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All sourcesNASA NTRSDOE OSTI
NASA NTRS2007

Thermal Testing and Analysis of an Efficient High-Temperature Multi-Screen Internal Insulation

Conventional multi-layer insulations exhibit excellent insulation performance but they are limited to the temperature range to which their components reflective foils and spacer materials are compatible. For high temperature applications, the internal multi-screen insulation IMI has been developed that utilizes unique ceramic material technology to produce reflective screens with high temperature stability. For analytical insulation sizing a parametric material model is developed that includes the main contributors for heat flow which are radiation and conduction. The adaptation of model-parameters based on effective steady-state thermal conductivity measurements performed at NASA Langley Research Center (LaRC) allows for extrapolation to arbitrary stack configurations and temperature ranges beyond the ones that were covered in the conductivity measurements. Experimental validation of the parametric material model was performed during the thermal qualification test of the X-38 Chin-panel, where test results and predictions showed a good agreement.

Weiland, Stefan↗
NASA NTRS2013

What Reliability Engineers Should Know about Space Radiation Effects

Space radiation in space systems present unique failure modes and considerations for reliability engineers. Radiation effects is not a one size fits all field. Threat conditions that must be addressed for a given mission depend on the mission orbital profile, the technologies of parts used in critical functions and on application considerations, such as supply voltages, temperature, duty cycle, and redundancy. In general, the threats that must be addressed are of two types-the cumulative degradation mechanisms of total ionizing dose (TID) and displacement damage (DD). and the prompt responses of components to ionizing particles (protons and heavy ions) falling under the heading of single-event effects. Generally degradation mechanisms behave like wear-out mechanisms on any active components in a system: Total Ionizing Dose (TID) and Displacement Damage: (1) TID affects all active devices over time. Devices can fail either because of parametric shifts that prevent the device from fulfilling its application or due to device failures where the device stops functioning altogether. Since this failure mode varies from part to part and lot to lot, lot qualification testing with sufficient statistics is vital. Displacement damage failures are caused by the displacement of semiconductor atoms from their lattice positions. As with TID, failures can be either parametric or catastrophic, although parametric degradation is more common for displacement damage. Lot testing is critical not just to assure proper device fi.mctionality throughout the mission. It can also suggest remediation strategies when a device fails. This paper will look at these effects on a variety of devices in a variety of applications. This paper will look at these effects on a variety of devices in a variety of applications. (2) On the NEAR mission a functional failure was traced to a PIN diode failure caused by TID induced high leakage currents. NEAR was able to recover from the failure by reversing the current of a nearby Thermal Electric Cooler (turning the TEC into a heater). The elevated temperature caused the PIN diode to anneal and the device to recover. It was by lot qualification testing that NEAR knew the diode would recover when annealed. This paper will look at these effects on a variety of devices in a variety of applications. Single Event Effects (SEE): (1) In contrast to TID and displacement damage, Single Event Effects (SEE) resemble random failures. SEE modes can range from changes in device logic (single-event upset, or SEU). temporary disturbances (single-event transient) to catastrophic effects such as the destructive SEE modes, single-event latchup (SEL). single-event gate rupture (SEGR) and single-event burnout (SEB) (2) The consequences of nondestructive SEE modes such as SEU and SET depend critically on their application--and may range from trivial nuisance errors to catastrophic loss of mission. It is critical not just to ensure that potentially susceptible devices are well characterized for their susceptibility, but also to work with design engineers to understand the implications of each error mode. -For destructive SEE, the predominant risk mitigation strategy is to avoid susceptible parts, or if that is not possible. to avoid conditions under which the part may be susceptible. Destructive SEE mechanisms are often not well understood, and testing is slow and expensive, making rate prediction very challenging. (3) Because the consequences of radiation failure and degradation modes depend so critically on the application as well as the component technology, it is essential that radiation, component. design and system engineers work togetherpreferably starting early in the program to ensure critical applications are addressed in time to optimize the probability of mission success.

DiBari, Rebecca↗
NASA NTRS1973

Multi-point release mechanism

A multi-point release mechanism used on the communications technology satellite. The mechanism is designed to jettison one large panel and to release a second panel; both panels have independent multi-point attachments to the spacecraft and require to be released in sequence. The solar array is stowed concertina fashion under 2 psi pressure to ensure that no movement occurs between the stowed folds of the array during the launch. One pair of linear pyrotechnic-actuators releases both the JBSA and the pressure plate via the release mechanism. This release mechanism has successfully passed qualification level vibration launch and thermal environment tests and has accumulated to date close to 30 successful releases.

