Rapid extraction and assay of uranium from environmental surface samples
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Barrett, Christopher A.↗
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Pulmonary lobe segmentation based on ridge surface sampling and shape model fitting
Purpose: Performing lobe-based quantitative analysis of the lung in computed tomography (CT) scans can assist in efforts to better characterize complex diseases such as chronic obstructive pulmonary disease (COPD). While airways and vessels can help to indicate the location of lobe boundaries, segmentations of these structures are not always available, so methods to define the lobes in the absence of these structures are desirable. Methods: The authors present a fully automatic lung lobe segmentation algorithm that is effective in volumetric inspiratory and expiratory computed tomography (CT) datasets. The authors rely on ridge surface image features indicating fissure locations and a novel approach to modeling shape variation in the surfaces defining the lobe boundaries. The authors employ a particle system that efficiently samples ridge surfaces in the image domain and provides a set of candidate fissure locations based on the Hessian matrix. Following this, lobe boundary shape models generated from principal component analysis (PCA) are fit to the particles data to discriminate between fissure and nonfissure candidates. The resulting set of particle points are used to fit thin plate spline (TPS) interpolating surfaces to form the final boundaries between the lung lobes. Results: The authors tested algorithm performance on 50 inspiratory and 50 expiratory CT scans taken from the COPDGene study. Results indicate that the authors' algorithm performs comparably to pulmonologist-generated lung lobe segmentations and can produce good results in cases with accessory fissures, incomplete fissures, advanced emphysema, and low dose acquisition protocols. Dice scores indicate that only 29 out of 500 (5.85%) lobes showed Dice scores lower than 0.9. Two different approaches for evaluating lobe boundary surface discrepancies were applied and indicate that algorithm boundary identification is most accurate in the vicinity of fissures detectable on CT. Conclusions: The proposed algorithm is effective for lung lobe segmentation in absence of auxiliary structures such as vessels and airways. The most challenging cases are those with mostly incomplete, absent, or near-absent fissures and in cases with poorly revealed fissures due to high image noise. However, the authors observe good performance even in the majority of these cases.
62 RADIOLOGY AND NUCLEAR MEDICINE↗
Microgravity Testing of a Surface Sampling System for Sample Return from Small Solar System Bodies
The return of samples from solar system bodies is becoming an essential element of solar system exploration. The recent National Research Council Solar System Exploration Decadal Survey identified six sample return missions as high priority missions: South-Aitken Basin Sample Return, Comet Surface Sample Return, Comet Surface Sample Return-sample from selected surface sites, Asteroid Lander/Rover/Sample Return, Comet Nucleus Sample Return-cold samples from depth, and Mars Sample Return [1] and the NASA Roadmap also includes sample return missions [2] . Sample collection methods that have been flown on robotic spacecraft to date return subgram quantities, but many scientific issues (like bulk composition, particle size distributions, petrology, chronology) require tens to hundreds of grams of sample. Many complex sample collection devices have been proposed, however, small robotic missions require simplicity. We present here the results of experiments done with a simple but innovative collection system for sample return from small solar system bodies.
Franzen, M. A.↗
Solar wind and terrestrial atmosphere effects on lunar sample surface composition
Samples returned from the Apollo missions have been shown to have undergone a partial surface oxidation with the degree of oxidation being dependent on the intensity and duration of exposure to a terrestrial or other oxidizing atmosphere. Exposure to atomic hydrogen at room temperature, or molecular hydrogen above 100 C results in a surface reduction. The adsorption of water vapor on a test sample was found to be only slightly dependent on the state of surface oxidation, a situation consistent with the formation of hydroxyl groups on the surface when a sample is exposed to hydrogen. That hydroxyl groups are indeed formed is substantiated by the release of water vapor (and by release of heavy water following exposure to deuterium), indicating that water vapor can be synthesized from solar wind hydrogen and sample oxygen. Observations of trace amounts of methane indicate that the reduction process is by no means restricted to the formation of water vapor.
Cadenhead, D. A.↗
Ball assisted device for analytical surface sampling
A system for sampling a surface includes a sampling probe having a housing and a socket, and a rolling sampling sphere within the socket. The housing has a sampling fluid supply conduit and a sampling fluid exhaust conduit. The sampling fluid supply conduit supplies sampling fluid to the sampling sphere. The sampling fluid exhaust conduit has an inlet opening for receiving sampling fluid carried from the surface by the sampling sphere. A surface sampling probe and a method for sampling a surface are also disclosed.
