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NASA NTRS1999

The Mars Environmental Compatibility Assessment (MECA)

The Mars Environmental Compatibility Assessment (MECA) will evaluate the Martian environment for soil and dust-related hazards to human exploration as part of the Mars Surveyor Program 2001 Lander. Sponsored by the Human Exploration and Development of Space (HEDS) enterprise, MECA's goal is to evaluate potential geochemical and environmental hazards that may confront future martian explorers, and to guide HEDS scientists in the development of high fidelity Mars soil simulants. In addition to objectives related to human exploration, the MECA data set will be rich in information relevant to basic geology, paleoclimate, and exobiology issues. The integrated MECA payload contains a wet-chemistry laboratory, a microscopy station, an electrometer to characterize the electrostatics of the soil and its environment, and arrays of material patches to study the abrasive and adhesive properties of soil grains. MECA is allocated a mass of 10 kg and a peak power usage of 15 W within an enclosure of 35 x 25 x 15 cm (figures I and 2). The Wet Chemistry Laboratory (WCL) consists of four identical cells that will accept samples from surface and subsurface regions accessible to the Lander's robotic arm, mix them with water, and perform extensive analysis of the solution. Using an array of ion-specific electrodes (ISEs), cyclic voltammetry, and electrochemical techniques, the chemistry cells will wet soil samples for measurement of basic soil properties of pH, redox potential, and conductivity. Total dissolved material, as well as targeted ions will be detected to the ppm level, including important exobiological ions such as Na, K+, Ca++, Mg++, NH4+, Cl, S04-, HC03, as well as more toxic ions such as Cu++, Pb++, Cd++, Hg++, and C104-. MECA's microscopy station combines optical and atomic-force microscopy (AFM) to image dust and soil particles from millimeters to nanometers in size. Illumination by red, green, and blue LEDs is augmented by an ultraviolet LED intended to excite fluorescence in the sample. Substrates were chosen to allow experimental study of size distribution, adhesion, abrasion, hardness, color, shape, aggregation, magnetic and other properties. To aid in the detection of potentially dangerous quartz dust, an abrasion tool measures sample hardness relative to quartz and a hard glass (Zerodur).

Meloy, Thomas P.↗

NASA NTRS1999

The MSP 2001 Mars Environmental Compatibility Assessment (MECA)

A chemical analysis of soil-water mixtures and the first microscopic images of martian soil will be among the results to be returned by the Mars Environmental Compatibility Assessment (MECA) payload on the Mars Surveyor Program 2001 Lander. Sponsored by the Human Exploration and Development of Space (HEDS) enterprise, MECA's primary goal is to evaluate potential geochemical and environmental hazards that may confront future martian explorers, and to guide HEDS scientists in the development of high fidelity Mars soil simulants. As a survey of soil properties, the MECA data set will also be rich in information relevant to basic geology, paleoclimate, and exobiology. The integrated MECA payload contains a wet-chemistry laboratory, a microscopy station, an electrometer to characterize the electrostatics of the soil and its environment, and arrays of material patches to study the abrasive and adhesive properties of soil grains. MECA is allocated a mass of 10 kg and a peak power usage of 15 W within an enclosure of 35 x 25 x 15 cm. The Wet Chemistry Laboratory (WCL) consists of four identical cells that will accept samples from surface and subsurface regions accessible to the Lander's robotic arm, mix them with water, and perform extensive analysis of the solution. Ion-selective electrodes and related sensors will evaluate total dissolved solids, redox potential, pH, and the concentration of many soluble ions and gases. Cyclic voltammetry will address oxidants, and anodic stripping voltammetry will probe potentially hazardous trace metals. MECA's microscopy station combines optical and atomic-force microscopy (AFM) in a controlled illumination environment to image dust and soil particles from millimeters to nanometers in size. Careful selection of substrates and an abrasion tool allows experimental study of size distribution, adhesion, abrasion, hardness, color, shape, aggregation, magnetic and other properties. Mounted on the end of the robot arm, MECA's electrometer consists of four types of sensors: an electric field meter, several triboelectricity monitors, an ion gauge, and a thermometer. Tempered only by ultra-violet- light-induced ions and a low-voltage break-down threshold, the dry, cold, dusty martian environment presents an imposing electrostatic hazard to both robots and humans. In addition, the electrostatic environment is key to transport of dust and, consequently, martian meteorology. MECA will also observe natural dust accumulation on engineering materials. Viewed with the robot arm camera, the abrasion and adhesion plates are strategically placed to allow direct observation of the inter-action between materials and soils on a macroscopic scale. Materials of graded hardness are placed directly under the robot arm scoop to sense wear and soil hardness. A second array, placed on the lander deck, is deployed after the dust plume of landing has settled. It can be manipulated in a primitive fashion by the arm, first having dirt deposited on it from the scoop and subsequently shaken clean. Dust accumulation as a function of conductivity, magnetic field strength, and other parameters will be explored. The MECA instruments described above will assess potential hazards that the Martian soil might present to human explorers and their equipment. In addition, MECA will provide information on the composition of ancient surface water environments, observing microscopic evidence of geological (and biological?) processes, inferring soil and dust transport, comminution and weathering mechanisms, and characterizing soil horizons that might be encountered during excavation. Additional information is contained in the original extended abstract.

