other quantitative analysis standards? Thanks Dr. Davide Levy, Ph.D. Director of XRD laboratory Wolfson Applied Materials Research Centre Tel Aviv University, Ramat Aviv, Tel Aviv 69978, Israel Phone: +972-3-6407815 Fax: +972-3-6407819 http://www3.tau.ac.il/wamrc/<https://nam03.safelinks.protection.outlook.com/?url=http%3A%2F%2Fwww3.tau.ac.il%2Fwamrc%2F&data=02%7C01%7C%7Cd70ad30d6d76437d2f4508d5625ca2fc%7C84df9e7fe9f640afb435%7C1%7C0%7C636523072368704117&sdata=6muD8adJgUeRj0vjYYNsRos0q7q9N9wWJ76nN6hz3p0%3D&reserved=0> ++ 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/<https://nam03.safelinks.protection.outlook.com/?url=http%3A%2F%2Fwww.mail-archive.com%2Frietveld_l%40ill.fr%2F&data=02%7C01%7C%7Cd70ad30d6d76437d2f4508d5625ca2fc%7C84df9e7fe9f640afb435%7C1%7C0%7C636523072368704117&sdata=FJ22qaHil9iXqM1dJoWRR%2BH6ugB%2BqCaiMjtkI%2FCEZUU%3D&reserved=0> ++ ++ 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: Alumina standard for quantitative analysis
davide, you can look the same dealers for neutron diffraction as well, or maybe some colleague can borrow some. (First guess) The other thing, if you are trying to reproduce data is to ask the people who performed it (and published in journal) to send you some quantity (second guess). Ask NIST if they can direct you to some other dealer (Third guess). I would ask X - Ray diffraction instrument builders as they normally have it to calibrate their instruments. (Fourth guess). I hope some of these can be of help El 23/01/2018 07:07, "Davide Levy" escribió: > Hi > > I would like to buy alumina standard to use for XRD quantitative analysis. > I looked in NIST website and it finished. Sigma-aldrich sells it but is > too expensive. > do you know other suppliers? Or other quantitative analysis standards? > > Thanks > > > > > > *Dr. Davide Levy, Ph.D.* > > > > *Director of XRD laboratoryWolfson Applied Materials Research Centre* > *Tel Aviv University,* > *Ramat Aviv, Tel Aviv 69978, Israel* > > *Phone: +972-3-6407815 <+972%203-640-7815>* > *Fax: +972-3-6407819 <+972%203-640-7819>* > *http://www3.tau.ac.il/wamrc/ <http://www3.tau.ac.il/wamrc/> * > > > > > > ++ > 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/ ++
Alumina standard for quantitative analysis
Hi I would like to buy alumina standard to use for XRD quantitative analysis. I looked in NIST website and it finished. Sigma-aldrich sells it but is too expensive. do you know other suppliers? Or other quantitative analysis standards? Thanks Dr. Davide Levy, Ph.D. Director of XRD laboratory Wolfson Applied Materials Research Centre Tel Aviv University, Ramat Aviv, Tel Aviv 69978, Israel Phone: +972-3-6407815 Fax: +972-3-6407819 http://www3.tau.ac.il/wamrc/ ++ 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: quantitative analysis - perovskites - preferred orientation
Dear Lukasz, First of all, in the majority of Rietveld programs the uniaxial preferred orientation (such as [100]) can not be handled adequately for cubic systems since the programs normally generate only one symmetrically equivalent hkl for a diffraction peak. In DDM, for such cases, I included a special option (Expanded hkl) to generate all equivalent hkl's for every peak. This option makes the refinement process slower and also may require some manual settings for initial parameter values. Another alternative for cubic systems is spherical harmonics. As for the estimated error of the refined PO component, it's really wise to check if it exceeds the refined value, but it should be done at the final stage only, as at initial stages all errors may be high due to the incompleteness of refinement. Best regards, Leonid *** Leonid A. Solovyov Institute of Chemistry and Chemical Technology 660036, Akademgorodok 50/24, Krasnoyarsk, Russia http://sites.google.com/site/solovyovleonid *** On Thursday, February 6, 2014 5:37 PM, Łukasz Kruszewski wrote: Dear Madam/Sir(s), I am performing Rietveld analysis for a sample containing perovskites (CaTiO3 and SrTiO3). When putting-in a preferred orientation (PO) correction (100 direction, as the crystals are cubic-like), I obtain better Rwp and GOF i.e. chi-squared values (9.63 and 1.5, respectively) than in the case of not using this correction (Rwp = 10.62 and GOF = 1.65). However, the values of the PO corrections are higher than the errors calculated. All the other parameters including the graphical fit, background etc., seem to be unchanged. I am also convinced about the correctness of any input, with my diffractometer calibrated with LaB6 and Si standards, and Beq / Uiso parameters taken directly from the CIF files provided, so that the microabsorption factor may likely be rejected (?). My guess is that putting in the preferred orientation might artificially, somehow, make the fit better, maybe due to some interdependence? Could you please kindly suggests if obtaining better statistics (Rwp, GOF) by getting a correction values below the corresponding errors could be treated as a good result? Best regards! -- Łukasz Kruszewski, Ph.D., adjunct Polish Academy of Sciences Institute of Geological Sciences X-Ray Diffraction Laboratory (coordinator) Twarda 51/55 str. 00-818 Warsaw Poland ++ 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/ ++
quantitative analysis - perovskites - preferred orientation
