Hi Luca,Thanks for sharing the links to your method - I hope we can try it the next time we get stuck on identification.
It is a shame to hear you were delayed for so long by J.Appl.Cryst. Did they ask you to cite some work from the Glasgow group as the commercial competitor? I have in mind that they were looking at measured profiles too (https://doi.org/10.1107/S002188980400038X, https://doi.org/10.1107/S0021889804011847).
Indeed I had overlooked your paper, so perhaps this list is still one of the better ways to reach some parts of the powder diffraction community!
With best regards, Jon On 06/09/2023 18:52, Luca Lutterotti wrote:
I am glad you find FPSM an inspiring idea, me and my co-workers will be quite happy if this will results in some citations. The FPSM publication back in 2019 was a troubled submission. It took us more than 3 years as initially was just rejected (for economical reasons, as it would be unfair against the traditional search-match software developed by companies; you read it right, that was the reason for rejection by the reviewer and the editor accepted it even if the other reviewer was for accepting it as it is). We had some discussion, but no way. Then we tried to change journal (www were hesitant as it would have had much less visibility on the powder diffraction community) but finally Daniel discussed with another editor of the same journal and we re-submitted and got some fair reviewers. But it was long and the first rejection a bit shocking. I thought before you have to reject for scientific reasons…….Now I am learning that not only at the academic level, but also some companies selling search-match software are including what they call WPF search-match, but no one cite the origin of the idea. I hope I don’t get a second Loopstra-Rietveld case….. ;-) Well in my case I wrote the software before publishing the idea. That software was re-written from scratch to optimise for the speed and the method. That’s why we can work with several thousand structures at the same speed the other softwares work on less than hundreds. I did not use Maud for that in fact.But I want you to know that the last version I developed on a recent EU project (not the one online), works also with turbostratic and modulated clay structures using your model (the Ufer et al.) to simulate them in the Rietveld. It is a fantastic trick that I use for texture analysis but also quantification and now in FPSM. Having a quick Rietveld help to search-match samples containing clays using data even at high angles (more than 60 degs). I indeed don’t pre-calculate and store structures because when you work with many of them it takes more time to load all the precalculations from a database (even the speedy ones) than to re-calculate everything.So I am glad we both made use of each other models/ideas! Best regards, Luca <http://www.unitn.it/> logo_unitrento_firma.png * Luca Lutterotti* Dipartimento di Ingegneria Industriale Università di Trento via Sommarive, 9 - 38123 Trento (Italy) tel. +39 0461 2824-14 (Office), -34 (X-Ray lab) ico_fb_32x32.pngico_twitter_32x32.pngico_insta_32x32.pngico_linkedin_32x32.pngico_youtube_32x32.png Maud: http://maud.radiographema.com <http://maud.radiographema>On 5 Sep 2023, at 13:49, Reinhard Kleeberg <kleeb...@mineral.tu-freiberg.de> wrote:Dear Luca,I completely agree and will be very happy to have a 1D detector with sufficient energy resolution to resolve a "pure" Cu Kalpha1/2 doublet from W Lalpha1. This would make routine work much easier. IMHO, the biggest improvements in XRPD instrumentation within the last decades came solely from the detector side, should be continued.Regarding search-match by Rietveld: Your FSPM method is a very inspiring idea. Nicola Doebelin has incorporated a simplified approach in PROFEX, too: https://www.youtube.com/watch?v=Oqj71TiifeI <https://www.youtube.com/watch?v=Oqj71TiifeI>I'm routinely applying a run of ~500 structures/minerals what we are commonly using (+- the former QPA database of Seifert AUTOQUAN or from the BGMN webpage) for a phase screening of unknown samples, needs ~ 5 min without interaction. Than running QPA refinement with the best matching structures, clicking on remaining peaks in the difference plot for getting a proposal of best matching main line positions in the database, and adding these structure(s) to the refinement, running again... This is a typical workflow in our lab, no need for peak search, background treatment, thinking about artifact peaks...Best regards ReinhardZitat von Luca Lutterotti <luca.luttero...