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> From: "Kaduk, Jim A" <[EMAIL PROTECTED]>
> To: "'RIETVELD_L Distribution List'" <[EMAIL PROTECTED]>
> Subject: RE: Accuracy and reproducibility of x-ray powder diffractometers
> Date: Wed, 12 Jan 2000 10:37:05 -0500
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> 
> We have several quality control procedures.
> 
> Each week, we measure the 20-60 deg portion of a reference specimen of
> NIST
> 640b dispersed in epoxy on each instrument, to monitor changes in
> intensity
> and position of the peaks (mostly to watch tube intensity decay).
> 
> From time to time, we measure full (20-140 deg) patterns of NIST 1976
> alumina plate, and use the patterns in Rietvedl refinements (GSAS) to
> determine new instrument parameters.  Most of our work involves Rietveld
> refinement, so these parameters serve as good QC.
> 
> We still do some "old fashioned" quantitative analyses, in which we
> measure
> the integrated areas of clusters of peaks (mostly for certain zeolite
> catalysts).  Each time we make such a measurement of a real sample, we
> measure the pattern of a reference specimen.
> 
> We find that the use of an internal standard (at a known concentration)
> for
> both profile intensities and peak positions reduces (not eliminates) most
> of
> the common errors associated with quantitative analysis using powder
> diffraction techniques.
> 
> Jim Kaduk
> [EMAIL PROTECTED]
> 
> > ----------
> > From:       Alan Hewat[SMTP:[EMAIL PROTECTED]]
> > Reply To:   RIETVELD_L Distribution List
> > Sent:       Thursday, January 06, 2000 4:24 AM
> > To:         [EMAIL PROTECTED]
> > Subject:    Accuracy and reproducibility of x-ray powder diffractometers
> > 
> > 
> > Question posted on behalf of Dr K.V.Rao <[EMAIL PROTECTED]>
> > 
> > >Recently we procured one x-ray powder diffractometer from a reputed
> > vendor. During installation we asked them to show us the accuracy and
> > reproducibility of the system. Initially they said that the quartz
> > standard
> > they have supplied with the instrument is not a very good crystalline
> > sample. So we have to procure a certified standard sample from some
> place
> > then they can demonstrate the accuracy and reproducibility on that
> sample.
> > When we told them that it is their responsibility to provide the proper
> > standard and demonstrate the specifications asked by us and quoted by
> > them,
> > they started telling that it is not possible to check the accuracy and
> > reproducibility at the site with the existing software available on the
> > system. These can be checked only at the manufacturing factory where
> they
> > have to use special measuring tools and software. So now we are unable
> to
> > accept the system just based on their brochure/manual specifications.
> > >
> > >Please let me know the following.
> > >1. What is the normal procedure followed to check the accuracy and
> > reproducibility of the powder diffractometer?
> > >2. Is it true that the accuracy and reproducibility can not be checked
> at
> > site and they can only be measured at the manufacturing factory?
> > >3. Is it true that they need special tools and separate software apart
> > from whatever they have  supplied with the instrument for this purpose?
> > >
> > >Please send your comments / suggestions to the following address
> > >
> > >Attn: Dr. K.V.Rao
> > >e-mail:  [EMAIL PROTECTED]
> > >
> > >or [EMAIL PROTECTED]
> > >
> > >Thanking you in advance
> > 
> > Alan Hewat, ILL Grenoble, FRANCE <[EMAIL PROTECTED]> tel (33) 4.76.20.72.13 
> > ftp://ftp.ill.fr/pub/dif  fax (33) 4.76.20.76.48  http://www.ill.fr/dif/
> > 
> 

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