Dear Madam/Sir(s), I am performing Rietveld analysis for a sample containing perovskites (CaTiO3 and SrTiO3). When putting-in a preferred orientation (PO) correction (100 direction, as the crystals are cubic-like), I obtain better Rwp and GOF i.e. chi-squared values (9.63 and 1.5, respectively) than in the case of not using this correction (Rwp = 10.62 and GOF = 1.65). However, the values of the PO corrections are higher than the errors calculated. All the other parameters including the graphical fit, background etc., seem to be unchanged. I am also convinced about the correctness of any input, with my diffractometer calibrated with LaB6 and Si standards, and Beq / Uiso parameters taken directly from the CIF files provided, so that the microabsorption factor may likely be rejected (?). My guess is that putting in the preferred orientation might artificially, somehow, make the fit better, maybe due to some interdependence? Could you please kindly suggests if obtaining better statistics (Rwp, GOF) by getting a correction values below the corresponding errors could be treated as a good result? Best regards! -- Łukasz Kruszewski, Ph.D., adjunct Polish Academy of Sciences Institute of Geological Sciences X-Ray Diffraction Laboratory (coordinator) Twarda 51/55 str. 00-818 Warsaw Poland ++ 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: Quantitative analysis
hi all, not only fibre like, but single component fibre, and with the fibre axis parrallel to the sample normal (i.e. "cyclic fibre". this is very restrictive and generally does not correspond to the real texture. Contrarilly to what has been said here or there, the March-Dollase does not ensure PO normalisation, but only the normalisation of this single component, there is then no physical restriction between all hkl lines in terms of crystal angles, which gives rise to a lot of fitting space with unreasonable solutions either in terms of QTA or QPA. A physically based correction for PO needs the calculation of the ODF, and more than a single pattern to be measured. But this is the price to pay for a corect estimate of phase amounts in textured samples. daniel -- Daniel Chateigner Professeur CRISMAT-ENSICAEN Bd. M. Juin 14050 Caen, France http://www.ecole.ensicaen.fr/~chateign/danielc/
Re: Quantitative analysis
[EMAIL PROTECTED] a écrit : Hi Blaise In Bragg-Brentano mode, sample spinning does nothin for PO. This is because the diffraction vector is normal to the sample surface, and sample spinning rotates along this vector. That's wrong! As I have already written, the empirical PO corrections like March-Dollase and Rietveld-Toraya suppose that the PO is fibre-like (axial symmetry). If your sample does not have fibre-like PO, you can create it by sample spinning. Radovan Spinning does increase your particle statistics, which almost always helps. If you're looking at a capillary, spinning the capillary does help with PO, but just being in a capillary helps PO. As to spinning speeds, a good guide is one revolution per data point. Cheers Matthew Matthew Rowles CSIRO Minerals Box 312 Clayton South, Victoria AUSTRALIA 3169 Ph: +61 3 9545 8892 Fax: +61 3 9562 8919 (site) Email: [EMAIL PROTECTED] -- Radovan Cerny Laboratoire de Cristallographie 24, quai Ernest-Ansermet CH-1211 Geneva 4, Switzerland Phone : [+[41] 22] 37 964 50, FAX : [+[41] 22] 37 961 08 mailto : [EMAIL PROTECTED] URL: http://www.unige.ch/sciences/crystal/cerny/rcerny.htm
RE: Quantitative analysis
Hi Blaise In Bragg-Brentano mode, sample spinning does nothin for PO. This is because the diffraction vector is normal to the sample surface, and sample spinning rotates along this vector. Spinning does increase your particle statistics, which almost always helps. If you're looking at a capillary, spinning the capillary does help with PO, but just being in a capillary helps PO. As to spinning speeds, a good guide is one revolution per data point. Cheers Matthew Matthew Rowles CSIRO Minerals Box 312 Clayton South, Victoria AUSTRALIA 3169 Ph: +61 3 9545 8892 Fax: +61 3 9562 8919 (site) Email: [EMAIL PROTECTED] From: Mibeck, Blaise [mailto:[EMAIL PROTECTED] Sent: Wednesday, 29 October 2008 01:25 To: rietveld_l@ill.fr Subject: RE: Quantitative analysis I am learning QPA and am worried about PO. I wonder why sample spinning isn't discussed more. I am luckily able to barrow time on a newer diffractometer with a sample spinner. Does this reduce PO? Or completely eliminate it? There is a set up variable in GSAS for whether you are spinning the sample - are there guidelines for how many revolutions to spin the sample if you just want to reduce PO? Thanks to all for there help!!! Blaise * * * * * * * * * * * * * Blaise Mibeck Research Scientist Energy & Environmental Research Center University of North Dakota 15 North 23rd Street, Stop 9018 Grand Forks, ND 58202-9018 Phone: (701) 777-5077 Email: [EMAIL PROTECTED]<mailto:[EMAIL PROTECTED]> -Original Message- From: David L. Bish [mailto:[EMAIL PROTECTED] Sent: Tuesday, October 28, 2008 9:09 AM To: Martin; [EMAIL PROTECTED]; rietveld_l@ill.fr Subject: RE: Quantitative analysis I agree that it's always best to avoid preferred orientation, but that is easier said than done on a routine basis. I have personally had good luck with the M-D PO correction on many known samples, as long as the PO was not severe. However, I imagine that Mario's problems are related to microabsorption in this case. Mario, if you can re-measure your data with a Co or Fe tube, it would be a good test of this. Dave Bish At 08:51 AM 10/28/2008 -0400, Martin wrote: Sorry to disagree. Experience tells me otherwise - the March-Dollase correction has nearly always led to poor quant results for me. It most