Hecht, M. H.↗

NASA NTRS2019

Sensor Analysis, Modeling, and Test for Robust Propulsion System Autonomy

An approach is presented supporting analysis, modeling, and test validation of operational flight instrumentation (OFI) that facilitates critical functions for the Space Launch System (SLS) main propulsion system (MPS). Certain types of OFI sensors were shown to exhibit highly nonlinear and non-gaussian noise characteristics during acceptance testing, motivating the development of advanced modeling and simulation (M&S) capability to support algorithm verification and flight certification. Hardware model and algorithm simulation fidelity was informed by a risk scoring metric; redesign of high-risk algorithms using test-validated sensor models significantly improved their expected performance as evaluated using Monte Carlo acceptance sampling methods. Autonomous functions include closed-loop ullage pressure regulation, pressurant leak detection, and fault isolation for automated safing and crew caution and warning (C&W).

Orr, Jeb S.↗

NASA NTRSDate not supplied

Risk-Based Methodology for the Determination of Hall Thruster Performance Specifications

This work adapts manufacturing and metrology industry standards to create a risk-based approach for the determination of electric propulsion performance specifications. The developed process is applied to 208 total thrust measurements acquired using three different NASA Hall Effect Rocket with Magnet Shielding (HERMeS) Technology Demonstration Unit (TDU) 12.5-kW Hall thrusters in three different test facilities in order to generate thrust specifications at the 300 V/6.25 kW, 400 V/8.33 kW, 500 V/10.42 kW, and 600 V/12.5 kW operating conditions. These thrust specifications are used to perform a set of sample acceptance tests to illustrate the importance of adding additional conservatism using a parameter known of the Test Accuracy Ratio in order to control the risk to the thruster producer and consumer from false rejection and acceptance of thruster units.

HERMeS↗

NASA NTRSDate not supplied

Risk-based Methodology for the Determination of Hall Thruster Performance Specifications

HERMeS↗

DOE OSTI2023

Chemical Characterization Results for Tank 40 Sludge Batch 10 Waste Acceptance Product Specifications (WAPS) Sample

A 3-L sample (HTF-40-23-24) obtained from Tank 40 following transfer of Tank 51 to achieve the final Sludge Batch 10 processing composition was received by Savannah River National Laboratory (SRNL). SRNL was tasked with characterization of the sample in accordance with requirements for reporting the Waste Acceptance Product Specifications. A representative subsample, approximately 500 mL, was prepared by continuously agitating the 3-L sample via a mixing blade inserted into the bottle. This subsample was then used for the chemical and physical characterization reported here. This characterization includes the following: (1) Supernate and slurry density; (2) Weight percent solids; (3) Mercury Analysis (supernate and slurry); (4) Anions; (5) Total Organic/Inorganic Carbon; (6) Free Hydroxide; (7) Other Base; (8) Elementals; (9) Volatile Organic Analysis and Semi-volatile Organic Analysis; and (10) Fissile Radionuclides and Uranium Enrichment. The results of this physical and chemical characterization of the sample are documented in this report.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Accelerating multilevel Markov Chain Monte Carlo using machine learning models

