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Methods, Problems and Solutions

GSAS (General Structure Analysis System) Rietveld powder diffraction and Single Crystal software

Applying Capillary Geometry Absorption Correction in GSAS

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[The reference to use for GSAS in any resulting publications is: A.C. Larson and R.B. Von Dreele, "General Structure Analysis System (GSAS)", Los Alamos National Laboratory Report LAUR 86-748 (1994).]

Via the Rietveld Mailing List

From: "Jie Shao" [[email protected]]
To: [email protected]
Subject: Absorption
Date: Fri, 02 Nov 2001 13:49:29 -0800


I'm using GSAS to process my XRD data (capillary geometry), and I'd like to
know how to correct the absorption effect (My sample contains heavy
elements). I measured the packing density of the sample capillary, and I can
calculate the mu based on it and the wavelength. However, according to the
GSAS manual, I need to input A = mu*R/lamda. What is R? What are the units I
should use for mu (cm-1?), R, and lamda (A?)? Thanks for your help.


Date: Mon, 05 Nov 2001 08:02:08 -0700
To: [email protected]
From: [email protected] (Bob Von Dreele)
Subject: Re: Absorption

Dear Jie (and anyone else),

According to the GSAS Manual (pp 138-140) the cylindrical absorption 
function requires mu*R/lambda. mu is the linear absorption coefficient for 
the sample in units that are commensurate with the radius of the cylinder 
(R). Usually one uses mu in cm-1 and R in cm. mu should be corrected for 
the packing efficiency which is typically 50%. The divide by lambda is a 
kluge to allow use of the absorption function for neutron TOF. Please note 
that the cylindrical absorption function is no good if mu*R exceeds ~30.

Bob Von Dreele


Date: Mon, 05 Nov 2001 08:02:08 -0700
To: [email protected]
From: [email protected] (Bob Von Dreele)
Subject: Re: Absorption

Dear Jie (and anyone else),

According to the GSAS Manual (pp 138-140) the cylindrical absorption 
function requires mu*R/lambda. mu is the linear absorption coefficient for 
the sample in units that are commensurate with the radius of the cylinder 
(R). Usually one uses mu in cm-1 and R in cm. mu should be corrected for 
the packing efficiency which is typically 50%. The divide by lambda is a 
kluge to allow use of the absorption function for neutron TOF. Please note 
that the cylindrical absorption function is no good if mu*R exceeds ~30.

Bob Von Dreele


Date: Mon, 05 Nov 2001 17:24:27 +0000
To: [email protected]
From: Lachlan Cranswick [[email protected]]
Subject: Re: Absorption
Reply-To: [email protected]


>According to the GSAS Manual (pp 138-140) the cylindrical absorption 
>function requires mu*R/lambda. mu is the linear absorption coefficient for 
>the sample in units that are commensurate with the radius of the cylinder 
>(R). Usually one uses mu in cm-1 and R in cm. mu should be corrected for 
>the packing efficiency which is typically 50%. The divide by lambda is a 
>kluge to allow use of the absorption function for neutron TOF. Please note 
>that the cylindrical absorption function is no good if mu*R exceeds ~30.

For handling high mu*R materials, one method that is applied in 
the CSIRO Minerals XRD lab is to dilute the sample with Industrial
Diamond powder.   This does not give too many extra peaks, it keeps
the background the same and the Diamond peaks can be used as an 
internal position standard.

Lachlan.

-----------------------
Lachlan M. D. Cranswick
Collaborative Computational Project No 14 (CCP14)
    for Single Crystal and Powder Diffraction
  Birkbeck University of London and Daresbury Laboratory 
Postal Address: CCP14 - School of Crystallography,
                Birkbeck College,
                Malet Street, Bloomsbury,
                WC1E 7HX, London,  UK
Tel: (+44) 020 7631 6849   Fax: (+44) 020 7631 6803
E-mail: [email protected]
WWW: http://www.ccp14.ac.uk/


From: "Yokochi, Alexandre" [[email protected]]
To: "'[email protected]'" [[email protected]]
Subject: RE: Absorption
Date: Mon, 5 Nov 2001 10:31:59 -0800 

Hi,

	As a further comment on the absorption correction, for a cylindrical
shaped sample and for angle dispersive instruments (i.e., not TOF, with
which I am not too familiar), the correction for absorption and extinction
can be handled separately from the structure refinement program, as it is
handled by a geometrical construct and (at least in my oppinion) it should
never have refinable parameters.  I think that there is a program called
something like CORRECT that will do this.

	For my lab X-rays, the diamond powder thing works very well.  LiF
also works well, but gives lots more lines.  However, LiF is a lot cheaper,
and usually readily available.

	AlexY


Dr. Alexandre F. T. Yokochi
Assistant Professor (Senior Research)
Director, X-ray Crystallographic Facilities
Department of Chemistry
Oregon State University
Corvallis, OR 97331-4003

Ph#  (541) 737-6724 Email: [email protected]
Fax# (541) 737-2062 Web Page: www.chem.orst.edu/yokochi


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