Formation of Homogenous dU/Nb Analytical Reference Materials via Mechanical Alloying
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Materials science↗
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Aerodynamic thermal simulation system. Part 3: Related reference material (instruction manual)
For abstract, see .
Kitchar, A. F.↗
Reflectance characteristics of reference materials used in lidar hard target calibration
Lidar hard target calibration is discussed, emphasizing the transfer target methodology. Characteristics of example calibratrion target surfaces are described in light of four reflectance mechanisms, specular, diffuse, retroreflection, and off-specular reflectance. The ideal transfer target is one which can be described as entirely diffusely reflecting, i.e., Lambertian. Correction for retroreflection is required when using the flowers of a sulfur transfer target at CO2 laser wavelengths. Corrections for specular and retroreflection for the integrating sphere are negligible; however, the off-specular reflectance of rough metal surfaces used in the integrating spheres is only qualitatively compared with the diffuse reflectance of flowers of sulfur.
Haner, David A.↗
Lidar Hard Target Calibration: Preliminary Study of Reference Materials for 2(sub mu)m Lidars
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hard target calibration 2↗
Developmental status of thermionic materials.
Reference materials selected for the major components of the unit cell of a thermonic fuel element are described. Out-of-pile and in-pile evaluation results are given. Current efforts for improving the life and performance of thermionic fuel element are outlined.
Yang, L.↗
National Aerospace Professional Societies and Associations and Organizations
This session will highlight several highly recognized National Technical and Professional Aerospace Societies, Associations and Organizations that are dedicated to the advancement of the theories, practices and unique applications of Science, Engineering and related Aerospace Activities ongoing in the United States. The emphasis will be on at least three (3) Aerospace Organizations, while reference many others. This paper will provide a wealth of educational references, information, opportunities and services available through many of the National and Local Chapter Affiliates, associated with the respective associations. Again, all experience and knowledge levels (K-12) will benefit from this information and reference material. Reference materials and other points of contact will be made available to all attendees.
Henderson, Arthur J., Jr.↗
Figures of Merit Software: Description, User's Guide, Installation Notes, Versions Description, and License Agreement
Figures of Merit (FoMs) and the FoM software provide a method for quantitatively evaluating the quality of a regolith simulant by comparing the simulant to a reference material. FoMs may be used for comparing a simulant to actual regolith material, specification by stating the value a simulant s FoMs must attain to be suitable for a given application and comparing simulants from different vendors or production runs. FoMs may even be used to compare different simulants to each other. A single FoM is conceptually an algorithm that computes a single number for quantifying the similarity or difference of a single characteristic of a simulant material and a reference material and provides a clear measure of how well a simulant and reference material match or compare. FoMs have been constructed to lie between zero and 1, with zero indicating a poor or no match and 1 indicating a perfect match. FoMs are defined for modal composition, particle size distribution, particle shape distribution, (aspect ratio and angularity), and density. This TM covers the mathematics, use, installation, and licensing for the existing FoM code in detail.
hoelzer, H. D.↗
Measuring Thermal Conductivity at LH2 Temperatures
For many years, the National Institute of Standards and Technology (NIST) produced reference materials for materials testing. One such reference material was intended for use with a guarded hot plate apparatus designed to meet the requirements of ASTM C177-97, "Standard Test Method for Steady-State Heat Flux Measurements and Thermal Transmission Properties by Means of the Guarded-Hot-Plate Apparatus." This apparatus can be used to test materials in various gaseous environments from atmospheric pressure to a vacuum. It allows the thermal transmission properties of insulating materials to be measured from just above ambient temperature down to temperatures below liquid hydrogen. However, NIST did not generate data below 77 K temperature for the reference material in question. This paper describes a test method used at NASA's Marshall Space Flight Center (MSFC) to optimize thermal conductivity measurements during the development of thermal protection systems. The test method extends the usability range of this reference material by generating data at temperatures lower than 77 K. Information provided by this test is discussed, as are the capabilities of the MSFC Hydrogen Test Facility, where advanced methods for materials testing are routinely developed and optimized in support of aerospace applications.
