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All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Triton Field Trials (TFiT) underwater noise - University of New Hampshire Living Bridge turbine Processed Data

In July 2021, a commercial-off-the-shelf hydrophone was deployed in a free-drifting configuration to measure underwater acoustic emissions and characterize a 25 kW-rated tidal turbine at the University of New Hampshire's Living Bridge Project in Portsmouth, New Hampshire. Sampling methods and analysis were performed in alignment with the recently published IEC 62600-40 Technical Specification for acoustic characterization of marine energy converters. Results from this study indicate acoustic emissions from the turbine were below ambient sound levels and therefore did not have a significant impact on the underwater noise levels of the project site. As a component of Pacific Northwest National Laboratory's Triton Field Trials (TFiT) described in a paper published in a Special Issue of Journal of Marine Energy Science and Engineering, this study provides a valuable use case for the IEC 62600-40 Technical Specification framework and further recommendations for cost-effective technologies and methods for measuring underwater noise at future current energy converter project sites. The paper can be accessed in the link bellow.

16 TIDAL AND WAVE POWER↗
DOE OSTI2026

Total Dissolved Nitrogen and Ammonia Data for the East River Watershed, Colorado (2015-2025)

This data package contains mean values for total dissolved nitrogen (TDN) and ammonia concentrations for water samples taken from the East River Watershed in Colorado. The East River is part of the Watershed Function Scientific Focus Area (WFSFA) located in the Upper Colorado River Basin, United States. TDN was analyzed using a Shimadzu Total Nitrogen Module (TNM-1) combined with the TOC-VCSH analyzer (Shimadzu Corporation, Japan). TNM-1 is a non-specific measurement of total nitrogen (TN). All nitrogen species in samples are combusted to nitrogen monoxide and nitrogen dioxide, then reacted with ozone to form an excited state of nitrogen dioxide. Upon returning to ground state, light energy is emitted. Then, TDN is measured using a chemiluminescence detector. Ammonia was determined using a Lachat's QuikChem 8500 Series 2 Flow Injection Analysis System (LACHAT Instruments, QuckChem 8500 series 2, Automated Ion Analyzer, Loveland, Colorado). When ammonia in water samples is heated (60 degrees C) with salicylate and hypochlorite in an alkaline phosphate buffer, an emerald green color is produced which is proportional to the ammonia concentration. The color is intensified by the addition of nitroprusside. Ethylenediaminetetraacetic acid (EDTA) is added to the buffer to prevent the interference of metal ions (Ca, Mg, and Fe etc.). Ammonia-N is then determined by LACHAT flow injection and a colorimetric assay at an absorbance wavelength 660 nm. (Reference: LACHAT Instruments: QuickChem Method 90-107-06-3-A, Determination of Ammonia by Flow Injection Analysis (High Throughput, Salicylate Method/DCIC) (Multi Matrix method). Written by Lynn Egan (Application group), February 08, 2011.) All files are labeled by location and variable, and data reported are the mean values upon replicate measurements. All samples were analyzed under a rigorous quality assurance and quality control (QA/QC) process as detailed in the methods. This data package contains (1) a zip file (tdn_ammonia_data_2015-2025.zip) containing a total of 299 files: 298 data files of ammonia and TDN data from across the Lawrence Berkeley National Laboratory (LBNL) Watershed Function Scientific Focus Area (SFA) which is reported in .csv files per location and a locations.csv (1 file) with latitude and longitude for each location; (2) a file-level metadata (v7_20260901_flmd.csv) file that lists each file contained in the dataset with associated metadata; (3) a data dictionary (v7_20260901_dd.csv) file that contains terms/column_headers used throughout the files along with a definition, units, and data type; (4) PDF and docx files for the determination of Method Detection Limits (MDLs) for TDN data, which has been updated in 2026-08; and (5) PDF and docx files for the detemination of Method Detection Limits (MDLs) for Ammonia and the Interferences by LACHAT Flow Injection Analysis. Missing values within the anion data files are noted as either "-9999" or "0.0" for not detectable (N.D.) data. There are a total of 105 locations containing TDN and Ammonia-N data. Update 2020-10-07: Updated the data files to remove times from the timestamps, so that only dates remain. The data values have not changed. Update 2021-04-11: Added Determination of Method Detection Limits (MDLs) for DIC, NPOC and TDN Analyses and Determination of Method Detection Limit for Ammonia and the Interferences by LACHAT Flow Injection Analysis documents, which can be accessed as PDFs or with Microsoft Word.Update on 6/10/2022: versioned updates to this dataset was made along with these changes: (1) updated total dissolved nitrogen and ammonia data for all locations up to 2021-12-31, (2) removal of units from column headers in datafiles, (3) added row underneath headers to contain units of variables, (4) restructure of units to comply with CSV reporting format requirements, (5) added -9999 for empty numerical cells, and (6) the addition of the file-level metadata (flmd.csv) and data dictionary (dd.csv) were added to comply with the File-Level Metadata Reporting Format. Update on 2022-09-09: Updates were made to reporting format specific files (file-level metadata and data dictionary) to correct swapped file names, add additional details on metadata descriptions on both files, add a header_row column to enable parsing, and add version number and date to file names (v2_20220909_flmd.csv and v2_20220909_dd.csv). Update on 2022-12-20: Updates were made to both the data files and reporting format specific files. Units were listed incorrectly, but have been fixed to reflect correct units (ug/L). File level metadata (flmd) and data dictionary (dd) files were updated to reflect the updated versions of these files. Available data was added up until 2022-06-01. Update on 2023-08-08: Updates were made to both the data files and reporting format specific files. New available anion data was added, up until 2023-01-05. The file level metadata and data dictionary files were updated to reflect the additional data added. Update on 2024-03-11: Updates were made to both the data files and reporting format specific files. New available anion data was added, up until 2023-10-27. Further, revisions to the data files were made to remove incorrect data points (from 1970 and 2001). The reporting format specific files were updated to reflect the additional data added. Revised versions of the PDF and docx files for determination of MDLs for TDN were added to replace previous versions. Update on 2025-05-15: Updates were made to both the data files and reporting format specific files. New available TDN and Ammonia-N data was added, up until the end of WY2024 (September 30, 2024). International Generic Sample Numbers (IGSNs), when registered, were added to the data files. The reporting format specific files were updated to reflect the additional data added. Update on 2026-09-01: Updates were made to both the data files and reporting format specific files. New available TDN and Ammonia-N data was added, up until the end of WY2025 (September 30, 2025). Updated versions, as of 2026-08-10, of the PDF and docx files for determination of MDLs for TDN data were added to this dataset.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2015

