.. perhaps I am not getting the point or it's just too stupid to be effective... but can't you just get the integrated intensity of the peak versus temperature and extrapolate down to zero? If you are really brave, just do it parametrically after you have done it free
Matteo ----------------------------------------------------------------- Matteo Leoni, PhD DICAM University of Trento via Mesiano, 77 38123 Trento Italy Tel +39 0461 282416 Fax +39 0461 282672 e-mail: matteo.le...@unitn.it ---------------------------------------------------------------- -----Messaggio originale----- Da: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] Per conto di Apu Sarkar Inviato: lunedì 5 maggio 2014 2.48 A: Tony Wang Cc: ILL Forum Oggetto: Re: Phase volume fraction Hi Tony, Thanks for your suggestion. Yes, I tried scanning the major peak of the second phase with increasing temperature. I have good data. However, still I have the doubt of detecting the exact temperature of dissolution of the second phase. Looking forward to meet you at AIF. Best regards Apu On 5/3/14, Tony Wang <ian...@126.com> wrote: > Hi Apu, > > > > As you are running in situ scanning you probably cannot scan the > sample for long time. > > If you are only care about the accurate phase transforming > temperature, you can localize the scan range to the major peak for > your second phase, which will largely improve the detection limit, as Matteo > suggested. > > Building some external calibration line may also help. > > > > Xiaodong (Tony) Wang > > Curtin University, coming to AIF > > > > From: rietveld_l-ow...@ill.fr [mailto:rietveld_l-ow...@ill.fr] On > Behalf Of Kurt Leinenweber > Sent: 2014年5月4日 6:05 > To: Habib Boughzala; ILL Forum > Subject: RE: Phase volume fraction > > > > Hi all, > > > > I think looking at the small diffraction peaks (or bumps) of the > low-fraction phase, and comparing them to any bumps that may or may > not be present in the actual data, could go a long way. But I do > agree that some more scientific analysis of the reliability of a very > low phase fraction would be merited. > > > > - Kurt > > > > _____ > > From: rietveld_l-requ...@ill.fr [rietveld_l-requ...@ill.fr] on behalf > of Habib Boughzala [habib.boughz...@ipein.rnu.tn] > Sent: Saturday, May 03, 2014 9:23 PM > To: ILL Forum > Subject: Re: Phase volume fraction > > > Hi everybody, > > > > I am very septic about the 1% of QPA detection limit and even less the > 0.1% in QPA e.s.d. since GSAS, FP, TOPAS, etc give different results > for the same sample with the same treatment. > > So I thing that we need drastically some scientific output in this field. > > > > Regards > > Habib > > > > Pr. Habib Boughzala > > I.P.E.I. Nabeul > > F.S.T Faculté des Sciences de Tunis > > A.T.C. Association Tunisienne de Cristallographie > > Tel 216 20523595 > > > > -------Original Message------- > > > > From: Leonid Solovyov <mailto:l_solov...@yahoo.com> > > Date: 02/05/2014 03:06:35 > > To: rietveld_l@ill.fr > > Subject: Re: Phase volume fraction > > > > Dear Martin, > > > > The main problems of the e.s.u. expressions used in Rietveld programs > are the neglect of correlations between residuals and the loss of > interrelations between particular residuals and particular parameters > in terms of their mutual influence. > > Some references on the topic: > > J. Appl. Cryst. (1979). 12, 554-563 > > Acta Cryst. (1982). A38, 264-269 > > J. Appl. Cryst. (1983). 16, 159-163 > > J. Appl. Cryst. (1986). 19, 10-18 > > J. Appl. Cryst. ( 1991). 24, 1-5 > > J. Appl. Cryst. (1994). 27, 802-844 > > > > Best regards, > > Leonid > > ******************************************************* > > Leonid A. Solovyov > Institute of Chemistry and Chemical Technology 660036, Akademgorodok > 50/24, Krasnoyarsk, Russia > <http://sites.google.com/site/solovyovleonid> > http://sites.google.com/site/solovyovleonid > ******************************************************* > > _____ > > From: Martin Fisch <m_fi...@bluewin.ch> > To: Leonid Solovyov <l_solov...