Selvidge, Shawn↗
The Genesis Non-flight Implant Sample Archive
Introduction: For the past 20 years the Genesis science community has been analyzing solar wind captured in sample collectors now curated at Johnson Space Center (JSC). Non-flown flight like collector materials (non-flight) considered reference material was always allocated by the JSC Genesis team for testing experimental procedures. However, to expedite Genesis science, distribution of non-flown reference materials were also provided by, D. S. Burnett (Genesis PI, Caltech) and A. J. G. Jurewicz (ASU) who were funded to aid all Genesis PIs by providing engineering test materials archived at Caltech pre-flight as well as ion implants into these materials [1]. Implanted materials (non-flight reference, flight-like semiconductor materials, and NIST SRM glass) received from the Caltech collection during a pilot project are being used to develop an accession procedure for the purpose of making these materials available to researchers in the future. These implant samples are important because they can be utilized as measurement standards [2]. This is a work in progress and this work reports progress in documentation and imaging. The pilot program received 63 implanted reference materials with known implanted ions. Genesis Non-Flight Database: The existing non-flight material database was modified to allow for the description of implant sessions and to allow correlation of the implant information to individual specimens. An implant session has three main components: a known ion, a known dose (ion/cm2), and a known energy (keV). Procedure: Laboratory Procedure. Upon receiving non-flight analytical standards (independently calibrated implants), or implant samples (nominally calibrated implants), they will be imaged in their current containers to capture any information written before being brought into the Genesis Sample Laboratory. Documentation is provided by the donor and used for correlating the data between the implant sessions and implant samples. This information is not verified by Genesis Curation. The microscope used to image samples in the laboratory has an automated stage with a stainless-steel plate to hold samples and a camera that utilizes the software Surveyor to take photomosaic images of the implant samples. The camera attached to the microscope is a QICAM High Performance IEEE 1394 FireWire Digital CCD Camera. This setup, shown in Fig. 1, allows for photomosaics of small-scale samples with a 10x objective or 25x objective. Examples of images taken with this microscope setup are shown in Fig.2 and Fig. 3. After imaging, samples get stored in a clean fluoroware container or polypropylene vial depending on sample size for long term storage. Database Procedure. The Genesis Non-Flight Database currently allows for the addition of implant sessions. The required fields for adding an implant session are the implant session ion, the implant session dose, and the implant session energy. There are also fields for the date and vendor of the sessions as well as a field for if the session was calibrated or not. Once an implant session has been inserted into the database, additional documentation from the session can be attached. The database will automatically assign an Implant Session Number. After inserting an implant session, the implanted samples can be inserted. The fields required for an implant sample are the material of the sample and the size of the sample. The Generic name for the implant sample with be automatically generated by the database once it has been inserted. Implant sample numbers begin with 3X to distinguish from flown Genesis sample numbers. There are also fields for processors to add the location (room, cabinet, tray) and container type (fluoroware, polypropylene vial). Once an implant session and an associated sample(s) have been inserted into the database the sample can be then tied to all associated implant sessions. An implant sample can be tied to multiple implant sessions. Future work: For curation, future work consists of creating an online catalogue for implant samples as well as updating the database with more samples as we receive them. For the scientific community these implant samples have many potential uses. For Genesis research, they are directly applicable for testing and, in some cases, as analytical standards. For non-Genesis research, implants (especially calibrated implants) could be used for calibrating other, unique planetary materials [1].
C D Calva↗
Mid-infrared reflectlance spectra (2.3-22 micions) of sulfur, gold, KBr, MgO, and halon
Biconical diffuse reflectance spectra in the mid-infrared are presented for powder and other solid forms of sulfur, gold, potassium bromide, magnesium oxide, and halon. Comparisons are made with previously published results of other investigators, and recommendations are made regarding the relative usefulnees of these materials as reflectance standards in the mid-IR. Sulfur has strong intrinsic bands at wavelengths greater than 7 microns that must be taken into account for its use as a reflectance standard. Some sulfur samples have hydrocarbon contaminants and in powder form may have adsorbed water, both of which produce bands in the 3-4-micron region. Potassium bromide has several weak intrinsic bands and is very sensitive to adsorbed water contamination; otherwise it is a good IR reference material. Magnesium oxide and halon have major bands structure and low reflectivity at wavelengths greater than 2.6 microns and thus are unsuitable as reference materials in the mid-IR. Vapor-deposited gold on fine sandpaper (600 grit) is very bright, spectrally flat, and fairly diffuse, so it is the superior material (of those examined) for reflectance reference material throughout the IR. Fine gold powder, on the other hand, is much less bright than evaporated gold, and its reflectivity at wavelengths greater than its particle size is highly sensitive to particle packing density.