33 ADVANCED PROPULSION SYSTEMS↗
Design and development of an air-ejector powered pneumatic surface sampling system
Pneumatic surface sampling device for use in simulated Mars environment
PNEUMATIC EQUIPMENT↗
Liquid Microjunction Surface Sampling Probe Fluid Dynamics: Computational and Experimental Analysis of Coaxial Intercapillary Positioning Effects on Sample Manipulation
A coaxial geometry liquid microjunction surface sampling probe (LMJ-SSP) enables direct extraction of analytes from surfaces for subsequent analysis by techniques like mass spectrometry. Solution dynamics at the probe-to-sample surface interface in the LMJ-SSP has been suspected to influence sampling efficiency and dispersion but has not been rigorously investigated. The effect on flow dynamics and analyte transport to the mass spectrometer caused by coaxial retraction of the inner and outer capillaries from each other and the surface during sampling with a LMJ-SSP was investigated using computational fluid dynamics and experimentation. A transparent LMJ-SSP was constructed to provide the means for visual observation of the dynamics of the surface sampling process. Visual observation, computational fluid dynamics (CFD) analysis, and experimental results revealed that inner capillary axial retraction from the flush position relative to the outer capillary transitioned the probe from a continuous sampling and injection mode through an intermediate regime to sample plug formationmode caused by eddy currents at the sampling end of the probe. The potential for analytical implementation of these newly discovered probe operational modes is discussed.
71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
Photoelectron spectrometer with means for stabilizing sample surface potential
An improved X-ray photoelectron spectrometer is disclosed, which includes circuit means to determine the surface potential of a sample, e.g., an insulator. The circuit means comprise an electron gun, whose potential is modulated at a preselected frequency above and below a selected potential with respect to the spectrometer common potential, e.g., ground. The beam of electrons is directed to the sample surface. The sample's surface potential is offset by an offset power supply with respect to the spectrometer common potential until the ac current which flows through the sample reaches a peak amplitude. A lock-in amplifier is included to measure the ac current in phase with the modulating frequency.
Grunthaner, F. J.↗
Laboratory Studies on Surface Sampling of Bacillus anthracis Contamination: Summary, Gaps, and Recommendations
This report summarizes previous laboratory studies to characterize the performance of methods for collecting, storing/transporting, processing, and analyzing samples from surfaces contaminated by Bacillus anthracis or related surrogates. The focus is on plate culture and count estimates of surface contamination for swab, wipe, and vacuum samples of porous and nonporous surfaces. Summaries of the previous studies and their results were assessed to identify gaps in information needed as inputs to calculate key parameters critical to risk management in biothreat incidents. One key parameter is the number of samples needed to make characterization or clearance decisions with specified statistical confidence. Other key parameters include the ability to calculate, following contamination incidents, the (1) estimates of Bacillus anthracis contamination, as well as the bias and uncertainties in the estimates, and (2) confidence in characterization and clearance decisions for contaminated or decontaminated buildings. Gaps in knowledge and understanding identified during the summary of the studies are discussed and recommendations are given for future studies.
59 BASIC BIOLOGICAL SCIENCES↗
Laboratory studies on surface sampling of Bacillus anthracis contamination: summary, gaps, and recommendations
This article summarizes previous laboratory studies to characterize the performance of methods for collecting, storing/transporting, processing, and analyzing samples from surfaces contaminated by Bacillus anthracis or related surrogates. The focus is on plate culture and count estimates of surface contamination for swab, wipe, and vacuum samples of porous and nonporous surfaces. Summaries of the previous studies and their results were assessed to identify gaps in information needed as inputs to calculate key parameters critical to risk management in biothreat incidents. One key parameter is the number of samples needed to make characterization or clearance decisions with specified statistical confidence. Other key parameters include the ability to calculate, following contamination incidents, the 1) estimates of Bacillus anthracis contamination, as well as the bias and uncertainties in the estimates, and 2) confidence in characterization and clearance decisions for contaminated or decontaminated buildings. Gaps in knowledge and understanding identified during the summary of the studies are discussed. Recommendations are given for future evaluations of data from existing studies and possible new studies.
anthrax↗
Sample processing approach for detection of ricin in surface samples
With several ricin contamination incidents reported over the past decade, rapid and accurate methods are needed for environmental sample analysis, especially after decontamination. A sample processing method was developed for common surface sampling devices to improve the limit of detection and avoid false negative/positive results for ricin analysis. Potential assay interferents from the sample matrix (bleach residue, sample material, wetting buffer), including reference dust, were tested using a Time-Resolved Fluorescence (TRF) immunoassay. Test results suggested that the sample matrix did not cause the elevated background fluorescence sometimes observed when analyzing post-bleach decontamination samples from ricin incidents. Furthermore, sample particulates (80 mg/mL Arizona Test Dust) did not enhance background fluorescence or interfere with ricin detection by TRF. These results suggested that high background fluorescence in this immunoassay could be due to labeled antibody quality and/or quantity issues. Centrifugal ultrafiltration devices were evaluated for ricin concentration as a part of sample processing. Up to 30-fold concentration of ricin was observed by the devices, which serve to remove soluble interferents and could function as the front-end sample processing step to other ricin analytical methods. Here, the procedure has the potential to be used with a broader range of environmental sample types and with other potential interferences and to be followed by other ricin analytical methods, although additional verification studies would be required.
