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NASA NTRS1985

Horizons and Opportunities in Lunar Sample Science

The Moon is the cornerstone of planetary science. Lunar sample studies were fundamental in developing an understanding of the early evolution and continued development of planetary bodies, and have led to major revisions in understanding of processes for the accumulation of planetesimals and the formation of planets. Studies of lunar samples have increased an understanding of impact cratering, meteoroid and micrometeoroid fluxes, the interaction of planetary surfaces with radiations and particles, and even the history of the Sun. The lunar sample research program was especially productive, but by no means have all the important answers been determined; continued study of lunar samples will further illuminate the shadows of our knowledge about the solar system. Further, the treasures returned through the Apollo program provide information that is required for a return to the Moon, beginning with new exploration (Lunar Geoscience Observer (LGO)), followed by intensive study (new sample return missions), and eventually culminating in a lunar base and lunar resource utilization. The few years during and following Apollo were a hectic time for lunar science. Since then, considerable maturation of the science and distinct changes in the mode of operation have developed. Funding (and hence the number of investigators) has naturally declined. Studies have become far more problem-oriented than descriptive. Many sample investigators have shifted their sights away from planetary evolution, for which the Moon holds considerable information, toward processes and materials in the pre-planetary solar nebula, for which the Moon has no direct evidence. Nonetheless, unique scientific opportunities are still supplied by the samples returned from the Apollo and Luna missions and by lunar meteorites. These 382 kg of samples constitute a priceless resource that still has enormous scientific potential. Continued interaction between NASA and the scientific community, especially through the advice of groups such as the Lunar and Planetary Sample Team (LAPST), is essential in maintaining the current level of excellence of the program. LAPST has reviewed its role, the role of the sample research community, and the perceived role of future researchers over the next decade in ensuring the effective use of lunar sample studies in space exploration and exploitation. The review encompasses: (I) lunar sample science; (2) lunar materials applications; (3) lunar sample studies and their relation to future space missions; and (4) lunar sample curation. Plans in all four areas are summarized in this document.