Here, this work presents an efficient approach for accelerating multilevel Markov Chain Monte Carlo (MCMC) sampling for large-scale problems using low-fidelity machine learning models. While conventional techniques for large-scale Bayesian inference often substitute computationally expensive high-fidelity models with machine learning models, thereby introducing approximation errors, our approach offers a computationally efficient alternative by augmenting high-fidelity models with low-fidelity ones within a hierarchical framework. The multilevel approach utilizes the low-fidelity machine learning model (MLM) for inexpensive evaluation of proposed samples thereby improving the acceptance of samples by the high-fidelity model. The hierarchy in our multilevel algorithm is derived from geometric multigrid hierarchy. We utilize an MLM to accelerate the coarse level sampling. Training machine learning model for the coarsest level significantly reduces the computational cost associated with generating training data and training the model. We present an MCMC algorithm to accelerate the coarsest level sampling using MLM and account for the approximation error introduced. We provide theoretical proofs of detailed balance and demonstrate that our multilevel approach constitutes a consistent MCMC algorithm. Additionally, we derive the expression for cost reduction due to machine learning model to facilitate cost analysis of the hierarchical sampling algorithm. Our technique is demonstrated on a standard benchmark inference problem in groundwater flow, where we estimate the probability density of a quantity of interest using a four-level MCMC algorithm. Our proposed algorithm accelerates multilevel sampling by a factor of two while achieving similar accuracy compared to sampling using the standard multilevel algorithm.

97 MATHEMATICS AND COMPUTING↗

NASA NTRS1998

How do the Properties of Allan Hills 84001 Compare With Accepted Criteria for Evidence of Ancient Life?

Criteria for Past Life: To be confident that any sample contains evidence of past life or biogenic activity, one must determine beyond a shadow of a doubt that certain well-established features or biomarker signatures are present in the sample. In the case of martian samples, the criteria for past life have not been established because if life existed on the planet, we have no way of knowing its detailed characteristics. Lacking independent evidence about the nature of possible past life on Mars, the scientific community must use, for the time being, the criteria established for ancient samples from the Earth: (1) Do we know the geologic context of the sample? Is it compatible with past life? (2) Do we know the age of the sample and its stratigraphic location? Are they understood enough to relate possible life to geologic history? (3) Does the sample contain evidence of cellular morphology? (4) What structural remains of colonies or communities exist within the samples? (5) Is there any evidence of biominerals showing chemical or mineral disequilibria? (6) Is there any evidence of stable isotope patterns unique to biology? (7) Are there any organic biomarkers present? (8) Are the features indigenous to the sample? For acceptance of past life in a geologic sample, essentially all of these criteria must he met.

Gibson, E. K., Jr.↗

NASA NTRS2017

Measuring Shock Stage of ltokawa Regolith Grains by Electron Back-Scattered Diffraction and Synchrotron X-Ray Diffraction

