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Description of the Round Robin SamplesThe SDPDRR Homepage is at http://www.cristal.org/SDPDRR/
 In order to help you to decide which method will be necessary, here
are the characteristics of both samples and all patterns (you may decide
to cope with only one of them). All data was collected at room temperature
:
 
 
 
Sample 1[Co(NH3)5CO3]NO3.H2OKindly supplied by Zhu Jianghai, Center for Analysis &  Measurement
Fudan University Shanghai.
 
Patterns:
Crystal system: monoclinic 
Cell : a = 7.673A, b = 9.628 A, c = 7.077 A, beta = 106.28° 
Space groups : P21/m or P21  
Pattern 1a) China - Highly packed sample
3 conventional X-ray (Cu K-alpha) 
Bragg Brentano  (minimal FWHM ~ 0.12° 2-theta)
 
Pattern 1b) Le Mans - Side-loaded sample
holder
Filename: Zhu1.*
Run on Rigaku D/max-B 
Rotating Anode Cu 
Wavelengths: 1.54056 and 1.54439 A 
Generator Power: 120mA, 40KV 
Goniometer Radius: 185mm 
Divergence Slit: 0.5°
Receiving Slit Aperture: 0.15mm 
Sollers Slit Acceptance Angle: 0.5° 
Diffracted Beam Monochromator: flat graphite crystal 
Start, Step, Stop: 10.06, 0.02, 120.04 
Counting time: 30sec/step 
Vertical Sample Holder: 20x20mm sample surface
No spinning (minimal FWHM ~ 0.13° 2-theta)
 
Pattern 1c) Le Mans - Sample dusted through
a sieve: free of preferred orientation (FWHM ~ 0.25° 2-theta)
Filename: Zhu2.*
Run on Siemens D501 
Tube Type Siemens Cu FF
Wavelengths: 1.54056 and 1.54439 A 
Generator Power: 28mA, 38KV 
Goniometer Radius: 200.5mm 
Divergence Slit: 0.3° 
Receiving Slit Aperture: 0.05° 
Sollers Slit Acceptance Angle: 2°
Diffracted beam curved graphite monochromator
Start, Step, Stop: 10.00, 0.02, 130.04 
Counting time: 24 seconds per point 
Horizontal Sample Holder: 40 x 20mm sample surface 
No Spinning 
Filename: zhu3.*
Run on Siemens D501, 
Tube Type Siemens Cu FF
Wavelengths: 1.54056 and 1.54056 A 
Generator Power: 28mA, 38KV 
Goniometer Radius: 200.5mm 
Divergence Slit: 1° 
Receiving Slit Aperture: 0.15° 
Sollers Slit Acceptance Angle: 2°
Diffracted beam curved graphite monochromator
Start, Step, Stop: 10.00, 0.02, 119.68 
Counting time: 28 seconds per point. 
Horizontal Sample Holder: 40 x 20mm sample surface
No Spinning 
 
Sample 2C22H24N2O8HClPharmaceutical :From the Aldrich Chemical Company Inc.
 Milwaukee, WI 53233 USA
 Reference : 25,016-3     [64-75-5]
 Tetracycline Hydrochloride 98%, 25g
 Lot : TQ
 No. : 14219PQ
 For laboratory use only.
 
Patterns:
Crystal system: orthorhombic 
Cell : a = 10.981 A, b = 12.853 A,c = 15.733 A,
Space group : P212121  
Pattern 2a) Le Mans - using a side-loaded
sample holder (minimal FWHM ~ 0.15° 2-theta)
Conventional X-ray (Cu K-alpha) - Bragg Brentano 
Capillary/Image-Plate system  
Pattern 2b) Daresbury - Beamline 9.1 -
Spinning Capillary run on Developmental Image Plate System (minimal FWHM
~ 0.05° 2-theta)
Filename: aldxconv.*
Run on Siemens D501 
Tube Type Siemens Cu FF 
Wavelengths: 1.54056 and 1.54439 A 
Generator Power: 28mA, 38KV 
Goniometer Radius: 200.5mm 
Divergence Slit: 0.3° 
Receiving Slit Aperture: 0.05° 
Sollers Slit Acceptance Angle: 2° 
Diffracted beam curved graphite monochromator 
Start, Step, Stop: 10.06, 0.02, 120.04 
Counting time: 48 sec./point 
Horizontal Sample Holder: 40x20 mm sample surface
No Spinning 
Filename: aldsync.* 
Run on Graham Bushnell-Wye, et al. 
Beam width and height: 0.5mmx0.5mm X-ray beam 
Wavelength: 0.692 A 
Distance from Sample to curved image plate: 350 mm 
Start, Step, Stop: 2.115, 0.005, 40.000 
Counting time: 5 hours 
Sample Holder: Sample packed in 0.5mm glass capilliary, 
References: 
"Development of Curved Image-Plate Techniques for Studies of Powder Diffraction,
Liquids and Amorphous Materials",M.A. Roberts, J. L. Finney, G. Bushnell-Wye
 Proceedings of EPDIC-5, Parma, Italy, 1997.
 
"Developments and Time-Resolved Studies using a Curved Image-Plate Detector",M.A. Roberts, J. L. Finney, G. Bushnell-Wye, W. A. Steer, Manuscript
in Preparation.
 
 Copyright ©
1998
L.M.D Cranswick &
A.
Le Bail
 
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