Source record↗

NASA NTRS2000

Mission Design Overview for Mars 2003/2005 Sample Return Mission

In May 2003, a new and exciting chapter in Mars exploration will begin with the launch of the first of three spacecraft that will collectively contribute toward the goal of delivering samples from the Red Planet to Earth. This mission is called Mars Sample Return (MSR) and will utilize both the 2003 and 2005 launch opportunities with an expected sample return in October 2008. NASA and CNES are major partners in this mission. The baseline mission mode selected for MSR is Mars orbit rendezvous (MOR), analogous in concept to the lunar orbit rendezvous (LOR) mode used for Apollo in the 1960s. Specifically, MSR will employ two NASA-provided landers of nearly identical design and one CNES-provided orbiter carrying a NASA payload of rendezvous sensors, orbital capture mechanisms, and an Earth entry vehicle (EEV). The high-level concept is that the landers will launch surface samples into Mars orbit, and the orbiter will retrieve the samples in orbit and then carry them back to Earth. The first element to depart for Mars will be one of the two landers. Currently, it is proposed that an intermediate class launch vehicle, such as the Boeing Delta 3 or Lockheed Martin Atlas 3A, will launch this 1800-kg lander from Cape Canaveral during the May 2003 opportunity. The lander will utilize a Type-1 transfer trajectory with an arrival at Mars in mid-December 2003. Landing will be aided by precision approach navigation and a guided hypersonic entry to achieve a touchdown accuracy of 10 km or better. Although the exact landing site has not yet been determined, it is estimated that lander resource constraints will limit the site to between 15 degrees north and south latitudes. Following touchdown, the lander will deploy a six-wheeled, 60-kg rover carrying an extensive suite of instruments designed to aid in the analysis of the local terrain and collection of core samples from selected rocks. The surface mission is currently designed around a concept called the surface traverse. Each traverse will involve the rover exploring a selected area of terrain up to 100 meters from the lander, the collection of rock core samples, and the delivery of the samples from the traverse back to a sample canister on the lander. Planning estimates indicate that up to three traverses may be possible during the expected 90-sol lifetime of the lander. The canister that will receive the samples from the rover will be attached to the top stage of a small solid-fueled rocket mounted to the deck of the lander. This rocket is called the Mars Ascent Vehicle (MAV) and consists of three stages weighing a total of about 140 kg. After the conclusion of the surface mission, the MAV will lift-off and insert the sample canister into a near-circular orbit with an altitude of about 600 km and inclination of 45 degrees. The sample canister will wait in this orbit until it is retrieved by the orbiter sometime in early 2007. In August 2005, the second lander and a CNES-provided orbiter weighing 2700 kg will depart for Mars. Currently, it is proposed that a single Ariane 5 provided by CNES will launch both of these two elements onto a Type-2 transfer trajectory. Although the orbiter and lander will be launched together, they will separate shortly after injection and will fly to Mars as two independent spacecraft. However, both spacecraft will perform a maneuver between 10 and 15 days after launch so that their arrival times at Mars differ by between 12 and 24 hours. This scheme will reduce the operational complexity at the encounter date. A set of four 60-kg surface probes will ride piggyback on the orbiter to Mars. These CNES-provided probes are called Netlanders and will serve as surface stations for scientific investigations independent of the Mars Sample Return goals. Starting approximately one month prior to arrival at Mars, the orbiter will begin to release the Netlanders one at a time. Each release cycle will take several days, and will include time for precision navigation to execute one or two maneuvers that will target the Netlanders to their proper landing site. All four deployment cycles will be completed prior to 10 days before arrival. Both the orbiter and lander will arrive in late-July 2006. Upon arrival, the lander will perform a precision landing and surface mission similar in concept to the one that was executed during the 2003 opportunity. Although the landing site for the 2005 opportunity has not been selected, it is expected to be different from the 2003 site to enhance the diversity of the collected samples. The orbiter's arrival at Mars will be highlighted by the first use of aerocapture to insert a spacecraft into a capture orbit around another planet. The choice of aerocapture, as opposed to a propulsive orbit insertion, was considered mission enabling due to a reduction of over 2000 m/s in mission AV. Aerocapture will be targeted to produce a 250 km x 1400 km capture orbit with an inclination of 45 degrees. Current analysis indicates that achieving this goal will require approximately six minutes of flight deep in the atmosphere with a targeted periapsis of approach of about 43 km. After factoring into account the penalty for carrying a heat shield to survive aerocapture, the net savings compared to a propulsive orbital insertion amounts to several hundred kilograms.

Lee, Wayne J.↗

NASA NTRS2000

NEA Multi-Chamber Sample Return Container with Hermetic Sealing

A sample return container is being developed by Honeybee Robotics to receive samples from a derivative of the Champollion/ST4 Sample Acquisition and Transfer Mechanism or other samplers such as the 'Touch and Go' Surface Sampler (TGSS), and then hermetically seal the samples for a sample return mission. The container is enclosed in a phase change material (PCM) chamber to prevent phase change during return and re-entry to earth. This container is designed to operate passively with no motors and actuators. Using the rotation axis of the TGSS sampler for interfacing, transferring and sealing samples, the container consumes no electrical power and therefore minimizes sample temperature change. The circular container houses multiple isolated canisters, which will be sealed individually for samples acquired from different sites or depths. The TGSS based sampler indexes each canister to the sample transfer position, below the index interface for sample transfer. After sample transfer is completed, the sampler indexes a seal carrier, which lines up seals with the openings of the canisters. The sampler moves to the sealing interface and seals the sample canisters one by one. The sealing interface can be designed to work with C-seals, knife edge seals and cup seals. This sample return container is being developed by Honeybee Robotics in collaboration with the JPL Exploration Technology program. A breadboard system of the sample return container has been recently completed and tested. Additional information is contained in the original extended abstract.

