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At least 145 records · Page 8

Introduction to Mars Sample Handling Workshop Series: Overview of Mars Sample Hazard Analysis

Samples returned from Mars should be contained and treated as though potentially hazardous until proven otherwise If sample containment cannot be verified en route to Earth, the sample and spacecraft should either be sterilized in space or not returned to Earth. Integrity of sample containment should be maintained through reentry and transfer to a receiving facility. Controlled distribution of unsterilized materials should only occur if analyses determine the sample not to contain a biological hazard. Planetary protection measures adopted for the first sample return should not be relaxed for subsequent missions without thorough scientific review and concurrence by an appropriate independent body

Rummel, John D.↗

Thermal design of the sample handling assembly in the sampling and caching subsystem on the Mars 2020 rover

The Mars 2020 Rover is scheduled to land on Mars on February 18, 2021. One of the primary mission objectives for the Mars 2020 Rover is to collect a set of Martian regolith samples for potential future return to Earth. Regolith and rock samples will be collected and placed into sample tubes using a coring drill, located at the end of a large Robotic Arm, on the outside of the rover. Filled sample tubes will be transferred from the outside of the Rover into the Adaptive Caching Assembly (ACA), located inside the Rover chassis, via the Bit Carousel. Once the filled sample tube is brought into the ACA, the Sample Handling Assembly (SHA) will transfer it to all of the internal processing stations of the ACA for volume assessment, sealing and finally drop-off on the Martian surface. The ACA is a volume within the rover chassis that is not temperature-controlled. Actuators inside the SHA and its End Effector (EE) must be warmed to above -55°C and -25°C, respectively, prior to use. This paper discusses the thermal design of the SHA that uses heaters and temperature sensors to warm up and maintain the temperature-sensitive arm components within temperature limits during operation. Thermal performance predictions for Mars surface operations are also presented.

Lee, Chern-Jiin↗

Thresholds of Temperature and Time for Mars Sample Return: Final Report of The Mars Sample Return Temperature-Time Tiger Team

The time-temperature tiger team (T4) was chartered by NASA and ESA to evaluate the risks to the scientific return of the MSR samples if they are exposed to temperatures between +30 and +60 ⁰C for different amounts of time. This team consists of 13 scientists, who were selected based on their scientific background to represent the scientific disciplines that are expected to be the ones that will be the most affected if such heating were to happen. The expertise of the team will help to understand whether exposing the MSR samples to temperatures between +30 and +60 ⁰C will pose any risk to the sample integrity and therefore, to future scientific investigations. Key processes identified by the T4 were: the release of volatiles by desorption and sublimation and release from condensed phases (interiors, decomposition, dehydration); chemical reactions including gas-gas and gas-solid; deliquescence of hygroscopic salts; acid/base interactions (potential for extreme pH conditions); aqueous redox reactions, isotopic exchange (aqueous phases, minerals, gasses, organic phases); condensation and freezing (in the after-heating cooling phase) and interactions with the sample tube materials. There is potential for multiple interactions and overlapping effects. For inorganic materials and the records they represent, over both long time scales (hours to days) and short time scales (minutes to hours) no temperature excursion above +30 °C could be accommodated without loss of science (Figure 1.1). While there will be some robust constituents (feldspars, quartz, pyroxenes, etc.) that are unaffected, there will also be some less robust constituents (salts, phyllosilicates, radicals, etc.) that are affected across all temperature ranges ≤60 °C. For organic materials, in particular organic biosignatures, the risks reflect that preservation is reliant on a number of processes, and a change in one component within a sample tube can affect another. For organic materials, over long timescales of hours to days no temperature excursion above +30 °C could be accommodated without loss of science, but over shorter time scales (minutes to hours), raising the temperature to 40 °C could be manageable without major disruption to science, whereas temperatures above 40 °C would lead to significant losses. The consideration of these findings by the MSR team will help to maintain the fidelity of samples returned from Mars in the future and maximize scientific return when analyzed in Earth laboratories.

Mark A Sephton↗

Solid phase sampling device and methods for point-source sampling of polar organic analytes

Sampling devices for sampling an aqueous source (e.g., field testing of ground water) for multiple different analytes are described. Devices include a solid phase extraction component for retention of a wide variety of targeted analytes. Devices include analyte derivatization capability for improved extraction of targeted analytes. Thus, a single device can be utilized to examine a sample source for a wide variety of analytes. Devices also include an isotope dilution capability that can prevent error introduction to the sample analysis and can correct for sample loss and degradation from the point of sampling until analysis as well as correction for incomplete or poor derivatization reactions. The devices can be field-deployable and rechargeable.

