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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
NASA NTRS2003

Quantitating Iron in Serum Ferritin by Use of ICP-MS

A laboratory method has been devised to enable measurement of the concentration of iron bound in ferritin from small samples of blood (serum). Derived partly from a prior method that depends on large samples of blood, this method involves the use of an inductively-coupled-plasma mass spectrometer (ICP-MS). Ferritin is a complex of iron with the protein apoferritin. Heretofore, measurements of the concentration of serum ferritin (as distinguished from direct measurements of the concentration of iron in serum ferritin) have been used to assess iron stores in humans. Low levels of serum ferritin could indicate the first stage of iron depletion. High levels of serum ferritin could indicate high levels of iron (for example, in connection with hereditary hemochromatosis an iron-overload illness that is characterized by progressive organ damage and can be fatal). However, the picture is complicated: A high level of serum ferritin could also indicate stress and/or inflammation instead of (or in addition to) iron overload, and low serum iron concentration could indicate inflammation rather than iron deficiency. Only when concentrations of both serum iron and serum ferritin increase and decrease together can the patient s iron status be assessed accurately. Hence, in enabling accurate measurement of the iron content of serum ferritin, the present method can improve the diagnosis of the patient s iron status. The prior method of measuring the concentration of iron involves the use of an atomic-absorption spectrophotometer with a graphite furnace. The present method incorporates a modified version of the sample- preparation process of the prior method. First, ferritin is isolated; more specifically, it is immobilized by immunoprecipitation with rabbit antihuman polyclonal antibody bound to agarose beads. The ferritin is then separated from other iron-containing proteins and free iron by a series of centrifugation and wash steps. Next, the ferritin is digested with nitric acid to extract its iron content. Finally, a micronebulizer is used to inject the sample of the product of the digestion into the ICPMS for analysis of its iron content. The sensitivity of the ICP-MS is high enough to enable it to characterize samples smaller than those required in the prior method (samples can be 0.15 to 0.60 mL).

Smith, Scott M.↗
NASA NTRS2017

Diffusivities of Redox-Sensitive Elements in Basalt vs. Oxygen Fugacity Determined by LA-ICP-MS

Several diffusion experiments were conducted in a piston cylinder device across a range of oxygen fugacities (FMQ-3 FMQ-1.2, FMQ+6) at 1 GPa and 1300 C. This was done to explore the effects of oxygen fugacity (fO2) on diffusivity of redox sensitive trace elements. This allows investigation of how these elements diffuse across the fO2 range encountered in different reservoirs on planets and moons in our solar system. The University of Rochester LA-ICP-MS system was used for analysis of samples. Analyses were conducted using an Agilent 7900 quadrupole mass spectrometer connected to a Photon Machines 193 nm G2 laser ablation (LA) system equipped with a HelEx 2-volume sample chamber. Spots used were 35 micrometers circles spaced at 65 micrometers intervals. Laser fluence was 7.81 J/cm^2 with a rep rate of 10 Hz. The iolite software package was used to reduce data collected from laser ablation analysis of experiments with Si-29 used as the internal standard isotope. Iolite's global fit module was used to simultaneously fit elements' diffusivities in each experiment while keeping the Matano interface constant. Elements analysed include V, Nb, W, Mo, La, Ce, Pr, Sm, Eu, Gd, Ta, and W. Figures

Szumila, Ian↗
NASA NTRS2005

Siderophile Element Profile Measurements in Iron Meteorites Using Laser Ablation ICP-MS

Understanding the behaviour of siderophile elements during cooling of iron meteorites can lead to insight into the general thermal histories of the meteorites as well as their respective parent bodies. Traditionally trace element analyses in meteorites have been done using techniques that only measure the average concentration in each phase. With these methods, all of the spatial information with respect to the distribution of an element within one phase is lost. Measuring concentration profiles of trace elements in meteorites is now possible, with the advent of high-resolution analytical techniques such as laser ablation, inductively coupled plasma mass spectrometry (LA-ICP-MS) with spatial resolution <20 microns. [e.g. 1,2] and secondary ion mass spectrometry [3]. These profiles can give more insight into both the partitioning and diffusive behavior of siderophile elements in metal systems relevant to iron meteorites, as well as parent body cooling rates.