Groskopfs, E.↗
NASA NTRS2004

Alternative Test Methods for Electronic Parts

It is common practice within NASA to test electronic parts at the manufacturing lot level to demonstrate, statistically, that parts from the lot tested will not fail in service using generic application conditions. The test methods and the generic application conditions used have been developed over the years through cooperation between NASA, DoD, and industry in order to establish a common set of standard practices. These common practices, found in MIL-STD-883, MIL-STD-750, military part specifications, EEE-INST-002, and other guidelines are preferred because they are considered to be effective and repeatable and their results are usually straightforward to interpret. These practices can sometimes be unavailable to some NASA projects due to special application conditions that must be addressed, such as schedule constraints, cost constraints, logistical constraints, or advances in the technology that make the historical standards an inappropriate choice for establishing part performance and reliability. Alternate methods have begun to emerge and to be used by NASA programs to test parts individually or as part of a system, especially when standard lot tests cannot be applied. Four alternate screening methods will be discussed in this paper: Highly accelerated life test (HALT), forward voltage drop tests for evaluating wire-bond integrity, burn-in options during or after highly accelerated stress test (HAST), and board-level qualification.

Plante, Jeannette↗
NASA NTRS2005

An Evolvable Approach to Launch Vehicles for Exploration

This paper presents ideas that may be used individually or in combination to mitigate high costs for separate developments of new crew and heavy-lift cargo launch vehicles, while providing the foundation for a highly reliable and evolvable approach to exploration. Consideration is given to reclassification of cargo for launch purposes into high value versus low value categories, rather than the presently-defined crew versus cargo categories. Objectives for the reclassification are to reduce the gap between payload mass requirements for crew and cargo payloads to better allow closure on a single moderately-sized common core vehicle to reduce development cost, achieve an economical balance between launch frequency and payload mass, and to improve total mission reliability and safety, as compared a light-weight crew vehicle and heavy cargo lift approach. Concepts to reduce design and flight qualification costs for a common core vehicle with derivatives are presented. Appropriate types and mass of cargo for each class of vehicle are identified. Utilization of existing infrastructure and flight hardware is considered to reduce costs and build on proven capabilities. The approach enables low-risk incorporation of international and commercial launch of relatively low-cost, easily replaceable assets as a means to evolve toward longer-duration and more distant missions. Benefits are identified for ground idrastructure, personnel, training, logistics, spares, and system evolution. Technology needs are compared with needs for other aspects of exploration. Technology development phasing, demonstration, and reliability growth opportunities are considered. Flexibility to adapt to future technologies such as advanced in-space propulsion is contrasted with an approach of sizing the cargo launch vehicle based on today's in-space propellants.

Cheuvront, David L.↗
DOE OSTI2024

Outcomes and Conclusions from the 2022 AM Bench Measurements, Challenge Problems, Modeling Submissions, and Conference

The Additive Manufacturing Benchmark Test Series (AM Bench) provides rigorous measurement data for validating additive manufacturing (AM) simulations for a broad range of AM technologies and material systems. AM Bench includes extensive in situ and ex situ measurements, simulation challenges for the AM modeling community, and a corresponding conference series. In 2022, the second round of AM Bench measurements, challenge problems, and conference were completed, focusing primarily upon laser powder bed fusion (LPBF) processing of metals, and both material extrusion processing and vat photopolymerization of polymers. In all, more than 100 people from 10 National Institute of Standards and Technology (NIST) divisions and 21 additional organizations were directly involved in the AM Bench 2022 measurements, data management, and conference organization. The international AM community submitted 138 sets of blind modeling simulations for comparison with the in situ and ex situ measurements, up from 46 submissions for the first round of AM Bench in 2018. Analysis of these submissions provides valuable insight into current AM modeling capabilities. The AM Bench data are permanently archived and freely accessible online. The AM Bench conference also hosted an embedded workshop on qualification and certification of AM materials and components.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Destructive PIE and Safety Testing of Six AGR-2 UO 2 Capsule 3 Compacts

