dear Natale,

I think a combination of Gandolfi spinning and 2D detector could indeed be interesting!
Both reorientation and detector height matter:

J Applied Crystallography (1994) 27: 855-859.

best

Miguel


---
michele gregorkiewitz
Dip Scienze Fisiche, della Terra e dell'Ambiente
Università di Siena
via Laterina 8, I-53100 Siena
gre...@unisi.it, +39'0577'233810


Il 2015-07-29 15:10 Jonathan WRIGHT ha scritto:
Dear Natale

 A good quality powder pattern starts with a good quality powder.
Using a 2D area detector is probably easier than trying to align a
small sample on a Gandolfi spinner, to increase grain statistics. Also
a lower resolution instrument will have fewer problems for grain
averaging. With a 0.1x0.1x0.1 mm sample volume it can be very
difficult to find the sample again after crushing it, assuming it has
not transformed during crushing.

 The following paper has nice examples when the sample was not
crushed:

 Application of synchrotron through-the-substrate microdiffraction to
crystals in polished thin sections. J. Rius, O. Vallcorba, C.
Frontera, I. Peral, A. Crespi and C. Miravitlles
 IUCrJ (2015) 2, 452-463
 http://dx.doi.org/10.1107/S2052252515007794 [2]

 It was done in ALBA at the MSPD beamline.

 We have some practice with the 3DXRD technique at the ID11 beamline
at the ESRF, see:

 Sørensen, H. O., Schmidt, S., Wright, J. P., Vaughan, G. B. M.,
Techert, S., Garman, E. F., Oddershede, J., Davaasambuu, J.,
Paithankar, K. S., Gundlach, C. & Poulsen, H. F. (2012). Z.
Kristallogr. 227, 63–78.
 http://dx.doi.org/10.1524/zkri.2012.1438 [3]

 This approach might be useful to characterize your sample, but it is
not the Rietveld method. Another approach would be diffraction
tomography ("XRD-CT"), which has a Rietveld based variant:

 J. Appl. Cryst. (2011). 44, 1111-1119    [
doi:10.1107/S0021889811024423 ]
 Hard X-ray diffraction scanning tomography with sub-micrometre
spatial resolution: application to an annealed [gamma]-U0.85Mo0.15
particle
 H. Palancher, R. Tucoulou, P. Bleuet, A. Bonnin, E. Welcomme and P.
Cloetens

 ... or a crystal indexing based variant:

 Impurity precipitation in atomized particles evidenced by nano x-ray
diffraction computed tomography ,  Anne Bonnin, Jonathan P. Wright,
Rémi Tucoulou and Hervé Palancher
 Appl. Phys. Lett. 105, 084103 (2014);
http://dx.doi.org/10.1063/1.4894009 [4]

 Obviously I am picking the citations closest to home. Most of these
approaches should be available in most of the x-ray synchrotrons in
Europe. For ESRF the next applications deadline is the 10th September.
Plenty of time to try to measure it on Simon's 4-circle before then
:-)

 Best,

 Jon

On 29/07/2015 14:10, Natale Perchiazzi wrote:

Hola Miguel,
A Gandolfi like setup would be definitely easier. I guess you
suggest alternatevely to crush and dilute the material in a matrix?
!
Cheers Natale

Inviato da Yahoo Mail su Android [1]
-------------------------

DA:"GREGORKIEWITZ MICHAEL" <michael.gregorkiew...@unisi.it>
DATA:Mer, 29 Lug, 2015 alle 12:16
OGGETTO:Re: synchrotron beamline info

Dear Natale,

do you think about a Gandolfi like setup? Or can the fragments be
crushed?

best

Miguel

---
michele gregorkiewitz
Dip Scienze Fisiche, della Terra e dell'Ambiente
Università di Siena
via Laterina 8, I-53100 Siena
gre...@unisi.it, +39'0577'233810

Il 2015-07-29 11:33 Natale Perchiazzi ha scritto:
Dear All,
I would need to get good quality powder pattern, suitable for
Rietveld
analysys, working on mineral microcrystalline fragments with
dimensions around 0.1-0.2 mm. From your experience, which could
be an
European synchrotron beamline with a suitable experimental setup
to
get these data?
best regards Natale Perchiazzi



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[2] http://dx.doi.org/10.1107/S2052252515007794
[3] http://dx.doi.org/10.1524/zkri.2012.1438
[4] http://dx.doi.org/10.1063/1.4894009
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