Boggess, Andrew J.↗

Solid-phase sampling device and methods for point-source sampling of polar organic analytes

Sampling devices for sampling an aqueous source (e.g., field testing of ground water) for multiple different analytes are described. Devices include a solid phase extraction component for retention of a wide variety of targeted analytes. Devices include analyte derivatization capability for improved extraction of targeted analytes. Thus, a single device can be utilized to examine a sample source for a wide variety of analytes. Devices also include an isotope dilution capability that can prevent error introduction to the sample analysis and can correct for sample loss and degradation from the point of sampling until analysis as well as correction for incomplete or poor derivatization reactions. The devices can be field-deployable and rechargeable.

Boggess, Andrew J.↗

CatMass : software for calculating optimal sample masses for X-ray absorption spectroscopy experiments involving complex sample compositions

This paper presents software for calculating the optimal mass of samples with complex compositions ( e.g. supported metal catalysts) for X-ray absorption spectroscopy (XAS) and scattering measurements. The ability to calculate the sample mass and other relevant parameters needed for an XAS measurement allows experimentalists to be better prepared in terms of detector selection, energy range of scan and overall time needed to complete the measurement, thus increasing efficiency. CatMass builds on existing sample mass calculators allowing users to determine the optimum sample preparation, collection geometry, usable energy range for a scan and approximate edge step of the absorption event. Visualization tools present the absorption calculation results in a format familiar to XAS experimentalists, with the added ability to save calculations and plots for future reference or recalculation. CatMass is a program broadly applicable in catalysis and is helpful for users with complex samples due to composition/stoichiometry or multiple competing elements.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Solvent hold tank sample results for MCU-16-53-55. January 2016 Monthly sample

Savannah River National Laboratory (SRNL) received one set of Solvent Hold Tank (SHT) samples (MCU-16-53-54-55), pulled on 01/25/2016 for analysis. The samples were combined and analyzed for composition. Analysis of the composite sample MCU-16-53-54-55 indicated the Isopar™L, and MaxCalix are at nominal levels. The modifier and TiDG concentrations are 3% and 23 % below their nominal concentrations. This analysis confirms the addition of TiDG, MaxCalix, and modifier to the solvent on November 28, 2015. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time. Periodic characterization and trimming additions to the solvent are recommended. No impurities above the 1000 ppm level were found in this solvent by the Semi-Volatile Organic Analysis (SVOA). No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). However, the Fourier transform infra-red spectroscopy (FTIR) method detected trace levels (a few ppm) of amides (a possible degradation product of TiDG). In addition, up to 21 ± 4 micrograms of mercury per gram of solvent (or 17.5 μg/mL) was detected in this sample. There appears to be a possible correlation between the mercury level and the TiDG concentration in the solvent. The current gamma level (9.16 E4 dpm/mL) confirmed that the gamma concentration has returned to previous level where the process operated normally and as expected. The laboratory will continue to monitor the quality of the solvent in particular for any new impurities or degradation of the solvent components.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Concomitant ion effects on isotope ratio measurements with liquid sampling – atmospheric pressure glow discharge ion source Orbitrap mass spectrometry

RATIONALE: The field of highly accurate and precise isotope ratio (IR) analysis has been dominated by inductively coupled plasma and thermal ionization mass spectrometers. While these instruments are considered the gold standard for IR analysis, the International Atomic Energy Agency desires a field deployable instrument capable of accurately and precisely measuring U isotope ratios. METHODS: The proposed system interfaces the liquid sampling – atmospheric pressure glow discharge (LS-APGD) ion source with a high resolution Exactive Orbitrap mass spectrometer. With this experimental setup certified U isotope standards and unknown samples were analyzed. The accuracy and precision of the system were then determined. RESULTS: The LS-APGD /Exactive instrument measures a certified reference material of natural U (235U/238U = 0.007258) as 0.007041 with a relative standard deviation of 0.158% meeting the International Target Values for Uncertainty for the destructive analysis of U. Additionally, when three unknowns measured and compared to the results from an ICP multi collector instrument, there is no statistical difference between the two instruments. CONCLUSIONS: The LS-APGD / Orbitrap system, while still in the preliminary stages of development, offers highly accurate and precise IR analysis that suggest a paradigm shift in the world of IR analysis. Furthermore, the portability of the LS-APGD as an elemental ion source combined with the low overhead and small size of the Orbitrap suggest that the instrumentation is capable of being field deployable. With liquid sampling glow discharge-Orbitrap MS, isotope ratio and precision performance improves with rejection of concomitant ion species.