The Advanced Gas Reactor (AGR) Fuel Development and Qualification Program’s second irradiation experiment (AGR-2) was irradiated in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL) from June 2010 to October 2013 (Collin 2014). The fuel compacts in this experiment held either tristructural isotropic (TRISO)-coated spherical kernels of uranium oxide (UO2) or TRISO-coated kernels containing both uranium carbide and uranium oxide phases (UCO). There were six separately monitored and controlled capsules in the AGR-2 test train. Capsule 3 held twelve compacts containing UO2-TRISO particles fabricated by BWX Technologies Nuclear Operations Group. The AGR-2 TRISO particles were fabricated in a pilot-scale fluidized-bed chemical vapor deposition (FB-CVD) furnace with a coating chamber inner diameter of 150 mm (Phillips, Barnes, and Hunn 2010), which was a change from the first irradiation experiment (AGR-1) particles that had been coated in a lab-scale FB-CVD coating system with a chamber inner diameter of 50 mm (Lowden 2006). The TRISO particles were overcoated with resinated graphite flake at Oak Ridge National Laboratory (ORNL), and the overcoated particles were pressed into one-inch-long, half-inch-diameter cylinders (Hunn, Montgomery, and Pappano 2010). Each cylindrical compact held an average of 1,543 TRISO particles with 9.6% enriched UO2 kernels that had a nominal diameter of 500 μm (Hunn, Savage, and Silva 2012). Capsule 3 compacts were irradiated to average calculated burnups of 9.01–10.69% fissions per initial metal atom (FIMA), and the average calculated fluences of fast neutrons with energies E n > 0.18 MeV were 3.05–3.53×10 25 n/m 2 (Sterbentz 2014). The calculated time-average, volume-average Capsule 3 compact temperatures were 996–1,062°C. However, Capsule 3 compact temperatures varied several hundred degrees across each compact, and the timeaverage minimum (TA min ) and time-average maximum (TA max ) temperatures were between 889–999°C and 1,072–1,105°C, respectively (Hawkes 2014). After irradiation, the AGR-2 test train was transferred from ATR to the INL Materials and Fuels Complex for inspection and disassembly (Ploger, Demkowicz, and Harp 2015). The initial inspection included dimensional metrology of the compacts and graphite fuel holders. Like all the AGR-2 compacts, the compacts in Capsule 3 shrank slightly during irradiation, as expected, with an average length reduction of 1.07–1.24% and an average diameter reduction of 0.13–0.41%. Post-irradiation examination (PIE) of the capsule components was completed to measure select fission products ( 90 Sr, 110m Ag, 134 Cs, 137 Cs, 144 Ce, and 154 Eu) outside the compacts (Stempien and Demkowicz 2020). This involved gamma counting of the graphite and graphoil spacers at the top and bottom of each capsule, acid leaching for radiochemical analysis of fission products on the metallic capsule components, and burn-leach analysis of the graphite holders. The total amount of 110mAg measured on the Capsule 3 components was 13% of the calculated capsule inventory. This was significantly lower than the amount of 110m Ag measured on the three UCO capsule components, which ranged from 32–70%. The lower 110m Ag release in Capsule 3 was likely due to lower peak temperatures compared with the UCO fuel capsules (Hawkes 2014). Measured inventories of the other select fission products were also lower in Capsule 3.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS1981

Guidelines for Line-Oriented Flight Training, Volume 1

Line-Oriented Flight Training (LOFT) is a developing training technology which synthesizes high-fidelity aircraft simulation and high-fidelity line-operations simulation to provide realistic, dynamic pilot training in a simulated line environment. LOFT is an augmentation of existing pilot training which concentrates upon command, leadership, and resource management skills. This report, based on an NASA/Industry workshop held in January, 1981, is designed to serve as a handbook for LOFT users. In addition to providing background information, guidelines are presented for designing LOFT scenarios, conducting real-time LOFT operations, pilot debriefing, and instructor qualification and training. The final chapter addressed other uses of LOFT and line-operations (or full-mission) simulation.