certainly cannot be applied safely. Martin -- M Vickers Dept of Chemistry UCL ____ > Subject: Re: Quantitative analysis > Date: Tue, 28 Oct 2008 02:53:20 -0700 > From: [EMAIL PROTECTED] > To: Rietveld_l@ill.fr > > Dear Mario, > > One more possible problem of applying preferred orientation corrections in > QPA is that not all of them are normalized. For example, the March-Dollase > correction is normalized and can be applied safely, but the Rietveld-Toraya > correction is inapplicable to QPA as it does not preserve the scale > normalization. > > Best regards, > Leonid > > *** > Leonid A. Solovyov > Institute of Chemistry and Chemical Technology > K. Marx av., 42 > 660049, Krasnoyarsk Russia > Phone: +7 3912 495663 > Fax: +7 3912 238658 > www.icct.ru/eng/content/persons/Sol_LA<http://www.icct.ru/eng/content/persons/Sol_LA> > For the best free wallpapers from MSN Click here!<http://wallpapers.msn.com/?ocid>
RE: Quantitative analysis
Spinning the sample doesn't reduce preferred orientation much. It does, however, improve ones counting statistics very nicely. Martin M Vickers Dept. of Chemistry UCL 20, Gordon Street London WC1E 0HX Subject: RE: Quantitative analysisDate: Tue, 28 Oct 2008 09:25:13 -0500From: [EMAIL PROTECTED]: rietveld_l@ill.fr I am learning QPA and am worried about PO. I wonder why sample spinning isn’t discussed more. I am luckily able to barrow time on a newer diffractometer with a sample spinner. Does this reduce PO? Or completely eliminate it? There is a set up variable in GSAS for whether you are spinning the sample – are there guidelines for how many revolutions to spin the sample if you just want to reduce PO? Thanks to all for there help!!! Blaise * * * * * * * * * * * * * Blaise Mibeck Research Scientist Energy & Environmental Research Center University of North Dakota 15 North 23rd Street, Stop 9018 Grand Forks, ND 58202-9018 Phone: (701) 777-5077 Email: [EMAIL PROTECTED] _ Discover Bird's Eye View now with Multimap from Live Search http://clk.atdmt.com/UKM/go/111354026/direct/01/
RE: Quantitative analysis
Thank you to all for your generous help... has been very important your information.. Mario. Mario, > > From the information that you just gave, it appears that the corundum 012 > and siderite 012 are not well resolved causing more of the siderite 012 > intensity to be attributed to the corundum 012 and an overestimation of > corundum. If it is a microabsorption problem, you wouldn't get a good QPA > data without PO correction to start with. If you can, reduce the receiving > slit size and run the sample again or don't correct for PO. > > Dipo Omotoso > > -Original Message- > From: [EMAIL PROTECTED] [mailto:[EMAIL PROTECTED] > Sent: October 28, 2008 8:24 AM > To: Rietveld_l@ill.fr > Subject: RE: Quantitative analysis > >>Dear all, > > the well-known data are: CaCO3 (20%), CaF2 (35%), SiO2 (1%), Al2O3 (20%), > and FeCO3 (24%). The data obtained without PO are: CaCO3 (24%), CaF2 > (36%), SiO2 (1%), Al2O3 (17%), and FeCO3 (23%). The data obtained with PO > are: CaCO3 (19%), CaF2 (32%), SiO2 (2%), Al2O3 (31%), and FeCO3 (16%). > it seems to have a problem among Al2O3 and FeCO3 data after PO. > > Mario. > > > Dear all, >> >> The data collection conditions is: hand grind (35 microns), scan: >> 2Theta/Theta Coupled, to steps 2 sec., target Cu, graphite >> monochromator, side loading. The correction of preferential >> orientation has been refined by March-Dollase model. >> >> Thanks a lot, >> >> Mario. >> >> >> >> >> Dear Mario, >>> >>> Please tell me a little about the data collection conditions you used >>> for this work:- >>> >>> How was the sample prepared (hand ground, micronised in McCrone mill >>> ) >>> What was the tube target Cu, Co, other ?? >>> >>> Cheers >>> Ian Madsen >>> >>> From: [EMAIL PROTECTED] [EMAIL PROTECTED] >>> Sent: Tuesday, October 28, 2008 2:48 AM >>> To: Rietveld_l@ill.fr >>> Subject: Quantitative analysis >>> >>> Dear all, >>> >>> I have this question, >>> >>> I have been refined one mixture (of well-know percentage composition) >>> of CaCO3, CaF2, SiO2 and Al2O3, with preferential orientation in >>> CaCO3 >>> (104) >>> and CaF2 (111) with good results. When I add to the mixture FeCO3 and >>> I refine with preferential orientation (104), it happens that when I >>> don´t apply the preferential orientation in all this phases, I have >>> correct values of percentage composition, but when I apply the >>> preferential orientation the refinement is good but with incorrect >>> values of percentage composition. This experiment has been taken in >>> Bragg Brentano geometry. >>> How I should refine this mixture? >>> >>> Thanks a lot by your help. >>> >>> Mario Macías >>> Universidad Industrial de Santander >>> Colombia >>> >>> >> >> >> >> > > > > >
RE: Quantitative analysis
