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Re: [sdpd] calibration problems with Silicon+gsas
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<p>On Tue, 10 Jun 2008 20:15:15 +0200 (CEST)<br>
Lubomir Smrcok <<a href="mailto:uachsmrk%40savba.sk";>uachsmrk...@savba.<wbr>sk</a>> wrote:<br>
> Hi,<br>
> we have been using Stoe Stadi_P for 16 years and have <br>
>never encountered <br>
> problems with positioning. My advice for you is to read <br>
> technical manual, part calibration ... Second, changing<br>
>the origin of a <br>
> spgr can hardly change indicated positions of the Bragg <br>
>diffractions, so <br>
> there is not the problem ...<br>
<br>
well, reflection conditions for special sites (only one in <br>
Si)? ;)<br>
<br>
> lubo<br>
> <br>
> <br>
> On Tue, 10 Jun 2008, Lujun...@EKM wrote:<br>
> <br>
>> Hello, All:<br>
>><br>
>> Thanks to the suggestion from Prof. Gottschalk, i took <br>
>>(1/8,1/8,1/<wbr>8) origin instead of (0,0,0). It is much <br>
>>improved and it shows the calibration sample has no <br>
>>problem, but current match cannot be better enough.<br>
>><br>
>> Nevertheless, whether the device's state was suitable <br>
>>for refinement analysis or not is still unclear, and i <br>
>>still doubt whether the peakshapes produced by the device <br>
>>can be well descriped by type-3 parameters.<br>
>> Moreover, i am also doubting whether this rough <br>
>>parameters, as shown in the webpage, are somehow <br>
>>reproducible for other materials when all the measurement <br>
>>conditions are the same.<br>
>><br>
>> The discussion webpage has been updated, please see more <br>
>>pictures via:<br>
>> <a href="http://www.physik.uni-augsburg.de/~lujun/";>http://www.physik.<wbr>uni-augsburg.<wbr>de/~lujun/</a><br>
>><br>
>> Faithfully<br>
>> Jun Lu<br>
>> ----------<br>
>> Lst. Prof. Lijie Qiao<br>
>> Department of Materials Physics and Chemistry<br>
>> University of Science and Technology Beijing<br>
>> 100083 Beijing<br>
>> P.R. China<br>
>> <a href="http://www.instrument.com.cn/ilog/handsomeland/";>http://www.instrume<wbr>nt.com.cn/<wbr>ilog/handsomelan<wbr>d/</a><br>
>><br>
>> Lst. Prof. Loidl and Lunkenheimer<br>
>> Experimental Physics V<br>
>> Center for Electronic Correlations and Magnetism (EKM)<br>
>> University of Augsburg<br>
>> Universitaetsstr. 2<br>
>> 86159 Augsburg<br>
>> Germany<br>
>> <a href="http://www.physik.uni-augsburg.de/exp5";>http://www.physik.<wbr>uni-augsburg.<wbr>de/exp5</a><br>
>><br>
>> ----- Original Message -----<br>
>> From: Matthias Gottschalk<br>
>> To: <a href="mailto:sdpd%40yahoogroups.com";>sdpd...@yahoogroups.<wbr>com</a><br>
>> Sent: Tuesday, June 10, 2008 6:58 PM<br>
>> Subject: Re: [sdpd] calibration problems with <br>
>>Silicon+gsas<br>
>><br>
>><br>
>> In spacegroup F d 3- m there a 2 origins.<br>
>> Put the Si on 1/8 1/8 1/8 instead of 0 0 0.<br>
>><br>
>> The Stadi P is a brilliant instrument (curved Ge<br>
>> monochromator, PSD). We use it (2 of them) in <br>
>>conjunction<br>
>> with GSAS now for 14 years without problems. However <br>
>>some<br>
>> crystallographic knowledge helps when doing Rietveld<br>
>> refinements.<br>
>><br>
>> Matthias Gottschalk<br>
>><br>
>> On Tue, 10 Jun 2008 17:09:03 +0200<br>
>> "Lujun...@EKM" <<a href="mailto:jun.lu%40physik.uni-augsburg.de";>jun.lu...@physik.<wbr>uni-augsburg.<wbr>de</a>> wrote:<br>