atmospheric pressure sampling↗

Estimating Sample Heterogeneity and Expected Scatter Due to Cracking in Packed Powder Samples Using a Two-Phase Model

High-precision Hugoniot measurements of heterogeneous materials are a key tool in creating accurate equations of state, but such measurements are prone to larger uncertainties than their homogeneous counterparts. To efficiently reduce these uncertainties one must estimate the relative contributions of different error sources. Sample cracking is one likely source. Here we estimate its contribution through modeling, using computed tomography scans of powdered single crystal quartz samples to estimate typical packing variation within and between samples. Samples were prepared using the same materials and methods. Furthermore, cracks were prominent in the samples. We describe a simple model to estimate shock transit time variation for a single shot due to cracking, and estimate that up to 3% variation can be attributed to these structures. This suggests that decreasing variation requires addressing such packing heterogeneities during target fabrication rather than experimental diagnostics.

36 MATERIALS SCIENCE↗

Solid matrix transformation and tracer addition using molten ammonium bifluoride salt as a sample preparation method for laser ablation inductively coupled plasma mass spectrometry

Solid sampling and analysis methods, such as laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), are challenged by matrix effects and calibration difficulties. Matrix-matched standards for external calibration are seldom available and it is difficult to distribute spikes evenly into a solid matrix as internal standards. While isotopic ratios of the same element can be measured to high precision, matrix-dependent effects in the sampling and analysis process frustrate accurate quantification and elemental ratio determinations. Here we introduce a potentially general solid matrix transformation approach entailing chemical reactions in molten ammonium bifluoride (ABF) salt that enables the introduction of spikes as tracers or internal standards. Proof of principle experiments show that the decomposition of uranium ore in sealed PFA fluoropolymer vials at 230 °C yields, after cooling, new solids suitable for direct solid sampling by LA. When spikes are included in the molten salt reaction, subsequent LA-ICP-MS sampling at several spots indicate that the spikes are evenly distributed, and that U-235 tracer dramatically improves reproducibility in U-238 analysis. Precisions improved from 17% relative standard deviation for U-238 signals to 0.1% for the ratio of sample U-238 to spiked U-235, a factor of over two orders of magnitude. These results introduce the concept of solid matrix transformation (SMT) using ABF, and provide proof of principle for a new method of incorporating internal standards into a solid for LA-ICP-MS. This new approach, SMT-LA-ICP-MS, provides opportunities to improve calibration and quantification in solids based analysis. Finally, looking forward, tracer addition to transformed solids opens up LA-based methods to analytical methodologies such as standard addition, isotope dilution, preparation of matrix-matched solid standards, external calibration, and monitoring instrument drift against external calibration standard

47 OTHER INSTRUMENTATION↗

Ensemble Sampling vs. Time Sampling in Molecular Dynamics Simulations of Thermal Conductivity

In this report we compare time sampling and ensemble averaging as two different methods available for phase space sampling. For the comparison, we calculate thermal conductivities of solid argon and silicon structures, using equilibrium molecular dynamics. We introduce two different schemes for the ensemble averaging approach, and show that both can reduce the total simulation time as compared to time averaging. It is also found that velocity rescaling is an efficient mechanism for phase space exploration. Although our methodology is tested using classical molecular dynamics, the ensemble generation approaches may find their greatest utility in computationally expensive simulations such as first principles molecular dynamics. For such simulations, where each time step is costly, time sampling can require long simulation times because each time step must be evaluated sequentially and therefore phase space averaging is achieved through sequential operations. On the other hand, with ensemble averaging, phase space sampling can be achieved through parallel operations, since each ensemble is independent. For this reason, particularly when using massively parallel architectures, ensemble sampling can result in much shorter simulation times and exhibits similar overall computational effort.

74 ATOMIC AND MOLECULAR PHYSICS↗

Preserving correlations between trajectories for efficient path sampling

Importance sampling of trajectories has proved a uniquely successful strategy for exploring rare dynamical behaviors of complex systems in an unbiased way. Carrying out this sampling, however, requires an ability to propose changes to dynamical pathways that are substantial, yet sufficiently modest to obtain reasonable acceptance rates. Satisfying this requirement becomes very challenging in the case of long trajectories, due to the characteristic divergences of chaotic dynamics. Here, we examine schemes for addressing this problem, which engineer correlation between a trial trajectory and its reference path, for instance using artificial forces. Our analysis is facilitated by a modern perspective on Markov chain Monte Carlo sampling, inspired by non-equilibrium statistical mechanics, which clarifies the types of sampling strategies that can scale to long trajectories. Viewed in this light, the most promising such strategy guides a trial trajectory by manipulating the sequence of random numbers that advance its stochastic time evolution, as done in a handful of existing methods. In cases where this “noise guidance” synchronizes trajectories effectively, as the Glauber dynamics of a two-dimensional Ising model, we show that efficient path sampling can be achieved for even very long trajectories.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Accuracy of tip-sample interaction measurements using dynamic atomic force microscopy techniques: Dependence on oscillation amplitude, interaction strength, and tip-sample distance