Mario, >From the information that you just gave, it appears that the corundum 012 and >siderite 012 are not well resolved causing more of the siderite 012 intensity >to be attributed to the corundum 012 and an overestimation of corundum. If it >is a microabsorption problem, you wouldn't get a good QPA data without PO >correction to start with. If you can, reduce the receiving slit size and run >the sample again or don't correct for PO. Dipo Omotoso -Original Message- From: [EMAIL PROTECTED] [mailto:[EMAIL PROTECTED] Sent: October 28, 2008 8:24 AM To: Rietveld_l@ill.fr Subject: RE: Quantitative analysis >Dear all, the well-known data are: CaCO3 (20%), CaF2 (35%), SiO2 (1%), Al2O3 (20%), and FeCO3 (24%). The data obtained without PO are: CaCO3 (24%), CaF2 (36%), SiO2 (1%), Al2O3 (17%), and FeCO3 (23%). The data obtained with PO are: CaCO3 (19%), CaF2 (32%), SiO2 (2%), Al2O3 (31%), and FeCO3 (16%). it seems to have a problem among Al2O3 and FeCO3 data after PO. Mario. Dear all, > > The data collection conditions is: hand grind (35 microns), scan: > 2Theta/Theta Coupled, to steps 2 sec., target Cu, graphite > monochromator, side loading. The correction of preferential > orientation has been refined by March-Dollase model. > > Thanks a lot, > > Mario. > > > > > Dear Mario, >> >> Please tell me a little about the data collection conditions you used >> for this work:- >> >> How was the sample prepared (hand ground, micronised in McCrone mill >> ) >> What was the tube target Cu, Co, other ?? >> >> Cheers >> Ian Madsen >> ____ >> From: [EMAIL PROTECTED] [EMAIL PROTECTED] >> Sent: Tuesday, October 28, 2008 2:48 AM >> To: Rietveld_l@ill.fr >> Subject: Quantitative analysis >> >> Dear all, >> >> I have this question, >> >> I have been refined one mixture (of well-know percentage composition) >> of CaCO3, CaF2, SiO2 and Al2O3, with preferential orientation in >> CaCO3 >> (104) >> and CaF2 (111) with good results. When I add to the mixture FeCO3 and >> I refine with preferential orientation (104), it happens that when I >> don´t apply the preferential orientation in all this phases, I have >> correct values of percentage composition, but when I apply the >> preferential orientation the refinement is good but with incorrect >> values of percentage composition. This experiment has been taken in >> Bragg Brentano geometry. >> How I should refine this mixture? >> >> Thanks a lot by your help. >> >> Mario Macías >> Universidad Industrial de Santander >> Colombia >> >> > > > >
Re: Quantitative analysis
The empirical PO corrections like March-Dollase or Rietveld-Toraya can correct only for fibre like PO, i.e. symmetrical around one axis. If it is not your case, you can make it fibre like by spinning, if you spin around the PO vector. If not than see J. Appl. Cryst. 28(1995)247-253. However, there are few other limitations, which are usually completly ignored: The distribution of crystallites around any pole hkl must be axially symmetrical either, so-called disc- or rod-shape like behavior. No way to do it by spinning ... Most of implementations of these corrections in the Rietveld codes also assume another condition: The texture axis is parallel (or perpendicular) to the diffraction vector for all measured hkls. This condition is fullfilled only in Bragg-Brentano or Debye-Scherrer geometries. Surprising that it still works ... Radovan Mibeck, Blaise a écrit : I am learning QPA and am worried about PO. I wonder why sample spinning isn’t discussed more. I am luckily able to barrow time on a newer diffractometer with a sample spinner. Does this reduce PO? Or completely eliminate it? There is a set up variable in GSAS for whether you are spinning the sample – are there guidelines for how many revolutions to spin the sample if you just want to reduce PO? Thanks to all for there help!!! Blaise * * * * * * * * * * * * * Blaise Mibeck Research Scientist Energy & Environmental Research Center University of North Dakota 15 North 23rd Street, Stop 9018 Grand Forks, ND 58202-9018 Phone: (701) 777-5077 Email: [EMAIL PROTECTED] <mailto:[EMAIL PROTECTED]> -Original Message- *From:* David L. Bish [mailto:[EMAIL PROTECTED] *Sent:* Tuesday, October 28, 2008 9:09 AM *To:* Martin; [EMAIL PROTECTED]; rietveld_l@ill.fr *Subject:* RE: Quantitative analysis I agree that it's always best to avoid preferred orientation, but that is easier said than done on a routine basis. I have personally had good luck with the M-D PO correction on many known samples, as long as the PO was not severe. However, I imagine that Mario's problems are related to microabsorption in this case. Mario, if you can re-measure your data with a Co or Fe tube, it would be a good test of this. Dave Bish At 08:51 AM 10/28/2008 -0400, Martin wrote: Sorry to disagree. Experience tells me otherwise - the March-Dollase correction has nearly always led to poor quant results for me. It most certainly cannot be applied safely. Martin -- M Vickers Dept of Chemistry UCL ---- Subject: Re: Quantitative analysis Date: Tue, 28 Oct 2008 02:53:20 -0700 From: [EMAIL PROTECTED] To: Rietveld_l@ill.fr Dear Mario, One more possible problem of applying preferred orientation corrections in QPA is that not all of them are normalized. For example, the March-Dollase correction is normalized and can be applied safely, but the Rietveld-Toraya correction is inapplicable to QPA as it does not preserve the scale normalization. Best regards, Leonid *** Leonid A. Solovyov Institute of Chemistry and Chemical Technology K. Marx av., 42 660049, Krasnoyarsk Russia Phone: +7 3912 495663 Fax: +7 3912 238658 www.icct.ru/eng/content/persons/Sol_LA <http://www.icct.ru/eng/content/persons/Sol_LA> For the best free wallpapers from MSN Click here! <http://wallpapers.msn.com/?ocid> -- Radovan Cerny Laboratoire de Cristallographie 24, quai Ernest-Ansermet CH-1211 Geneva 4, Switzerland Phone : [+[41] 22] 37 964 50, FAX : [+[41] 22] 37 961 08 mailto : [EMAIL PROTECTED] URL: http://www.unige.ch/sciences/crystal/cerny/rcerny.htm
RE: Quantitative analysis
