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Radiochemical Processing Laboratory

Spectroscopic Capabilities

FTIR Spectrometer with Microscopy Capability
FTIR Spectrometer with Microscopy Capability

The RPL is equipped with a variety of state-of-the-art spectroscopic equipment for applications to both radioactive and non-radioactive materials. These capabilities include:

  • Fourier transform infrared spectrometers, including an infrared microscope.
  • A tunable argon ion pumped, Ti:Sapphire Raman system.
  • Fiber optic Raman and UV-Vis spectroscopic systems.

These instruments are routinely used for studies on highly radioactive materials such as tank waste and spent fuel and can be modified for specific characterization. Limits on radioactive materials use are typically dependent on sample dispersibility and sample dose. Procedures are in place for proper sample immobilization and reduced exposure handling. Furthermore, procedures can be quickly modified to accommodate higher dose conditions.

Infrared spectroscopy is routinely used for identification of organic and inorganic materials. A number of projects have recently utilized RPL spectrometers for the infrared spectra of new O17, N15 labeled radioactive inorganic salts. The RPL currently houses three Nicolet 750 infrared spectrometers with tandem IR/TGA (Seiko 5200) and IR/ mass spectroscopy (Extrel) capability. The TGA/mass spectroscopic experiment is available as well. These have been used to understand binding phenomena and decomposition kinetics of pure materials but are also commonly used to understand complex systems such as Hanford tank wastes and high concentration Pu bearing mixtures.

A Nicolet infrared microscope has been used for surface characterization of crystalline and amorphous materials. The microscope is set up as an external accessory to the main infrared bench and can be used in reflectance or transmission mode. The spectrometer also has photoacoustic and depth profiling capability.

Raman Spectrometer and Optical Bench
Raman Spectrometer and Optical Bench

The RPL has two instruments to carry out Raman spectroscopy experiments. The first is an Ocean Optics spectrometer, which uses the output of a 100 mWatt cw laser at 532 nm. Both the laser and collection optics are contained in a probe that is coupled to the spectrometer by fiberoptic cable. The probe and sample positioners are enclosed in a laser safe aluminum box. The instrument is routinely used for thin film, solids, and solution measurements. The second Raman instrument is a laser-based system, which provides experimental versatility. The system includes a Spex 500 M monochrometer capable of 0.02 nm resolution, and a liquid nitrogen cooled Spex CCD array detector. The argon laser can be used in multi-line or single line mode and can be used to pump a Lexel (479) Ti:sapphire laser. The Ti:sapphire laser potentially provides tuning from the blue end of the spectrum to beyond 1 micron and therefore allows the resonance Raman experiment as well as numerous other modifications, such as fluorescence experiments.

Speciation and kinetic studies of highly radioactive materials in solution are routinely carried out using a fiber-optic based UV-VIS spectrometer. The instrument uses a CCD array detector and is equipped with standard tungsten and deuterium lamps for wavelength scans from 350 nm to 980 nm. The most commonly used setup is the dip probe. The probe material is inert over a wide range of pH and is immersed directly into solution. Solutions can be measured in standard cuvettes as well; furthermore accessories are available that will allow this equipment to be used to investigate solids by reflectance measurements.

Point of Contact:
Sam Bryan, Radiochemical Science Team
Phone: (509) 375-5648

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A National Asset with Multiple Missions
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