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At least 235 records · Page 13

Small Punch Testing of Molybdenum-99 Targets

Northstar Medical Radioisotopes is developing an accelerator-based method to produce 99 Mo, which is a parent isotope of the commonly used 99m Tc medical isotope. The Mo targets being designed for the accelerator will be produced from enriched 100 Mo, also known as aMo . Pressed and sintered powder feedstock is used to fabricate aMo targets, producing 29 mm disk-shaped targets. The targets are subjected to 1–6 days in line of an electron beam with subsequent dissolution of the disk to retain the 99 Mo, which decays to 99m Tc at radio-pharmacies. The press and sinter method is advantageous because the inherent porosity produced by this method enables increased surface area and therefore increased flow of dissolution media, decreasing the dissolution time and reducing the need for a highly acidic media. Although porosity aids in dissolution, it reduces the mechanical strength and ductility. Targets require good mechanical integrity when subjected to the conditions in the accelerator. Therefore, Northstar is seeking methods to rapidly test disk samples after fabrication to assure mechanical performance metrics are achieved. This report details the design and testing of a small punch test (SPT) that accommodates the 29 mm disk. Initial data were used to relate the SPT data to tensile properties, such as the yield strength (YS), ultimate tensile strength (UTS), and total elongation to failure. Although the SPT has been established as a somewhat reliable method for testing metallic materials, few studies have applied the SPT to refractory materials such as Mo. Based on tensile testing performed at Oak Ridge National Laboratory on different Mo samples, correlation between the Mo tensile and SPT properties could be performed, establishing a standard calibration that could be applied to other Mo samples. To test the efficacy of the SPT with Mo, multiple different disk batches were fabricated under different conditions (e.g., pressure, lubricant) with commercially available pure Mo powder. Generally, only a UTS could be well defined because the press and sinter disks failed under brittle fracture, making it difficult to determine the YS and elongation. Compared with disks fabricated with aMo powder, the aMo samples underperformed their pure nat Mo counterparts. This report summarizes the current status of the SPT, but further evaluation is needed before it can be applied as a reliable quality assurance tool.

62 RADIOLOGY AND NUCLEAR MEDICINE↗

The Impact of Increased Requirements for Verification Measurements of Category III and IV Receipts

As part of the regular nuclear material accounting and control process, sites that have accountable nuclear material regularly perform measurements of the material in their possession. The expectation for the type of measurements and their frequency is set out in Department of Energy (DOE) Order 474.2, and further detailed in each site’s respective material control and accountability (MC&A) plan and associated controlling documents. The measurements of interest in this report are those performed on external (between DOE sites) transfer receipts of Category III or IV accountable materials. In 2020, a revision of DOE Order 474.2 was proposed that would significantly increase the requirement that measurements be performed upon receipt of material, and further, that those measurements be quantitative verification (rather than qualitative confirmatory) measurements. A survey was performed of DOE sites to discuss the impact on their MC&A measurements program if more rigorous verification measurements requirements for Category III and IV receipts were implemented. An assessment of nondestructive assay (NDA) measurement instruments to meet those needs was also performed. Across the board, sites indicated that personnel and budget would cause the largest impact. Sites which are qualified as Category I/II indicated a reduced impact as these sites already have the measurement capabilities and some personnel but would require the acquisition of additional measurement systems. Category III/IV sites indicated a much larger impact as these sites generally have smaller MC&A programs. A few smaller sites stated a measurement program would need to be created to handle the demand. Calorimetry, quantitative gamma spectroscopy and neutron coincidence counting systems were identified as common systems that could meet the verification measurement requirements. The other, and perhaps larger issue is the need for calibration standards for the calorimetry and neutron coincidence counting systems. It is proposed that a comparative study be performed for ISOCS and ISOTOPICS, qualification of a COTS calorimetry system be performed, and development of an AWCC system that uses a neutron generator.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

Dataset_for_Molecular_Motion_Below_the_Glass_Transition_A_Solid-State_NMR_Study_of_Siloxane_Polymer_Dynamics Study