Development of an Ultra-Low Background Liquid Scintillation Counter for Trace Level Analysis

Low-level liquid scintillation counting (LSC) has been established as one of the radiation detection techniques useful in elucidating environmental processes and environmental monitoring around nuclear facilities. The Ultra-Low Background Liquid Scintillation Counter (ULB-LSC) under construction in the Shallow Underground Laboratory at Pacific Northwest National Laboratory aims to further reduce the MDAs and/or required sample processing. Through layers of passive shielding in conjunction with an active veto and 30 meters water equivalent overburden, the background reduction is expected to be 10 to 100 times below typical analytic low-background liquid scintillation systems. Simulations have shown an expected background of around 14 counts per day. A novel approach to the light collection will use a coated hollow light guide cut into the inner copper shielding. Demonstration LSC measurements will show low-energy detection, spectral deconvolution, and alpha/beta discrimination capabilities, from trials with standards of tritium, strontium-90, and actinium-227, respectively. An overview of the system design and expected demonstration measurements will emphasize the potential applications of the ULB-LSC in environmental monitoring for treaty verification, reach-back sample analysis, and facility inspections.

Erchinger, Jennifer L.↗
DOE OSTI2023

Gas-Phase Composition as a Predictive Metric for Calendar Life Behavior of Next-Generation Silicon Anodes