I am learning QPA and am worried about PO. I wonder why sample spinning isn't discussed more. I am luckily able to barrow time on a newer diffractometer with a sample spinner. Does this reduce PO? Or completely eliminate it? There is a set up variable in GSAS for whether you are spinning the sample - are there guidelines for how many revolutions to spin the sample if you just want to reduce PO? Thanks to all for there help!!! Blaise * * * * * * * * * * * * * Blaise Mibeck Research Scientist Energy & Environmental Research Center University of North Dakota 15 North 23rd Street, Stop 9018 Grand Forks, ND 58202-9018 Phone: (701) 777-5077 Email: [EMAIL PROTECTED] -Original Message- From: David L. Bish [mailto:[EMAIL PROTECTED] Sent: Tuesday, October 28, 2008 9:09 AM To: Martin; [EMAIL PROTECTED]; rietveld_l@ill.fr Subject: RE: Quantitative analysis I agree that it's always best to avoid preferred orientation, but that is easier said than done on a routine basis. I have personally had good luck with the M-D PO correction on many known samples, as long as the PO was not severe. However, I imagine that Mario's problems are related to microabsorption in this case. Mario, if you can re-measure your data with a Co or Fe tube, it would be a good test of this. Dave Bish At 08:51 AM 10/28/2008 -0400, Martin wrote: Sorry to disagree. Experience tells me otherwise - the March-Dollase correction has nearly always led to poor quant results for me. It most certainly cannot be applied safely. Martin -- M Vickers Dept of Chemistry UCL ____ > Subject: Re: Quantitative analysis > Date: Tue, 28 Oct 2008 02:53:20 -0700 > From: [EMAIL PROTECTED] > To: Rietveld_l@ill.fr > > Dear Mario, > > One more possible problem of applying preferred orientation corrections in QPA is that not all of them are normalized. For example, the March-Dollase correction is normalized and can be applied safely, but the Rietveld-Toraya correction is inapplicable to QPA as it does not preserve the scale normalization. > > Best regards, > Leonid > > *** > Leonid A. Solovyov > Institute of Chemistry and Chemical Technology > K. Marx av., 42 > 660049, Krasnoyarsk Russia > Phone: +7 3912 495663 > Fax: +7 3912 238658 > www.icct.ru/eng/content/persons/Sol_LA > For the best free wallpapers from MSN Click here! <http://wallpapers.msn.com/?ocid>
RE: Quantitative analysis
>Dear all, the well-known data are: CaCO3 (20%), CaF2 (35%), SiO2 (1%), Al2O3 (20%), and FeCO3 (24%). The data obtained without PO are: CaCO3 (24%), CaF2 (36%), SiO2 (1%), Al2O3 (17%), and FeCO3 (23%). The data obtained with PO are: CaCO3 (19%), CaF2 (32%), SiO2 (2%), Al2O3 (31%), and FeCO3 (16%). it seems to have a problem among Al2O3 and FeCO3 data after PO. Mario. Dear all, > > The data collection conditions is: hand grind (35 microns), scan: > 2Theta/Theta Coupled, to steps 2 sec., target Cu, graphite monochromator, > side loading. The correction of preferential orientation has been refined > by March-Dollase model. > > Thanks a lot, > > Mario. > > > > > Dear Mario, >> >> Please tell me a little about the data collection conditions you used >> for >> this work:- >> >> How was the sample prepared (hand ground, micronised in McCrone mill >> ) >> What was the tube target Cu, Co, other ?? >> >> Cheers >> Ian Madsen >> >> From: [EMAIL PROTECTED] [EMAIL PROTECTED] >> Sent: Tuesday, October 28, 2008 2:48 AM >> To: Rietveld_l@ill.fr >> Subject: Quantitative analysis >> >> Dear all, >> >> I have this question, >> >> I have been refined one mixture (of well-know percentage composition) of >> CaCO3, CaF2, SiO2 and Al2O3, with preferential orientation in CaCO3 >> (104) >> and CaF2 (111) with good results. When I add to the mixture FeCO3 and I >> refine with preferential orientation (104), it happens that when I don´t >> apply the preferential orientation in all this phases, I have correct >> values of percentage composition, but when I apply the preferential >> orientation the refinement is good but with incorrect values of >> percentage >> composition. This experiment has been taken in Bragg Brentano geometry. >> How I should refine this mixture? >> >> Thanks a lot by your help. >> >> Mario Macías >> Universidad Industrial de Santander >> Colombia >> >> > > > >
RE: Quantitative analysis
I agree that it's always best to avoid preferred orientation, but that is easier said than done on a routine basis. I have personally had good luck with the M-D PO correction on many known samples, as long as the PO was not severe. However, I imagine that Mario's problems are related to microabsorption in this case. Mario, if you can re-measure your data with a Co or Fe tube, it would be a good test of this. Dave Bish At 08:51 AM 10/28/2008 -0400, Martin wrote: Sorry to disagree. Experience tells me otherwise - the March-Dollase correction has nearly always led to poor quant results for me. It most certainly cannot be applied safely. Martin -- M Vickers Dept of Chemistry UCL -- > Subject: Re: Quantitative analysis > Date: Tue, 28 Oct 2008 02:53:20 -0700 > From: [EMAIL PROTECTED] > To: Rietveld_l@ill.fr > > Dear Mario, > > One more possible problem of applying preferred orientation corrections in QPA is that not all of them are normalized. For example, the March-Dollase correction is normalized and can be applied safely, but the Rietveld-Toraya correction is inapplicable to QPA as it does not preserve the scale normalization. > > Best regards, > Leonid > > *** > Leonid A. Solovyov > Institute of Chemistry and Chemical Technology > K. Marx av., 42 > 660049, Krasnoyarsk Russia > Phone: +7 3912 495663 > Fax: +7 3912 238658 > www.icct.ru/eng/content/persons/Sol_LA > -- For the best free wallpapers from MSN Click here!
