Providing Lab-wide emergency response
and supporting the Lab’s weapons mission
C-CDE is home to unique experimental capabilities, spanning advanced surface science, polymer compounding, and 3D printing. Niche analytical instrumentation supports efforts in weapons materials, threat reduction, applied energy, public health, and the environment.
CDE is routinely asked to analyze uranium metal, uranium oxide, uranium hydride, and uranium nitride for chemical identification, isotopic composition, sample homogeneity, and purity. We have several different methods to characterize uranium, including laser induced breakdown spectroscopy (LIBS), laser ablation inductively coupled mass spectrometry (LA-ICP-MS), and solution ICP-MS.
Capabilities
- Chemical Processes and Applied Technologies
- Trace Analytical and Material Characterization
- Soft Matter Polymers
Techniques
This state-of-the-art 4-dimensional gas chromatography / mass spectrometry instrument, GCxGC High-Resolution Time-of-Flight Mass Spectrometer enables new methods for analyzing complex samples for organic constituents. The instrument supports R&D in analysis of polychlorinated biphenyl (PCB) contamination, inorganic polymers, biopolymers, and bacterial metabolites.
Mössbauer spectroscopy is a versatile technique used to probe the chemical environment of an element — oxidation state, magnetic environment, ligand effects, etc. The method is based on the Mössbauer effect and consists of recoil-free, resonant absorption and emission of gamma rays in solids. Combined with Doppler shifts, the hyperfine transitions between the excited and ground states of the nucleus can be probed.
X-Ray Photoelectron Spectroscopy (XPS) is a surface science technique used to measure a material’s element composition and the chemical/electronic state of atoms in the material. Operating the system at ambient pressure, enabling the study of materials in real-world conditions. This capability supports research in areas of corrosion, materials aging, fuel cells, and nuclear fuel cycle.
LA-ICP-MS (Laser Ablation Inductively Coupled Plasma Mass Spectrometry) is a robust analytical technique that requires little to no sample preparation, allowing for high throughput. A sample is analyzed directly enabling mapping capability and allowing spatial information to be maintained. The ablated material is transferred from the sample chamber via a carrier gas to the ICP-MS for ionization and detection. The technique is mostly used for trace metal analysis (ppm – low wt% level) but bulk analysis can be done with appropriate standards.
Analysis of a uranium – molybdenum alloy is shown below where the homogeneity of Mo and 235U can be seen.
CDE is often asked to analyze the purity of metals and oxides, including uranium. Isotopic composition is also important when analyzing uranium samples. Solution phase ICP-MS is a robust analytical instrument that uses an argon plasma to ionize a sample. The triple quad iCAP Q separates the elements based on m/z. Certified elemental standards and isotopic standards are used for quantification and in calculating the isotopic composition of the sample. In addition, UTEVA columns are typically utilized to separate uranium from the impurities in the sample to achieve lower limits of detection.
LIBS is a rapid, optical spectroscopy technique that uses a focused pulsed laser to ablate nanograms of material. The material is vaporized, ionized, and then emits light at characteristic wavelengths of the material sampled. With a commercial off the shelf handheld LIBS system from SciAps, we have developed a method to determine if uranium corrosion is uranium hydride or uranium oxide. The application program is on the HH LIBS and rapidly analyzes the sample to report results in second.