54 ENVIRONMENTAL SCIENCES↗
Combining Laser Ablation/Liquid Phase Collection Surface Sampling and High-Performance Liquid Chromatography Electrospray Ionization Mass Spectrometry
This paper describes the coupling of ambient pressure transmission geometry laser ablation with a liquid phase sample collection method for surface sampling and ionization with subsequent mass spectral analysis. A commercially available autosampler was adapted to produce a liquid droplet at the end of the syringe injection needle while in close proximity to the surface to collect the sample plume produced by laser ablation. The sample collection was followed by either flow injection or a high performance liquid chromatography (HPLC) separation of the extracted components and detection with electrospray ionization mass spectrometry (ESI-MS). To illustrate the analytical utility of this coupling, thin films of a commercial ink sample containing rhodamine 6G and of mixed isobaric rhodamine B and 6G dyes on glass microscope slides were analyzed. The flow injection and HPLC/ESI-MS analysis revealed successful laser ablation, capture and, with HPLC, the separation of the two compounds. The ablated circular area was about 70 m in diameter for these experiments. The spatial sampling resolution afforded by the laser ablation, as well as the ability to use sample processing methods like HPLC between the sample collection and ionization steps, makes this combined surface sampling/ionization technique a highly versatile analytical tool.
Laser Ablation↗
Continuous Flow Liquid Microjunction Surface Sampling Probe Connected On-line with HPLC/MS for Spatially Resolved Analysis of Small Molecules and Proteins
RATIONALE: A continuous flow liquid microjunction surface sampling probe extracts soluble material from surfaces for direct ionization and detection by MS. Demonstrated here is the on-line coupling of such a probe with HPLC/MS enabling extraction, separation and detection of small molecules and proteins from surfaces in a spatially resolved (~0.5 mm diameter spots) manner. Methods: A continuous flow liquid microjunction surface sampling probe was connected to a 6-port, 2-position valve for extract collection and injection to an HPLC column. A QTRAP 5500 hybrid triple quadrupole linear ion trap equipped with a Turbo V ion source operated in positive ESI mode was used for all experiments. System operation was tested with extraction, separation and detection of propranolol and associated metabolites from drug dosed tissues and proteins from dried sheep blood spots on paper. Results: Confirmed in the tissue were the parent drug and two different hydroxypropranolol glucuronides. The mass spectrometric response for these compounds from different locations in the liver showed an increase with increasing extraction time (5, 20 and 40 s extractions). For on-line separation and detection/identification of extracted proteins from dried sheep blood spots, two major protein peaks dominated the chromatogram and could be correlated with the expected masses for the hemoglobin and chains. Conclusions: Spatially resolved sampling, separation, and detection of small molecules and proteins from surfaces can be accomplished using a continuous flow liquid microjunction surface sampling probe coupled on-line with HPLC/MS detection.
dried blood spots↗
Characterization of the March 2017 tank 10 surface sample (combination of HTF-10-17-30 AND HTF-10-17-31) and variable depth sample (combination of HTF-10-17-32 and HTF-10-17-33)
Two surface samples (HTF-10-17-30 and HTF-10-17-31) and two variable depth samples (HTF-10-17-32 and HTF-10-17-33) were collected from SRS Tank 10 during March 2017 and submitted to SRNL for characterization. At SRNL, the two surface samples were combined in one container, the two variable depth samples (VDSs) were combined in another container, and then the two composite samples were each characterized by a series of physical, ionic, radiological, and elemental analysis methods. The surface sample composite was characterized primarily for Tank Farm corrosion control purposes, while the VDS composite was characterized primarily for Tank Closure Cesium Removal (TCCR) purposes.
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
The Viking gas exchange experiment results from Chryse and Utopia surface samples
Immediate gas changes occurred when untreated Martian surface samples were humidified and/or wet by an aqueous nutrient medium in the Viking lander gas exchange experiment. The evolutions of N2, CO2, and Ar are mainly associated with soil surface desorption caused by water vapor, while O2 evolution is primarily associated with decomposition of superoxides inferred to be present on Mars. On recharges with fresh nutrient and test gas, only CO2 was given off, and its rate of evolution decreased with each recharge. This CO2 evolution is thought to come from the oxidation of organics present in the nutrient by gamma Fe2O3 in the surface samples. Atmospheric analyses were also performed at both sites. The mean atmospheric composition from four analyses is N2, 2.3%; O2, not greater than 0.15%; Ar, 1.5% and CO2, 96.2%.