RE: Quantitative analysis
While my coffee pot gurgles away here's my tuppence worth As mentioned by previous answers prevention is MUCH better than cure. Having said that a couple of comments. If there's significant PO then it's a pretty sure thing that the particles are not spherical - so you can forget the Brindley correction which assumes spherical (and also monodisperse BTW) particles. PO is also strongly suggestive (but not certain) of fairly large particles, so microabsorption could be pretty severe. In this case with FeCO3 and Cu radiation microabsorption is going to be an issue independent of whether the PO correction preserves the scale normalization. Pam Dr Pamela Whitfield MRSC CChem Energy Materials Institute for Chemical Process and Environmental Technology (ICPET) Building M12 National Research Council Canada 1200 Montreal Road Ottawa ON K1A 0R6 CANADA Tel: (613) 998-8462Fax: (613) 991 2384 Email: [EMAIL PROTECTED] -Original Message- From: Leonid Solovyov [mailto:[EMAIL PROTECTED] Sent: October 28, 2008 5:53 AM To: Rietveld_l@ill.fr Subject: Re: Quantitative analysis Dear Mario, One more possible problem of applying preferred orientation corrections in QPA is that not all of them are normalized. For example, the March-Dollase correction is normalized and can be applied safely, but the Rietveld-Toraya correction is inapplicable to QPA as it does not preserve the scale normalization. Best regards, Leonid *** Leonid A. Solovyov Institute of Chemistry and Chemical Technology K. Marx av., 42 660049, Krasnoyarsk Russia Phone: +7 3912 495663 Fax: +7 3912 238658 www.icct.ru/eng/content/persons/Sol_LA *** --- On Mon, 10/27/08, [EMAIL PROTECTED] <[EMAIL PROTECTED]> wrote: > From: [EMAIL PROTECTED] <[EMAIL PROTECTED]> > Subject: Quantitative analysis > To: Rietveld_l@ill.fr > Date: Monday, October 27, 2008, 3:48 PM > Dear all, > > I have this question, > > I have been refined one mixture (of well-know percentage > composition) of > CaCO3, CaF2, SiO2 and Al2O3, with preferential orientation > in CaCO3 (104) > and CaF2 (111) with good results. When I add to the mixture > FeCO3 and I > refine with preferential orientation (104), it happens that > when I don´t > apply the preferential orientation in all this phases, I > have correct > values of percentage composition, but when I apply the > preferential > orientation the refinement is good but with incorrect > values of percentage > composition. This experiment has been taken in Bragg > Brentano geometry. > How I should refine this mixture? > > Thanks a lot by your help. > > Mario Macías > Universidad Industrial de Santander > Colombia
RE: Quantitative analysis
Dear all, The data collection conditions is: hand grind (35 microns), scan: 2Theta/Theta Coupled, to steps 2 sec., target Cu, graphite monochromator, side loading. The correction of preferential orientation has been refined by March-Dollase model. Thanks a lot, Mario. Dear Mario, > > Please tell me a little about the data collection conditions you used for > this work:- > > How was the sample prepared (hand ground, micronised in McCrone mill ) > What was the tube target Cu, Co, other ?? > > Cheers > Ian Madsen > > From: [EMAIL PROTECTED] [EMAIL PROTECTED] > Sent: Tuesday, October 28, 2008 2:48 AM > To: Rietveld_l@ill.fr > Subject: Quantitative analysis > > Dear all, > > I have this question, > > I have been refined one mixture (of well-know percentage composition) of > CaCO3, CaF2, SiO2 and Al2O3, with preferential orientation in CaCO3 (104) > and CaF2 (111) with good results. When I add to the mixture FeCO3 and I > refine with preferential orientation (104), it happens that when I don´t > apply the preferential orientation in all this phases, I have correct > values of percentage composition, but when I apply the preferential > orientation the refinement is good but with incorrect values of percentage > composition. This experiment has been taken in Bragg Brentano geometry. > How I should refine this mixture? > > Thanks a lot by your help. > > Mario Macías > Universidad Industrial de Santander > Colombia > >
RE: Quantitative analysis
Mario, You may want to check for the presence of solid solution in your siderite (especially Ca and Mg). In my experience refining the PO in siderite with measurable amounts of Ca or Mg correlates significantly with the occupancy if the Fe/(Ca or Mg) ratio is not constrained to the true chemistry. The chemistry may be estimated by the d104 shift. Dipo Omotoso Natural Resources Canada CETC-Devon #1 Oil Patch drive, Devon AB. T9G 1A8. -Original Message- From: [EMAIL PROTECTED] [mailto:[EMAIL PROTECTED] Sent: Mon 10/27/2008 7:10 PM To: [EMAIL PROTECTED]; Rietveld_l@ill.fr Subject: RE: Quantitative analysis Dear Mario, Please tell me a little about the data collection conditions you used for this work:- How was the sample prepared (hand ground, micronised in McCrone mill ) What was the tube target Cu, Co, other ?? Cheers Ian Madsen From: [EMAIL PROTECTED] [EMAIL PROTECTED] Sent: Tuesday, October 28, 2008 2:48 AM To: Rietveld_l@ill.fr Subject: Quantitative analysis Dear all, I have this question, I have been refined one mixture (of well-know percentage composition) of CaCO3, CaF2, SiO2 and Al2O3, with preferential orientation in CaCO3 (104) and CaF2 (111) with good results. When I add to the mixture FeCO3 and I refine with preferential orientation (104), it happens that when I don´t apply the preferential orientation in all this phases, I have correct values of percentage composition, but when I apply the preferential orientation the refinement is good but with incorrect values of percentage composition. This experiment has been taken in Bragg Brentano geometry. How I should refine this mixture? Thanks a lot by your help. Mario Macías Universidad Industrial de Santander Colombia
Re: Quantitative analysis
