instrumentation and applications of xrd2 for …instrumentation and applications of xrd2 for...
TRANSCRIPT
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Bob He, Bruker AXS
Instrumentation and Applications of XRD2 for Pharmaceutics
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This document was presented at PPXRD -Pharmaceutical Powder X-ray Diffraction Symposium
Sponsored by The International Centre for Diffraction Data
This presentation is provided by the International Centre for Diffraction Data in cooperation with the authors and presenters of the PPXRD symposia for the express purpose of educating the scientific community.
All copyrights for the presentation are retained by the original authors.
The ICDD has received permission from the authors to post this material on our website and make the material available for viewing. Usage is restricted for the purposes of education and scientific research.
ICDD Website - www.icdd.comPPXRD Website – www.icdd.com/ppxrd
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X-ray Applications for typical pharmaceutical samples
XRD & XRD2 Single Crystal
Several Grains
Powder Finished Product
Solutions
Qualitative Phase ID Ф Ф Ф Ф Ф
Quantitative Rietveld analysis
Quantitative analysis with standards
X-ray movie, Non-Ambient Ф Ф Ф Ф Ф
Structure solution, Indexing Ф
Microdiffraction/ Mapping Ф Ф Ф
Shape analysis Ф Ф Ф
HTS Ф Ф Ф
Grain-Size det. Ф Ф
%Crystallinity Ф Ф Ф Ф
- can be performed by either XRD or XRD2
Ф – better with XRD2
- accept performance and accurate results only with XRD2
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Basic Concept – XRD2
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Conventional X-ray Diffractometer
Divergence slit
Detector-slit
Tube
Antiscatterslit
Sample
Mono-chromator
Bragg-Brentano Geometry.
Scanning over 2 range to collect XRD pattern.
Corundum Powder Diffraction
0
2000
4000
6000
8000
10000
12000
14000
16000
18000
20000
20 25 30 35 40 45 50
Two Theta
Inte
nsit
y
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XRD2: Two-dimensional X-ray Diffraction
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XRD2: Single Frame from Battery Anode Collected with Vantec-500 Detector
2 coverage: 70 at 8 cm detector distance
Contains information on phase, stress, texture and grain size
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Fundamental Equations and Diffraction Vector Approach
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XRD2: Diffraction Vector as
a Function of 2 and
cos2sin
sin2sin
12cos10ss
H
l
k
h
)(
)(
)(
0
0
0
ssc
ssb
ssa
hkl
hkld
1sin20
H
ss
sin2 hkld
Laue equations with 3 lattice axes: The magnitude of the vector
Leads to Bragg law:
Introduce for XRD2:
Diffraction
condition in vector
hklHss
0
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XRD2: Sample Space and Unit Diffraction Vector
The components of the unit
vector hS in the sample
coordinates S1S2S3 is then
given by
Or
in expanded form
for Eulerian
geometry:
z
y
x
h
h
h
aaa
aaa
aaa
h
h
h
333231
232221
131211
3
2
1
)sincoscossin(sinsincos
cossincoscos)coscossinsin(sinsin1
h
)sinsincossin(cossincos
coscoscoscos)cossinsinsin(cossin2
h
h3 sin cos sin cos sin cos cos cos cos sin
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XRD2: Diffraction Vector as
a Function of
Unit vector:
Stress and strain: Texture (pole-figure):
Crystal size:
3
2
1
h
h
h
sh
jiij hh ),,,(,sin 3
1 h2
2
2
1
11coshh
h
z
y
x
h
h
h
Lh
4
i
ihkls
v
VfpN
so
s s- o
D
1
2
s
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Sources & Optics
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How to make brighter source I: Microfocus sources
Large spot
Quasi-one dimensional heat flow limits power loading
Small spot
Two dimensional heat flow (more efficient cooling)
Relative performance improved by 10 times
)2ln(
2 0max
r
TTp m
Brightness (B) is proportional to power loading (p) >99% power turns to heat and needs to be removed Power loading is higher for smaller spot focus
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ImS microfocus source
• Intensity 3x1010 X-rays/mm2-sec (Cu K)
• 8 times higher than conventional 5.4 kW rotating anode
• Typical lifetime >5 years
• High reliability
• 3 year warranty
• >300 installed
• Air-cooled
• Available in Cr, Cu, Mo, Ag
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ImS & VÅNTEC-2000 vs. Classic Set-up Corundum Comparison
Sealed Tube with Göbel Mirror
45kV, 40mA, (1800 W)
0.3mm collimator
total counts: 78K
Microsource (ImS)TM
45kV, 0.650mA, (30 W)
0.3mm collimator
total counts: 1235K
Intensity: 15.8x; Efficiency: 948x !
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NEW: Liquid metal sources
• High-speed liquid-metal-jet anode
• Anode is regenerative
• No longer limited by melting
• >500 kW/mm2 e-beam power density
• Rotating anode limited to maximum 50 kW/mm2
6/15/2016 17
E-beam
Interaction
point
Metal jet
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Source Spectrum and Brightness
Spot size
[µm, FWHM]
Voltage
[kV]
Power
[W]
Ga Kα Brightness
[Photons/(s×mm2×mrad2×line]
5 60 50 1.5×1011
10 60 100 7.6×1010
20 60 200 3.8×1010
10 20 30 40 50 600
200
400
600
800
1000
Photon Energy (keV)
Bri
gh
tne
ss (
a.u
.)
Ga Kα: 9.25 keV (Cu replacement)
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So, is it possible to put a synchrotron beamline on a table top?
