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INE-Beamline

Background

INE / ACT - experimental stations

The INE Beamlines  (INE-Beamline and the ACT station at the CAT-ACT Beamline) at the KIT-synchrotron are dedicated to actinide research with X-ray spectroscopic techniques. Both are operated by the Institute for Nuclear Waste Disposal (INE).

INE Fig1 Immobilisation

Schematic sketch visualizing some of the actinide mobilization / retention processes possibly following actinide release from corroded HAW.

Research and development at INE are largely aimed at long term safety assessment of proposed deep geological repositories for high-level, heat producing nuclear waste (HAW) disposal. To ensure sound safety assessment, a molecular understanding of processes determinant in the fate of radionuclides, notably the actinides, and thermodynamic quantification is essential. Of central importance in such investigations is determination of actinide speciation (i.e., their chemical and physical form). X-ray spectroscopic methods have proved to be valuable tools for actinide speciation research. Investigations on non-fissile radioisotopes up to 106 times the legal exemption limit and fissile radioisotopes (Pu-239, U-235) up to 200mg, contained within two layers of protection, are possible.

The synchrotron-based activities at the INE-Beamline are embedded in INE’s in-house research, thereby allowing a combination of analytical and instrumental methods, notably laser techniques and microscopic methods.

 

In situ X-ray spectroscopic investigations on radioactive samples are routinely performed at the INE Beamlines for studying, e.g., actinide containing solid-water interface chemical reactions, not possible at other facilities. A special protocol for working with radioactive samples at both INE beamlines exists and is supervised by INE’s own radiation protection officers. The unique aspect of the INE Beamlines is its close proximity to INE’s active laboratories on-site KIT north campus. The design is for a multi-purpose beamline, where a number of methods are possible on one and the same sample.

 

The INE Beamlines serves three general functional areas:

  • Research = user facility (INE in-house, HGF NUSAFE program, via strategic research cooperation with KIT-INE)
  • Education and dissemination (maintaining nuclear competence)
  • Development & upgrades (adaption of methods, serving user needs)

 

Layout

INE-Beamline DCM insight
Lemonnier-type double crystal X-ray monochromator (DCM) developed in cooperation with the Universität Bonn (Physikalisches Institut).

INE Fig2 BL schema

INE-Beamline – layout of optics and experimental stage.

 

The compact design and pressure inside the DCM vacuum housing of ~10-6 mbar allows fast crystal changes without long pumping times (see figure beside).

The experimental station is flexibel designed to adapt different configuration setups as low energy with special chambers for sample, microfocus setup, etc... (see "experiment" for more information).

 

INE-Beamline standard setup

 

                 
                                 

                 

 


 


 


Experiment

Detectors

 

Detector Type Main specs
Fluorescence

4 element SDD Vortex (SIINT)

 

Vortex-60EX SDD (SIINT)

130 eV at 6 keV; 45 mm2 active area/element; 25 µm Be window

130 eV at 6 keV; 50 mm2 active area; 25 µm Be window

Absorption

3 ionization chambers (Poikat / Hamburg

low-energy set-up with single entrance window (Oken Ltd. ionization chambers, Japan)

window 12.5 or 25 µm KAPTON, FEMTO low current amplifiers DLPCA-200

ionization chambers and sample chamber form windowless volume – gas tight insertion of SDD into sample chamber for high quality fluorescence spectra


 

Sample holder (HUBER goniometer):

 

Movement Range
z stage 40 mm; 40 nm/step
phi circle 360°; 0.0001°/step
psi cradle 30°; 0.0001°/step
theta cradle 30°; 0.0001°/step



                    INE Fig4 microfocus
                   Setup for confocal measurements with a µ-focused beam at the INE-Beamline.

 

 

Sample environment

 

Standard holder for transmission and fluorescence measurements of radioactive and non-radioactive samples, e.g., 400 µl and 2 ml PE-tubes, pellets.

Special sample chambers for grazing incidence measurements of flat samples (up to 3 inch diameter)

Liquid sample cell for the investigation of redox labile systems under electrochemically controlled conditions

High T / pressure cell setup

Environment: atmosphere, inert gas (existing supplies: He, N2, Ar)

Liquid N2 cryostat (OI OptistatDN) for low temperature measurements


                      INE - High T /P cell

                                                  High T / pressure cell for liquid samples.

 

Methods

 

 

XAFS characterization of bulk species by XANES/EXAFS
XAFS/XRD characterization of phase - pair distribution relationships
XRF measure elemental concentrations
Surface sensitive with grazing incidence (GI) techniques
GI-XAFS characterization of surface sorbed species
X-ray reflectivity determination of surface layer thickness and roughness
X-ray standing waves characterization of surface sorbed and incorporated species
Spatial resolution with focused beam for ‘micro’ or µ-techniques
µ-XAFS chemical state imaging
µ-XRF elemental mapping
µ-XRD identification and distribution mapping of phases
Combination of methods combined X-ray methods or X-ray method combined with other techniques, e.g., laser, Raman or UV/VIS spectroscopy

 

Characteristics

Radioactive work Infrastructure and licensing for activities 106 times the legal exemption limit as well as Pu-239 and U-235 up to 200mg.
Energy range 2.1 keV - 25 keV (P to Pd K-edge, actinides up to Cf L3 edge)
Source 1.5 T Bending magnet (Ec=6keV)
Optics • Double crystal monochromator, water-cooled first crystal, mechanically coupled movement of the second crystal to ensure fixed exit, D-MOSTAB, exchangeable crystal pairs InSb(111), Si(111), Si(311), Ge(422)
• Rh coated silicon mirrors (1st mirror vertical collimating, 2nd mirror vert. and horiz. focusing)
• SESO X-ray beam position monitor
• Optical microscope for sample positioning
• Set of polycapillary half lenses (IfG) for confocal detection of sample fluorescence yield at ~25 µm spatial (3D) resolution
• Single bounce capillary lens (IfG) with long focal distance for diffraction measurements at ~35 µm lateral resolution
 
Beam size at sample position

~500µm × 500µm (standard beam size)

~25µm with secondary focusing optic

Flux at sample position ~2×1010 photons/s at Zr K-/Pu L3-edges using Ge(422)
Experimental set-up/ sample positioning

• Standard sample holders for radioactive samples, other dimensions can be accommodated
• High precision HUBER sample positioning system, goniometer cradles, and motorized auxiliary slits for both standard XAFS and surface sensitive GI techniques
• Hexapod (PI) for positioning of secondary focusing optics
• Heavy load hexapod (PI) for precise positioning of Johann spectrometer or other heavy equipment
• Liquid N2 cryostat (OI OptistatDN) for low temperature measurements
• 1.2 × 3 m2 breadboard optical table
• Sealed media feed-through chicanes and separate ventilation / filter system for experimental hutch
• Access through lock-room with hand / foot-contamination monitor
 

Experimental set-up/ detectors • Ionization chambers for nominally high energies (transmission mode)
• Ionization chambers for nominally low energies (Oken Ltd, Japan)
• Setup for total electron yield (TEY) measurements
• XRD-setup using image plates (autoradiography films)
• PIN diode to measure photon flux at sample position
• Silicon drift detector 4 elements (Vortex, SII NanoTechnology)
• Silicon drift detector (Vortex-60EX, SII NanoTechnology)
• Fully digital fluorescence detector read-out (XIA)
 
Team INE / ACT Beamline
Name Tel. E-Mail
kathy dardenneHtd0∂kit edu
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