JRP CALL information
Supported By

European Commission

CEA, Commissatiat à l'Energie Atomique, Marcoule, France

The LN1 Laboratory within the ATALANTE facility in Marcoule is dedicated to molecular chemistry of all actinides in solution, solid state and at interfaces. It brings together selected techniques to obtain structural information, speciation and thermodynamic properties. Four glove boxes are dedicated to classical chemical experiments, essential to synthesize and purify specific actinide compounds. Nine other glove boxes are used for the preparation of samples before examination by the different techniques. The experimental results can be compared with theoretical approach of phenomena, with the help of the experts in modeling in the team LILA.

Mass spectrometry: the Brucker Esquire-LC quadrupole ion trap is equipped with Electrospray Ionization, and Atmospheric Pressure Chemical Ionization interface and linked to a glove box. Positive or negative ionization modes can be used.
EI is useful for metal-ligand analysis (information on stoichiometry and stability) and APCI allows a structural identification of organic compounds.

FTIR and Raman spectrometry: FTIR vibrational spectra can be recorded with the EQUINOX 55 from Bruker. Two detector types have been installed for medium and far infrared and an ATR device is available in glove box. A LabRAM system from Dylor, equipped with optic fibers, is installed to allow Raman studies on active samples. Two excitation lasers are available (633 and 532nm). Vibrational spectrometry provides information for solid and liquid compounds: metal-ligand vibration energy, coordination of ligands around the metal.

Microcalorimetry: two Thermal Activity Monitor microcalorimeters from Thermometric with a highly stable temperature-controlled bath containing up to four calorimetry units are available, one is connected to a glove box. The sensor bulbs inserted in the units are capable of measuring heat flows in static or titration systems. Microcalorimetry provides information on heats of reaction at low level (10-1 mJ), and equilibrium constants of reactions (complexation, extraction, dilution, sorption).

Time resolved Induced laser Fluorescence Spectroscopy: specific laser line using a pulsed Nd-Yag laser (PL8000, Excel Technology), an Optical Parametric Oscillator (Sunlite, Excel technology) and a light frequency doublers (FX1, Excel Technolgy). This equipment is well suited to detect fluorescent elements like U(VI), Cm(III), Am(III)) and Eu(III) at low concentration levels. The method allows furthermore the speciation in presence of complexing ligands and the determination of hydration numbers in the first coordination shell by analyzing fluorescence lifetimes.

NMR spectrometry: Varian INOVA 400MHz equipped with three channels, wave form generator, Z-gradient and a 100W proton amplifier for solid samples decoupling. Two glove boxes, next to the magnet room, are dedicated to prepare radioactive liquid samples in the NMR tubes. 5mm broad band and reverse commercial probes, both with Z-gradient, are used. A special probe head is under study for MAS experiments with powder samples.

NMR gives access to structure of compounds, stability constants and dynamic behaviour in solids and solutions.

Diffractometry: 4 circles Brucker ASX Kappa CCD (Nonius), allowing fast data acquisition. The goniometer is equipped with a low temperature device coupled with an air drying system. An optical microscope equipped with a camera is used to fulfill the crystal selection and to introduce it in a quartz capillary. Single crystal X-ray diffraction is the key tool in elucidating the geometric structure of solid phases.


The LN1 Laboratory has been commissioned in April 2005. The work on any radionuclide is allowed with limits set by regulations and dose rates at the work bench.



Atalante facility in Marcoule


LN1 Laboratory

 

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More information

www.cea.fr

 

Contact person

Marie-Christine CHARBONNEL


The LN1 Laboratory within the ATALANTE facility in Marcoule is dedicated to molecular chemistry of all actinides in solution, solid state and at interfaces. It brings together selected techniques to obtain structural information, speciation and thermodynamic properties. Four glove boxes are dedicated to classical chemical experiments, essential to synthesize and purify specific actinide compounds. Nine other glove boxes are used for the preparation of samples before examination by the different techniques. The experimental results can be compared with theoretical approach of phenomena, with the help of the experts in modeling in the team LILA.