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Nuclear Materials Analysis

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Chemical, Biological & Physical Sciences Chemical & Biological Signature Science Applied Physics Detection Systems Radio Chemical Analysis Radiation Detection & Nuclear Sciences Nuclear Materials Analysis

"Analytical Sciences for Nonproliferation Applications"
The Nuclear Materials Analysis Group offers world-class capabilities for advanced microscopic, trace elemental, and isotopic analysis of low level nuclear, environmental, and advanced materials. Cutting edge research is performed to advance the state of the art in these areas and to provide the highest quality measurements to serve our nation's national security, environment, energy, and scientific interests.

Key Capabilities

  • Expertise runs the gamut from radiochemical separations to mass spectrometric detection and characterization.
  • NuMAG research is primarily focused in two areas:
    • Use-inspired basic research leading to innovative radiochemical separations, new analytical methods for chemical analysis, and new instrument development.
    • Analytical services that provide state-of-the-art and one-of-a-kind results to various national security clients and nonproliferation applications.
  • Mass Spectrometry expertise includes Thermal Ionization Mass Spectrometry (TIMS), Secondary Ionization Mass Spectrometry (SIMS), and Inductively Coupled Plasma Mass Spectrometry (ICPMS), including a high-precision multi-collector, to provide unparalleled analytical services.
  • Optical and advanced microscopies are utilized to perform material selection for analysis, material characterization, and TIMS source preparation.
  • NuMAG is strategically matrixed to PNNL'S Radiochemical Analysis Group to exploit advanced radiochemical separations that purify and concentrate samples for efficient, rapid and accurate analyses.

Related Facilities

  • Clean-room capabilities (rad & non-rad)
  • "Quiet" labs for electron microscopy
  • Marine sciences lab (clean room space)
  • Mass spectrometry instrument development wing
  • WSU Triga reactor (collaborators)

Instrumentation

Separations

  • High-pressure ion chromatography (HPIC)—anion/cation—with in-line beta for orthogononal detection HPIC
  • In-line electrochemically-modulated separations

Solids Analysis Introduction

  • Femtosec and nanosec laser ablation
  • Microscopy
  • Optical microscopy/sample preparation
  • Scanning electron microscopes
  • Automated scanning electron microscopy
  • Electron microprobes
  • Micro-XRF
  • Transmission electron microscope field emission
  • Micro-XRD

Mass Spectrometry

  • Custom and commercial Thermal Ionization Mass Spectrometry (TIMS): actinide sector, negative ion sector and quadrupole
  • High Precision Isotope Ratio (MC-ICPMS and MC-TIMS)
  • Cameca 4f SIMS upgraded with bright primary source
  • Elemental ICP-mass spectrometry and ICP-optical emission spectrometry
  • ICP-MS, including quadrupole, collision cell, time-of-flight, distance-of-flight, high-resolution orbitrap
  • Noble gas isotope ratio mass spectrometry

Projects

Research projects within the Nuclear Materials Analysis Group support a variety of clients including the National Nuclear Security Administration's non-proliferation verification and detection research (NA-24) and the Department of Homeland Security Chemistry and Biology research endeavors. Additionally, the group's work enables NSD's mission to detect the production, characteristics, and movement of weapons of mass destruction and effect. Projects include:

All the Signal, All the Time
Charles Barinaga

Objective: An advanced ion detector will be developed and tested for isotopic mass spectrometry. This novel, enabling technology will have direct application to nuclear nonproliferation by improving nuclear isotope measurements - with performance enhancements in isotope coverage, sensitivity, precision, dynamic range, and background noise level. The approach depends on the unique design and development of a direct charge detection array coupled with novel, multiplexed, high-speed, low-noise electronics to produce an array ion detector capable of simultaneously monitoring a wide mass range with high sensitivity and wide dynamic range. Improved elemental and isotopic signature capability for nuclear proliferation detection and forensics will result.

Funding: NA-22
Partners: University of Arizona, Indiana University, iMAGERLABS
More information: https://labweb.pnl.gov/Pages/20110616095218.aspx

ASAT Array Detector Board and Chip

Plutonium and Uranium
Sandra Hazelton

Objective: Signal enhancement and matrix elimination are important for the analysis of actinides which often exist at very low concentrations. Separation of plutonium and uranium has been demonstrated at an oxidized glassy carbon surface by electrochemical modulation in a flow configuration (see photo). Accumulation for U and Pu can be individually controlled by application of an electrode voltage, which is used to turn deposition "on" and "off."

Funding: NA-22
Partners: Oak Ridge National Laboratory
More information:

Electrochemical modulation in a flow configuration

Material Accountability Measurements
Sandra Hazelton

Objective: Accurate and timely analysis of accountable materials such as Pu is important to nuclear safeguards, however, the complexity of spent nuclear fuel sample matrices hinders both non-destructive and destructive analyses. The objective of this project is to design a large-scale electrochemically flow cell (see photo) that can rapidly and efficiently separate large quantities Pu and U from spent nuclear fuel in a simple on-line configuration.

Funding: NA-22

Large-scale electrochemically flow cell

Multi-Collector ICP-MS for Uranium Analysis
Gregory Eiden

Objective: The project seeks to significantly improve the mass spectrometric analysis of actinides by combining breakthroughs in femtosecond (fs) laser ablation (LA) with the first multi-collector ICP/MS (MC-ICP/MS) built specifically for low level, high precision actinide analysis. This goal is being addressed by exploring quantitatively how the integrated system performs as the next generation analytical measurement tool.