Watson, H. C.↗
DOE OSTI2025

Preliminary Insights Into the Feasibility of Determining the Purification Date of Enriched Uranium by Direct Measurement of the 230 Th/ 234 U Ratio Using an All-Faraday Detector Configuration on the Neoma MC-ICP-MS

Rationale: Mass spectrometric measurement of the 230 Th/ 234 U ratio to calculate the purification age of enriched uranium is typically conducted via a combination of ion counters and faraday detectors, thus requiring an inter-detector calibration scheme. Here, our aim is to understand whether the pursuit of a simplified measurement scheme involving only faraday detectors is feasible. Methods: We investigate the possibility of determining U-Th model ages for two enriched uranium standards (NBL U630 and U850) by direct measurement of the 230 Th/ 234 U ratio (without chromatographic separation or isotope dilution) on a ThermoFisher Scientific Neoma MC-ICP-MS utilizing both solution and laser ablation (LA)-based sampling techniques and an all-faraday detector configuration. Results: For the solution mode analyses conducted on aliquots containing sub μg/mL total U, we produce composite average 230 Th/ 234 U model dates of May 19, 1988 (± 351 days), and March 26, 1961 (± 2.5 years) using the directly measured 230 Th/ 234 U ratios for the NBL U630 and U850 uranium standards, which have certified purification dates of June 6, 1988 (± 190 days), and December 31, 1957 (± 36.5 days), respectively. The ages produced by LA-based sampling of dried residues of the same standards deposited onto cotton TexWipes are less accurate and of poorer precision (June 23, 2004 ± 8.7 years for U630 and December 21, 1965 ± 7.9 years for U850) but still yield meaningful information in regards to the purification date. Conclusions: We believe that further refinement of the all faraday detector measurement approach to include development of a more robust Th/U relative sensitivity factor determination, signal cutoff selection, and data processing protocols will allow for this approach to be confidently applied to enriched uranium materials with unknown purification histories. Potential advantages of the method include the reduced sample handling and infrastructure requirements as well as the ability to simultaneously generate a broad picture of the uranium isotopic composition in tandem with the U-Th age determination.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS2017

Determination of Trace and Volatile Element Abundance Systematics of Lunar Pyroclastic Glasses 74220 and 15426 Using LA-ICP-MS

Since their recognition as pyroclastic glasses generated by volcanic fire fountaining on the Moon, 74220 and 15426 have garnered significant scientific interest. Early studies recognized that the glasses were particularly enriched in volatile elements on their surfaces. More recently, detailed analyses of the interiors of the glasses, as well as of melt inclusions within olivine grains associated with the 74220 glass beads, have determined high H2O, F, Cl and S contents. Such elevated volatile contents seem at odds with evidence from moderately volatile elements (MVE), such as Zn and K, for a volatile- depleted Moon. In this study, we present initial results from an analytical campaign to study trace element abundances within the pyroclastic glass beads. We report trace element data determined by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for 15426 and 74220.

McIntosh, E. Carrie↗
NASA NTRS2014

The Effect of Aqueous Alteration in Antarctic Carbonaceous Chondrites from Comparative ICP-MS Bulk Chemistry

Terrestrial ages of Antarctic carbonaceous chondrites (CC) indicate that these meteorites have been preserved in or on ice for, at least, tens of thousands of years. Due to the porous structure of these chondrites formed by the aggregation of silicate-rich chondrules, refractory inclusions, metal grains, and fine-grained matrix materials, the effect of pervasive terrestrial water is relevant. Our community defends that pristine CC matrices are representing samples of scarcely processed protoplanetary disk materials as they contain stellar grains, but they might also trace parent body processes. It is important to study the effects of terrestrial aqueous alteration in promoting bulk chemistry changes, and creating distinctive alteration minerals. Particularly because it is thought that aqueous alteration has particularly played a key role in some CC groups in modifying primordial bulk chemistry, and homogenizing the isotopic content of fine-grained matrix materials. Fortunately, the mineralogy produced by parent-body and terrestrial aqueous alteration processes is distinctive. With the goal to learn more about terrestrial alteration in Antarctica we are obtaining reflectance spectra of CCs, but also performing ICP-MS bulk chemistry of the different CC groups. A direct comparison with the mean bulk elemental composition of recovered falls might inform us on the effects of terrestrial alteration in finds. With such a goal, in the current work we have analyzed some members representative of CO and CM chondrite groups.

Alonso-Azcarate, J.↗
DOE OSTI2025

Online collection of LC effluent as droplets for automatic injection into ICP-MS

A sample introduction technique was developed to allow for online, dropwise injection of effluent into a mass spectrometer (MS). This allowed for the coupling of chromatography systems that were not driven by pumps without altering the set-up or separation performance. This capability combined the benefits of coupling separation and measurement while also enabling accurate chromatographic evaluation that would generally be performed offline. The incorporation of a flowing rinse into the system made dropwise resolution possible for any liquid capable of forming drops under ambient conditions. The technique was demonstrated utilizing gas pressurized extraction chromatography (GPEC) and inductively coupled plasma-time-of-flight mass spectrometry (ICP-TOFMS) to illustrate the qualitative applications for rapid separation development and procedure evaluation. This method's quantitative applications were evaluated using single and double isotope dilution mass spectrometry (IDMS) with an external mass bias correction to measure analytes across entire elutions including volumes as small as single drops. In conclusion, the total neodymium values afforded by both single and double IDMS were within the uncertainty of the calculated value for evaluation of full elution peaks and for most of the single drops analyzed that reached above 10k cps Nd-144.

