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Re: [sdpd] calibration problems with Silicon+gsas



Hi,
we have been using Stoe Stadi_P for 16 years and have never encountered 
problems with positioning.  My advice for you is to read 
technical manual, part calibration ... Second, changing the origin of a 
spgr can hardly change indicated positions of the Bragg diffractions, so 
there is not the problem ...
lubo


On Tue, 10 Jun 2008, Lujun...@EKM wrote:

> Hello, All:
>
> Thanks to the suggestion from Prof. Gottschalk, i took (1/8,1/8,1/8) origin instead of (0,0,0). It is much improved and it shows the calibration sample has no problem, but current match cannot be better enough.
>
> Nevertheless, whether the device's state was suitable for refinement analysis or not is still unclear, and i still doubt whether the peakshapes produced by the device can be well descriped by type-3 parameters.
> Moreover, i am also doubting whether this rough parameters, as shown in the webpage, are somehow reproducible for other materials when all the measurement conditions are the same.
>
> The discussion webpage has been updated, please see more pictures via:
> http://www.physik.uni-augsburg.de/~lujun/
>
> Faithfully
> Jun Lu
> ----------
> Lst. Prof. Lijie Qiao
> Department of Materials Physics and Chemistry
> University of Science and Technology Beijing
> 100083 Beijing
> P.R. China
> http://www.instrument.com.cn/ilog/handsomeland/
>
> Lst. Prof. Loidl and Lunkenheimer
> Experimental Physics V
> Center for Electronic Correlations and Magnetism (EKM)
> University of Augsburg
> Universitaetsstr. 2
> 86159 Augsburg
> Germany
> http://www.physik.uni-augsburg.de/exp5
>
>  ----- Original Message -----
>  From: Matthias Gottschalk
>  To: sdpd...@yahoogroups.com
>  Sent: Tuesday, June 10, 2008 6:58 PM
>  Subject: Re: [sdpd] calibration problems with Silicon+gsas
>
>
>  In spacegroup F d 3- m there a 2 origins.
>  Put the Si on 1/8 1/8 1/8 instead of 0 0 0.
>
>  The Stadi P is a brilliant instrument (curved Ge
>  monochromator, PSD). We use it (2 of them) in conjunction
>  with GSAS now for 14 years without problems. However some
>  crystallographic knowledge helps when doing Rietveld
>  refinements.
>
>  Matthias Gottschalk
>
>  On Tue, 10 Jun 2008 17:09:03 +0200
>  "Lujun...@EKM" <jun.lu...@physik.uni-augsburg.de> wrote:
>  > Hello, crystallographical experts:
>  >
>  > i had never got a satisfying refinement solution for
>  >my interesting materials, so i began to doubt our X-ray
>  >device (STADI-P, STOE Company): was it capable of
>  >structural refining or just not well calibrated? This is
>  >the motivation for my calibration refining work.
>  > The raw data was collected and can be easily indexed.
>  >i was happy for a while, but when the refinement work was
>  >tried, i became dispointed. Whatever i tried, the match
>  >betrween raw data and calculation was always bad: there
>  >were no calculation intensities in some positions where
>  >should be, and in other positions also were there no
>  >experimental peaks where should be.
>  > Would anyone like to point out some reasons for such
>  >situation? In particular, the most important question for
>  >me is whether our STADI-P device suitable for refinement
>  >experiments or not. If so, i have no choice but to throw
>  >away all my previous refinement work. :(
>  >
>  > All the related files has been attached along with this
>  >mail (raw data with raw format, gsas format and ascii
>  >format; instrument data where parameters are estimated
>  >using CMPR programme; one well-cited published CIF file
>  >for silicon; and the hkl files after indexing with
>  >PowderX).
>  >
>  > Your reply will be quite appreciated.
>  >
>  >
>  >
>  >Faithfully
>  > Jun Lu
>  > ----------
>  > Lst. Prof. Lijie Qiao
>  > Department of Materials Physics and Chemistry
>  > University of Science and Technology Beijing
>  > 100083 Beijing
>  > P.R. China
>  > http://www.instrument.com.cn/ilog/handsomeland/
>  >
>  > Lst. Prof. Loidl and Lunkenheimer
>  > Experimental Physics V
>  > Center for Electronic Correlations and Magnetism (EKM)
>  > University of Augsburg
>  > Universitaetsstr. 2
>  > 86159 Augsburg
>  > Germany
>  > http://www.physik.uni-augsburg.de/exp5
>  >
>  >
>  > [Non-text portions of this message have been removed]
>  >
>
>
>
>
>
> [Non-text portions of this message have been removed]
>
>

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