Rafeek, Shaheed↗

NASA NTRS2000

A Sample Return Container with Hermetic Seal

A sample return container is being developed by Honeybee Robotics to receive samples from a derivative of the Champollion/ST4 Sample Acquisition and Transfer Mechanism or other samplers and then hermetically seal samples for a sample return mission. The container is enclosed in a phase change material (PCM) chamber to prevent phase change during return and re-entry to earth. This container is designed to operate passively with no motors and actuators. Using the sampler's featured drill tip for interfacing, transfer-ring and sealing samples, the container consumes no electrical power and therefore minimizes sample temperature change. The circular container houses a few isolated canisters, which will be sealed individually for samples acquired from different sites or depths. The drill based sampler indexes each canister to the sample transfer position, below the index interface for sample transfer. After sample transfer is completed, the sampler indexes a seal carrier, which lines up seals with the openings of the canisters. The sampler moves to the sealing interface and seals the sample canisters one by one. The sealing interface can be designed to work with C-seals, knife edge seals and cup seals. Again, the sampler provides all sealing actuation. This sample return container and co-engineered sample acquisition system are being developed by Honeybee Robotics in collaboration with the JPL Exploration Technology program.

Kin Yuen Kong↗

NASA NTRS2009

Device Acquires and Retains Rock or Ice Samples

The Rock Baller is a sample acquisition tool that improves sample retention. The basic elements of the Rock Baller are the tool rotation axis, the hub, the two jaws, and the cutting blades, which are located on each of the jaws. The entire device rotates about the tool rotation axis, which is aligned parallel to the nominal normal direction of the parent rock surface. Both jaws also rotate about the jaw axis, which is perpendicular to the tool rotation axis, at a rate much slower than the rotation about the tool rotation axis. This movement gradually closes the jaws into a nearly continuous hemispherical shell that encloses the sample as it is cut from the parent rock. When required the jaws are opened to release the sample. The hemispherical cutting method eliminates the sample retention problems associated with existing sample acquisition methods that employ conventional cylindrical cutting. The resulting samples are hemispherical, or nearly hemispherical, and as a result the aspect ratio (sample depth relative to sample radius) is essentially fixed. This fixed sample aspect ratio may be considered a drawback of the Rock Baller method, as samples with a higher aspect ratio (more depth, less width) may be considered more scientifically valuable because such samples would allow for a broader inspection of the geological record. This aspect ratio issue can be ameliorated if the Rock Baller is paired with a device similar to the Rock Abrasion Tool (RAT) used on the Mars Exploration Rovers. The RAT could be used to first grind into the surface of the parent rock, after which the Rock Baller would extract a sample from a depth inside the rock that would not have been possible without first using the RAT. Other potential applications for this technology include medical applications such as the removal of tissue samples or tumors from the body, particularly during endoscopic, laparoscopic, or thoracoscopic surgeries.

Giersch, Louis R.↗

NASA NTRS2014

X-Ray Micro-Computed Tomography of Apollo Samples as a Curation Technique Enabling Better Research

X-ray micro-computed tomography (micro-CT) is a technique that has been used to research meteorites for some time and many others], and recently it is becoming a more common tool for the curation of meteorites and Apollo samples. Micro-CT is ideally suited to the characterization of astromaterials in the curation process as it can provide textural and compositional information at a small spatial resolution rapidly, nondestructively, and without compromising the cleanliness of the samples (e.g., samples can be scanned sealed in Teflon bags). This data can then inform scientists and curators when making and processing future sample requests for meteorites and Apollo samples. Here we present some preliminary results on micro-CT scans of four Apollo regolith breccias. Methods: Portions of four Apollo samples were used in this study: 14321, 15205, 15405, and 60639. All samples were 8-10 cm in their longest dimension and approximately equant. These samples were micro-CT scanned on the Nikon HMXST 225 System at the Natural History Museum in London. Scans were made at 205-220 kV, 135-160 microamps beam current, with an effective voxel size of 21-44 microns. Results: Initial examination of the data identify a variety of mineral clasts (including sub-voxel FeNi metal grains) and lithic clasts within the regolith breccias. Textural information within some of the lithic clasts was also discernable. Of particular interest was a large basalt clast (approx.1.3 cc) found within sample 60639, which appears to have a sub-ophitic texture. Additionally, internal void space, e.g., fractures and voids, is readily identifiable. Discussion: It is clear from the preliminary data that micro-CT analyses are able to identify important "new" clasts within the Apollo breccias, and better characterize previously described clasts or igneous samples. For example, the 60639 basalt clast was previously believed to be quite small based on its approx.0.5 sq cm exposure on the surface of the main mass. These scans show the clast to be approx.4.5 g, however (assuming a density of approx.3.5 g/cc). This is large enough for detailed studies including multiple geo-chronometers. This basalt clast is of particular interest as it is the largest Apollo 16 basalt, and it is the only mid-TiO2 basalt in the Apollo sample suite. By identifying the location of interesting clasts or grains within a sample, we will be able to make more informed decisions about where to cut a sample in order to best expose clasts of interest for future study. Moreover, knowing the location of internal defects (e.g., fractures) will allow more precise chipping and extraction of clasts or grains. By combining micro-CT scans with compositional techniques like micro x-ray fluorescence (particularly on sawn slabs), we will be able to provide even more comprehensive information to scientists trying to best select samples that fit their scientific needs.