@yahoo.com> > Sent: Friday, May 2, 2014 2:59 PM > Subject: Re: Phase volume fraction > > > > Hi Leonid > > Everyone says that Rietveld s.u.'s are underestimated. Why is this? Is > there any reference to this? > > Cheers, > Martin > > > > On 02.05.2014 09:57, Leonid Solovyov wrote: > > Dear Apu, > > > > If you use the Rietveld-based QPA you may assess the detection limit > for a phase from the estimated standard uncertainty of its weight (or > volume) fraction. In this case one should also take into account the > fact that the Rietveld standard uncertainties of QPA are underestimated about > 2-3 times. > To have more realistic uncertainties you may use DDM: > > http://sites.google.com/site/ddmsuite/ > > http://sourceforge.net/p/ddmsuite > > > > Best regards, > > Leonid > > > > ******************************************************* > Leonid A. Solovyov > Institute of Chemistry and Chemical Technology 660036, Akademgorodok > 50/24, Krasnoyarsk, Russia > <http://sites.google.com/site/solovyovleonid> > http://sites.google.com/site/solovyovleonid > ******************************************************* > > _____ > > From: Apu Sarkar <mailto:apusar...@gmail.com> <apusar...@gmail.com> > To: "Leoni, Matteo" <mailto:matteo.le...@unitn.it> > <matteo.le...@unitn.it> > > Cc: <mailto:rietveld_l@ill.fr> "rietveld_l@ill.fr" > <mailto:rietveld_l@ill. > fr> <rietveld_l@ill.fr> > Sent: Friday, May 2, 2014 3:41 AM > Subject: Re: Phase volume fraction > > > Yes, I meant detection limit. > In my sample I have a second phase which dissolves at some > temperature. I tried to identify the dissolution temperature using > XRD. With increasing temperature the peak intensity for the second > phase decreased. After certain temperature the peak disappeared. I > understand that is not exactly the dissolution temperature. There is a > limit of XRD to detect the phase. > > Thanks > Apu > > Department of Nuclear Engineering > NC State University > Raleigh, USA > > > > On 5/1/14, Leoni, Matteo <matteo.le...@unitn.it> wrote: >> I guess you are talking about detection limit only, not >> quantification limit, right? >> The answer largely depends on your material (scattering power, domain > size), >> tube (sampling volume) and counting time. I have seen cases where you >> can clearly see something below 0.1 wt% and cases where already the >> percent > was >> off limits. >> Matteo >> >> ----------------------------------------------------------------- >> >> Matteo Leoni, PhD >> >> DICAM >> University of Trento >> via Mesiano, 77 >> 38123 Trento >> Italy >> >> Tel +39 0461 282416 Fax +39 0461 282672 >> >> e-mail: matteo.le...@unitn.it >> ---------------------------------------------------------------- >> >> >> -----Messaggio originale----- >> Da: rietveld_l-requ...@ill.fr [mailto:rietveld_l-requ...@ill.fr] Per >> conto di Apu Sarkar >> Inviato: giovedì 1 maggio 2014 22.24 >> A: rietveld_l@ill.fr >> Oggetto: Phase volume fraction >> >> Hi, >> Can any one tell me what is the minimum phase volume fraction that >> can be detected by a laboratory X-ray diffractometer. In there any >> reference for this. >> >> I am using the new Empyrean from PANalytical. >> >> Thanks >> Apu >> >> Department of Nuclear Engineering >> NC State University >> Raleigh, USA >> > > > -- > Apu Sarkar > Postdoctoral Research Scholar > Department of Nuclear Engineering > North Carolina State University > > > Raleigh > USA > > > Mobile: 919-561-9244 > Website: https://sites.google.com/a/ncsu.edu/apu/ > > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > Please do NOT attach files to the whole list > <alan.he...@neutronoptics.com> Send commands to <lists...@ill.fr> eg: > HELP as the subject with no body text The Rietveld_L list archive is > on http://www.mail-archive.com/rietveld_l@ill.fr/ > ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ > > > > > > > > > > > > > <http://www.incredimail.com/app/?tag=IM2_Default_Stamp_EN&id=509&lang= > 9&did= > 10500&ppd=2672,201106231034,1125,1,1953940704990396415&rui=156769540&a > pp_tes > t_id=0&sd=20140503> > > -- Apu Sarkar Postdoctoral Research Scholar Department of Nuclear Engineering North Carolina State University Raleigh USA Mobile: 919-561-9244 Website: https://sites.google.com/a/ncsu.edu/apu/
++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Please do NOT attach files to the whole list <alan.he...@neutronoptics.com> Send commands to <lists...@ill.fr> eg: HELP as the subject with no body text The Rietveld_L list archive is on http://www.mail-archive.com/rietveld_l@ill.fr/ ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++