This dataset contains solid-state 1H and 13C NMR relaxometry data, differential scanning calorimetry (DSC) data, and size exclusion chromatography (SEC/GPC) data supporting the study of sub-glass-transition (sub-Tg) molecular dynamics in a composition- and sequence-controlled series of diphenyl-substituted polysiloxanes (PDMS, 14Ph, 33Ph, 50Ph, 67Ph, and 100Ph; 0–100% diphenylsiloxane content by mole).All solid-state NMR data were acquired on a 200 MHz Bruker Avance III HD spectrometer using a static 7 mm HX probe or a 4 mm HX probe under 4 kHz magic-angle spinning. Raw Bruker TopSpin experiment folders are included for: (1) variable-temperature 1H lineshape measurements used to determine linewidth (FWHM) as a function of temperature across the glass transition; (2) 1H T1 (saturation recovery with solid-echo detection), probing nanosecond-scale dynamics near the 1H Larmor frequency; (3) 1H T1rho (direct spin-lock, 62.5 kHz), probing microsecond-scale segmental dynamics; (4) 13C-detected Lee–Goldburg cross-polarization 1H T1rho (LGCPH T1rho) for 33Ph and 50Ph, resolving aromatic and aliphatic proton environments; and (5) 13C T1 relaxation for 33Ph and 50Ph. Differential scanning calorimetry data (TA Instruments DSC 25, −150 to +120 °C, up to +300 °C for 100Ph, 10 °C/min) are included for all six compositions and support the glass-transition temperatures in Table 1 and Figure 1. Size exclusion chromatography data (Agilent 1200 Series, PL-Gel 300 mixed-C column, THF mobile phase, polystyrene calibration standards) are included for the three synthesized copolymers (33Ph, 50Ph, 67Ph) and support the number-average molecular weights in Table 1. Processed data include per-composition relaxation-time summaries (Excel), curve-fitting and Bloembergen-Purcell-Pound (BPP) model analysis notebooks (Jupyter/Python), and Igor Pro (.pxp) master files used to generate the manuscript's figures.

Bloembergen-Purcell-Pound theory↗

As-Built Simulation of the High Flux Isotope Reactor

The Oak Ridge National Laboratory High Flux Isotope Reactor (HFIR) is an 85 MWt flux trap-type research reactor that supports key research missions, including isotope production, materials irradiation, and neutron scattering. The core consists of an inner and an outer fuel element containing 171 and 369 involute-shaped plates, respectively. The thin fuel plates consist of a U 3 O 8 -Al dispersion fuel (highly enriched), an aluminum-based filler, and aluminum cladding. The fuel meat thickness is varied across the width of the involute plate to reduce thermal flux peaks at the radial edges of the fuel elements. Some deviation from the designed fuel meat shaping is allowed during manufacturing. A homogeneity scan of each fuel plate checks for potential anomalies in the fuel distribution by scanning the surface of the plate and comparing the attenuation of the beam to calibration standards. While typical HFIR simulations use homogenized fuel regions, explicit models of the plates were developed under the Low-Enriched Uranium Conversion Program. These explicit models typically include one inner and one outer fuel plate with nominal fuel distributions, and then the plates are duplicated to fill the space of the corresponding fuel element. Therefore, data extracted from these simulations are limited to azimuthally averaged quantities. To determine the reactivity and physics impacts of an as-built outer fuel element and generate azimuthally dependent data in the element, 369 unique fuel plate models were generated and positioned. This model generates the three-dimensional (i.e., radial–axial–azimuthal) plate power profile, where the azimuthal profile is impacted by features within the adjacent control element region and beryllium reflector. For an as-built model of the outer fuel element, plate-specific homogeneity data, 235 U loading, enrichment, and channel thickness measurements were translated into the model, yielding a much more varied azimuthal power profile encompassed by uncertainty factors in analyses. These models were run with the ORNL-TN and Shift Monte Carlo tools, and they contained upwards of 500,000 cells and 100,000 unique tallies.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Near-infrared Spectral Characterization of Solar-type Stars in the Northern Hemisphere

Although solar-analog stars have been studied extensively over the past few decades, most of these studies have focused on visible wavelengths, especially those identifying solar-analog stars to be used as calibration tools for observations. As a result, there is a dearth of well-characterized solar analogs for observations in the near-infrared, a wavelength range important for studying solar system objects. We present 184 stars selected based on solar-like spectral type and V−J and V−K colors whose spectra we have observed in the 0.8–4.2 μm range for calibrating our asteroid observations. Each star has been classified into one of three ranks based on spectral resemblance to vetted solar analogs. Of our set of 184 stars, we report 145 as reliable solar-analog stars, 21 as solar analogs usable after spectral corrections with low-order polynomial fitting, and 18 as unsuitable for use as calibration standards owing to spectral shape, variability, or features at low to medium resolution. We conclude that all but five of our candidates are reliable solar analogs in the longer wavelength range from 2.5 to 4.2 μm. The average colors of the stars classified as reliable or usable solar analogs are V−J = 1.148, V−H = 1.418, and V−K = 1.491, with the entire set being distributed fairly uniformly in R.A. across the sky between −27° and +67° in decl.