We have been analyzing Itokawa samples in order to definitively establish the degree of shock experienced by the regolith of asteroid Itokawa, and to devise a bridge between shock determinations by standard light optical petrography, crystal structures as determined by electron and X-ray diffraction techniques. We are making measurements of olivine crystal structures and using these to elucidate critical regolith impact processes. We use electron back-scattered diffraction (EBSD) and synchrotron X-ray diffraction (SXRD). We are comparing the Itokawa samples to L and LL chondrite meteorites chosen to span the shock scale experienced by Itokawa, specifically Chainpur (LL3.4, Shock Stage 1), Semarkona (LL3.00, S2), Kilabo (LL6, S3), NWA100 (L6, S4) and Chelyabinsk (LL5, S4). In SXRD we measure the line broadening of olivine reflections as a measure of shock stage. In this presentation we concentrate on the EBSD work. We employed JSC's Supra 55 variable pressure FEG-SEM and Bruker EBSD system. We are not seeking actual strain values, but rather indirect strain-related measurements such as extent of intra-grain lattice rotation, and determining whether shock state "standards" (meteorite samples of accepted shock state, and appropriate small grain size) show strain measurements that may be statistically differentiated, using a sampling of particles (number and size range) typical of asteroid regoliths. Using our system we determined that a column pressure of 9 Pa and no C-coating on the sample was optimal. We varied camera exposure time and gain to optimize mapping performance, concluding that 320x240 pattern pixilation, frame averaging of 3, 15 kV, and low extractor voltage yielded an acceptable balance of hit rate (>90%), speed (11 fps) and map quality using an exposure time of 30 ms (gain 650). We found that there was no strong effect of step size on Grain Orientation Spread (GOS) and Grain Reference Orientation Deviation angle (GROD-a) distribution; there was some effect on grain average Kernel Average Misorientation (KAM) (reduced with smaller step size for the same grain), as expected. We monitored GOS, Maximum Orientation Spread (MOS) and GROD-a differences between whole olivine grains and sub-sampled areas, and found that there were significant differences between the whole grain dataset and subsets, as well as between subsets, likely due to sampling-related "noise". Also, in general (and logically) whole grains exhibit greater degrees of cumulative lattice rotation. Sampling size affects the apparent strain character of the grain, at least as measured by GOS, MOS and GROD-a. There were differences in the distribution frequencies of GOS and MOS between shock stages, and in plots of MOS and GOS vs. grain diameter. These results are generally consistent with those reported this year. However, it is unknown whether the differences between samples of different shock states exceeds the clustering of these values to the extent that shock stage determinations can still be made with confidence. We are investigating this by examination of meteorites with higher shock stage 4 to 5. Our research will improve our understanding of how small, primitive solar system bodies formed and evolved, and improve understanding of the processes that determine the history and future of habitability of environments on other solar system bodies. The results will directly enrich the ongoing asteroid and comet exploration missions by NASA and JAXA, and broaden our understanding of the origin and evolution of small bodies in the early solar system, and elucidate the nature of asteroid and comet regolith.

Zolensky, Michael↗

NASA NTRS2013

Automated, Ultra-Sterile Solid Sample Handling and Analysis on a Chip

There are no existing ultra-sterile lab-on-a-chip systems that can accept solid samples and perform complete chemical analyses without human intervention. The proposed solution is to demonstrate completely automated lab-on-a-chip manipulation of powdered solid samples, followed by on-chip liquid extraction and chemical analysis. This technology utilizes a newly invented glass micro-device for solid manipulation, which mates with existing lab-on-a-chip instrumentation. Devices are fabricated in a Class 10 cleanroom at the JPL MicroDevices Lab, and are plasma-cleaned before and after assembly. Solid samples enter the device through a drilled hole in the top. Existing micro-pumping technology is used to transfer milligrams of powdered sample into an extraction chamber where it is mixed with liquids to extract organic material. Subsequent chemical analysis is performed using portable microchip capillary electrophoresis systems (CE). These instruments have been used for ultra-highly sensitive (parts-per-trillion, pptr) analysis of organic compounds including amines, amino acids, aldehydes, ketones, carboxylic acids, and thiols. Fully autonomous amino acid analyses in liquids were demonstrated; however, to date there have been no reports of completely automated analysis of solid samples on chip. This approach utilizes an existing portable instrument that houses optics, high-voltage power supplies, and solenoids for fully autonomous microfluidic sample processing and CE analysis with laser-induced fluorescence (LIF) detection. Furthermore, the entire system can be sterilized and placed in a cleanroom environment for analyzing samples returned from extraterrestrial targets, if desired. This is an entirely new capability never demonstrated before. The ability to manipulate solid samples, coupled with lab-on-a-chip analysis technology, will enable ultraclean and ultrasensitive end-to-end analysis of samples that is orders of magnitude more sensitive than the ppb goal given in the Science Instruments.