Nash, D. B.↗
ORNL Report of Analysis for the Verification of NRMP CRM U030A
In support of the Certified Reference Material (CRM) program managed by the Nuclear Reference Material Program (NRMP), the Material Signatures and Isotopic Standards (MSIS) group of Oak Ridge National Laboratory (ORNL) was asked to prepare a set of CRM U030A units for use as standards for isotopic analysis using multicollector thermal ionization mass spectrometry (TIMS) and inductively coupled plasma mass spectrometry (ICP-MS) instruments. This report documents the results of the verification measurements performed on three randomly selected units by the MSIS group’s ISO/IEC 17025:2017 accredited operating procedure CSD-AM-CIMS-IN20, Determination of Uranium and Plutonium Isotopic Composition using Thermal Ionization Mass Spectrometry [1], and in accordance with the quality assurance plan as described in QAP-X-96-CSD/RML-001, Nuclear Analytical Chemistry Laboratory Section Quality Assurance Plan [2].
Mathew, Kattathu [Oak Ridge National Laboratory (O↗
Boron isotopic analysis in bulk silicate materials using the Neoma MS/MS MC-ICP-MS
Boron (B) isotopes are a valuable tracer with applications ranging from geological, environmental, and nuclear studies because B isotopic fractionation is highly sensitive to chemical processes yielding distinct isotopic trends in natural and anthropogenic systems. Despite this wide applicability, there remain relatively few measurements on well-described reference materials and in some cases, poor agreement between various methods. We report a method for boron isotope ratio measurement in solution on the Neoma MS/MS MC-ICP-MS specifically targeting bulk silicates. We evaluate the performance of the method and instrument as it relates to the measurement of the absolute boron isotope ratio ( 10 B/ 11 B). The results indicate that the method produces data in agreement with literature values and that the sample–standard bracketing technique is appropriate for the Neoma MS/MS MC-ICP-MS which has been in use for decades on previous generation instruments. Careful tuning of the MS/MS lenses is required to obtain precision comparable to non MS/MS equipped MC-ICP-MS. With careful tuning, internal and external precisions of ∼0.3‰ were achieved. However, when the MS/MS is not properly tuned external precisions exceed 3‰. Nevertheless, our results for IAEA B-6, BCR-2, BHVO-2 and W-2a reference materials overlap the 1σ range of previously reported 10 B/ 11 B. Data are reported for total boron quantities down to a few tens of nanograms. Our procedure yielded blanks as low as 3 ng but up to 29 ng, making blank corrections important for small samples sizes in the few 10s of nanogram range. We report B isotope ratios for AGV-2G, SL-1G, GSC-2G, GSD-2G, GSE-2G, RLS-132, RLS-140, NKT-1G, and T1-G glass reference materials that have not been previously reported in the literature.
Scott, Sean R. [Pacific Northwest National Laborat↗
Genesis Solar Wind Sample Curation Documentation
Introduction: A scientist with experience as a sample science analyst, provider of flight hardware for multiple missions, and senior engineer in an ISO 2000-rated manufacturing plant has described the timeline of key participants in any PI-led sample return mission, the breadth of the organizations involved [1,2], and, of interest to this meeting, choosing the types of data to preserve and issues of future data accessibility. This work broadens that perspective by giving similar lessons from Genesis sample curation point-of-view. Curation participation regarding data gathering was part of the mission review process from the beginning. Genesis’ story illustrates outcome of several choices about types of data to record and preserve. Precision analysis of solar wind atoms captured in pure, ultraclean substrates is the driving science goal; therefore, detailed documentation was captured from all mission and curation phases and from investigator laboratories because these processes affect the final analytical results [3]. Pre-flight: Design and fabrication of the spacecraft. Like many modern small sample return missions, Genesis was a tightly managed team integrated across science, engineering and curation. Communication across the team was excellent, and, for the most part, the hands-on engineering technicians understood the impacts of “small choices” they routinely make, and the eyes-on oversight of manufacturing processes by scientists was mindful of details. The payload was designed by the Jet Propulsion Laboratory and the spacecraft by Lockheed Martin. Solar wind collectors and instruments were fabricated by multiple vendors and laboratories. The main portion of the payload was assembled at JSC. Fabrication procedures and contamination-control data (with witness coupons) were stored primarily at JSC. The original composition, dimensions and configuration of components, results of thermal testing, etc. are still needed for interpretation of analytical data. At times, these must be estimated from secondary information acquired pre-flight. Moreover, some files (e.g., original 3-D models and early Powerpoint) cannot be opened using software. Archived curation data includes 2-D drawings, material usage lists, QA documentation and analyses of consumables used during fabrication. Important chemical information still resides in archived hardware, paints and lubricants, material coupons, cleaning coupons, environmental