79 ASTRONOMY AND ASTROPHYSICS↗

Chemical ionization mass spectrometry utilizing benzene cations for measurements of volatile organic compounds and nitric oxide

We evaluate the capability of chemical ionization mass spectrometry (CIMS) using benzene cations as reagent ions (benzene CIMS) for detecting atmospheric trace gases. We characterize the ionization pathways and product ion distributions for 27 analytes spanning diverse chemical classes. To interpret the complex ion chemistry involving two reagent ions (C 6 H$^{+}_{6}$ and (C 6 H 6 )$^{+}_{2}$) and multiple ionization pathways (charge transfer, proton transfer, adduct formation, and hydride abstraction), we introduce a thermodynamics-based framework that classifies analytes into three categories based on their ionization energy (IE), relative to those of benzene monomer (9.24 eV) and dimer (8.69 eV). Each class exhibits distinct ionization mechanisms and product ions. Analytes with IE smaller than 8.69 eV (low IE) undergo charge transfer with both reagent ions; analytes with IE between 8.69 and 9.24 eV (mid IE) undergo charge transfer with C 6 H$^{+}_{6}$ and potential adduct formation with (C 6 H 6 )$^{+}_{2}$; analytes with IE larger than 9.24 eV (high IE) could undergo adduct formation, proton transfer, or hydride abstraction. Analytes within each class also show similar sensitivity, enabling sensitivity estimation for compounds lacking calibration standards. In addition to volatile organic compounds (VOCs), benzene CIMS detects nitric oxide (NO) with a detection limit of 5 pptv for 1 min integration time, exceeding the performance of most commercial NOx analyzers. Field deployments in Chicago and St. Louis demonstrate good agreement with reference NO measurements. Isoprene measurements show good agreement with a co-located gas chromatography–photoionization detector (GC-PID) in St. Louis, but exhibit substantial positive bias in Chicago, likely due to interferences from anthropogenic VOCs in the polluted urban environment. These results highlight the potential of benzene CIMS for concurrent measurements of NO, VOCs, and their oxidation products using a single instrument, while also underscoring challenges in complex atmospheric conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Constraining the sensitivity of iodide adduct chemical ionization mass spectrometry to multifunctional organic molecules using the collision limit and thermodynamic stability of iodide ion adducts

Abstract. The sensitivity of a chemical ionization mass spectrometer (ions formed per number density of analytes) is fundamentally limited by the collision frequency between reagent ions and analytes, known as the collision limit, the ion–molecule reaction time, and the transmission efficiency of product ions to the detector. We use the response of a time-of-flight chemical ionization mass spectrometer (ToF-CIMS) to N2O5, known to react with iodide at the collision limit, to constrain the combined effects of ion–molecule reaction time, which is strongly influenced by mixing and ion losses in the ion–molecule reaction drift tube. A mass spectrometric voltage scanning procedure elucidates the relative binding energies of the ion adducts, which influence the transmission efficiency of molecular ions through the electric fields within the vacuum chamber. Together, this information provides a critical constraint on the sensitivity of a ToF-CIMS towards a wide suite of routinely detected multifunctional organic molecules for which no calibration standards exist. We describe the scanning procedure and collision limit determination, and we show results from the application of these constraints to the measurement of organic aerosol composition at two different field locations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Validation of Multiresidue Method for Analysis of 31 Pesticides in Rice Using Gas Chromatography-Tandem Mass Spectrometry

Five modified QuEChERS were tested for the multiresidue analysis of 31 pesticides in rice. Rice was spiked with mixture solution of pesticides at 10 ng/g. Method selection was based on the LODs (sensitivity) and recovery tests (accuracy) of the pesticides. Analysis was done in GC-tandem MS in multiple reaction monitoring mode with a total run time of approximately 37 min. The selected method was validated after spiking rice at 20 and 100 ng/g in rice. The performance characteristics of the method impacted for all selected pesticides were acceptable according to the guidelines for method validation (recovery of 70-120% with an RSD of <20% and r2value of ≥0.99). For rice, matrix effect on the signals of the compounds was corrected by using matrixmatched calibration standards. The LOQs met the requirements of the maximum residue limits for pesticides in rice. The developed method allowed for the simultaneous determination and confirmation of a large number of different groups of pesticides and was fast, simple, inexpensive, and useful for the routine analysis of rice.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Cryogenic thermocouple calibration tables

Thermocouple calibration standards are developed for low-temperature thermocouple materials. Thermovoltage, thermopower, and the thermopower derivative are presented in tabular and graphical form.