Ziegler, R. A.↗

NASA NTRS2018

Curating NASA's Past, Present, and Future Extraterrestrial Sample Collections

As codified in NASA Policy Directive 7100.10F, the Astromaterials Acquisition and Curation Office at NASA Johnson Space Center (hereafter JSC Curation) is charged with curation of all extraterrestrial material under NASA control, including future NASA missions. JSC Curation curates all or part of nine astromaterial collections in seven clean room suites: (1) Apollo Samples (1969; ISO 6-7), (2) Luna Samples (from USSR; 1972; ISO 7), (3) Antarctic Meteorites (1976; ISO 7), (4) Cosmic Dust (1981; ISO 5), (5) Microparticle Impact Collection (formerly called Space Exposed Hardware; 1985; ISO 5), (6) Genesis Solar Wind Atoms (2004; ISO 4); (7) Stardust Comet Particles (2006; ISO 5), (8) Stardust Interstellar Particles (2006; ISO 5), (9) Hayabusa Asteroid Particles (from JAXA; 2010; ISO 5). In addition to the labs that house the samples, we have installed and maintained a wide variety of facilities and infrastructure required to support the clean-rooms: more than 10 different HEPA-filtered air-handling systems, ultrapure dry gaseous nitrogen systems, an ultrapure water system (UPW) and cleaning facilities to provide clean tools and equipment for the labs. We also have sample preparation facilities for making thin sections, microtome sections, and even focused ion-beam (FIB) sections to meet the research requirements of scientists. To ensure that we are keeping the samples as pristine as possible, we routinely monitor the cleanliness of our clean rooms and infrastructure systems. This monitoring includes: daily monitoring of the quality of our UPW, weekly airborne particle counts in the labs, monthly monitoring of the stable isotope composition of the gaseous N2 system, and annual measurements of inorganic or organic contamination in processing cabinets. We track within our databases the current and ever-changing characteristics of more than 250,000 individual samples across our various collections (including the 19,141 samples on loan to 433 Principal Investigators in 24 countries). The next sample return missions that NASA will participate in are Hayabusa2 and OSIRIS-REx (Origins Spectral Interpretation Resource Identification Security - Regolith Explorer). The designs for a new state-of-the-art suite of clean rooms to house these samples at JSC have been finalized. This includes separate ISO class 5 clean rooms to house each collection, a common ISO class 7 area for general use, an ISO class 7 microtome laboratory, and a separate thin section lab. Additionally, a new cleaning facility is being designed and procedures developed that will allow for enhanced cleaning of cabinets and tools in an inorganically, organically, and biologically clean manner. We are also designing a large multi-purpose Advanced Curation laboratory that will allow us to develop the techniques necessary to fully support the Hayabusa2 and OSIRIS-REx missions, as well as future possible sample return missions (e.g., Lunar Polar Volatiles, Mars, Comet Surface). A micro-CT (micro Computed Tomography) laboratory dedicated to the study of astromaterials has come online within JSC Curation, and we plan to add additional facilities that will enable non-destructive (or minimally-destructive) analyses of astromaterials in the near future (e.g., micro-XRF (micro X-Ray Fluorescence), confocal imaging Raman Spectroscopy). These facilities will be available to: (1) develop sample handling and storage techniques for future sample return missions, (2) be utilized by PET (Positron Emission Tomography) for future sample return missions, (3) for retroactive PET-style analyses of our existing collections, and (4) for periodic assessments of the existing sample collections.