Atomic force microscopy (AFM) is a versatile surface characterization method that can map a sample’s topography with high spatial resolution while simultaneously interrogating its surface chemistry through the site-specific high-resolution quantification of the forces acting between the sample and the probe tip. Thanks to considerable advances in AFM measurement technology, such local measurements of chemical properties have gained much popularity in recent years. To this end, dynamic AFM methodologies are implemented where either the oscillation frequency or the oscillation amplitude and phase of the vibrating cantilever are recorded as a function of tip-sample distance and subsequently converted to reflect tip-sample forces or interaction potentials. Such conversion has, however, been shown to produce non-negligible errors when applying the most commonly used mathematical conversion procedures if oscillation amplitudes are of the order of the decay length of the interaction. Extending on these earlier findings, the computational study presented in this paper reveals that the degree of divergence from actual values may also critically depend on both the overall strength of tip-sample interaction and the distance at which the interaction is obtained. These systematic errors can, however, be effectively eliminated by using oscillation amplitudes that are sufficiently larger than the decay length of the interaction potential.

Electrical properties and parameters↗

A COMPLETE SAMPLE OF BRIGHT SWIFT LONG GAMMA-RAY BURSTS. I. SAMPLE PRESENTATION, LUMINOSITY FUNCTION AND EVOLUTION

We present a carefully selected sub-sample of Swift long gamma-ray bursts (GRBs) that is complete in redshift. The sample is constructed by considering only bursts with favorable observing conditions for ground-based follow-up searches, which are bright in the 15-150 keV Swift/BAT band, i.e., with 1-s peak photon fluxes in excess to 2.6 photons s{sup -1} cm{sup -2}. The sample is composed of 58 bursts, 52 of them with redshift for a completeness level of 90%, while another two have a redshift constraint, reaching a completeness level of 95%. For only three bursts we have no constraint on the redshift. The high level of redshift completeness allows us for the first time to constrain the GRB luminosity function and its evolution with cosmic times in an unbiased way. We find that strong evolution in luminosity ({delta}{sub l} = 2.3 {+-} 0.6) or in density ({delta}{sub d} = 1.7 {+-} 0.5) is required in order to account for the observations. The derived redshift distributions in the two scenarios are consistent with each other, in spite of their different intrinsic redshift distributions. This calls for other indicators to distinguish among different evolution models. Complete samples are at the base of any population studies. In future works we will use this unique sample of Swift bright GRBs to study the properties of the population of long GRBs.

79 ASTRONOMY AND ASTROPHYSICS↗

Dark Energy Survey Year 6 results: Clustering redshifts and importance sampling of self-organized-maps 𝑛⁡(𝑧) realizations for 3 × 2 ⁢pt samples

This work is part of a series establishing the redshift framework for the 3 × 2 ⁢pt analysis of the Dark Energy Survey Year 6 (DES Y6). For DES Y6, photometric redshift distributions are estimated using self-organizing maps (SOMs), calibrated with spectroscopic and many-band photometric data. To overcome limitations from color-redshift degeneracies and incomplete spectroscopic coverage, we enhance this approach by incorporating clustering-based redshift constraints (clustering-z, or WZ) from angular cross-correlations with BOSS and eBOSS galaxies and eBOSS quasar samples. We define a WZ likelihood and apply importance sampling to a large ensemble of SOM-derived 𝑛⁡(𝑧) realizations, selecting those consistent with the clustering measurements to produce a posterior sample for each lens and source bin. The analysis uses angular scales corresponding to 1.5–5 Mpc to optimize signal-to-noise ratio while mitigating modeling uncertainties and marginalizes over redshift-dependent galaxy bias and other systematics informed by the N-body simulation CARDINAL . While a sparser spectroscopic reference sample limits WZ constraining power at 𝑧 >1.1, particularly for source bins, we demonstrate that combining SOM with WZ improves redshift accuracy and enhances the overall cosmological constraining power of DES Y6. As a result, we estimate an improvement in 𝑆 8 of approximately 10% for cosmic shear and 3 ×2⁢pt analysis, primarily due to the WZ calibration of the source samples.

Cosmological parameters↗