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Trace Analytical and Material Characterization

Developing and supporting programs through chemical analysis, analytical methods and development, and material R&D

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  • Group Leader
  • Peter Stark
  • Deputy Group Leader
  • Dan Kelly
  • Group Office
  • (505) 667-5740

Chemical Analysis, Material R&D, and Development of Analytical Instrumentation

SEM image of UH3 grown under applied load, considered “born dense”
SEM image of UH3 grown under applied load, considered “born dense”

The Trace Analytical and Material Characterization Team in Chemistry Division's Chemical Diagnostics and Engineering group provides analytical chemistry and R&D science and engineering for a wide variety of LANL programs including Science and Engineering Campaigns, WR Pit and Detonator Production, and the Weapons Directorate. This work involves multidisciplinary staff and is materials science-based with analytical capabilities spanning the periodic table, from atomic to macroscopic length scales.

Our team develops and employs a variety of chemical analytical instrumentation (over 30 instruments), including laser induced breakdown spectroscopy (LIBS), gas chromatography mass spectrometry (GC-MS), x-ray photoelectron spectroscopy (XPS), x-ray fluorescence spectroscopy (XRF), scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS), near- and mid-Fourier transform infrared spectroscopy (FTIR), ultraviolet-visible spectroscopy (UV-vis), to name a few.

Uranium and Plutonium Corrosion Studies

Our team extensively studies the mechanisms of uranium corrosion, and the compatibility of plutonium with Pit Manufacturing materials. Recent studies of uranium hydriding have elucidated the physical properties and mechanical behavior of the growing UH3 reaction product.

Small volume reactor cells
Small Volume Reactor Cells for low temperature low pressure studies
Keyence VHX-6000 microscope measurements of topography and dimensions of hydride blisters
Keyence VHX-6000 microscope measurements of topography and dimensions of hydride blisters
SEM image of UH3 grown under applied load, considered “born dense”
SEM image of UH3 grown under applied load, considered “born dense”
The growing hydride applies 1000s of pounds and moves neighboring materials 100s of mils. Has implications on storage of uranium metal and type of containers used for storage.
The growing hydride applies 1000s of pounds and moves neighboring materials 100s of mils. Has implications on storage of uranium metal and type of containers used for storage.
Anodization: Surface treatment to promote thick oxide passivation layer. Sulfuric acid anodization increases induction period of uranium hydriding by a factor of 3
Anodization: Surface treatment to promote thick oxide passivation layer. Sulfuric acid anodization increases induction period of uranium hydriding by a factor of 3!

Uranium metal corrodes when in contact with O2 and H2 which induces stress within the metal and neighboring materials. The Chemical Diagnostics and Engineering group has the capability of investigating corrosion varying the environmental conditions of the metal and performing analytical measurements to understand the changes to the metal, neighboring materials, and environment under relevant storage conditions.

Polymeric Materials for Engineered Applications

Our team has expertise in polymeric materials used for cushioning in high-performance engineered applications. We have provided engineers and designers SME support and analysis from development to WR production. This work helps ensure process control at the production agency.

FT-IR analysis of a silicone pad; this analysis shows residual PTFE on a surface. These results led to a root cause analysis determining the production agency was using unapproved PTFE-based mold releases.
FT-IR analysis of a silicone pad; this analysis shows residual PTFE on a surface. These results led to a root cause analysis determining the production agency was using unapproved PTFE-based mold releases.

In addition to supporting current systems, we also develop technology for evaluation for future systems, often using Additive Manufacturing (AM). We have developed better aging silicone resins that are used in Direct Ink Write (DIW) technology to produce pads. In collaboration with MST-7, we are evaluating WR-production grade DIW equipment and also Selective Laser Sintering (SLS) as a method to produce complex thermoplastic components.

R&D DIW experimental setup and microscope images of a printed pad. Silicones are extruded through a 250 mm nozzle in various patterns to meet mechanical response requirements
R&D DIW experimental setup and microscope images of a printed pad. Silicones are extruded through a 250 mm nozzle in various patterns to meet mechanical response requirements.
Laser-Induced Breakdown Spectroscopy (LIBS)

Our team has developed LIBS methods for radiological material and continues to collaborate within the Chemical Diagnostics and Engineering group and Chemistry Division.

LIBS team supporting DTRA effort
LIBS team supporting DTRA effort.

LIBS is a laser-based technique that involves the use of a focused pulse laser beam to generate a microplasma. The emission from the plasma is wavelength resolved using a spectrograph/detector/computer system to determine the elemental composition of the samples of interest. We focus on building systems, optimizing COTS systems, and developing data analysis programs and user interfaces that are application specific.

A handheld LIBS unit is being developed for use in gloveboxes to quickly distinguish between uranium hydride and uranium oxide.
A handheld LIBS unit is being developed for use in gloveboxes to quickly distinguish between uranium hydride and uranium oxide.
Gas Chromatography Analysis

Our team has extensive expertise in gas chromatography (GC) methods used to support environmental protection efforts, weapons production, and exploratory weapons research. C-CDE applies a variety of detection methods to qualitatively identify and quantify compounds of interest in liquid and gas-phase sample matrices.

Gas chromatography-mass spectrometry (GC-MS) and two-dimensional GCMS (GCXGC-MS) methods have been developed to help mitigate the presence of legacy environmental contaminants present around the laboratory complex.

A GC x GC chromatogram of PCB aroclor 1254
A GC x GC chromatogram of PCB aroclor 1254 (left) analyzed on a Leco HRT+4D TOFMS with Thermal Modulation Technology (right).

Additionally, GC coupled with thermal conductivity detectors (TCD) and nitrogen-phosphorus detectors (NPD) have been used to quantify analytes of interest in gas-phase samples collected from radiolysis and thermal aging studies. Moreover, our GC-MS systems are always on standby to support emergency analyses when identification of potentially hazardous compounds is needed.

Our laboratory can assist with the detection of nearly all volatile and semi-volatile compounds using a range of unique instrumentation.

Two of our Agilent GC Systems used for analyzing analytes in pressurized and sub-atmospheric gas-phase matrices. Gases for analysis can either be pressurized, or injected under vacuum depending on sample pressure.
Two of our Agilent GC Systems used for analyzing analytes in pressurized and sub-atmospheric gas-phase matrices. Gases for analysis can either be pressurized, or injected under vacuum depending on sample pressure.
Chemical Certification and Compatibility Lab

The Chemical Certification and Compatibility Lab (C3Lab) is managed as part of the Trace Analytical and Materials Characterization Team.

Chemical Certification and Compatibility Lab (C3Lab)

C3Lab is an analytical lab operating to NAP-24A Weapons Quality policy, in support of LANL’s missions in Pit and Detonator manufacturing. This work certifies incoming materials, conducts multi-material compatibility testing, and develops new analytical capability in support of War Reserve Manufacturing at LANL.

Capabilities