Hall, W. J.↗

Improved relay chatter detector

Detector provides go/no-go sensing of momentary relay or contact opening during vibration testing. Device compares duration of unwanted openings to calibrated standard and lights indicator if standard is exceeded. Stability and reliability are higher than in any other comparable device.

Reynolds, R. K.↗

Snow-extent mapping and lake ice studies using ERTS-1 MSS together with NOAA-2 VHRR

Five snow extent maps of the 5,601 sq km American River Basin were prepared using a Zoom Transfer Scope from ERTS-1 MSS band 4 imagery. The maps were generally completed within one hour. A snowmelt curve based on ERTS-1 imagery was used as a calibration standard or comparison for maps prepared from NOAA-2 VHRR imagery in the same manner. Cost comparisons with U-2 derived imagery indicate that ERTS-1 snow mapping of the basins is six times faster. Conservative estimates of comparable aircraft snow survey flights yields a cost figure 200 times that of the ERTS-1 snow map. Snow mapping attempts in the Lake Ontario Basin demonstrated that ERTS-1 is not well suited to large basins. Optimum size of basins for ERTS studies is believed to range from about 250 sq km to 30,000 sq km. The value of the ERTS-1 MSS for Great Lake ice evaluation was proved during the past winter on Lake Erie. Not only were ice features and types of ice identified, but melting ice was detected through the combined use of band 5 and band 7. Ice movement (direction and speed) was mapped by examining imagery from two successive days.

Wiesnet, D. R.↗

Review of Terrestrial Photovoltaic Measurements Workshop

Measurement methods for terrestrial solar cells require calibration standards to set simulator irradiance levels or to monitor solar irradiance in outdoor measurements. Measurements of solar cell performance in terrestrial sunlight are the most acceptable, but an artificial light source can be used for laboratory measurements.

Brandhorst, H. W., Jr.↗

90-GHz flux-density measurements of variable radio sources

Results are presented for measurements of the flux densities of 10 variable extragalactic sources at 85.2 or 90 GHz, which were made over a period of almost seven years with the NRAO 36-ft millimeter-wave antenna. The primary flux-density calibration standards used include Jupiter, Saturn, Mars, and the small-diameter Galactic source DR 21. Measured flux densities are given as a function of time (in years) for the sources 3C 84, NRAO 150, 3C 120, OJ 287, 4C 39.25, 3C 273, 3C 279, 3C 345, BL Lac, and 3C 454.3. No statistically meaningful flux-density changes during an observing interval (1 to 3 days) are detected for any source, and a high degree of correlation between flux-density variations at 85.2 or 90 GHz and those observed at lower frequencies is found in all 10 sources. Some variations observed at different frequencies in several individual sources are briefly discussed.

Hobbs, R. W.↗

A review of issues and strategies in nondestructive evaluation of fiber reinforced structural composites

Techniques for quantitative assessment of the mechanical strength and integrity of fiber composites during manufacture and service and following repair operations are presented. Problems and approaches are discussed relative to acceptance criteria, calibrating standards, and methods for nondestructive evaluation of composites in strength-critical applications. Acousto-ultrasonic techniques provide the methods of choice in this area.

Vary, A.↗

Results of the 1978 NASA/JPL balloon flight solar cell calibration program

The 1978 scheduled solar cell calibration balloon flight was successfully completed. Thirty six modules were carried to an altitude of above 36 kilometers. Recovery of telemetry and flight packages was without incident. These calibrated standard cells are used as reference standards in simulator testing of cells and arrays with similar spectral response characteristics. The factors affecting the spectral transmission of the atmosphere at various altitudes are summarized.

Seaman, C. H.↗

Further laboratory studies and stratospheric flight of a mass spectrometer beam system

A gas expansion system combined with a mass spectrometer has been tested and flown successfully in the stratosphere. Through a sequence of orifices and high speed pumping, gas particles were formed into a molecular beam and analyzed by a sensitive mass spectrometer. During two balloon flights, vertical profiles of all major atmospheric constituents as well as O3, CO2, H2O and others were obtained. Gases such as AR38 and O16;O17 provided in-flight calibration standards. The sensitivity of the system was such that gases with mixing ratios of 10 ppb at an ambient pressure of about 10 mbar were detectable.

Mauersberger, K.↗