PNNL NeptunePlus MC-ICP/MS Detector array
PNNL NeptunePlus MC-ICP/MS Detector array. The angled line in the figure is the focal plane of the instrument's magnetic sector. Various masses of uranium isotopes are shown along with various detectors available for their detection. These detectors include full size secondary electron multipliers (SEM), compact discrete dynode (CDD) multipliers, and Faraday Cup (FC) detectors. In some cases, 235 and 238 in the instance shown here, multiple detectors are available for detection of a given mass. Which detector is used depends on the amount of sample and thus the intensity of the ion beam to be detected. For minor abundance ion beams such as 234 in natural uranium, a Retardation Potential Quadrupole (RPQ) is available to reduce interference from nearby, intense beams (e.g., 238).

High-Resolution Mass Spectrometry (HiRes)
Charles Barinaga

Objective: The goal of High-Resolution MS for Proliferation Detection Using New Technology (HiRes) is to develop, demonstrate, evaluate, and apply novel high mass resolution techniques (instrumental and gas-phase chemical) to the determination of actinides and other signature isotopes.

Our approach is to develop a new ICP-Orbitrap MS capability by the interfacing of ICPMS with Orbitrap MS technology, as well as by the design and development of a new ICPMS interface, and by chemical resolution techniques, if necessary.

The results thus far have been three fold: ICP has been interface to LTQ-Orbitrap, various interface designs have been designed and tested, and high resolution mass separations (>200,000 m/?m) have been obtained.

Funding: NA-22

High-resolution MS for proliferation detection using new technology (HiRes)

Surrogate Nuclear Explosion Debris
Gregory Eiden

Objective: In this project, we are developing laboratory methods to produce surrogate nuclear explosion debris (SNED) that could be used for nuclear-explosion related research and development and operational program applications. A key premise of this work is that laboratory plasmas may be able to mimic the conditions found in the cooling fireball following a nuclear explosion, at least once the latter has cooled to the point where chemical bonds are thermodynamically stable.

SEM Image showing micron scale spherical particles produced in a laboratory plasma
SEM Image showing micron scale spherical particles produced in a laboratory plasma. These particles are illustrative of one form of SNED that may be of interest.

Electron Mass Spectrometry Separations
Doug Duckworth


Automation of a Particle Process
Jim McKinley


Staff Bios

Douglas C. Duckworth
Primary expertise in basic research on separations technologies for radionuclides with additional experience in the area of radiological, nuclear, biological, and chemical forensics. Background includes instrument development and applications for advancing chemical separations and analysis; developing research programs in isotopic and elemental analysis; providing technical expertise for elemental and isotopic analysis of nuclear, environmental, materials and forensic sample support services; and developing light and heavy isotope technologies to identify isotopic signatures. Duckworth's expertise has been recognized with collaborative research and/or funding from the DOE's Office of Basic Energy Sciences, Department of Homeland Security (DHS), National Institutes of Justice, and the National Nuclear Security Administration (NNSA). Duckworth's specific expertise is critical to expanding PNNL's support to the national security community in forensics and to helping NNSA and DHS deliver on their missions.

Susan McKinley
Susan McKinley is currently the Program Manager for a long-standing environmental analysis project. She is responsible for the management of technical activities, quality control, reporting, laboratory-client interaction, and finances for this project. The project performs analysis and characterization of client provided environmental samples. The work includes; sample receipt and processing, sample analysis and characterization by polarized light microscopy, electron microscopy, mass spectrometry, alpha and gamma counting, data review and data reporting. Samples are analyzed for elemental and isotopic constituents of various radioisotopes as requested by the client. Methods development work to directly support the client's analytical needs is also performed.

Dr. Gregory C. Eiden
Dr. Eiden has over 20 years experience in the development of mass spectrometry methods including nearly every type of mass analyzer in common use (time-of-flight, Paul traps, multi-sector field, quadrupole). Other areas of expertise include optical spectroscopic methods (especially resonant multi-photon ionization based spectroscopies), the chemistry of gas phase cations, plasma processing for semiconductor manufacturing, and surface analysis. His research at PNNL has focused on elemental, isotopic, and molecular mass spectrometry instrument and method development and applications. Recently, Dr. Eiden has begun exploring laboratory methods for creating synthetic nuclear debris using laboratory plasmas to create the environment of a cooling nuclear fireball. He is a co-inventor of "chemical resolution" mass spectrometry, an approach that is now recognized worldwide (1996 R&D 100 Award, 1997 Federal Laboratory Consortium Award, 2004 FLC Award for Excellence in Technology Transfer, Special Journal Issues) as a new paradigm in addressing one of the main obstacles (spectral interference) to better sensitivity in elemental and isotopic mass spectrometry.


images using scanning electron microscopy
PNNL scientists research materials that mimic the chemical and physical aspects of debris from nuclear explosions in the environment and discover signatures that can be used to prevent proliferation of nuclear weapons. Shown here is a sheet of iron exposed to a plasma flame (~8300 degrees Celsius) for several seconds. The image was taken by scientists Alison Eckberg and Ben Garcia of material created by Martin Liezers, through a project managed by Greg Eiden.

For more information, contact Douglas C. Duckworth at (509) 375-7225

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