Zeigler, Ryan A.↗

DOE OSTI2017

Purpose-Built UAVs for Physical Sampling of Trace Contamination at the Portsmouth Gaseous Diffusion Plant - 17331

The sampling of trace amounts of contamination, particularly of low-energy byproducts such as americium, presents a challenge for non-contact sensing. In many cases, such as determining the need for cleaning inside the exhaust shaft of the Waste Isolation Pilot Plant or sampling the walls of the enormous Gaseous Diffusion Plant at Portsmouth, it may be desirable to take physical swab samples at carefully distributed sample locations for analysis by mass spectrometry. Because of the danger posed to human workers in such scenarios, including risk of falls from lethal heights and exposure to low levels of radiation and the hassle of donning and doffing PPE, a low-cost robotic solution is desired. The inaccessibility of the heights involved suggest Unmanned Aerial Vehicle (UAV) solutions, rather than Unmanned Ground Vehicle (UGV) solutions, but conventional quadrotor UAVs are ill-suited to precise physical interaction with their surroundings. Quadrotors are under-actuated, rendering them non-holonomic and preventing the dexterous application of arbitrary generalized force/torques in interaction with the environment. At Purdue University, the authors have developed a number of novel UAV platforms suitable for dexterous interaction with the environment, making them ideal for such applications. These platforms can independently control forces in all directions, allowing for controlled application of the swab to the surface. Because of the scale of these structures (over 2 km in the case of the Gaseous Diffusion Plant), flight efficiency is of supreme importance. The Purdue team is took a variety of vehicles to the Gaseous Diffusion Plant for field trials on site in August, 2016. (With results available prior to the meeting.) The Purdue Dexterous Hexrotor is a fully-actuated Hexrotor capable of exerting forces in all six directions of force and torque. Operating alone or in swarms, the Dexterous Hexrotor can fly in free space, transition to contact through impact control, and sample the surface through force control. The Purdue I-BoomCopter is a tri-copter with an extra horizontal propeller that enables long-distance flight without pitching and the ability to apply closed-loop forces horizontally. Finally, the Purdue Tiltrotor VTOL is an under-actuated hybrid UAV that combines tilting rotors for vertical takeoff and landing, with a fixed-wing, flying-body design that is ultra-efficient for long-distance flight. The Dexterous Hexrotor provided two demonstrations of physical sampling of walls and crane rails. In sampling the large open sections of the inside of the plant, a small swarm of three UAVs is commanded to sample three distinct points on an internal map of the building. Human-supervised autonomy permits the UAVs to take off by themselves, find a clear elevation at which to fly through uncluttered space, navigate to their designated sampling points, and pause for confirmation by the human supervisor. The supervisor is presented with a video image of the intended sampling spot, which, if confirmed, the UAV will automatically approach and sample. The UAVs then autonomously return to the take-off spot. The second demo involved a single UAV searching upwards, then transitioning into 3-D SLAM mode to wait for a safe sampling spot on the 3-D scan to acquire the sample from the crane rail. The human supervisor, in this case, is responsible for ensuring the absence of cables and other obstacles. I-BoomCopter demonstrated its high-speed, long-distance coverage ability by making a few fast passes before homing in on a mock-up electrical panel with door, which it opened and closed. The dexterity of the I-BoomCopter results from its large propellers, which allow for controlled hovering and the horizontal thruster for applying forces of significant magnitude. Finally, the Tiltrotor VTOL is highly efficient in fixed-wing mode, but the tilt-rotor is under-actuated in hover. The tilt-rotor will take off vertically, then transition to high-speed, long-distance flight to make a number of passes inside the facility. The significance of these demos is the low-cost implementation of physical sampling over prescribable locations in difficult-to-reach areas of potentially contaminate facilities. To make this tractable over very large facilities, the demonstration of combinations of dexterous hovering ability and long-distance/high-speed flight is also in evidence. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2015

An Open Port Sampling Interface for Liquid Introduction Atmospheric Pressure Ionization Mass Spectrometry