Lauber, J. K.↗
NASA NTRS2013

Affordable Development and Qualification Strategy for Nuclear Thermal Propulsion

Nuclear Thermal Propulsion (NTP) is a concept which uses a nuclear reactor to heat a propellant to high temperatures without combustion and can achieve significantly greater specific impulse than chemical engines. NTP has been considered many times for human and cargo missions beyond low earth orbit. A lot of development and technical maturation of NTP components took place during the Rover/NERVA program of the 60's and early 70's. Other NTP programs and studies followed attempting to further mature the NTP concept and identify a champion customer willing to devote the funds and support the development schedule to a demonstration mission. Budgetary constraints require the use of an affordable development and qualification strategy that takes into account all the previous work performed on NTP to construct an existing database, and include lessons learned and past guidelines followed. Current guidelines and standards NASA uses for human rating chemical rocket engines is referenced. The long lead items for NTP development involve the fuel elements of the reactor and ground testing the engine system, subsystem, and components. Other considerations which greatly impact the development plans includes the National Space Policy, National Environmental Policy Act, Presidential Directive/National Security Council Memorandum #25 (Scientific or Technological Experiments with Possible Large-Scale Adverse Environmental Effects and Launch of Nuclear Systems into Space), and Safeguards and Security. Ground testing will utilize non-nuclear test capabilities to help down select components and subsystems before testing in a nuclear environment to save time and cost. Existing test facilities with minor modifications will be considered to the maximum extent practical. New facilities will be designed to meet minimum requirements. Engine and test facility requirements are based on the driving mission requirements with added factors of safety for better assurance and reliability. Emphasis will be placed on small engines, since the smaller the NTP engine, the easier it is to transport, assemble/disassemble, and filter the exhaust during tests. A new ground test concept using underground bore holes (modeled after the underground nuclear test program) to filter the NTP engine exhaust is being considered. The NTP engine system design, development, test, and evaluation plan includes many engine components and subsystems, which are very similar to those used in chemical engines, and can be developed in conjunction with them Other less mature NTP engine components and subsystems (e.g., reactor) will be thoroughly analyzed and tested to acceptable levels recommended by the referenced standards and guidelines. The affordable development strategy also considers a prototype flight test, as a final step in the development process. Preliminary development schedule estimates show that an aggressive development schedule (without much margin) will be required to be flight ready for a 2033 human mission to Mars.

Gerrish, Harold P., Jr.↗
NASA NTRS2013

Affordable Development and Qualification Strategy for Nuclear Thermal Propulsion

Nuclear Thermal Propulsion (NTP) is a concept which uses a nuclear reactor to heat a propellant to high temperatures without combustion and can achieve significantly greater specific impulse than chemical engines. NTP has been considered many times for human and cargo missions beyond low earth orbit. A lot of development and technical maturation of NTP components took place during the Rover/NERVA program of the 60's and early 70's. Other NTP programs and studies followed attempting to further mature the NTP concept and identify a champion customer willing to devote the funds and support the development schedule to a demonstration mission. Budgetary constraints require the use of an affordable development and qualification strategy that takes into account all the previous work performed on NTP to construct an existing database, and include lessons learned and past guidelines followed. Current guidelines and standards NASA uses for human rating chemical rocket engines is referenced. The long lead items for NTP development involve the fuel elements of the reactor and ground testing the engine system, subsystem, and components. Other considerations which greatly impact the development plans includes the National Space Policy, National Environmental Policy Act, Presidential Directive/National Security Council Memorandum #25 (Scientific or Technological Experiments with Possible Large-Scale Adverse Environmental Effects and Launch of Nuclear Systems into Space), and Safeguards and Security. Ground testing will utilize non-nuclear test capabilities to help down select components and subsystems before testing in a nuclear environment to save time and cost. Existing test facilities with minor modifications will be considered to the maximum extent practical. New facilities will be designed to meet minimum requirements. Engine and test facility requirements are based on the driving mission requirements with added factors of safety for better assurance and reliability. Emphasis will be placed on small engines, since the smaller the NTP engine, the easier it is to transport, assemble/disassemble, and filter the exhaust during tests. A new ground test concept using underground bore holes (modeled after the underground nuclear test program) to filter the NTP engine exhaust is being considered. The NTP engine system design, development, test, and evaluation plan includes many engine components and subsystems, which are very similar to those used in chemical engines, and can be developed in conjunction with them Other less mature NTP engine components and subsystems (e.g., reactor) will be thoroughly analyzed and tested to acceptable levels recommended by the referenced standards and guidelines. The affordable development strategy also considers a prototype flight test, as a final step in the development process. Preliminary development schedule estimates show that an aggressive development schedule (without much margin) will be required to be flight ready for a 2033 human mission to Mars.

Gerrish, Harold P., Jr.↗
NASA NTRS2018

Body of Knowledge for Graphics Processing Units (GPUs)

Graphics Processing Units (GPU) have emerged as a proven technology that enables high performance computing and parallel processing in a small form factor. GPUs enhance the traditional computer paradigm by permitting acceleration of complex mathematics and providing the capability to perform weighted calculations, such as those in artificial intelligence systems. Despite the performance enhancements provided by this type of microprocessor, there exist tradeoffs in regards to reliability and radiation susceptibility, which may impact mission success. This report provides an insight into GPU architecture and its potential applications in space and other similar markets. It also discusses reliability, qualification, and radiation considerations for testing GPUs.

