in-situ light scattering as a tool for sample control ... in-situ light scattering as a tool for...
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In-situ light scattering as a tool for sample control during
Small Angle Neutron Scattering
Tobias E. SchraderJülich Centre for Neutron Science, Garching, Germany.
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Deliverables
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Motivation
Komplex of a PGK enzyme Measurement of a PGK enzyme with Small Angle Neutron Scatteringfor different concentrations
Inoue, ; Biehl, R. ; Rosenkranz, T. ; Fitter, J. ; Monkenbusch, M. ;Radulescu,A. ;Farago, ; Richter, D.:Large Domain Fluctuations on 50-ns Timescale Enable Catalytic Activity in Phosphoglycerate Kinase, In: Biophysical Journal 99 (2010),
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Motivation
control of the sample quality in a short time(possible degradation behavior)
measurement of larger length scales possible(aggregates)
-> save neutron time
non-destructible method, delivering additional information on the sample
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Measurement of particle size at one freely chosen angle
Dynamic Light Scattering (DLS)
20 nm to some µm
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Dynamic Light Scattering (DLS)
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Dynamic Light Scattering (DLS)
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Static Light Scattering (SLS)
Measurement of many scattering angles (Goniometer)
angular intensity-distribution
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observable particle sizes
Static Light Scattering Small Angle Neutron Scattering
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Previous experiments using In-situ light scattering found in publications
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A high pressure cell for small angle neutron scattering up to 500 MPa in combination with light scattering to investigate liquid samples
FIG. 5. Schematic sketch of the setup which allows simultaneous SANS andDLS measurements.
Rev. Sci. Instrum. 78, 125101 2007
J. Kohlbrecher, A. Bollhalder, and R. VavrinaLaboratory for Neutron Scattering, ETH Zurich and Paul Scherrer Institut, 5232 Villigen PSI, SwitzerlandG. MeierIFF, weiche Materie, FZ-Jülich, Postfach 1913, 52428 Jülich, Germany
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New sample environment opportunities on D11
P. Lindner & R Schweins
Figure 1: DLS-SANS set-up at D11 (courtesy of Th. Nawroth, U Mainz).The red arrow marks the incident laser light direction, the blue arrowthe incident neutron beam direction and the green arrow highlightsthe stopped-flow mixing device.
ILL news - number 51 –december 2009
Mol.Pharmaceutics 2011,8, 2162-2172
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The two possible configurationsgoniometer / fibre - configuration
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advantage: possible to use sample changer
Fibre configuration
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Goniometer Configuration
advantage: many scattering angles accessible
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Goniometer Configuration
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Lab measurements
test of the set up
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Measurements
SLS data with theoretical plot on a cylindrical cuevette - not suitable for neutron scattering
sample:
Nanoparticles77,5 nm radius
result:
jump in the refractionindex leads to an
error in the SLS data
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MeasurementsDLS data
sample:
Nanoparticles(77,5 nm radius)
result:
hydrodynamicradius measured
65 – 85 nm
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combined SANS and light scattering measurements at KWS-2
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Goniometer set upgoniometer configuration at KWS2
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Measurementsgoniometer configuration at KWS2
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MeasurementsSLS data at KWS2 – goniometer configuration with rectangular cuvette - suitable for neutron scattering
sample:
Nanoparticles(7,5 nm radius)
results:
limited q-Range
jump in therefraction index
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limitet q-range (rectangular cuvette)
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Dynamic Light Scattering (goniometer configuration)
sample:
Nanoparticlesradius: 7,5 nm
result:
hydrodynamicradius:
50 nm 509 nm
Measurements
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Poor fit and poor result from SANS data alone
SANS data at KWS2 – goniometer configuration
sample:
Nanoparticles(7,5 nm radius)
result:
radius measured:18 nm
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Measurements
sample:
ST-40 Nanoparticlesradius: 7,5 nm
result:
measuredradius: 9 nm
SANS data at KWS2 – goniometer configuration
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fibre - configuration
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Fibre configuration
advantage: possible to use sample changer
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Measurementsfibre configuration at KWS2
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Measurementsfibre configuration at KWS2
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advantage: possible to use sample changer
Fibre configuration
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Measurementsfibre configuration at KWS2
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Measurementsfibre configuration at KWS2
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sample: mixture of 15 nm particles (0,36 wt%) with an artificial pollution of 799 nm particles (0,11 wt%)
Measurements
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Measurements: fibre configurationDLS data at KWS2 – fibre configuration
sample:
mix of:
Nanoparticles(7,5 nm radius)
Nanoparticles(399,5 nm radius)
result:
hydrodynamicradius measured:
392 nm
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MeasurementsSANS data at KWS2 – fibre configuration
sample:
mix of:
Nanoparticles(7,5 nm radius)
Nanoparticles(399,5 nm radius)
result:
radius measured:8,8 nm
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Summary
Dynamic Light Scattering: applicable results with goniometer-/fibre-configuration
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Summary
Dynamic Light Scattering: applicable results with goniometer-/fibre-configuration
− Static Light Scattering: significant errorToluene bath; use custom made cuvette
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Summary
Dynamic Light Scattering: applicable results with goniometer-/fibre-configuration
− Static Light Scattering: significant error Toluene bath; use custom made cuvette
In-situ measurements: additional informationdata correctionadditional scientific applications possible
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Thank you for your attention !
Thanks to:
Raimund HeiglAurel RadulescuSimon StarringerNoemi SzekelyThomas GlomannJörg Stellbrink
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Current set up