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Analysis of impurities in magnesium oxide materials by mass spectrographic, chemical, thermogravimetric, vacuum-fusion furnace, quartz tube graphite crucible furnace techniques
We present a detailed chemical abundance analysis of the brightest star in the ultrafaint dwarf (UFD) galaxy candidate Cetus II from high-resolution Magellan/MIKE spectra. For this star, DES J011740.53-173053, abundances or upper limits of 18 elements from carbon to europium are derived. Its chemical abundances generally follow those of other UFD galaxy stars, with a slight enhancement of the α-elements (Mg, Si, and Ca) and low neutron-capture element (Sr, Ba, and Eu) abundances supporting the classification of Cetus II as a likely UFD. The star exhibits lower Sc, Ti, and V abundances than Milky Way (MW) halo stars with similar metallicity. This signature is consistent with yields from a supernova originating from a star with a mass of ∼11.2 M$_{⊙}$. In addition, the star has a potassium abundance of [K/Fe] = 0.81, which is somewhat higher than the K abundances of MW halo stars with similar metallicity, a signature that is also present in a number of UFD galaxies. A comparison including globular clusters and stellar stream stars suggests that high K is a specific characteristic of some UFD galaxy stars and can thus be used to help classify objects as UFD galaxies.
Mass spectrographic impurity analysis of magnesium oxide powders and compacts
Impurity analysis of nonconductors and gases by spark-source mass spectrography techniques
Mass and emission spectrographic analyses of magnesium oxide and tantalum carbide to determine impurities
A newsletter article to appear in the FY 2022 Q1 issue of the LDRD Quarterly Highlights, https://www.lanl.gov/projects/ldrd-tri-lab/quarterly-highlights.php.
Summary of lunar sample chemical analyses scheme
Presentation to be presented during the Site-Directed Research and Development (SDRD) program FY 2021 review meeting (Webex), September 22–23, 2021.
An apparatus is provided which can process numerous samples that must be chemically analyzed by the application of fluids such as liquid reagents, solvents and purge gases, as well as the application of dumps for receiving the applied fluid after they pass across the sample, in a manner that permits numerous samples to be processed in a relatively short time and with minimal manpower. The processor includes a rotor which can hold numerous cartridges containing inert or adsorbent material for holding samples, and a pair of stators on opposite sides of the rotor. The stators form stations spaced along the path of the cartridges which lie in the rotor, and each station can include an aperture in one stator through which a fluid can be applied to a cartridge resting at that station, and an aperture in the other stator which can receive the fluid which has passed through the cartridge. The stators are sealed to the ends of the cartridges lying on the rotor, to thereby isolate the stations from one another.
As part of a detailed NASA-sponsored study of chemical composition/property sensitivity of the LARC-160 polymerization of monomeric reactants (PMR) polyimide system, a number of liquid chromatographic techniques have been employed. The ester monomers in this system are characterized by a reverse-phase ion-suppression method. Mono, di, and triesters of the 3,3',4,4'-benzophenonetetracarboxylic acid ingredient are identified and their isomeric forms resolved. The 5-norbornene-2,3-dicarboxylic acid ester (nadic ester) endcapper is detected by low wavelength ultraviolet sensing. A second method, reverse-phase ion-pair chromatography, is employed for determining unreacted amines. The extent of resin B-staging is monitored through analysis of the ester/amine oligomers.
Mass spectroscopy and chemical deposition techniques for determining hydroxyl content in magnesium oxide
The Hyperspectral X-ray Imaging (HXI) project will enable non-destructive chemical-state determination of nano-scale samples in the electron microscope for nuclear safeguards applications. To efficiently measure chemical state through electron-excited X-ray emission requires a combination of wide spectral bandwidth, high resolution, and high count rate capability. We are building a next-generation X-ray detector based on an array of transition edge sensors (TESs) to make these measurements possible and routine in the scanning electron microscope (SEM). Leveraging the large pixel densities afforded by microwave multiplexing readout and continuous, uninterrupted operation of a cryogen-free dilution refrigerator, this instrument will have efficiency to allow chemical species identification of nano-scale samples in hours instead of days to weeks. We describe prototype pixel designs for this HXI instrument, comprising three pixel types that will make up the hybrid TES array. Engineering design of the integrated HXI cryostat and SEM system is in progress, with full detector commissioning expected in Spring 2021 followed closely by full-scale integration with the SEM. Furthermore, we also report on the commissioning of a complementary TES-based X-ray emission spectroscopy platform for bulk samples to build a spectral library for HXI sample identification.