Mora, Maria F.↗

DOE OSTI2011

ISOLOK VALVE ACCEPTANCE TESTING FOR DWPF SME SAMPLING PROCESS

Evaluation of the Defense Waste Processing Facility (DWPF) Chemical Process Cell (CPC) cycle time identified several opportunities to improve the CPC processing time. Of the opportunities, a focus area related to optimizing the equipment and efficiency of the sample turnaround time for DWPF Analytical Laboratory was identified. The Mechanical Systems & Custom Equipment Development (MS&CED) Section of the Savannah River National Laboratory (SRNL) evaluated the possibility of using an Isolok{reg_sign} sampling valve as an alternative to the Hydragard{reg_sign} valve for taking process samples. Previous viability testing was conducted with favorable results using the Isolok sampler and reported in SRNL-STI-2010-00749 (1). This task has the potential to improve operability, reduce maintenance time and decrease CPC cycle time. This report summarizes the results from acceptance testing which was requested in Task Technical Request (TTR) HLW-DWPF-TTR-2010-0036 (2) and which was conducted as outlined in Task Technical and Quality Assurance Plan (TTQAP) SRNL-RP-2011-00145 (3). The Isolok to be tested is the same model which was tested, qualified, and installed in the Sludge Receipt Adjustment Tank (SRAT) sample system. RW-0333P QA requirements apply to this task. This task was to qualify the Isolok sampler for use in the DWPF Slurry Mix Evaporator (SME) sampling process. The Hydragard, which is the current baseline sampling method, was used for comparison to the Isolok sampling data. The Isolok sampler is an air powered grab sampler used to 'pull' a sample volume from a process line. The operation of the sampler is shown in Figure 1. The image on the left shows the Isolok's spool extended into the process line and the image on the right shows the sampler retracted and then dispensing the liquid into the sampling container. To determine tank homogeneity, a Coliwasa sampler was used to grab samples at a high and low location within the mixing tank. Data from the two locations were compared to determine if the contents of the tank were well mixed. The Coliwasa sampler is a tube with a stopper at the bottom and is designed to obtain grab samples from specific locations within the drum contents. A position paper (4) was issued to address the prototypic flow loop issues and simulant selections. A statistically designed plan (5) was issued to address the total number of samples each sampler needed to pull, to provide the random order in which samples were pulled and to group samples for elemental analysis. The TTR required that the Isolok sampler perform as well as the Hydragard sampler during these tests to ensure the acceptability of the Isolok sampler for use in the DWPF sampling cells. Procedure No.L9.4-5015 was used to document the sample parameters and process steps. Completed procedures are located in R&D Engineering job folder 23269.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Thermally stable and self-healable lignin-based polyester

The increased use of plastics and the associated environmental impact has catalyzed research on the development of bio-derived polymers. Bio-based polyesters have gained increased attention due to the abundance of their starting materials and ease of processing. Lignin is naturally occurring in biomass with rich carbon content, whose functionality and rigidity make it an ideal bio-derived candidate for bio-based polyesters. Herein, a lignin-based polyester with good thermal stability and self-repairability was synthesized from carboxylated lignin and epoxidized soybean oil. The synthesized lignin/epoxidized soybean oil (ESO) vitrimer was brittle such that its mechanical performance could not be recorded. However, when polyethylene glycol (PEG) was incorporated as a plasticizer, polymer samples exhibited acceptable ductility. From thermomechanical analysis of the synthesized polyesters, the plasticizer did not impair thermal stability of polymers, but greatly enhanced mechanical properties. Notably, all samples exhibited stability at high temperatures, and good glass transition temperatures (51.0 ± 0.9–78.0 ± 1.2 °C). The highest tensile strength (3.983 ± 0.1 MPa) and storage modulus (1463.67 ± 12.6 MPa) were recorded for the polyester containing 6 % w/w PEG. Moreover, the polymer samples exhibited self-healing capability at 180 °C. This work expands on valorization of lignin through the synthesis of bio-derived materials.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Statistical Sampling Plan for AGR-5/6/7 Fuel Materials

Kernels, coated particles, and compacts will be manufactured to predefined specifications for irradiation in the AGR 5/6/7 experiments. Many tests will be performed for quality assurance and most of these tests correspond to criteria that have to be met with 95% confidence, based on random samples. This report describes the statistical acceptance testing methods and gives minimum sample sizes for kernels to achieve 95% confidence. Coated particles and compacts will be addressed in revisions to this report. The methods used for sample size determination are described in detail in INL/EXT 05 00349, Statistical Methods Handbook for Advanced Gas Reactor Fuel Materials (Einerson 2005). The statistical approach is to collect a representative sample, apply an acceptance test to the sample, and accept or reject the product based on this test for each criterion. The criteria or “product specifications” are contained in SPC-1352, “AGR 5/6/7 Fuel Specification,” Revision 1 and are duplicated in this plan.