RATIONALE: A simple method to introduce unprocessed samples into a solvent for rapid characterization by liquid introduction atmospheric pressure ionization mass spectrometry has been lacking. The continuous flow, self-cleaning open port sampling interface introduced here fills this void. METHODS: The open port sampling interface used a vertically aligned, co-axial tube arrangement enabling solvent delivery to the sampling end of the device through the tubing annulus and solvent aspiration down the center tube and into the mass spectrometer ionization source via the commercial APCI emitter probe. The solvent delivery rate to the interface was set to exceed the aspiration rate creating a continuous sampling interface along with a constant, self-cleaning spillover of solvent from the top of the probe. RESULTS: Using the open port sampling interface with positive ion mode APCI and a hybrid quadrupole time of flight mass spectrometer, rapid, direct sampling and analysis possibilities are exemplified with plastics, ballpoint and felt tip ink pens, skin, and vegetable oils. These results demonstrated that the open port sampling interface could be used as a simple, versatile and self-cleaning system to rapidly introduce multiple types of unprocessed, sometimes highly concentrated and complex, samples into a solvent flow stream for subsequent ionization and analysis by mass spectrometry. The basic setup presented here could be incorporated with any self-aspirating liquid introduction ionization source (e.g., ESI, APCI, APPI, ICP, etc.) or any type of atmospheric pressure sampling ready mass spectrometer system. CONCLUSIONS: The open port sampling interface provides a means to introduce and quickly analyze unprocessed solid or liquid samples with liquid introduction atmospheric pressure ionization source without fear of sampling interface or ionization source contamination.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2016

Evaluating Composite Sampling Methods of Bacillus Spores at Low Concentrations

Restoring facility operations after the 2001 Amerithrax attacks took over three months to complete, highlighting the need to reduce remediation time. The most time intensive tasks were environmental sampling and sample analyses. Composite sampling allows disparate samples to be combined, with only a single analysis needed, making it a promising method to reduce response times. We developed a statistical experimental design to test three different composite sampling methods: 1) single medium single pass composite: a single cellulose sponge samples multiple coupons; 2) single medium multi-pass composite: a single cellulose sponge is used to sample multiple coupons; and 3) multi-medium post-sample composite: a single cellulose sponge samples a single surface, and then multiple sponges are combined during sample extraction. Five spore concentrations of Bacillus atrophaeus Nakamura spores were tested; concentrations ranged from 5 to 100 CFU/coupon (0.00775 to 0.155CFU/cm 2 , respectively). Study variables included four clean surface materials (stainless steel, vinyl tile, ceramic tile, and painted wallboard) and three grime coated/dirty materials (stainless steel, vinyl tile, and ceramic tile). Analysis of variance for the clean study showed two significant factors: composite method (p-value < 0.0001) and coupon material (p-value = 0.0008). Recovery efficiency (RE) was higher overall using the post-sample composite (PSC) method compared to single medium composite from both clean and grime coated materials. RE with the PSC method for concentrations tested (10 to 100 CFU/coupon) was similar for ceramic tile, painted wall board, and stainless steel for clean materials. RE was lowest for vinyl tile with both composite methods. Statistical tests for the dirty study showed RE was significantly higher for vinyl and stainless steel materials, but significantly lower for ceramic tile. These results suggest post-sample compositing can be used to reduce sample analysis time when responding to a Bacillus anthracis contamination event of clean or dirty surfaces.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2012

Analysis of the Tank 5f Final Characterization Samples-2011

The Savannah River National Laboratory (SRNL) was requested by SRR to provide sample preparation and analysis of the Tank 5F final characterization samples to determine the residual tank inventory prior to grouting. Two types of samples were collected and delivered to SRNL: floor samples across the tank and subsurface samples from mounds near risers 1 and 5 of Tank 5F. These samples were taken from Tank 5F between January and March 2011. These samples from individual locations in the tank (nine floor samples and six mound Tank 5F samples) were each homogenized and combined in a given proportion into 3 distinct composite samples to mimic the average composition in the entire tank. These Tank 5F composite samples were analyzed for radiological, chemical and elemental components. Additional measurements performed on the Tank 5F composite samples include bulk density and water leaching of the solids to account for water soluble species. With analyses for certain challenging radionuclides as the exception, all composite Tank 5F samples were analyzed and reported in triplicate. The target detection limits for isotopes analyzed were based on customer desired detection limits as specified in the technical task request documents. SRNL developed new methodologies to meet these target detection limits and provide data for the extensive suite of components. While many of the target detection limits were met for the species characterized for Tank 5F, as specified in the technical task request, some were not met. In a few cases, the relatively high levels of radioactive species of the same element or a chemically similar element precluded the ability to measure some isotopes to low levels. The Technical Task Request allows that while the analyses of these isotopes is needed, meeting the detection limits for these isotopes is a lower priority than meeting detection limits for the other specified isotopes. The isotopes whose detection limits were not met in all cases included the following: Al-26, Sn-126, Sb-126, Sb-126m, Eu-152 and Cf-249. SRNL, in conjunction with the plant customer, reviewed all these cases and determined that the impacts were negligible.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2012