@unitn.it <mailto:luca.luttero...@unitn.it>>:Dear Reinhard and Rietvelders,It is always a compromise. Ideally we would like the fastest instrument with a lot of intensity (so, 1D or 2D detectors) but no lines outside the Kalpha or even just the Kapha1 like the one of James Cline. But this means a monochromator on the incident beam and you get fluorescence background. Now I like your solution of the Si Drift detector, so you just cut the fluorescence and you don’t need the monochromator in the first place. So we are working and we are testing some lab prototypes of a 1D Si Drift like detector to get the best of both world. It is only a lot of electronic, but one day we will have wonderful instrument with only the lines we need and no fluorescence for the background. Actually we use fluorescence for the chemical analysis (quantitative).About the search-match problem. Have a look on our FPSM method (http://fpsm.radiographema.com/ <http://fpsm.radiographema.com/>) where we don’t care about extra lines as it is a Rietveld search-match. We don’t need to identify or search peaks. We don’t use peak positions, we just fit with the Rietveld. It is slower indeed, but every day is becoming faster and in a few years it will run quickly on our cellphones (I have a prototype running there).Best regards, Luca <http://www.unitn.it/ <http://www.unitn.it/>> Luca Lutterotti Dipartimento di Ingegneria Industriale Università di Trento via Sommarive, 9 - 38123 Trento (Italy) tel. +39 0461 2824-14 (Office), -34 (X-Ray lab) Maud:http://maud.radiographema.com <http://maud.radiographema.com/><http://maud.radiographema/ <http://maud.radiographema/>>Begin forwarded message: From: Reinhard Kleeberg <kleeb...@mineral.tu-freiberg.de> Subject: Re: [EXT] [External] Re: Step-like basline Date: 5 September 2023 at 08:56:15 CEST To: rietveld_l@ill.fr Reply-To: Reinhard Kleeberg <kleeb...@mineral.tu-freiberg.de> Dear Luca,I completely agree with your opinion, and want to add that even for "trivial" tasks in XRPD like phase analysis and standard Rietveld refinements the satellites/spectral impurities do cause significant trouble:- The K beta and W L satellites of strong peaks of major phases like quartz, carbonates or cubic structures in geomaterials are typically not automatically recognized in the standard peak search procedures and therefore misinterpreted to be K alpha peaks and added to the peak list. I can't tell you how often I was asked from colleagues for explanation of such "unidentified peaks", and how much time people have spent for searching for explanation of such artefact lines. - In Rietveld analysis our software must generate the peaks at least for the measured angular range. Depending on the method how the software is doing this, we run into problems with the satellites. If the software generates the reflections from the positions of K alpha peaks from the start lattice parameters and the (extended) upper measured angle, K beta satellites of K alpha peaks outside this angular range will maybe not generated and remain unfitted in the pattern. If the software generates the peaks depending on the shortest wavelength in the wavelength profile (more intelligent approach), the software must generate much more reflections (with maxima outside the measured angular range) and all these peaks must be calculated over an extremely broad angular range. In the case of low symmetry structures with big cells or disordered structures described by partial structure factors and the resulting extreme high numbers of peaks, the "extension effect" will cause significantly prolonged time for calculations, without any positive effect.That's why I prefer to use instrumentation with better monochromatic radiation (monochromators, high energy resolution detectors) even in the daily business of phase analysis. We do use our 1D detector Mythen2 with Fe filter (Co radiation) only for "quick and dirty" measurements.Best regards Reinhard Zitat von Luca Lutterotti <luca.luttero...@unitn.it>:Dear Habib,Reinhard is right, and what he explained is exactly what you observed. Now I would add that I may not define your Bruker clean and optimised, because for this kind of samples, wafers and extremely textured thin films, it would be better to have a monochromator in the incident beam and not a Ni filtered (I would more say it is a requirement). It was already showed many times in the past as a monochromator in the incident beam is a necessity for this materials to avoid all the "physical artifacts" created by the strong intensity and not clean Kalpha radiation.Best regards, Luca <http://www.unitn.it/> Luca Lutterotti Dipartimento di Ingegneria Industriale Università di Trento via Sommarive, 9 - 38123 Trento (Italy) tel. +39 0461 2824-14 (Office), -34 (X-Ray lab)  Maud: http://maud.radiographema.com <http://maud.radiographema/>On 4 Sep 2023, at 12:20, Habib Boughzala <habib.boughz...