>> > Hello, crystallographical experts:<br>
>> ><br>
>> > i had never got a satisfying refinement solution for<br>
>> >my interesting materials, so i began to doubt our <br>
>>X-ray<br>
>> >device (STADI-P, STOE Company): was it capable of<br>
>> >structural refining or just not well calibrated? This <br>
>>is<br>
>> >the motivation for my calibration refining work.<br>
>> > The raw data was collected and can be easily indexed.<br>
>> >i was happy for a while, but when the refinement work <br>
>>was<br>
>> >tried, i became dispointed. Whatever i tried, the <br>
>>match<br>
>> >betrween raw data and calculation was always bad: <br>
>>there<br>
>> >were no calculation intensities in some positions <br>
>>where<br>
>> >should be, and in other positions also were there no<br>
>> >experimental peaks where should be.<br>
>> > Would anyone like to point out some reasons for such<br>
>> >situation? In particular, the most important question <br>
>>for<br>
>> >me is whether our STADI-P device suitable for <br>
>>refinement<br>
>> >experiments or not. If so, i have no choice but to <br>
>>throw<br>
>> >away all my previous refinement work. :(<br>
>> ><br>
>> > All the related files has been attached along with <br>
>>this<br>
>> >mail (raw data with raw format, gsas format and ascii<br>
>> >format; instrument data where parameters are estimated<br>
>> >using CMPR programme; one well-cited published CIF <br>
>>file<br>
>> >for silicon; and the hkl files after indexing with<br>
>> >PowderX).<br>
>> ><br>
>> > Your reply will be quite appreciated.<br>
>> ><br>
>> ><br>
>> ><br>
>> >Faithfully<br>
>> > Jun Lu<br>
>> > ----------<br>
>> > Lst. Prof. Lijie Qiao<br>
>> > Department of Materials Physics and Chemistry<br>
>> > University of Science and Technology Beijing<br>
>> > 100083 Beijing<br>
>> > P.R. China<br>
>> > <a href="http://www.instrument.com.cn/ilog/handsomeland/";>http://www.instrume<wbr>nt.com.cn/<wbr>ilog/handsomelan<wbr>d/</a><br>
>> ><br>
>> > Lst. Prof. Loidl and Lunkenheimer<br>
>> > Experimental Physics V<br>
>> > Center for Electronic Correlations and Magnetism <br>
>>(EKM)<br>
>> > University of Augsburg<br>
>> > Universitaetsstr. 2<br>
>> > 86159 Augsburg<br>
>> > Germany<br>
>> > <a href="http://www.physik.uni-augsburg.de/exp5";>http://www.physik.<wbr>uni-augsburg.<wbr>de/exp5</a><br>
>> ><br>
>> ><br>
>> > [Non-text portions of this message have been removed]<br>
>> ><br>
>><br>
>><br>
>><br>
>><br>
>><br>
>> [Non-text portions of this message have been removed]<br>
>><br>
>><br>
<br>
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#ygrp-sponsor #ov li{
list-style-type: square;
padding: 6px 0;
font-size: 77%;
}
#ygrp-sponsor #ov li a{
text-decoration: none;
font-size: 130%;
}
#ygrp-sponsor #nc{
background-color: #eee;
margin-bottom: 20px;
padding: 0 8px;
}
#ygrp-sponsor .ad{
padding: 8px 0;
}
#ygrp-sponsor .ad #hd1{
font-family: Arial;
font-weight: bold;
color: #628c2a;
font-size: 100%;
line-height: 122%;
}
#ygrp-sponsor .ad a{
text-decoration: none;
}
#ygrp-sponsor .ad a:hover{
text-decoration: underline;
}
#ygrp-sponsor .ad p{
margin: 0;
}
o{font-size: 0; }
.MsoNormal{
margin: 0 0 0 0;
}
#ygrp-text tt{
font-size: 120%;
}
blockquote{margin: 0 0 0 4px;}
.replbq{margin:4}
-->
</style>
</head>
<!--~-|**|PrettyHtmlEnd|**|-~-->
</html><!--End group email -->
</x-html>