+↗

DOE OSTI2012

Adaptive Algebraic Multigrid for Finite Element Elliptic Equations with Random Coefficients

This thesis presents a two-grid algorithm based on Smoothed Aggregation Spectral Element Agglomeration Algebraic Multigrid (SA-ρAMGe) combined with adaptation. The aim is to build an efficient solver for the linear systems arising from discretization of second-order elliptic partial differential equations (PDEs) with stochastic coefficients. Examples include PDEs that model subsurface flow with random permeability field. During a Markov Chain Monte Carlo (MCMC) simulation process, that draws PDE coefficient samples from a certain distribution, the PDE coefficients change, hence the resulting linear systems to be solved change. At every such step the system (discretized PDE) needs to be solved and the computed solution used to evaluate some functional(s) of interest that then determine if the coefficient sample is acceptable or not. The MCMC process is hence computationally intensive and requires the solvers used to be efficient and fast. This fact that at every step of MCMC the resulting linear system changes, makes an already existing solver built for the old problem perhaps not as efficient for the problem corresponding to the new sampled coefficient. This motivates the main goal of our study, namely, to adapt an already existing solver to handle the problem (with changed coefficient) with the objective to achieve this goal to be faster and more efficient than building a completely new solver from scratch. Our approach utilizes the local element matrices (for the problem with changed coefficients) to build local problems associated with constructed by the method agglomerated elements (a set of subdomains that cover the given computational domain). We solve a generalized eigenproblem for each set in a subspace spanned by the previous local coarse space (used for the old solver) and a vector, component of the error, that the old solver cannot handle. A portion of the spectrum of these local eigen-problems (corresponding to eigenvalues close to zero) form the coarse basis used to define the new two-level method of our interest. We illustrate the performance of this adaptive two-level procedure with a large set of numerical experiments that demonstrate its efficiency over building the solvers from scratch.

97 MATHEMATICS AND COMPUTING↗

NASA NTRS2001

Improved Detection Technique for Solvent Rinse Cleanliness Verification

The NASA White Sands Test Facility (WSTF) has an ongoing effort to reduce or eliminate usage of cleaning solvents such as CFC-113 and its replacements. These solvents are used in the final clean and cleanliness verification processes for flight and ground support hardware, especially for oxygen systems where organic contaminants can pose an ignition hazard. For the final cleanliness verification in the standard process, the equivalent of one square foot of surface area of parts is rinsed with the solvent, and the final 100 mL of the rinse is captured. The amount of nonvolatile residue (NVR) in the solvent is determined by weight after the evaporation of the solvent. An improved process of sampling this rinse, developed at WSTF, requires evaporation of less than 2 mL of the solvent to make the cleanliness verification. Small amounts of the solvent are evaporated in a clean stainless steel cup, and the cleanliness of the stainless steel cup is measured using a commercially available surface quality monitor. The effectiveness of this new cleanliness verification technique was compared to the accepted NVR sampling procedures. Testing with known contaminants in solution, such as hydraulic fluid, fluorinated lubricants, and cutting and lubricating oils, was performed to establish a correlation between amount in solution and the process response. This report presents the approach and results and discusses the issues in establishing the surface quality monitor-based cleanliness verification.