@ipein.rnu.tn> wrote: Many thanks Reinhard,That's exactly what I wanted to say by "I can assure that our Bruker D8 is clean and optimized!" Otherwise, in some other cases of well conditioned thin film no similar phenomenon is observed!So, yes, it's obviously possible that your point of view is right. Regards Habib ------ Message d'origine ------De "Reinhard Kleeberg" <kleeb...@mineral.tu-freiberg.de <mailto:kleeb...@mineral.tu-freiberg.de>>À "Habib Boughzala" <boughz...@yahoo.com <mailto:boughz...@yahoo.com>> Cc rietveld_l@ill.fr <mailto:rietveld_l@ill.fr> Date 04/09/2023 11:07:50 Objet Re: Re[2]: [EXT] Re: [External] Re: Step-like baslineDear Habib,the phenomenom "satellites or edges" originates from the diffraction process. The critical parameters are: - spectral pureness of the primary beam (primary beam monochromator, tube spectral contamination like W...)- the use of K beta absorbtion filter (and its thickness) - the energy resolution ("window") of the detector system.Even a D8 system may be equipped with different types of detectors, slits and energy limits can be set differently for an identical configuration, and quite often satellite peaks may appear later in the time of use (aging of the tube produces more W L, Fe filters may corrode and get perforated...). So it is strictly recommended to check the instrument peridically, by measuring a full pattern of a profile standard (LaB6 or Si or similar).Greetings Reinhard Zitat von Habib Boughzala <boughz...@yahoo.com <mailto:boughz...@yahoo.com>>:Dear all, I would like to send you my witness related to this kind of observation. I can assure that our Bruker D8 is clean and optimized!In many cases of well conditioned thin film (spin coating or controlled diffusion) material this kind of phenomenon is visible around the highest reflection, especially when the preferred orientation is drastically present.So, in my opinion, Reinhard and Alan are right, and what is observed is just like reflections broadening, asymmetry, shifting ...etc ... and can be related to the material behavior. Now, what is the physical (crystallographic!) property responsible of this phenomenon? let's open the floor for a large discussion.Habib ------ Message d'origine ------De "Alan W Hewat" <alan.he...@neutronoptics.com <mailto:alan.he...@neutronoptics.com>> À "Reinhard Kleeberg" <kleeb...@mineral.tu-freiberg.de <mailto:kleeb...@mineral.tu-freiberg.de>>Cc rietveld_l@ill.fr <mailto:rietveld_l@ill.fr> Date 04/09/2023 09:29:08 Objet Re: [EXT] Re: [External] Re: Step-like baslineReinhard is right that it is best to improve the instrument to produce cleaner data. I'm concerned about the advice to model all kinds of features whose origin is not fully understood, simply to obtain a better fit. Shay has told us nothing about his instrument or his conditions of data collection. He asks "Is it a sample preparation problem", to which the obvious reply is "Do you see this with other samples or different materials" ? Only he can answer that. If the answer is yes, he might try modifying his instrument (remove filters etc) to see what effect that has on the pattern from a simple well characterised material. Again only he can do that. Data collection is an experimental science, and data refinement should not be reduced to a "black box" computer program where extra parameters can be added to reduce the R-factor.Alan.On Mon, 4 Sept 2023 at 08:18, Reinhard Kleeberg <kleeb...@mineral.tu-freiberg.de <mailto:kleeb...@mineral.tu-freiberg.de>> wrote:Can be modeled in the BGMN peak profile model as well, by modifying the *.lam file by a series of additional Lorentzians on the 1/lambda scale, see figure. The same can be done for other spectral impurities, e.g. W L satellites. Also "electronic effects" on the wavelength distribution profile like the "edges" from the ROI settings of Si drift detectors can be modelled in such a convolution based approach. However, better to have a pure/simple wavelength distribution (clear alpha1/2 doublet) by a monochromator or high energy resolution detector, as any satellites make trouble in trace phase analysis and do cause prolonged calculation time in complicated Rietveld refinements. Reinhard Zitat von Matthew Rowles <rowle...