This paper continues the annual tradition of summarizing at this conference the results of chemical analyses performed on archival potable water samples returned from the International Space Station (ISS). 2016 represented a banner year for life on board the ISS, including the successful conclusion for two crew members of a record one-year mission. Water reclaimed from urine and/or humidity condensate remained the primary source of potable water for the crew members of ISS Expeditions 46-50. The year 2016 was also marked by the end of a long-standing tradition of U.S. sampling and monitoring of Russian Segment potable water sources. Two water samples taken during Expedition 46 in February 2016 and returned on Soyuz 44, represented the final Russian Segment samples to be collected and analyzed by the U.S. side. Although anticipated for 2016, a rise in the total organic carbon (TOC) concentration of the product water from the U.S. water processor assembly due to breakthrough of organic contaminants from the system did not materialize, as evidenced by the onboard TOC analyzer and archive sample results.
This paper continues the annual tradition, at this conference, of summarizing the results of chemical analyses performed on archival potable water samples returned from the International Space Station (ISS). 2016 represented a banner year for life aboard the ISS, including the successful conclusion for 2 crewmembers of a record 1-year mission. Water reclaimed from urine and/or humidity condensate remained the primary source of potable water for the crewmembers of ISS Expeditions 46-50. The year was also marked by the end of a long-standing tradition of U.S. sampling and monitoring of Russian Segment potable water sources. Two water samples, taken during Expedition 46 and returned on Soyuz 44 in March 2016, represented the final Russian Segment samples to be collected and analyzed by the U.S. side. Although anticipated for 2016, a rise in the total organic carbon (TOC) concentration of the product water from the U.S. water processor assembly due to breakthrough of organic contaminants from the system did not materialize, as evidenced by the onboard TOC analyzer and archival sample results.
Analytical chemical techniques for refractory metals, metal carbides, and metal oxides
Measure the elemental composition in both random meteors and in the bolides forming specific meteor streams (these are traceable to specific small bodies in the solar system). These will yield the average chemical composition and degree of chemical variability in a statistically significant number of planetesimals. CAPO-SUMS is functionally equivalent to a series of multiple, small-body sample analysis missions, but provides much more analytical capability than is possible on any orbital or flyby mission due to the vaporization, ionization and ultraviolet emission from the ablating bolide as it enters the atmosphere. CAPO-SUMS will provide a chemical context from which the detailed analytical studies provided by a cometary or asteroidal lander mission can be interpreted.
The detonation of high explosives produces a wide variety of particulate matter (PM) with distinct properties, not all of which are traditionally studied for chemical composition, formation processes, and forensic applications. We report particle-resolved measurements of Composition B detonation soot using soot particle aerosol mass spectrometry (SP-AMS), identifying carbonaceous species and metals not previously characterized on a single-particle basis. Results are combined with scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS) to enhance source-dependent signatures. Black carbon, including graphitic carbon and detonation nanodiamonds, contributed 50.5-71.4% of PM 2.5 mass, while 22.5-43.4% was non-refractory organic carbon, a previously overlooked component that exhibited a complex and varying composition. Detonations were performed with and without PMMA confinement and under steady and overdriven conditions. Distinct particles enriched with polycyclic aromatic hydrocarbons (PAHs) were observed in experiments utilizing confinement, with quantities dependent on manufacturing method. SEM-EDS validated SP-AMS findings of metals internally mixed with carbonaceous species and extended the particle size range to 100 µm. This work makes detecting non-refractory organics using single-particle techniques more feasible for detonation forensics and understanding high-energy soot formation. While this analysis uses offline sample collection, SP-AMS could be deployed for in-situ measurements of detonation PM 2.5 transported in the atmosphere.
Numerous 'extended impacts' found in both leading and trailing edge capture cells were successfully analyzed for the chemical composition of projectile residues by secondary ion mass spectrometry (SIMS). Most data were obtained from the trailing edge cells where 45 of 58 impacts were classified as 'probably natural' and the remainder as 'possibly man-made debris.' This is in striking contrast to leading edge cells where 9 of 11 impacts so far measured are definitely classified as orbital debris. Although all the leading edge cells had lost their plastic entrance foils during flight, the rate of foil failure was similar to that of the trailing edge cells, 10 percent of which were recovered intact. Ultraviolet embrittlement is suspected as the major cause of failure on both leading and trailing edges. The major impediment to the accurate determination of projectile chemistry is the fractionation of volatile and refractory elements in the hypervelocity impact and redeposition processes. This effect had been noted in a simulation experiment but is more pronounced in the LDEF capture cells, probably due to the higher average velocities of the space impacts. Surface contamination of the pure Ge surfaces with a substance rich in Si, but also containing Mg and Al, provides an additional problem for the accurate determination of impactor chemistry. The effect is variable, being much larger on surfaces that were exposed to space than in those cells that remained intact. Future work will concentrate on the analyses of more leading edge impacts and the development of new SIMS techniques for the measurement of elemental abundances in extended impacts.