witness plates and reference materials from manufacturing facilities. Purity and cleanliness of collector substrates. Semi-conductor vendors provided surface cleanliness data and some purity data. Purity for specific elements of interest was verified by science team members in their laboratories [4]. Curation archived procurement and shipping records, analysis reports, and non-proprietary fabrication data. A physical archive of flight collector reference materials is maintained for future use so additional data can be collected as analytical techniques improve. These are of increased value due to the hard landing upon re-entry. Cleaning and cleanliness assessments of flight hardware. Cleaning of the science canister payload was performed at JSC in a dedicated ISO 4 cleanroom using ultrapure water (UPW). The cleanliness of this UPW was monitored throughout processing. The archive for the clean lab also includes airborne particle counts, airborne molecular and inorganic contamination measurements as well as cleanroom construction material coupons and witness coupons. Hardware cleanliness was assessed by particle counts in rinse water batches. This information is recorded in batch cleaning forms and logbooks, and are, perhaps, of decreased value due to the hard landing. Post-flight: Curation-generated data. The curation handling history of each Genesis sample is documented in a typical astromaterials sample database which captures sample location, physical description and characterization data. Samples have a “shelf life”. Crucial to the preservation of samples is ongoing documentation of the sample environment, initially under curatorial control but is now a separate facility function with requires coordination. PI-generated data. Data on sample characterization and cleaning techniques continues to be generated by sample users [5]. These are often captured in LPSC abstracts, but these “engineering” results often are not publishable as stand-alone papers. We are actively looking for ways to make this information more accessible to users. Ion implants into samples have aided science return and can be shared among investigators. These (and similar) materials should be added to the curatorial collection with appropriate process and characterization data generated externally. Summary: Complete data archives for returned astromaterial samples must be broad in types and formats, and inclusive of environmental monitoring.
Genesis↗
Developmental status of thermionic materials.
Description of the reference materials selected for the major components of the unit cell of a thermionic pile element (TFE), the out-of-pile and in-pile test results, and current efforts for improving the life and performance of thermionic fuel elements. The component materials are required to withstand the fuel burnup and fast neutron fluence dictated by the thermionic reactor system. Tungsten was selected as the cladding material because of its compatibility with both the carbide and the oxide fuel materials. Niobium was selected as the collector material because its thermal expansion coefficient matches closely with that of the thin aluminum oxide layer used to electrically insulate the collector from the TFE sheath. An unfueled converter has performed stably over 41,000 hr. Accelerated irradiation tests have attained burnups equivalent to that for 40,000 hr of the thermionic reactor under consideration.
Yang, L.↗
High sensitivity measurement of femtogram-level 238 Pu by thermal ionization mass spectrometry with correction of background 238 U
Low-concentration plutonium isotopic measurements provide a valuable fingerprint to identify possible material origins in the context of environmental contamination monitoring, environmental tracing, nuclear safeguards, nuclear forensics, and treaty monitoring. Thermal ionization mass spectrometry (TIMS) has long been recognized as one of the most sensitive techniques for plutonium isotopic measurement, but has not generally been utilized for 238 Pu determination, especially at low concentrations, due to an isobaric interference from 238 U, prevalent as background. Here, this work demonstrates a new analytical technique for correction of background 238 U from the 238 Pu counts collected during a TIMS analysis. The technique takes advantage of the higher ionization temperature of U relative to Pu and uses a 235 U tracer added after plutonium purification chemistry for 238 U semi-quantitative determination. This technique has been successfully applied to the determination of 238 Pu concentration and the 238 Pu/ 239 Pu ratio in sample types including single-isotope standards, isotopic certified reference materials, matrix-containing environmental reference materials, and simulated nuclear detonation debris. The results have been directly compared on a sample-by-sample basis to alpha spectrometry results. The detection limit by this new technique is 0.23 fg 238 Pu, which was previously unachievable by mass spectrometry and is possible in around 1 h of analysis time post-chemistry compared to weeks of required counting time by alpha spectrometry (at the same atom amount). We also present original, high precision data for Pu isotope concentrations in IAEA-384, Fangataufa Sediment, including 242 Pu results for the first time. The new technique allows measurement of a key isotope, 238 Pu, that was previously not measured in small environmental or nuclear forensics collections.