The expansion of renewable technologies and electrification of the transportation sector is driving increased demand for next-generation battery materials that provide higher power and energy density with superior cycling and calendar life stability. Silicon (Si) has a theoretical capacity nearly 10x that of graphite, and is therefore a promising anode material candidate to meet these rigorous performance demands. While leading Si anode battery demonstrations are approaching target metrics for cycle life, a series of complex and interrelated modes of reactivity lead to reduced calendar life and therefore challenge practical adoption of these materials. Deconvoluting the degradation processes that impact Si calendar life is critical to informing the rational and accelerated design of improved Si materials. In the present work, we employ novel sampling techniques and GC-MS-FID characterization to measure gas-phase composition during initial Si cycling, which we tie to selective mechanisms of Si passivation. We utilize a tiered analysis approach to identify and quantify the gas-phase reaction products associated with three advanced Si material candidates under practical operating conditions. Ex situ analysis of Si powders (pure chemical reactivity) is coupled with nondestructive in situ sampling of Si electrodes in a practical pouch-cell format (coupled chemical and electrochemical reactivity). We link the observed gas-phase species evolution to electrochemical behavior and measured calendar life of the three Si materials. Further, we evaluate the voltage-resolved evolution of gas-phase species for one such Si nanomaterial, where nonmonotonic gas generation implies competition between passivating reaction pathways. The measured gas-phase compositional data serves as a critical input for our advanced electrochemical SEI models to identify favorable vs unfavorable reaction pathways to stabilize Si. In addition to bolstering a fundamental understanding of Si reactivity, the present approach informs specific and quantifiable gas-phase metrics tied to calendar life improvements in Si, which can streamline and accelerate the process of next-generation material development.

DIRECT ENERGY CONVERSION,ENERGY STORAGE↗
NASA NTRS1979

Lunar sample analysis

The surface composition of two samples from the highly shocked, glass-coated lunar basalt (12054) and from four glass-coated fragments from the 1-2 mm (14161) fines were examined by X-ray photoemission spectroscopy to determine whether the agglutination process itself is responsible for the difference between their surface and bulk compositions. Auger electron spectroscopy of glass balls from the 15425 and 74001 fines were analyzed to understand the nature, extent, and behavior of volatile phases associated with lunar volcanism. Initial results indicate that (1) volatiles, in the outer few atomic layers sampled, vary considerably from ball to ball; (2) variability over the surface of individual balls is smaller; (3) the dominant volatiles on the balls are S and Zn; and (4) other volatiles commonly observed are P, Cl, and K.

Housley, R. M.↗
NASA NTRS1985

Quasi non-intrusive sampling and analysis of gases associated with the boundary layer on the tethered satellite and similar supersonic and hypersonic research vehicles

The effect that one candidate inlet, an assembly of capillary openings in a thin glass plate (a multichannel plate), might have on the overall sampling process is considered. The flow characteristics of the plate, under a variety of conditions of external pressure and mass flow, is evaluated. A review of capillary flow theory is presented with some development of the pertinent equations. The predicted mass flow will be compared to that determined perimentally to assess the effect that mass flow through one capillary might have upon a neighboring capillary. Mass spectrometric measurements of mixtures flowing through the multichannel plate (MCP) is also considered. In the first part of the experiments, the flow was in a direction normal to the surface of the plate. The experimental gases were Argon and mixtures of carbon dioxide in air. Ongoing experiments are discussed which are conducted with the flow parallel to the surface of the plate, a simulation of the kind of flow that a flight vehicle would experience.

Fishel, C.↗
DOE OSTI2013

Mechanical characterization of copper coated carbon nanotubes reinforced aluminum matrix composites

In this investigation, carbon nanotube (CNT) reinforced aluminum composites were prepared by the molecular-level mixing process using copper coated CNTs. The mixing of CNTs was accomplished by ultrasonic mixing and ball milling. Electroless Cu-coated CNTs were used to enhance the interfacial bonding between CNTs and aluminum. Scanning electron microscope analysis revealed the homogenous dispersion of Cu-coated CNTs in the composite samples compared with the uncoated CNTs. The samples were pressureless sintered under vacuum followed by hot rolling to promote the uniform microstructure and dispersion of CNTs. In 1.0 wt.% uncoated and Cu-coated CNT/Al composites, compared to pure Al, the microhardness increased by 44% and 103%, respectively. As compared to the pure Al, for 1.0 wt.% uncoated CNT/Al composite, increase in yield strength and ultimate tensile strength was estimated about 58% and 62%, respectively. However, in case of 1.0 wt.% Cu-coated CNT/Al composite, yield strength and ultimate tensile strength were increased significantly about 121% and 107%, respectively. - Graphical Abstract: Copper coated CNTs were synthesized by the electroless plating process. Optimizing the plating bath to (1:1) by wt CNTs with Cu, thickness of Cu-coated CNTs has been reduced to 100 nm. Cu-coated CNTs developed the stronger interfacial bonding with the Al matrix which resulted in the efficient transfer of load. Highlights: • Copper coated CNTs were synthesized by the electroless plating process. • Thickness of Cu-coated CNTs has been reduced to 100 nm by optimized plating bath. • In 1.0 wt.% Cu-coated CNT/Al composite, microhardness increased by 103%. • Cu-coated CNTs transfer load efficiently with stronger interfacial bonding. • In 1.0 wt.% Cu-coated CNT/Al composite, Y.S and UTS increased by 126% and 105%.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Microstructural Characterization of Irradiated Fuels and Materials for the United States High Performance Research Reactor Fuel Development Program and the Fuel Cycle Research and Development Program