Analysis of the Tank 5F Final Characterization Samples-2011 (U)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2012

DEVELOPMENT OF A TAMPER RESISTANT/INDICATING AEROSOL COLLECTION SYSTEM FOR ENVIRONMENTAL SAMPLING AT BULK HANDLING FACILITIES

Environmental sampling has become a key component of International Atomic Energy Agency (IAEA) safeguards approaches since its approval for use in 1996. Environmental sampling supports the IAEA's mission of drawing conclusions concerning the absence of undeclared nuclear material or nuclear activities in a Nation State. Swipe sampling is the most commonly used method for the collection of environmental samples from bulk handling facilities. However, augmenting swipe samples with an air monitoring system, which could continuously draw samples from the environment of bulk handling facilities, could improve the possibility of the detection of undeclared activities. Continuous sampling offers the opportunity to collect airborne materials before they settle onto surfaces which can be decontaminated, taken into existing duct work, filtered by plant ventilation, or escape via alternate pathways (i.e. drains, doors). Researchers at the Savannah River National Laboratory and Oak Ridge National Laboratory have been working to further develop an aerosol collection technology that could be installed at IAEA safeguarded bulk handling facilities. The addition of this technology may reduce the number of IAEA inspector visits required to effectively collect samples. The principal sample collection device is a patented Aerosol Contaminant Extractor (ACE) which utilizes electrostatic precipitation principles to deposit particulates onto selected substrates. Recent work has focused on comparing traditional swipe sampling to samples collected via an ACE system, and incorporating tamper resistant and tamper indicating (TRI) technologies into the ACE system. Development of a TRI-ACE system would allow collection of samples at uranium/plutonium bulk handling facilities in a manner that ensures sample integrity and could be an important addition to the international nuclear safeguards inspector's toolkit. This work was supported by the Next Generation Safeguards Initiative (NGSI), Office of Nonproliferation and International Security (NIS), National Nuclear Security Administration (NNSA).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2014

Pneumatic Microvalve-Based Hydrodynamic Sample Injection for High-Throughput, Quantitative Zone Electrophoresis in Capillaries

A hybrid microchip/capillary CE system was developed to allow unbiased and lossless sample loading and high throughput repeated injections. This new hybrid CE system consists of a polydimethylsiloxane (PDMS) microchip sample injector featuring a pneumatic microvalve that separates a sample introduction channel from a short sample loading channel and a fused silica capillary separation column that connects seamlessly to the sample loading channel. The sample introduction channel is pressurized such that when the pneumatic microvalve opens briefly, a variable-volume sample plug is introduced into the loading channel. A high voltage for CE separation is continuously applied across the loading channel and the fused silica capillary separation column. Analytes are rapidly separated in the fused silica capillary with high resolution. High sensitivity MS detection after CE separation is accomplished via a sheathless CE/ESI-MS interface. The performance evaluation of the complete CE/ESI-MS platform demonstrated that reproducible sample injection with well controlled sample plug volumes could be achieved by using the PDMS microchip injector. The absence of band broadening from microchip to capillary indicated a minimum dead volume at the junction. The capabilities of the new CE/ESI-MS platform in performing high throughput and quantitative sample analyses were demonstrated by the repeated sample injection without interrupting an ongoing separation and a good linear dependence of the total analyte ion abundance on the sample plug volume using a mixture of peptide standards. The separation efficiency of the new platform was also evaluated systematically at different sample injection times, flow rates and CE separation voltages.