• Yes, at least the equivalent of a typical present generation bending magnet beamline
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Detector
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June 15, 2016 21
LYNXEYE XE
• Silicon strip technology
• Best Energy Discriminator of any 1D detector
• 0D, 1D and 2D modes
• Ideal detector for random powders and RSMs
• No Maintenance
VANTEC 500
• Detector with the Largest Active Area
• Radiation Hard
• Can take the direct beam and strong reflections
• No Maintenance
PILATUS3 R 100K-A
• Hybrid Photon Counting (HPC) technology
• High count rate capability
• Sensitivity: Co, Cu + hard radiation (Mo, Ag)
• Active area: 83,8 x 33,5 (2.807) mm2No Maintenance
• Pixel size: 172µm (195 x 487 pixel )
Choice of Detectors: 0D/1D/2D
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Large active area: 140 mm in dia.
Frame size: 2048 x 2048 pixels 1024 x 1024 pixels 512 x 512 pixels
Pixel size: 68 mm x 68 µm 136 mm x 136 µm 272 mm x 272 µm
High sensitivity: 80% DQE for Cu
High max linear count rate: 0.9 Mcps – global; 160 kcps/reflection -local
Low background noise: <10-5 cps/pix
Maintenance-free: no re-gassing
VÅNTEC-500 – Outperforms all previous gaseous detectors.
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XRD2 : Detector Orientation:
-optimized vs. 2 optimized
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XRD2 : Choice of Detectors:
Active Area and Orientation
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optimized – 0°Mode 2 optimized – 90°Mode
June 15, 2016 26
30 mm 50 mm & offset 19deg
50 mm
10 mm & 20 deg off
XRD2 : Detector Orientation and
Distance: frames collected with Aspirin
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Sample Stage & System Configuration
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June 15, 2016 28
Centric Eulerian Cradle
• Most versatile stage on the market
• Ψ, φ, X, Y and Z are always mounted
Universal Motion Concept Stages
• Sits in front of the goniometer
• Allows more weight and travel
• UMC 1516
• Ψ, φ, X, Y and Z
• UMC 150 HTS
• Designed for Reflection and Transmission
• 96 well plates
• X, Y and Z
Accessory Attachments
• Attach directly to the XY table
• Standard Powder Adapter (included)
• Dome Temperature stages
• Capillary Attachment
• Wafer Chucks
XRD2 : Sample Stages for Various
Application
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Horizontal System
Horizontal th-2th, CEC
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No barrier between 0D/1D/2D
Vertical theta-theta, CEC for microdiffraction/stress/texture
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High-throughput Screening (HTS)
Vertical theta-theta, Reflection/Transmission
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October 2011 D8 DISCOVER 32
D8 DISCOVER High Throughput Screening
VÅNTEC-500
IµS
UMC150 HTS
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Phase Identification
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XRD2: Phase ID Measurement Geometry
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XRD2: Single Frame Covering All
Multilayer battery anode.
2 coverage: 70 at 8 cm detector distance
A single frame showing information on phase, stress, texture and grain size
2D detector is essential for In-situ measurement
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Ibuprofen Integrated to 1-D data
01.07.2011 DXC 2011 36
t Dist Beam
15 s 15cm 300 mm
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15.06.2016 37 Bruker Confidential
XRD2: Data Collection:
Acetaminophen powder Lin
(C
ps)
0
1
2
2-Theta - Scale
9 10 20 30 40
5 second data collection 30 second data collection
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XRD2: Frame Merge and Integration
4 frames at 20 cm
Merged frames 2 coverage: 100
Integrated profile for phase ID search/match
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XRD2: Mapping: API Distribution in a Pill
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Easy and accurate sample positioning without touching the sample surface
Video image of each material library spot can be automatically stored during data scan
XRD2: High throughput screening Laser/video sample alignment
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PolySNAP for Combined Analysis: Correlation among XRD, Raman and other probes
Cell display
Dendrogram
3D plots
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Particle/Crystal Size
6/15/2016 42
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15.06.2016
XRD2: Crystal Size by profile analysis:
Organic glass for food & drugs
*Courtesy of Prof. Lian Yu, U. of Wisconsin - Madison 43
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15.06.2016 44 Bruker Confidential
XRD2: Data Collection:
Acetaminophen powder
The spotty diffraction ring is due to the large crystallites compared to the sampling volume (beam size).
The number of spots on the ring is determined by crystallite size, instrumental window (-range), multiplicity of the crystal plane, and effective diffraction volume.
The size of jelly beans and candy bin determines how many you can fill.
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15.06.2016 45 Bruker Confidential
XRD2: Particle size measurement by profile analysis:
so
s s- o
D
1
2
s
For XRD2, the instrumental window is given by
)]2/sin(arcsin[cos221 D
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XRD2: Particle size measurement by profile analysis:
For XRD2 in reflection mode, the crystallite size is given by
where m is the linear absorption coefficient
For transmission mode with the incident beam perpendicular to the sample surface, the crystallite size is given by
where t is the sample thickness.
k is the instrument calibration factor or can be calculated from: if the instrument broadening in 2 direction is known.
31
2
2
)]2/sin(arcsin[cos
D
s
hkl
N
bpkd
m
31
2 )]2/sin(arcsin[cos
D
s
ihkl
N
tbpkd
31
4
3
k
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XRD2: Particle Size Analysis
1 nm 10 nm 100 nm 1 mm 10 mm 100 mm 1 mm
2 profile analysis profile analysis
particle size range in pharmaceutical systems
Scherrer equation:
cosB
Ct
Gold nano-particle
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December 8, 2010 48 15. Juni 2016 48 © Copyright Bruker Corporation. All rights reserved