Martin, The reason of your bad experience with March-Dollase can be different, however, Leonid was right. The March-Dollase is normalized, the Rietveld-Toraya not. It can be easily normalized (see for example J. Appl. Cryst. 28(1995)247-253) but in all Rietveld codes I know it is not. Best radovan Martin a écrit : Sorry to disagree. Experience tells me otherwise - the March-Dollase correction has nearly always led to poor quant results for me. It most certainly cannot be applied safely. Martin -- M Vickers Dept of Chemistry UCL > Subject: Re: Quantitative analysis > Date: Tue, 28 Oct 2008 02:53:20 -0700 > From: [EMAIL PROTECTED] > To: Rietveld_l@ill.fr > > Dear Mario, > > One more possible problem of applying preferred orientation corrections in QPA is that not all of them are normalized. For example, the March-Dollase correction is normalized and can be applied safely, but the Rietveld-Toraya correction is inapplicable to QPA as it does not preserve the scale normalization. > > Best regards, > Leonid > > *** > Leonid A. Solovyov > Institute of Chemistry and Chemical Technology > K. Marx av., 42 > 660049, Krasnoyarsk Russia > Phone: +7 3912 495663 > Fax: +7 3912 238658 > www.icct.ru/eng/content/persons/Sol_LA > For the best free wallpapers from MSN Click here! <http://wallpapers.msn.com/?ocid=[B001MSN42A0716B]> -- Radovan Cerny Laboratoire de Cristallographie 24, quai Ernest-Ansermet CH-1211 Geneva 4, Switzerland Phone : [+[41] 22] 37 964 50, FAX : [+[41] 22] 37 961 08 mailto : [EMAIL PROTECTED] URL: http://www.unige.ch/sciences/crystal/cerny/rcerny.htm
RE: Quantitative analysis
Sorry to disagree. Experience tells me otherwise - the March-Dollase correction has nearly always led to poor quant results for me. It most certainly cannot be applied safely. Martin -- M Vickers Dept of Chemistry UCL > Subject: Re: Quantitative analysis> Date: Tue, 28 Oct 2008 02:53:20 -0700> > From: [EMAIL PROTECTED]> To: Rietveld_l@ill.fr> > Dear Mario,> > One more > possible problem of applying preferred orientation corrections in QPA is that > not all of them are normalized. For example, the March-Dollase correction is > normalized and can be applied safely, but the Rietveld-Toraya correction is > inapplicable to QPA as it does not preserve the scale normalization. > > Best > regards,> Leonid> > ***> > Leonid A. Solovyov> Institute of Chemistry and Chemical Technology> K. Marx > av., 42> 660049, Krasnoyarsk Russia> Phone: +7 3912 495663> Fax: +7 3912 > 238658> www.icct.ru/eng/content/persons/Sol_LA> _ See the most popular videos on the web http://clk.atdmt.com/GBL/go/115454061/direct/01/
Re: Quantitative analysis
Dear Mario, One more possible problem of applying preferred orientation corrections in QPA is that not all of them are normalized. For example, the March-Dollase correction is normalized and can be applied safely, but the Rietveld-Toraya correction is inapplicable to QPA as it does not preserve the scale normalization. Best regards, Leonid *** Leonid A. Solovyov Institute of Chemistry and Chemical Technology K. Marx av., 42 660049, Krasnoyarsk Russia Phone: +7 3912 495663 Fax: +7 3912 238658 www.icct.ru/eng/content/persons/Sol_LA *** --- On Mon, 10/27/08, [EMAIL PROTECTED] <[EMAIL PROTECTED]> wrote: > From: [EMAIL PROTECTED] <[EMAIL PROTECTED]> > Subject: Quantitative analysis > To: Rietveld_l@ill.fr > Date: Monday, October 27, 2008, 3:48 PM > Dear all, > > I have this question, > > I have been refined one mixture (of well-know percentage > composition) of > CaCO3, CaF2, SiO2 and Al2O3, with preferential orientation > in CaCO3 (104) > and CaF2 (111) with good results. When I add to the mixture > FeCO3 and I > refine with preferential orientation (104), it happens that > when I don´t > apply the preferential orientation in all this phases, I > have correct > values of percentage composition, but when I apply the > preferential > orientation the refinement is good but with incorrect > values of percentage > composition. This experiment has been taken in Bragg > Brentano geometry. > How I should refine this mixture? > > Thanks a lot by your help. > > Mario Macías > Universidad Industrial de Santander > Colombia
RE: Quantitative analysis
Dear Mario, My experience of quant Rietveld is much the same as yours - poor quant result if using any sort of PO function. Advise as others have here - reduce PO. Capillary geometry may help in many instances but in this case could then have problems with absorption seeing as you will most likely be having to use Co radiation to avoid fluorescence from the iron. Good luck, Martin _ Win an Xbox 360 or £200 Top Shop Vouchers http://clk.atdmt.com/GBL/go/115454062/direct/01/
RE: Quantitative analysis
Dear Mario, Please tell me a little about the data collection conditions you used for this work:- How was the sample prepared (hand ground, micronised in McCrone mill ) What was the tube target Cu, Co, other ?? Cheers Ian Madsen From: [EMAIL PROTECTED] [EMAIL PROTECTED] Sent: Tuesday, October 28, 2008 2:48 AM To: Rietveld_l@ill.fr Subject: Quantitative analysis Dear all, I have this question, I have been refined one mixture (of well-know percentage composition) of CaCO3, CaF2, SiO2 and Al2O3, with preferential orientation in CaCO3 (104) and CaF2 (111) with good results. When I add to the mixture FeCO3 and I refine with preferential orientation (104), it happens that when I don´t apply the preferential orientation in all this phases, I have correct values of percentage composition, but when I apply the preferential orientation the refinement is good but with incorrect values of percentage composition. This experiment has been taken in Bragg Brentano geometry. How I should refine this mixture? Thanks a lot by your help. Mario Macías Universidad Industrial de Santander Colombia
RE: Quantitative analysis