@gmail.com <mailto:rowle...@gmail.com>>:Topas can model them quite well. The functionality was introduced in version 5.On Mon, 4 Sep 2023, 00:54 Kurt Leinenweber, <ku...@asu.edu <mailto:ku...@asu.edu>> wrote:Hi, Are these things modeled in Rietveld programs, by chance? It seems like a lot of baggage to put in a refinement but if it makes the results better… - Kurt*From:* rietveld_l-requ...@ill.fr <mailto:rietveld_l-requ...@ill.fr> <rietveld_l-requ...@ill.fr <mailto:rietveld_l-requ...@ill.fr>> *On BehalfOf *Thomas Gegan *Sent:* Sunday, September 3, 2023 9:16 AM*To:* Bish, David L <b...@indiana.edu <mailto:b...@indiana.edu>>; Shay Tirosh <stiro...@gmail.com <mailto:stiro...@gmail.com>>;Fernando Igoa <fer.igoa.1...@gmail.com <mailto:fer.igoa.1...@gmail.com>>*Cc:* Rietveld List (rietveld_l@ill.fr <mailto:rietveld_l@ill.fr>) <rietveld_l@ill.fr <mailto:rietveld_l@ill.fr>>*Subject:* RE: [EXT] Re: [External] Re: Step-like baslineI agree with a Ni absorption edge, possibly with a Kβ peak around 38° 2θ.*Tom Gegan* Chemist IIIPhone: +1 732 205-5111, Email: tom.ge...@basf.com <mailto:tom.ge...@basf.com>Postal Address: BASF Corporation, , 25 Middlesex Essex Turnpike, 08830 Iselin, United States*From:* rietveld_l-requ...@ill.fr <mailto:rietveld_l-requ...@ill.fr> <rietveld_l-requ...@ill.fr <mailto:rietveld_l-requ...@ill.fr>> *On BehalfOf *Bish, David L *Sent:* Sunday, September 3, 2023 7:08 AM*To:* Shay Tirosh <stiro...@gmail.com <mailto:stiro...@gmail.com>>; Fernando Igoa <fer.igoa.1...@gmail.com <mailto:fer.igoa.1...@gmail.com>>*Cc:* Rietveld List (rietveld_l@ill.fr <mailto:rietveld_l@ill.fr>) <rietveld_l@ill.fr <mailto:rietveld_l@ill.fr>>*Subject:* [EXT] Re: [External] Re: Step-like basline Some people who received this message don't often get email from b...@indiana.edu <mailto:b...@indiana.edu>. Learn why this is important <https://urldefense.com/v3/__https:/aka.ms/LearnAboutSenderIdentification__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjKqH-aqqA$> Hello Shay,I think it is probably related to "tube tails". You can read about this inthe literature (e.g., on the BGMN web site) and you can model it in some Rietveld software such as Topas. You don't normally notice this but it becomes apparent with higher-intensity peaks. Regards, Dave ------------------------------*From:* rietveld_l-requ...@ill.fr <mailto:rietveld_l-requ...@ill.fr> <rietveld_l-requ...@ill.fr <mailto:rietveld_l-requ...@ill.fr>> on behalf of Fernando Igoa <fer.igoa.1...@gmail.com <mailto:fer.igoa.1...@gmail.com>>*Sent:* Sunday, September 3, 2023 3:06 AM *To:* Shay Tirosh <stiro...@gmail.com <mailto:stiro...@gmail.com>>*Cc:* Rietveld List (rietveld_l@ill.fr <mailto:rietveld_l@ill.fr>) <rietveld_l@ill.fr <mailto:rietveld_l@ill.fr>>*Subject:* [External] Re: Step-like baslineThis message was sent from a non-IU address. Please exercise caution whenclicking links or opening attachments from external sources. Hey Shay, Are you using a motorized slit during the measurement? These may open upabruptly to compensate for the angular dependence of the footprint and thusgenerate an abrupt increase in the intensity. Hope it helps :)On Sun, Sep 3, 2023, 8:50 AM Shay Tirosh <stiro...@gmail.com <mailto:stiro...@gmail.com>> wrote:Dear Rietvelders I am attaching a zoom-in on a diffraction profile.My question is what is the origin of the step-like profile next to a verylarge reflection peak? Is it a sample preparation problem? Is it part of the baseline? Thanks Shay -- ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++Please do NOT attach files to the whole list <alan.he...@neutronoptics.com <mailto:alan.he...@neutronoptics.com>>Send commands to <lists...@ill.fr <mailto:lists...@ill.fr>> eg: HELP as the subject with no bodytext The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/ <https://urldefense.com/v3/__http:/www.mail-archive.com/rietveld_l@ill.fr/__;!!IKRxdwAv5BmarQ!fFhSHn4S5iEzkW-O9lvWG-OzoqK_2SKhRniGa71nxuOL3GcxiyD83i2mnNN0Z48HPkn4zjJTf8rNHg$> ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++Please do NOT attach files to the whole list <alan.he...@neutronoptics.com <mailto:alan.he...@neutronoptics.com>>Send commands to <lists...@ill.fr <mailto:lists...@ill.fr>> eg: HELP as the subject with no bodytext The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/ ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++-- TU Bergakademie Freiberg Dr. R. 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