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GSAS (General Structure Analysis System) Rietveld powder diffraction and Single Crystal software
Setting up POLA or IPOLA and POLA correctly for a powder XRD system containing a diffracted beam
Graphite Monochromator in GSAS
The CCP14 Homepage is at http://www.ccp14.ac.uk
[Back to Problems and Solutions] [Back to GSAS Hints/Resources]
[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).]
[The reference to cite in any resulting publications for using EXPGUI is: B. H. Toby, EXPGUI, a graphical user interface for GSAS, J. Appl. Cryst. (2001). 34,
210-213]
About POLA and IPOLA
(Summary: Differences between the "ideal" polarisation values for a Graphite Monochromator and "rened" values
are expected due to other effects such as Mosaic spread. )
From: "Bob Von Dreele"
Subject: Difference between using POLA only and IPOLA/POLA
To: Lachlan Cranswick [l.m.d.cranswick@dl.ac.uk]
Date: Wed, 09 Oct 2002 08:58:49 -0700
The two functions are "identical" in effect but differ by
a scaling factor. IPOLA=1 is in there to match the
"traditional" Azaroff function for diffracted beam
monochromators. The difference between theory &
measurement for POLA is "expected". The IPOLA=0 function
is my adaption so that POLA is the polarized fraction.
POLA=0.50 for no polarization and POLA=1.0 for perfect
polarization nearly realized in synchrotron radiation &
vertical diffraction.
The following two methods show how to setup for the Graphite Monochromator by rening on a suitable standard. In
this case, annealed Y2O3. Users of the DBW derived CSIRO Riet7 software or Koalariet would probably feel more
at ease using the second IPOLA/POLA method. (In Koalariet, the 2-theta value is inserted).
Click here to obtain GSAS exp and data les of Y2O3 data for determining Polarisation by both methods. (Data from
the IUCr CPD Quantitative Phase Analysis Round Robin)
Philips 3020 Goniometer with PW3710 Controller (17.3cm Goniometer Radius).
Copper Long Fine Focus X-ray Tube set at 40kV and 40mA
Flat-plate Bragg-Brentano, reflection geometry
Sample backpacked into standard Philips sample holders
For non Pharmaceutical Samples: Step Scan from 5 to 150,
at 0.02 degree steps and 3 seconds per step
1 degree divergence slit
Incident beam Sollers Slit
Unspun sample
0.3mm receiving slit
Setting up POLA or IPOLA and POLA correctly for a powde... http://www.ccp14.ac.uk/solution/gsas/graphite_monochromat...
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Diffracted beam Sollers slit
1 degree scatter slit
Diffracted beam curved Graphite Monochromator
Proportional Counter
002 reection of Graphite: 2-theta with Cu X-rays = 26.603 (d=3.3480). Calculated cos^2 2-theta = 0.80
Using "POLA only method" to handle a Graphite Monochomator within GSAS
The overall advice is to determine the best polarisation value by systematic renement on an appropriate standard;
where data collected up to the angular limit of the Powder XRD (140 to 160 degrees 2-theta). It can be advisable to t
the prole with a Le Bail t, then x prole parameters, "shft" offset correction and unit cell values. Be wary that
there can be considerable correlation between the polarisation values, thermal values and the background. Using a
standard (like cubic annealed Y2O3) where peaks are well separated is advised.
First you may want to x the thermals at reasonable values, then systematically vary the POLA values and see what
this does to the R-factors.
Then you may want to repeat the above but allow the thermals to vary.
Finally, set POLA at extreme values and see if it renes with the thermals to consistent values. If the renement looks
robust, then use this value of POLA for samples generated by this diffractometer. In the following table, POLA
consistently renes to a value of 0.523(3) for this particular XRD conguration with a Graphite Monochromator.
Results from rening cubic Y2O3 using the above described strategy
POLA R F**2 Rwp Y1thermal Y2thermal O1Thermal Thermals
(fixed)
0.40 0.0745 0.1148 0.00400 0.00400 0.00800 Fixed
0.45 0.0525 0.1022 0.00400 0.00400 0.00800 Fixed
0.50 0.0333 0.0952 0.00400 0.00400 0.00800 Fixed
0.55 0.0270 0.0937 0.00400 0.00400 0.00800 Fixed
0.60 0.0377 0.0972 0.00400 0.00400 0.00800 Fixed
0.65 0.0497 0.1040 0.00400 0.00400 0.00800 Fixed
0.70 0.0624 0.1130 0.00400 0.00400 0.00800 Fixed
0.75 0.0751 0.1299 0.00400 0.00400 0.00800 Fixed

0.40 0.0551 0.1051 0.00162 0.00065 -0.00379 Refined
0.45 0.0370 0.0969 0.02763 0.00170 -0.00076 Refined
0.50 0.0264 0.0933 0.00366 0.00276 0.00177 Refined