NASA Electronic Parts and Packaging (NEPP) Program↗
NASA NTRS2007

Radiation Test Challenges for Scaled Commerical Memories

As sub-100nm CMOS technologies gather interest, the radiation effects performance of these technologies provide a significant challenge. In this talk, we shall discuss the radiation testing challenges as related to commercial memory devices. The focus will be on complex test and failure modes emerging in state-of-the-art Flash non-volatile memories (NVMs) and synchronous dynamic random access memories (SDRAMs), which are volatile. Due to their very high bit density, these device types are highly desirable for use in the natural space environment. In this presentation, we shall discuss these devices with emphasis on considerations for test and qualification methods required.

LaBel, Kenneth A.↗
DOE OSTI2021

Draft ASME Boiler and Pressure Vessel Code Cases and Technical Bases for Use of Alloy 617 for Constructions of Nuclear Component Under Section III, Division 5

The American Society of Mechanical Engineers (ASME) Boiler and Pressure Vessel Code currently only allows five materials for use in construction of nuclear components for high temperature service. These are: 2.25Cr-1Mo and V-modified 9Cr-1Mo steels, Types 304 and 316 stainless steels and the high nickel Alloy 800H. Since 2005, the US high temperature gas-cooled reactor program has been characterizing elevated temperature mechanical properties of Alloy 617 as the leading candidate construction material for the intermediate heat exchanger. After analysis of these experimental results, along with historical data and additional results available through the Generation IV International Forum, Very High Temperature Reactor, Materials Program Management Board Materials Handbook, a draft ASME Code Case to allow nuclear construction with Alloy 617 for temperatures up to 1750°F (954°C) has been developed. This report contains the Code Case for Low Temperature Service Construction of Section III, Division 5, Subsection HB, Subpart A, Class A and Subsection HC, Subpart A, Class B components, which has been approved in Section II, Materials, and Section III, Rules for Construction of Nuclear Facility Components. Supporting technical justification for the low temperature Code Case is also included. This Code Case allows use of Alloy 617 up to 800°F (425°C). This report also contains an updated draft of a Section III, Division 5, Subsection HB, Subpart B, Class A Code Case for Alloy 617 to qualify it for use in construction of nuclear components up to 1750°F (954°C) for service life up to 100,000 hours. The draft contained in Appendix 4, subject to editorial revision and approval by the ASME Special Task Group on Alloy 617 Code Qualification, will be submitted for approval by letter ballot by the appropriate ASME Committees. The technical justification supporting the Code Case is presented in Appendix 5 of this report. This background document is part of the information package that will be submitted with the Code Case for ballot.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Summary of Leach-Burn-Leach Round-Robin Test Results

Tristructural isotropic (TRISO) coated particle fuel is of interest to multiple member states associated with the Generation IV International Forum (GIF). Qualification and acceptance testing of TRISO fuel includes the determination of particle defect fractions and impurities in the as-fabricated TRISO fuel particle and/or composited fuel form, which are typically determined using burn-leach (BL) or leach-burn-leach (LBL) analysis methods. A round-robin test focusing on LBL analysis was undertaken by the GIF Very High Temperature Reactor System Fuel and Fuel Cycle Project Management Board. Participating in this LBL round-robin test were research staff from the Institute of Nuclear and New Energy Technology (INET) in the People’s Republic of China, the Korean Atomic Energy Research Institute (KAERI) in the Republic of Korea, and Oak Ridge National Laboratory (ORNL) in the United States of America. The motivation of this LBL benchmarking exercise was to explore consistency in results generated by LBL and to elucidate the potential influence of variations in the procedures used by the participating members on the accurate determination of the measured fuel properties.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2026

Commercialization of Reflected Target Non-Intrusive Assessment (ReTNA) Tool, for Indoor Optical Analysis of Heliostats

Under HelioCon, NLR began developing a new optical measurement system, called Reflected Target Non-Intrusive Assessment (ReTNA). ReTNA has shown promise towards addressing metrology gaps for heliostat used in concentrated solar thermal (CST) plant. This project is focused on advancing this measurement system from the laboratory into industry, where it can provide valuable information for heliostat developers during research, development, and qualification of a heliostat design, and be used for quality assurance during heliostat manufacture. Over the course of this project, ReTNA was deployed at several commercial heliostat facilities. The system developed and deployed with the primary project partner, Solar Dynamics LLC, is described in detail. The report discusses each project Milestone, the ending status, the achieved value, and how these Milestones improve and qualify the ReTNA measurement tool. Finally, the final report covers the market advancements, path forward, commercial successes, and lessons learned. Final Technical report for TCF Base Technology-Specific project TCF-23-20118, Commercialization of Reflected Target Non-Intrusive Assessment (ReTNA) tool, for indoor optical analysis of Heliostats.