238Pu↗
Plutonium isotope ratio measurements by total evaporation-thermal ionization mass spectrometry (TE-TIMS): an evaluation of uncertainties using traceable standards from the New Brunswick Laboratory
The accuracy and precision of isotope amount ratio measurements using thermal ionization mass spectrometry (TIMS) instrumentation are described, and the measurement of Pu materials is emphasized. The mass fractionation observed for Am, Ga, Pu, and U for isotope amount ratio measurements using the total evaporation (TE) technique is compared with theoretical estimates to demonstrate the advantage of the TE methodology and to investigate systematic biases in the major isotope amount ratios of U and Pu certified reference material (CRM) standards from the U.S. provider of CRMs. The quality of the Pu isotopic data generated by TIMS instruments in an analytical laboratory is demonstrated by the application of the double ratio technique to estimate the 241 Pu half-life. Analytical data on traceable Pu CRMs from the New Brunswick Laboratory (NBL), generated as part of routine measurements supporting various programs, are used for this half-life estimation. Although the 241 Pu abundances in CRMs of 136, 137, 138, and 126-A are approximately 200–2000× smaller than those in the 241 Pu material used in the previous Institute for Reference Materials and Measurements (IRMM) evaluation of the 241 Pu half-life, the half-life value estimated in this work shows excellent agreement with the currently accepted value from the IRMM. This agreement also demonstrates the pedigree of the Pu isotopic standards from the NBL and the quality of the isotope amount ratio measurements using TIMS instrumentation. For both the major and minor Pu isotope amount ratios, this report describes the relative importance of the factors affecting the uncertainty of TIMS measurements, which are considered the gold standard in isotope ratio measurements (LA-UR-24-29199).
07 ISOTOPE AND RADIATION SOURCES↗
Quantitative Technique for Comparing Simulant Materials through Figures of Merit
The 1989 workshop report entitled Workshop on Production and Uses of Simulated Lunar Materials and the Lunar Regolith Simulant Materials: Recommendations for Standardization, Production, and Usage, NASA Technical Publication both identified and reinforced a need for a set of standards and requirements for the production and usage of the Lunar simulant materials. As NASA prepares to return to the Moon, and set out to Mars, a set of early requirements have been developed for simulant materials and the initial methods to produce and measure those simulants have been defined. Addressed in the requirements document are: 1) a method for evaluating the quality of any simulant of a regolith, 2) the minimum characteristics for simulants of Lunar regolith, and 3) a method to produce simulants needed for NASA's Exploration mission. As an extension of the requirements document a method to evaluate new and current simulants has been rigorously defined through the mathematics of Figures of Merit (FoM). Requirements and techniques have been developed that allow the simulant provider to compare their product to a standard reference material through Figures of Merit. Standard reference material may be physical material such as the Apollo core samples or material properties predicted for any landing site. The simulant provider is not restricted to providing a single "high fidelity" simulant, which may be costly to produce. The provider can now develop "lower fidelity" simulants for engineering applications such as drilling and mobility applications.
Rickman, Doug↗
Design and Materials of Reference Electrodes for Radioactive Waste Tank Service – A Literature Review
The Hanford site stores approximately 55 million gallons of radioactive and chemically hazardous wastes from the production of weapons materials. The wastes are stored in 177 underground, carbon steel storage tanks, 149 of these are single shell tanks (SSTs) and 28 of these are double shell tanks (DSTs). The DSTs provide critical retrieval and interim storage before the waste is vitrified in the Waste Treatment and Isolation Plant (WTP). The DSTs have been in service for 38 to 56 years and current plans indicate that WTP operations will be completed in 2075. Thus, the tanks will need to remain in service far beyond the initial 40-year life expectancy. For life extension of the tanks, effective corrosion control practices must remain in force. This effort includes direct measurements of the extent of corrosion (e.g., ultrasonic measurements and corrosion coupons) and electrochemical processes (e.g., linear polarization measurements).
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