In an effort to contribute to the development of advanced nuclear fuel for research reactors, monolithic and dispersion plate fuels will be examined to determine how irradiation parameters such as fission density, fission rate, and irradiation temperature, as well as mechanical parameters such as composition and fabrication, affect the final microstructure of the fuel, post irradiation. Electron Backscatter Detection (EBSD) analysis capabilities of irradiated materials will be developed as well as improvements on irradiated sample preparation in order to provide higher quality samples for SEM, FIB, and TEM. In addition, image analysis techniques developed at Idaho National Laboratory (INL) will be employed to examine microstructural features such as fission product precipitates and fission gas bubbles. The main goals are to further develop EBSD capabilities on irradiated material; characterize microstructure of irradiated fuel to support qualification; develop a consistent, effective process for image analysis using INL developed software; and provide repeatable, statistically-confident, critically assessed data to further modeling efforts. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

On the measurement of shape: With applications to lunar regolith

With the renewed commitment from NASA and other commercial entities for a presence on the Moon, the importance of understanding the characteristics of lunar regolith and how to utilize it have become the target of increasing scrutiny. Much of what is known about lunar regolith was collected during and immediately after the Apollo program, however, analytical techniques and instrumentation have advanced in leaps and bounds in the subsequent decades. Specifically, dynamic image analysis systems have advanced to the point that millions of particles can have morphological characteristics automatically determined in relatively short time frames. Particle morphological data was collected on several lunar samples and a pair of widely used regolith simulants to ascertain the accuracy of these simulants and to explore statistical analysis methods of these large datasets. It is found that these morphology datasets can vary widely depending on the particle size of the particles, and simple averaging of the data skews the results heavily towards the numerically abundant size ranges, the fines. Different reporting methods are suggested to ameliorate these problems. When applied to the lunar regolith, the particles are noted to be less morphologically complex than initially suspected. Compared to the lunar material, the simulants are found to contain some more morphological variability and angular grains. Such difference is likely due to the wildly different comminution processes that these different powder systems are subjected to.

2D shape↗
NASA NTRS1984

Trends in Planetary Data Analysis. Executive summary of the Planetary Data Workshop

Planetary data include non-imaging remote sensing data, which includes spectrometric, radiometric, and polarimetric remote sensing observations. Also included are in-situ, radio/radar data, and Earth based observation. Also discussed is development of a planetary data system. A catalog to identify observations will be the initial entry point for all levels of users into the data system. There are seven distinct data support services: encyclopedia, data index, data inventory, browse, search, sample, and acquire. Data systems for planetary science users must provide access to data, process, store, and display data. Two standards will be incorporated into the planetary data system: Standard communications protocol and Standard format data unit. The data system configuration must combine a distributed system with those of a centralized system. Fiscal constraints have made prioritization important. Activities include saving previous mission data, planning/cost analysis, and publishing of proceedings.