14 SOLAR ENERGY↗
NASA NTRS2010

NASA Aerospace Flight Battery Program: Generic Safety, Handling and Qualification Guidelines for Lithium-Ion (Li-Ion) Batteries; Availability of Source Materials for Lithium-Ion (Li-Ion) Batteries; Maintaining Technical Communications Related to Aerospace Batteries (NASA Aerospace Battery Workshop)

This NASA Aerospace Flight Battery Systems Working Group was chartered within the NASA Engineering and Safety Center (NESC). The Battery Working Group was tasked to complete tasks and to propose proactive work to address battery related, agency-wide issues on an annual basis. In its first year of operation, this proactive program addressed various aspects of the validation and verification of aerospace battery systems for NASA missions. Studies were performed, issues were discussed and in many cases, test programs were executed to generate recommendations and guidelines to reduce risk associated with various aspects of implementing battery technology in the aerospace industry. This report contains the Appendices to the findings from the first year of the program's operations.

Manzo, Michelle A.↗
NASA NTRS2005

Design and Development of the Space Technology 5 (ST5) Solar Arrays

The National Aeronautics and Space Administration's (NASA's) Space Technology 5 (ST5) is designed to flight-test the concept of miniaturized 'small size" satellites and innovative technologies in Earth's magnetosphere. Three satellites will map the intensity and direction of the magnetic fields within the inner magnetosphere. Due to the small area available for the solar arrays, and to meet the mission power requirements, very high-efficiency multijunction solar cells were selected to power the spacecraft built by NASA Goddard Space Flight Center (GSFC). This was done in partnership with the Air Force Research Lab (AFRL) through the Dual-Use Science and Technology (DUS&T) program. Emcore's InGaP/lnGaAs/Ge Advanced triple-junction (ATJ) solar cells, exhibiting an average air mass zero (AMO) efficiency of 28.0% (one-sun, 28 C), were used to populate the arrays. Each spacecraft employs 8 identical solar panels (total area of about 0.3 square meters), with 15 large-area solar cells per panel. The requirement for power is to support on-orbit average load of 13.5 W at 8.4 V, with plus or minus 5% off pointing. The details of the solar array design, development and qualification considerations, as well as ground electrical performance & shadowing analysis results are presented.

Lyons, John↗
DOE OSTI2020

Development of Direct Injection/Ionization Mass Spectrometry Methods for Whole Molecule Characterization

The objective of this work is to adapt ambient ionization mass spectrometry (AMS) techniques for the rapid analysis of intact uranium complexes, stable strontium, cerium, and explosive compounds. The methods used were “soft ionization” techniques, which facilitate the detection of whole molecule complexes. The soft ionization mass spectrometry (MS) techniques that were investigated include paper spray ionization (PSI), matrix-assisted ionization (MAI), electrospray ionization (ESI) and direct analysis in real time (DART). For the first time, PSI-MS methods were successfully developed for whole molecule uranium-containing analytes (uranyl acetate, uranyl nitrate, and uranyl-tributylphosphate complexes). This was also the first demonstration of uranium complex detection and characterization and one of the few examples of inorganic analysis using MAI techniques. Proof of concept experiments also putatively identified matrix-derived ions and ion complexes that have not previously been described in the literature. Additionally, PSI-MS on cotton swipe samples doped with a multi-element standard containing μg levels of U, Bi, Pb, Cd, Fe, and Zn were directly analyzed without purification, representing a major improvement over existing methods. Both PSI and MAI methods demonstrated limits of detection (LODs) in the 10 - 100’s ng for various uranyl species within a range of 10’s ppm - 100’s ppb, dependent on analytical method and analyte species. AMS methods were also developed for other inorganics, including Ce and Sr, and organic explosive residues to address specific challenges in environmental monitoring and forensics. Further refinement and qualification of the AMS techniques developed within this effort would lead to significant cost reduction and timeliness by facilitating the triage and queueing of samples for subsequent more sensitive and time-consuming analyses.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