Hornung, S. D.↗

DOE OSTI2020

Glycolate Analysis in Tank 22: Developing and Testing Analytical Methods for the Savannah River Site Liquid Waste System

Researchers developed and tested a range of techniques to support a low mg/L Limit of Quantitation (LOQ) of glycolate in radioactive Tank 22 waste solution by Ion Chromatography (IC) and by proton NMR. For the IC method, Dionex OnGuard II cartridges were tested as a means of removing alkali earth and transition metals that can interfere during ion chromatography applications especially when analyzing for low-concentration, chelating analytes. Additionally, concentrations of nitrate in the raw Tank 22 sample (5,000 to 10,000 mg/L) were managed by using reasonable levels of sample dilution. The resulting IC performance quality was enhanced by improving the baseline, increasing sensitivity [Limit of Quantitation (LOQ) of 12 mg/L and Limit of Detection (LOD) of 4.0 mg/L], and resolving analytes into well-defined Gaussian peaks when using the Dionex OnGuard II H⁺ cartridges to remove matrix interferences. High concentrations of nitrate limited the performance of the IC method. To achieve an acceptable baseline, samples with high nitrate content require more dilution, resulting in higher detection limits. Tests on samples with higher concentrations of nitrate (Tank 30 and 32 supernate with approximately 150000 mg/L nitrate) suggested that IC detection limits for glycolate in these samples would be > 500 mg/L. Thus, an LOQ of 12 mg/L is not feasible by this IC method on evaporator feed samples. An alternative method of glycolate analysis, using proton nuclear magnetic resonance (H NMR), was developed by the research team. In initial tests, the H NMR technique provided reasonable quantitation of glycolate in Tank 22 conditions by direct observation of the liquid. The H NMR method may provide improved detection limits for solutions with higher nitrate concentrations. We recommend further development of this analysis for high nitrate LWS samples such as evaporator feed and evaporator drop tank content. A method for pretreatment of samples using crystalline silicotitanate (CST) was developed and tested. The objective of the pretreatment was to facilitate analysis of samples with higher levels of radioactivity. The pretreatment did not influence the glycolate concentration in solution, and the pretreatment is projected to reduce Cs 137 activity in a sample by a factor of 16,200. The double strike CST pretreatment was demonstrated and would allow milliliters of higher activity samples to be transferred from the Shielded Cells and handled in a containment unit for glycolate analysis. The various studies validated IC and H NMR methods for glycolate analysis, defined the range of applicability, and demonstrated key supporting analytical protocols. Based on the results, high quality glycolate analysis of Tank 22 is feasible down to approximately 12 mg/L, with the potential for broader applicability of the methods to other conditions in the Savannah River Site Liquid Waste System (LWS).

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2017

Recent Bremsstrahlung-based Assays of 210Pb in Lead and Comments on Current Availability of Low-Background Lead in North America

Abstract Low-background lead for radiation measurement shielding is often assayed for 210Pb to ensure acceptable backgrounds. Samples of lead assayed with a germanium spectrometer calibrated for bremsstrahlung-based assay of 210Pb provide a view into the 210Pb content of commercial lead in the U.S. (other than stockpiled Doe Run lead). Results suggest that the loss of lead smelting in the U.S. has eliminated the traditional supply of “low background” lead (~30 Bq·kg-1), and indicate current commercial supplies contain roughly an order of magnitude higher 210Pb levels.

Low background, gamma spectroscopy, lead, bremsstr↗

DOE OSTI2015

The effect of ultraviolet irradiation on the ultra-thin HfO{sub 2} based CO gas sensor

In this work, an effort has been made to fabricate ultrathin HfO{sub 2}/Al{sub 2}O{sub 3} sample by atomic layer deposition method for the fast detection of CO gas at room temperature. The effect of the operating temperature and the UV light on the gas sensing characteristics has been studied. We investigated the optimum operating temperature for the sample by sensing 25 ppm CO and CO{sub 2} gases from room temperature to 150 °C for 10 °C steps. The maximum response was obtained at 150 °C for both gases in the measurement temperature range. Also, the photoresponse measurements clearly show the effect of UV light on the sample. At room temperature, sensor showed superior response (14%) for 5 ppm CO gas. The response time of sensor is 6 s to 5 ppm CO gas concentration. The ultrathin HfO{sub 2} based sample shows acceptable gas sensitivity for 5 ppm CO gas at room temperature under UV light irradiation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