Oyama, V. I.↗
Development of Surface Sampling Techniques for the Canister Deposition Field Demonstration (FY22 Update)
This report describes the proposed surface sampling techniques and plan for the multi-year Canister Deposition Field Demonstration (CDFD). The CDFD is primarily a dust deposition test that will use three commercial 32PTH2 NUHOMS welded stainless steel storage canisters in Advanced Horizontal Storage Modules, with planned exposure testing for up to 10 years at an operating ISFSI site. One canister will be left at ambient condition, unheated; the other two will have heaters to achieve canister surface temperatures that match, to the degree possible, spent nuclear fuel (SNF) loaded canisters with heat loads of 10 kW and 40 kW. Surface sampling campaigns for dust analysis will take place on a yearly or bi-yearly basis. The goal of the planned dust sampling and analysis is to determine important environmental parameters that impact the potential occurrence of stress corrosion cracking on SNF dry storage canisters. Specifically, measured dust deposition rates and deposited particle sizes will improve parameterization of dust deposition models employed to predict the potential occurrence and timing of stress corrosion cracks on the stainless steel SNF canisters. The size, morphology, and composition of the deposited dust and salt particles will be quantified, as well as the soluble salt load per unit area and the rate of deposition, as a function of canister surface temperature, location, time, and orientation. Previously, a preliminary sampling plan was developed, identifying possible sampling locations on the canister surfaces and sampling intervals; possible sampling methods were also described. Further development of the sampling plan has commenced through three different tasks. First, canister surface roughness, a potentially important parameter for air flow and dust deposition, was characterized at several locations on one of the test canisters. Second, corrosion testing to evaluate the potential lifetime and aging of thermocouple wires, spot welds, and attachments was initiated. Third, hand sampling protocols were developed, and initial testing was carried out. The results of those efforts are presented in this report. The information obtained from the CDFD will be critical for ongoing efforts to develop a detailed understanding of the potential for stress corrosion cracking of SNF dry storage canisters.
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Laser Ablation Sampling of Materials Directly into the Formed Liquid Microjunction of a Continuous Flow Surface Sampling Probe/Electrospray Ionization Emitter for Mass Spectral Analysis and Imaging
Transmission geometry laser ablation directly into a formed liquid microjunction of a continuous flow liquid microjunction surface sampling probe/electrospray ionization emitter was utilized for molecular and elemental detection and mass spectrometry imaging. The ability to efficiently capture and ionize ablated material was demonstrated by the detection of various small soluble n-mers of polyaniline and silver ion solvent clusters formed from laser ablation of electropolymerized polyaniline and silver thin films, respectively. In addition, analysis of surfaces that contain soluble components was accomplished by coating or laminating the sample with an insoluble film to enable liquid junction formation without directly extracting material from the surface. The ability to perform mass spectrometry imaging at a spatial resolution of about 50 m was illustrated by using laminated inked patterns on a microscope slide. In general, these data demonstrate at least an order of magnitude signal enhancement compared to the non-contact, laser ablation droplet capture-based surface sampling/ionization approaches that have been previously presented.
electrospray ionization (ESI)↗
FY23 Update: Surface Sampling Activities for the Canister Deposition Field Demonstration
This report describes the results of a field demonstration of the proposed surface sampling techniques and plan for the multi-year Canister Deposition Field Demonstration (CDFD). The CDFD will evaluate salt deposition rates on three commercial 32PTH2 NUHOMS welded stainless steel storage canisters in Advanced Horizontal Storage Modules. Exposure testing is planned for up to 10 years and will incorporate periodic surface sampling campaigns. The goal of the planned dust sampling and analysis is to determine important environmental parameters that impact the potential occurrence of stress corrosion cracking on spent nuclear fuel (SNF) dry storage canisters. Specifically, measured dust deposition rates and deposited particle sizes will improve parameterization of dust deposition models employed to predict the potential occurrence and timing of stress corrosion cracks on the stainless steel SNF canisters. Previously, a preliminary sampling plan was developed, identifying possible sampling locations on the canister surfaces and sampling intervals; possible sampling methods were also described. Building from previous work, this report documents hand sampling from a spent nuclear fuel canister on a transfer skid mockup designed by Sandia National Laboratories. The sampling took place from a boom lift and salts were collected from mounted sample plates. The results of these efforts are presented in this report and compared to previous laboratory-controlled tests. The information obtained from the CDFD will be critical for ongoing efforts to develop a detailed understanding of the potential for stress corrosion cracking of SNF dry storage canisters.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