0.55 0.0266 0.0933 0.00471 0.00382 0.00432 Refined
0.60 0.0339 0.0961 0.00576 0.00488 0.00694 Refined
0.65 0.0434 0.1006 0.00681 0.00593 0.00907 Refined
0.70 0.0526 0.1062 0.00787 0.00698 0.01112 Refined
0.75 0.0613 0.1124 0.00891 0.00800 0.01296 Refined
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Refining POLA from (and Thermals starting at Y1=0.004, Y2=0.004, O1=0.008)
0.40 0.523 0.0247 0.0930 0.00415 0.00326 0.00291 Refined
0.50 0.523 0.0248 0.0929 0.00415 0.00326 0.00292 Refined
0.75 0.523 0.0248 0.0929 0.00415 0.00326 0.00292 Refined
Background Refining POLA from 0.5 (and Thermals starting at Y1=0.004, Y2=0.004, O1=0.008)
POLA R F**2 Rwp Y1thermal Y2thermal O1Thermal Thermals
2 term Shifted Cheby 0.472 0.0345 0.1420 0.00203 0.00087 -0.00018 Refined
3 term Shifted Cheby 0.555 0.0309 0.1215 0.00537 0.00451 0.00319 Refined
4 term Shifted Cheby 0.529 0.0335 0.1124 0.00462 0.00417 0.00307 Refined
5 term Shifted Cheby 0.517 0.0327 0.1025 0.00460 0.00370 0.00268 Refined
6 term Shifted Cheby 0.532 0.0307 0.0932 0.00494 0.00452 0.00238 Refined
7 term Shifted Cheby 0.527 0.0291 0.0877 0.00490 0.00394 0.00326 Refined
8 term Shifted Cheby 0.530 0.0263 0.0850 0.00497 0.00423 0.00358 Refined
9 term Shifted Cheby 0.529 0.0252 0.0844 0.00491 0.00415 0.00307 Refined
10 term Shifted Cheby 0.529 0.0268 0.0841 0.00490 0.00415 0.00293 Refined
11 term Shifted Cheby 0.530 0.0264 0.0831 0.00495 0.00422 0.00348 Refined
12 term Shifted Cheby 0.529 0.0247 0.0829 0.00492 0.00419 0.00356 Refined
13 term Shifted Cheby 0.528 0.0250 0.0826 0.00483 0.00413 0.00383 Refined
14 term Shifted Cheby 0.530 0.0226 0.0821 0.00498 0.00424 0.00329 Refined
15 term Shifted Cheby 0.530 0.0243 0.0820 0.00507 0.00431 0.00309 Refined
16 term Shifted Cheby 0.529 0.0247 0.0809 0.00491 0.00419 0.00294 Refined
17 term Shifted Cheby 0.529 0.0245 0.0804 0.00489 0.00416 0.00308 Refined
18 term Shifted Cheby 0.528 0.0247 0.0804 0.00488 0.00415 0.00310 Refined
19 term Shifted Cheby 0.530 0.0249 0.0795 0.00501 0.00447 0.00223 Refined
20 term Shifted Cheby 0.529 0.0243 0.0793 0.00500 0.00437 0.00244 Refined
--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+--+
Using neutron derived thermals from Smrcok L, Duris P (1989) P. 375-378 - 8 term Cheby Background
POLA R F**2 Rwp Y1thermal Y2thermal O1Thermal Thermals
Refined value
0.40 0.549 0.0295 0.0862 0.00760 0.00510 0.00460 Fixed
0.45 0.549 0.0295 0.0862 0.00415 0.00326 0.00291 Fixed
0.50 0.549 0.0295 0.0862 0.00415 0.00326 0.00292 Fixed
0.55 0.549 0.0295 0.0862 0.00415 0.00326 0.00292 Fixed
0.60 0.549 0.0295 0.0862 0.00415 0.00326 0.00292 Fixed
0.65 0.549 0.0295 0.0862 0.00415 0.00326 0.00292 Fixed
0.70 0.549 0.0295 0.0862 0.00415 0.00326 0.00292 Fixed
0.75 0.549 0.0295 0.0862 0.00415 0.00326 0.00292 Fixed
Using POLA and IPOLA=1 to handle a Graphite Monochomator within GSAS
As explained above by Bob, set IPOLA to 1 (numeral one), then enter the calculated POLA value as "cos^2 2-theta"
for the monochromator. (coefcient in formula for polarisation correction when using a monochromator.)
Then for a graphite monochromator, calculate the "cos^2 2-theta" of the 002 graphite reection (For Cu X-rays this is
at an angle of 26.6 degrees 2-theta). The calculated value should be 0.80. Enter this value into the POLA eld and
rene the structure. Near the end of the renement, allow POLA to rene (which in this case renes to 0.91(1)).
Similarly to the above "POLA only method", it would be best to do similar systematics to ensure you have a robust
and reliable result.
Setting up POLA or IPOLA and POLA correctly for a powde... http://www.ccp14.ac.uk/solution/gsas/graphite_monochromat...
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[Back to Problems and Solutions] [Back to GSAS Hints/Resources]
[Generating and Manipulating Fourier Maps from Powder Data in GSAS]
[Getting back the Forplot Menu after plotting a Windows Fourier Map]
[Generating a VRML based 3D Structure and Electron Density Contour Map in GSAS]
[Viewing GSAS Fourier Contour Maps in 3rd party programs Using Scott Belmonte's GPL'd FOUE software]
[CCP14 Home: (Frames | No Frames)]
CCP14 Mirrors: [UK] | [CA] | [US] | [AU]
What's New Introduction Site Map
Search the CCP14 Download Programs
What do you want to do?
(lists of software by crystallographic method)
Tutorials Solutions
(This Webpage Page in No Frames Mode)
If you have any queries or comments, please feel free to contact the CCP14
Setting up POLA or IPOLA and POLA correctly for a powde... http://www.ccp14.ac.uk/solution/gsas/graphite_monochromat...
4 of 4 05/05/2012 14:55