Eletrophoresis↗

DOE OSTI2022

Analysis of DWPF Sludge Batch 6 (Macrobatch 7): Pour Stream Glass Samples

The Defense Waste Processing Facility (DWPF) began processing Sludge Batch 6 (SB6), also referred to as Macrobatch 7 (MB7), in June 2010. SB6 is a blend of the heel of Tank 40 from Sludge Batch 5 (SB5), H-Canyon Np transfers and SB6 that was transferred to Tank 40 from Tank 51.1 SB6 was processed using Frit 418. Sludge is received into the DWPF Chemical Processing Cell (CPC) and is processed through the Sludge Receipt and Adjustment Tank (SRAT) and Slurry Mix Evaporator Tank (SME). The treated sludge slurry is then transferred to the Melter Feed Tank (MFT) and fed to the melter. During processing of each sludge batch, the DWPF is required to take at least one glass sample to meet the objectives of the Glass Product Control Program (GPCP) and to complete the necessary Production Records so that the final glass product may be disposed of at a Federal Repository. The DWPF requested various analyses of radioactive glass samples obtained from the melter pour stream during processing of SB6 as well as reduction/oxidation (REDOX) analysis of MFT samples to determine the impact of Argon bubbling. Sample analysis followed the Task Technical and Quality Assurance Plan (TTQAP) and an Analytical Study Plan (ASP). Four Pour Stream (PS) glass samples and two MFT slurry samples were delivered to the Savannah River National Laboratory (SRNL) from the DWPF. Table 1-1 lists the sample information for each pour stream glass sample. SB6 PS3 (S03472) was selected as the official pour stream sample for SB6 and full analysis was requested. This report details the visual observations of the as-received SB6 PS No.3 glass sample as well as results for the chemical composition, Product Consistency Test (PCT), radionuclide content, noble metals, and glass density. REDOX results will be provided for all four pour stream samples and vitrified samples of MFT-558 and MFT-568A. Where appropriate, data from other pour stream samples will be provided.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2012

Analysis of the Tank 5F Final Characterization Samples-2011 (U)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2016

Analysis of Tank 38H (HTF-38-16-80, 81) and Tank 43H (HTF-43-16-82, 83) Samples for Support of the Enrichment Control and Corrosion Control Programs

SRNL analyzed samples from Tank 38H and Tank 43H to support ECP and CCP. The total uranium in the Tank 38H surface sample was 57.6 mg/L, while the sub-surface sample was 106 mg/L. The Tank 43H samples ranged from 50.0 to 51.9 mg/L total uranium. The U-235 percentage was consistent for all four samples at 0.62%. The total uranium and percent U-235 results appear consistent with recent Tank 38H and Tank 43H uranium measurements. The Tank 38H plutonium results show a large difference between the surface and sub-surface sample concentrations and somewhat higher concentrations than previous samples. The Pu-238 concentration is more than forty times higher in the Tank 38H sub-surface sample than the surface sample. The surface and sub-surface Tank 43H samples contain similar plutonium concentrations and are within the range of values measured on previous samples. The four samples analyzed show silicon concentrations somewhat higher than the previous sample with values ranging from 104 to 213 mg/L.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2019

Analysis of Tank 38H (HTF-38-19-18, -19) and Tank 43H (HTF-43-19-20, -21) Samples for Support of the Enrichment Control and Corrosion Control Programs

SRNL analyzed samples from Tank 38H and Tank 43H to support ECP and CCP. Overall, the results of the analysis indicate the concentrations of species in the Tank 38H surface sample increased significantly from the previous sample with the sodium concentration increasing from 1.09 M in the previous sample to 3.19 M in the current sample. However, it should be noted that the previous Tank 38H surface sample was very dilute compared with typical Tank 38H samples of the recent past. The Tank 38H sub-surface sample shows a composition fairly similar to the previous sample’s composition. Both the Tank 43H surface and sub-surface samples appear slightly more dilute than the previous samples based on the sodium concentrations. For both Tank 38H and Tank 43H, the subsurface samples appear slightly more concentrated for most species than the surface samples. These results indicate some success in increasing the salt solution concentration and reducing stratification in Tank 38H, but some stratification is still evident in both Tank 38H and Tank 43H.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