Dear Mario, If the quantity of FeCO3 appears to be smaller than the actual value, then it could be due to absorption. If you are using a copper source (CuKalpha) then that excites iron fluorescence, which is radiated equally in all directions... this means that the beam does not penetrate the FeCO3 particles entirely, and results in incomplete diffraction from these particles. There are programs that correct for this problem, but as far as I know there is no freeware to deal with this effect. - Kurt * Kurt Leinenweber Dept. of Chemistry and Biochemistry Arizona State University Tempe, AZ 85287-1604 phone (480)-965-8853 fax (480)-965-2747 *** -Original Message- From: [EMAIL PROTECTED] [mailto:[EMAIL PROTECTED] Sent: Monday, October 27, 2008 8:48 AM To: Rietveld_l@ill.fr Subject: Quantitative analysis Dear all, I have this question, I have been refined one mixture (of well-know percentage composition) of CaCO3, CaF2, SiO2 and Al2O3, with preferential orientation in CaCO3 (104) and CaF2 (111) with good results. When I add to the mixture FeCO3 and I refine with preferential orientation (104), it happens that when I don´t apply the preferential orientation in all this phases, I have correct values of percentage composition, but when I apply the preferential orientation the refinement is good but with incorrect values of percentage composition. This experiment has been taken in Bragg Brentano geometry. How I should refine this mixture? Thanks a lot by your help. Mario Macías Universidad Industrial de Santander Colombia
Re: Quantitative analysis
Dear Mario, I only use PO to check if it applies. If yes, I make a new preparation to avoid PO. Also, graininess may look similar to PO, and this would surely bias QPA if PO refinement is allowed for. So my advice is: grind, grind, grind. Best miguel On 27 Oct 2008 at 10:48, [EMAIL PROTECTED] wrote: > Dear all, > > I have this question, > > I have been refined one mixture (of well-know percentage composition) of > CaCO3, CaF2, SiO2 and Al2O3, with preferential orientation in CaCO3 (104) > and CaF2 (111) with good results. When I add to the mixture FeCO3 and I > refine with preferential orientation (104), it happens that when I don´t > apply the preferential orientation in all this phases, I have correct > values of percentage composition, but when I apply the preferential > orientation the refinement is good but with incorrect values of percentage > composition. This experiment has been taken in Bragg Brentano geometry. > How I should refine this mixture? > > Thanks a lot by your help. > > Mario Macías > Universidad Industrial de Santander > Colombia > > > -- Miguel Gregorkiewitz Dip Scienze della Terra, Università via Laterina 8, I-53100 Siena, Europe fon +39'0577'233810 fax 233938 email [EMAIL PROTECTED]
Quantitative analysis
Dear all, I have this question, I have been refined one mixture (of well-know percentage composition) of CaCO3, CaF2, SiO2 and Al2O3, with preferential orientation in CaCO3 (104) and CaF2 (111) with good results. When I add to the mixture FeCO3 and I refine with preferential orientation (104), it happens that when I don´t apply the preferential orientation in all this phases, I have correct values of percentage composition, but when I apply the preferential orientation the refinement is good but with incorrect values of percentage composition. This experiment has been taken in Bragg Brentano geometry. How I should refine this mixture? Thanks a lot by your help. Mario Macías Universidad Industrial de Santander Colombia
RE: Laboratory supplies/equipments for application of the Rietveld Method (quantitative analysis)
Thank you very much man!!! We are right now making a zero background sample holder, with a quartz cutted 6 degrees form its c axis. We are buying Cab-O-Sil (fumed silica) as well, trying to reduce preferred orientation in our samples using the method of Blount and Vassilou (1979). Subject: Re: Laboratory supplies/equipments for application of the Rietveld Method (quantitative analysis)Date: Wed, 26 Sep 2007 10:51:00 -0400From: [EMAIL PROTECTED]: [EMAIL PROTECTED] the gem dugout for zero background sample holders, and angle/intensity standards. http://www.thegemdugout.com/ On Sep 26, 2007, at 9:30 AM, Leandro Bravo wrote: Hi All!! I´m searching for some equipments, supplies that could be useful to the application of the Rietveld Method (quantitative analisys) like zero-background sample holders, mill etc... in other words, equipments for sample prepare to avoid preferred orientation, microabsorption, etc.. We are trying to buy a Mccrone Micronizing Mill but we just can manage to contact the company (Mccrone Lab Supplies), any of you know other place where I can buy the Mccrone Mill?!?! In other hand, if we don´t buy the Mccrone Mill is there any other equipment that could be useful in our lab?!?! Receba as últimas notícias do Brasil e do mundo direto no seu Messenger com Alertas MSN! É GRÁTIS! Assine já! _ Receba as últimas notícias do Brasil e do mundo direto no seu Messenger com Alertas MSN! É GRÁTIS! http://alertas.br.msn.com/
Re: Laboratory supplies/equipments for application of the Rietveld Method (quantitative analysis)
Try the gem dugout for zero background sample holders, and angle/ intensity standards. http://www.thegemdugout.com/ On Sep 26, 2007, at 9:30 AM, Leandro Bravo wrote: Hi All!! I´m searching for some equipments, supplies that could be useful to the application of the Rietveld Method (quantitative analisys) like zero-background sample holders, mill etc... in other words, equipments for sample prepare to avoid preferred orientation, microabsorption, etc.. We are trying to buy a Mccrone Micronizing Mill but we just can manage to contact the company (Mccrone Lab Supplies), any of you know other place where I can buy the Mccrone Mill?!?! In other hand, if we don´t buy the Mccrone Mill is there any other equipment that could be useful in our lab?!?! Receba as últimas notícias do Brasil e do mundo direto no seu Messenger com Alertas MSN! É GRÁTIS! Assine já!
Laboratory supplies/equipments for application of the Rietveld Method (quantitative analysis)
Hi All!! I´m searching for some equipments, supplies that could be useful to the application of the Rietveld Method (quantitative analisys) like zero-background sample holders, mill etc... in other words, equipments for sample prepare to avoid preferred orientation, microabsorption, etc.. We are trying to buy a Mccrone Micronizing Mill but we just can manage to contact the company (Mccrone Lab Supplies), any of you know other place where I can buy the Mccrone Mill?!?! In other hand, if we don´t buy the Mccrone Mill is there any other equipment that could be useful in our lab?!?! _ Receba as últimas notícias do Brasil e do mundo direto no seu Messenger com Alertas MSN! É GRÁTIS! http://alertas.br.msn.com/
