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RE: [sdpd] Protection of samples



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<TITLE>RE: [sdpd] Protection of samples</TITLE>
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<P><FONT SIZE=2>I also favour the solution provided by Dr. Leinenweber.&nbsp; We have designed our own sample holders.&nbsp; They consist of a regular powder sample holder onto which a half sphere can be mounted.&nbsp; In the half sphere, a slot is machined away and this is sealed with mylar foil (regular, not metallised)&nbsp; In that way, the X-rays always fall perpendicular to the windows and there is no diffraction.&nbsp; The absorption is really minimal.&nbsp; On the other hand, we will have to change the design somewhat, because the minimum measuring angle is too high (the windows don't come low enough).&nbsp; Eventually, we could go to a really air-tight design with beryllium windows.&nbsp; As we are working with hazardous materials, this could provide us with a local air-tight sample holder, which is much easier than putting the entire diffractometer in a glove box.</FONT></P>

<P><FONT SIZE=2>Kind regards,</FONT>
</P>

<P><FONT SIZE=2>Sven</FONT>
</P>

<P><FONT SIZE=2>&gt; -----Original Message-----</FONT>
<BR><FONT SIZE=2>&gt; From: Kurt Leinenweber [<A HREF="mailto:KURTL...@asu.edu";>mailto:KURTL...@asu.edu</A>]</FONT>
<BR><FONT SIZE=2>&gt; Sent: Monday 18 June 2001 19:41</FONT>
<BR><FONT SIZE=2>&gt; To: sdpd...@yahoogroups.com</FONT>
<BR><FONT SIZE=2>&gt; Subject: RE: [sdpd] Protection of samples</FONT>
<BR><FONT SIZE=2>&gt; </FONT>
<BR><FONT SIZE=2>&gt; </FONT>
<BR><FONT SIZE=2>&gt; Hi all,</FONT>
<BR><FONT SIZE=2>&gt; </FONT>
<BR><FONT SIZE=2>&gt; I generally prefer to use a dry cell with the Kapton or mylar </FONT>
<BR><FONT SIZE=2>&gt; away from the</FONT>
<BR><FONT SIZE=2>&gt; sample, so it is not in diffracting position, and </FONT>
<BR><FONT SIZE=2>&gt; perpendicular to the x-ray</FONT>
<BR><FONT SIZE=2>&gt; beam so there is no absorption correction for the dry cell </FONT>
<BR><FONT SIZE=2>&gt; cover when a</FONT>
<BR><FONT SIZE=2>&gt; Rietveld refinement is performed (ie the cover is a </FONT>
<BR><FONT SIZE=2>&gt; semicircle about 2-3 cm</FONT>
<BR><FONT SIZE=2>&gt; above the sample).&nbsp; It requires some design but seems to be </FONT>
<BR><FONT SIZE=2>&gt; worth it; since</FONT>
<BR><FONT SIZE=2>&gt; I designed this one (for the Siemens D-5000) I have had </FONT>
<BR><FONT SIZE=2>&gt; requests to have new</FONT>
<BR><FONT SIZE=2>&gt; ones made for 8 different research groups at our University!</FONT>
<BR><FONT SIZE=2>&gt; </FONT>
<BR><FONT SIZE=2>&gt; &nbsp;&nbsp;&nbsp;&nbsp;&nbsp; &nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp; &nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp;&nbsp; - Kurt Leinenweber</FONT>
<BR><FONT SIZE=2>&gt; </FONT>
<BR><FONT SIZE=2>&gt; -----Original Message-----</FONT>
<BR><FONT SIZE=2>&gt; From: Greg Beis [<A HREF="mailto:bgreg...@iesl.forth.gr";>mailto:bgreg...@iesl.forth.gr</A>]</FONT>
<BR><FONT SIZE=2>&gt; Sent: Monday, June 18, 2001 9:59 AM</FONT>
<BR><FONT SIZE=2>&gt; To: sdpd...@yahoogroups.com</FONT>
<BR><FONT SIZE=2>&gt; Subject: [sdpd] Protection of samples</FONT>
<BR><FONT SIZE=2>&gt; </FONT>
<BR><FONT SIZE=2>&gt; </FONT>
<BR><FONT SIZE=2>&gt; Dear all,</FONT>
<BR><FONT SIZE=2>&gt; I have a question concerning ways of protecting air sensitive samples.</FONT>
<BR><FONT SIZE=2>&gt; I am doing powder diffraction on some extremely air sensitive </FONT>
<BR><FONT SIZE=2>&gt; compounds. For</FONT>
<BR><FONT SIZE=2>&gt; that reason, I use aluminized mylar in order to seal them on </FONT>
<BR><FONT SIZE=2>&gt; the holder.</FONT>
<BR><FONT SIZE=2>&gt; Unfortunately, the mylar gives a very broad peak at around 20-30 deg.</FONT>
<BR><FONT SIZE=2>&gt; 2theta, in an area where I expect many small reflections of </FONT>
<BR><FONT SIZE=2>&gt; my samples which</FONT>
<BR><FONT SIZE=2>&gt; I cannot distinguish them.</FONT>
<BR><FONT SIZE=2>&gt; Does anyone of you know any other &quot;protective&quot; material, </FONT>
<BR><FONT SIZE=2>&gt; except mylar, for</FONT>
<BR><FONT SIZE=2>&gt; that purpose? Any suggestions are more than wellcome.</FONT>
<BR><FONT SIZE=2>&gt; </FONT>
<BR><FONT SIZE=2>&gt; Thank you in advance,</FONT>
<BR><FONT SIZE=2>&gt; Gregory</FONT>
<BR><FONT SIZE=2>&gt; </FONT>
<BR><FONT SIZE=2>&gt; </FONT>
<BR><FONT SIZE=2>&gt; </FONT>
<BR><FONT SIZE=2>&gt; </FONT>
<BR><FONT SIZE=2>&gt; </FONT>
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