Evans, N.↗
DOE OSTI2017

Delayed Gamma-ray Spectroscopy for Safeguards Applications

The delayed gamma-ray assay technique utilizes an external neutron source (D-D, D-T, or electron accelerator-driven), and high-resolution gamma-ray spectrometers to perform characterization of SNM materials behind shielding and in complex configurations such as a nuclear fuel assembly. High-energy delayed gamma-rays (2.5 MeV and above) observed following the active interrogation, provide a signature for identification of specific fissionable isotopes in a mixed sample, and determine their relative content. Potential safeguards applications of this method are: 1) characterization of fresh and spent nuclear fuel assemblies in wet or dry storage; 2) analysis of uranium enrichment in shielded or non-characterized containers or in the presence of a strong radioactive background and plutonium contamination; 3) characterization of bulk and waste and product streams at SNM processing plants. Extended applications can include warhead confirmation and warhead dismantlement confirmation in the arms control area, as well as SNM diagnostics for the emergency response needs. In FY16 and prior years, the project has demonstrated the delayed gamma-ray measurement technique as a robust SNM assay concept. A series of empirical and modeling studies were conducted to characterize its response sensitivity, develop analysis methodologies, and analyze applications. Extensive experimental tests involving weapons-grade Pu, HEU and depleted uranium samples were completed at the Idaho Accelerator Center and LLNL Dome facilities for various interrogation time regimes and effects of the neutron source parameters. A dedicated delayed gamma-ray response modeling technique was developed and its elements were benchmarked in representative experimental studies, including highresolution gamma-ray measurements of spent fuel at the CLAB facility in Sweden. The objective of the R&D effort in FY17 is to experimentally demonstrate the feasibility of the delayed gamma-ray interrogation of shielded SNM samples with portable neutron sources suitable for field applications.

61 RADIATION PROTECTION AND DOSIMETRY↗
DOE OSTI2015

Analysis of Nb{sub 3}Sn surface layers for superconducting radio frequency cavity applications

We present an analysis of Nb{sub 3}Sn surface layers grown on a bulk Niobium (Nb) coupon prepared at the same time and by the same vapor diffusion process used to make Nb{sub 3}Sn coatings on 1.3 GHz Nb cavities. Tunneling spectroscopy reveals a well-developed, homogeneous superconducting density of states at the surface with a gap value distribution centered around 2.7 ± 0.4 meV and superconducting critical temperatures (T{sub c}) up to 16.3 K. Scanning transmission electron microscopy performed on cross sections of the sample's surface region shows an ∼2 μm thick Nb{sub 3}Sn surface layer. The elemental composition map exhibits a Nb:Sn ratio of 3:1 and reveals the presence of buried sub-stoichiometric regions that have a ratio of 5:1. Synchrotron x-ray diffraction experiments indicate a polycrystalline Nb{sub 3}Sn film and confirm the presence of Nb rich regions that occupy about a third of the coating volume. These low T{sub c} regions could play an important role in the dissipation mechanisms occurring during RF tests of Nb{sub 3}Sn-coated Nb cavities and open the way for further improving a very promising alternative to pure Nb cavities for particle accelerators.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2018

Pathways towards Valid Data: Assessment of Optimized Packaging Strategies for Core Components - 18158

Every company that runs nuclear power plants needs a strategy for disposal of the radioactive waste and for decommissioning and dismantling of its nuclear reactors. The dismantling progress of several German NPPs is already in an advanced stage. Hence, particularly highly activated core components have to be disposed of as radioactive waste. Nevertheless, this is also an issue during the operating phase due to necessary replacements of highly activated core components such as PWR control elements or RPV heads. The conditioning of waste packages for final disposal in the German repository Konrad requires the core components to be dismantled, packaged and dried. Therefore, a qualified packaging strategy is needed to ensure a reliable compliance with the protection objectives of the repository and an optimized utilization of prescribed contingents. Exemplified by PWR control elements a pathway is drawn how to perform an optimized packaging strategy in compliance with the protection objectives of the repository based on only few relevant radionuclides derived from activation calculations. For these calculations, particularly the influence of trace impurities in the materials has to be considered and their amounts have to be verified or analyzed by sampling. Furthermore, low nuclide activities from contamination cannot simply be neglected because some of them are obliged to be declared or their radiological relevance has not been sufficiently determined. Due to various influence factors, qualified sampling strategies need carefully considered concepts. Therefore, detailed planning facilitates the qualification and approval process and reduces the costs for analyses and the number of containers. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2017

Visualization and prediction of supercritical CO 2 distribution in sandstones during drainage: An in situ synchrotron X-ray micro-computed tomography study

Pore-scale distribution of supercritical CO 2 (scCO 2 ) exerts significant control on a variety of key hydrologic as well as geochemical processes, including residual trapping and dissolution. Despite such importance, only a small number of experiments have directly characterized the three-dimensional distribution of scCO 2 in geologic materials during the invasion (drainage) process. Here, we present a study which couples dynamic high-resolution synchrotron X-ray micro-computed tomography imaging of a scCO 2 /brine system at in situ pressure/temperature conditions with quantitative pore-scale modeling to allow direct validation of a pore-scale description of scCO2 distribution. The experiment combines high-speed synchrotron radiography with tomography to characterize the brine saturated sample, the scCO 2 breakthrough process, and the partially saturated state of a sandstone sample from the Domengine Formation, a regionally extensive unit within the Sacramento Basin (California, USA). The availability of a 3D dataset allowed us to examine correlations between grains and pores morphometric parameters and the actual distribution of scCO 2 in the sample, including the examination of the role of small-scale sedimentary structure on CO2 distribution. The segmented scCO 2 /brine volume was also used to validate a simple computational model based on the local thickness concept, able to accurately simulate the distribution of scCO 2 after drainage. The same method was also used to simulate Hg capillary pressure curves with satisfactory results when compared to the measured ones. Finally, this predictive approach, requiring only a tomographic scan of the dry sample, proved to be an effective route for studying processes related to CO 2 invasion structure in geological samples at the pore scale.

3D quantitative morphometric analysis↗
NASA NTRS2011

Receiver Gain Modulation Circuit

A receiver gain modulation circuit (RGMC) was developed that modulates the power gain of the output of a radiometer receiver with a test signal. As the radiometer receiver switches between calibration noise references, the test signal is mixed with the calibrated noise and thus produces an ensemble set of measurements from which ensemble statistical analysis can be used to extract statistical information about the test signal. The RGMC is an enabling technology of the ensemble detector. As a key component for achieving ensemble detection and analysis, the RGMC has broad aeronautical and space applications. The RGMC can be used to test and develop new calibration algorithms, for example, to detect gain anomalies, and/or correct for slow drifts that affect climate-quality measurements over an accelerated time scale. A generalized approach to analyzing radiometer system designs yields a mathematical treatment of noise reference measurements in calibration algorithms. By treating the measurements from the different noise references as ensemble samples of the receiver state, i.e. receiver gain, a quantitative description of the non-stationary properties of the underlying receiver fluctuations can be derived. Excellent agreement has been obtained between model calculations and radiometric measurements. The mathematical formulation is equivalent to modulating the gain of a stable receiver with an externally generated signal and is the basis for ensemble detection and analysis (EDA). The concept of generating ensemble data sets using an ensemble detector is similar to the ensemble data sets generated as part of ensemble empirical mode decomposition (EEMD) with exception of a key distinguishing factor. EEMD adds noise to the signal under study whereas EDA mixes the signal with calibrated noise. It is mixing with calibrated noise that permits the measurement of temporal-functional variability of uncertainty in the underlying process. The RGMC permits the evaluation of EDA by modulating the receiver gain using an external signal. Without the RGMC, samples of calibrated references from radiometers form an ensemble data set of the natural occurring fluctuations within a receiver. By driving the gain of an otherwise stable receiver with an external signal, the conceptual framework and generalization of the mathematics of EDA can be tested. A series of measurements was conducted to evaluate and characterize the performance of the RGMC. Test signals stepped the RGMC across its dynamic range of performance using a radiometer that sampled four noise references; analysis indicates that the RGMC successfully modulated the receiver gain with an external signal. Calibration algorithms applied to four noise references demonstrate the RGMC produced ensemble data sets of the external signal.

Jones, Hollis↗
DOE OSTI2022

Psilocybin: crystal structure solutions enable phase analysis of prior art and recently patented examples

Psilocybin {systematic name: 3-[2-(dimethylamino)ethyl]-1 H -indol-4-yl dihydrogen phosphate} is a zwitterionic tryptamine natural product found in numerous species of fungi known for their psychoactive properties. Following its structural elucidation and chemical synthesis in 1959, purified synthetic psilocybin has been evaluated in clinical trials and has shown promise in the treatment of various mental health disorders. In a recent process-scale crystallization investigation, three crystalline forms of psilocybin were repeatedly observed: Hydrate A, Polymorph A, and Polymorph B. The crystal structure for Hydrate A was solved previously by single-crystal X-ray diffraction. This article presents new crystal structure solutions for the two anhydrates, Polymorphs A and B, based on Rietveld refinement using laboratory and synchrotron X-ray diffraction data, and density functional theory (DFT) calculations. Utilizing the three solved structures, an investigation was conducted via Rietveld method (RM) based quantitative phase analysis (QPA) to estimate the contribution of the three different forms in powder X-ray diffraction (PXRD) patterns provided by different sources of bulk psilocybin produced between 1963 and 2021. Over the last 57 years, each of these samples quantitatively reflect one or more of the hydrate and anhydrate polymorphs. In addition to quantitatively evaluating the composition of each sample, this article evaluates correlations between the crystal forms present, corresponding process methods, sample age, and storage conditions. Furthermore, revision is recommended on characterizations in recently granted patents that include descriptions of crystalline psilocybin inappropriately reported as a single-phase `isostructural variant.' Rietveld refinement demonstrated that the claimed material was composed of approximately 81% Polymorph A and 19% Polymorph B, both of which have been identified in historical samples. In this article, we show conclusively that all published data can be explained in terms of three well-defined forms of psilocybin and that no additional forms are needed to explain the diffraction patterns.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

First Cosmology Results using Supernovae Ia from the Dark Energy Survey: Survey Overview, Performance, and Supernova Spectroscopy

We present details on the observing strategy, data-processing techniques, and spectroscopic targeting algorithms for the first three years of operation for the Dark Energy Survey Supernova Program (DES-SN). This five-year program using the Dark Energy Camera mounted on the 4 m Blanco telescope in Chile was designed to discover and follow supernovae (SNe) Ia over a wide redshift range (0.05 < z < 1.2) to measure the equation-of-state parameter of dark energy. We describe the SN program in full: strategy, observations, data reduction, spectroscopic follow-up observations, and classification. From three seasons of data, we have discovered 12,015 likely SNe, 308 of which have been spectroscopically confirmed, including 251 SNe Ia over a redshift range of 0.017 < z < 0.85. We determine the effective spectroscopic selection function for our sample and use it to investigate the redshift-dependent bias on the distance moduli of SNe Ia we have classified. The data presented here are used for the first cosmology analysis by DES-SN (“DES-SN3YR”), the results of which are given in Dark Energy Survey Collaboration et al. The 489 spectra that are used to define the DES-SN3YR sample are publicly available at https://des.ncsa.illinois.edu/releases/sn.

79 ASTRONOMY AND ASTROPHYSICS↗
NASA NTRS1993

Verification of thermal analysis codes for modeling solid rocket nozzles

One of the objectives of the Solid Propulsion Integrity Program (SPIP) at Marshall Space Flight Center (MSFC) is development of thermal analysis codes capable of accurately predicting the temperature field, pore pressure field and the surface recession experienced by decomposing polymers which are used as thermal barriers in solid rocket nozzles. The objective of this study is to provide means for verifications of thermal analysis codes developed for modeling of flow and heat transfer in solid rocket nozzles. In order to meet the stated objective, a test facility was designed and constructed for measurement of the transient temperature field in a sample composite subjected to a constant heat flux boundary condition. The heating was provided via a steel thin-foil with a thickness of 0.025 mm. The designed electrical circuit can provide a heating rate of 1800 W. The heater was sandwiched between two identical samples, and thus ensure equal power distribution between them. The samples were fitted with Type K thermocouples, and the exact location of the thermocouples were determined via X-rays. The experiments were modeled via a one-dimensional code (UT1D) as a conduction and phase change heat transfer process. Since the pyrolysis gas flow was in the direction normal to the heat flow, the numerical model could not account for the convection cooling effect of the pyrolysis gas flow. Therefore, the predicted values in the decomposition zone are considered to be an upper estimate of the temperature. From the analysis of the experimental and the numerical results the following are concluded: (1) The virgin and char specific heat data for FM 5055 as reported by SoRI can not be used to obtain any reasonable agreement between the measured temperatures and the predictions. However, use of virgin and char specific heat data given in Acurex report produced good agreement for most of the measured temperatures. (2) Constant heat flux heating process can produce a much higher heating rate than the radiative heating process. The results show that heating rates of 125 C/s (225 F/s) can be achieved. (3) The electrical resistance of the FM 5055 samples were about 150 Omega in the virgin state, and decreased to about 35 Omega when charred. A reliable scheme must be developed to electrically insulate the composite from the heater foil in order to prevent any current leakage into the sample which can result in volumetric heating of the char zone of the composite.

Keyhani, M.↗