GPEC↗
DOE OSTI2024

The Curious Case of Pu + : Insight on 5f Orbital Activity from Inductively Coupled Plasma Tandem Mass Spectrometry (ICP-MS/MS) Reactions

A comprehensive understanding of when and how 5f orbitals participate in complex chemical bonding is important for a variety of applications. The actinides are unique in that they possess 5f orbitals and can access high oxidation states, which make them attractive for use in catalysis. Fundamental studies of actinide–ligand interactions offer a mechanism to examine the activation of the 5f orbitals so that the selectivity of 5f orbitals can be assessed. A previous study examined the reaction of Pu + + CO 2 and determined that the reaction efficiency is restricted by a barrier, namely, promotion from the Pu + ground-state configuration, 5f 6 7s, to a reactive-state configuration, 5f 5 6d 2 . Here, the present study illustrates the benefit of activation of Pu’s 5f orbitals when studying the reaction of Pu + + NO. In this reaction, PuO + forms in an exothermic, barrierless process. The 5f orbitals can and do participate in forming a linear intermediate, [N-Pu-O] + , and this drives the exothermic reaction. Understanding the conditions under which 5f orbitals are active in chemical bonding is the key to exploiting the actinides’ selective catalytic capabilities.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Lithium isotope analysis on the Neoma MS/MS MC-ICP-MS

Accurate and precise lithium isotopic composition measurements are achieved on the Neoma MS/MS after careful tuning of the prefilter lenses to allow both Li ion beams to pass through unimpeded.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2024

Minimum Detectable Intakes and Doses for Uranium Bioassays—Comparison between Alpha Spectrometry and ICP-MS

Naturally occurring uranium complicates monitoring for occupational exposures. There are several retroactive methods that can be used to monitor for occupational exposures, with benefits and drawbacks to each. Analysis of uranium in urine by mass spectrometry and alpha spectrometry is compared, and methods of determining an occupational exposure are presented. Furthermore, the minimum detectable concentrations from each analysis and a method for intake determination based on the analytical results are compared for various solubility types and mixtures. Mass spectrometry with radiochemical separation was found to be the most sensitive analysis for detecting occupational exposures to anthropogenic mixtures based on minimum detectable doses calculated from the proposed method for intake determination.

bioassay↗
DOE OSTI2024

Comparison of the sensitivity of 236 U measurements in environmental samples by MC-ICP-MS and ATONA based high precision U TIMS measurements

The ATONA project is focused upon exploring the improvements in uranium isotope ratio measurements by thermal ionization mass spectrometry (TIMS) provided by a new, capacitor-based, amplifier technology. These “ATONA” Faraday amplifiers (Isotopx Ltd, UK) promise accurate, low-noise measurements of very small signals (< 1 femto-amp) in a traditional Faraday cup, which was only previously possible using an ion counter. This report outlines a series of experiments that were performed to assess the performance of the system in samples that test our rapid analysis procedures, and then compare the results against other mass spectrometry techniques currently available for environmental analyses. The following major goals were achieved: (1) illustrated the importance of 236 U measurements for the screening and analysis of environmental samples; (2) improved sensitivity for 236 U, and then identified 236 U in the 4350B standard at ultra-trace levels (3) Provided comparison of the 236 U sensitivity to multi-collector inductively coupled mass spectrometry techniques (4) Illustrated high TRL for the ATONA based measurement technique. This completes the reporting requirements for task 4 in the project LCP and highlights the utility of the system to make highly sensitive 236 U measurements in programmatically relevant sample matrices and at relevant uranium concentrations.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2024

ICP-MS For Analysis of Lithium Isotopic Ratios in Materials Highly Enriched in 7 Li (CRADA 626) Final Report

The intent of this project was to determine appropriate methodologies for analysis of lithium isotopes for 1) quasi-online monitoring of isotope separations, and 2) high-precision characterization of end-products, including lithium fluoride and lithium-beryllium fluoride (FLiBe). Traditionally, isotopic analysis requires the use of expensive, sophisticated instrumentation with often relatively long analytical timelines. We determined that the use of cheaper, smaller, and easier-to-operate instruments are sufficient for rapid analysis of lithium isotopes to monitor isotope separation efficiencies. In addition, we found that the analytical precision afforded by these lower-cost instruments is comparable to the more sophisticated (i.e., more expensive) instrumentation when the isotopic composition of lithium becomes highly depleted in 6Li. This finding will ultimately help lower costs of manufacturing of depleted lithium that is required for operation of certain designs of Generation IV nuclear reactors.

07 ISOTOPE AND RADIATION SOURCES↗
NASA NTRS2003

Laser-Ablation ICP-MS Analyses of Meteoritic Metal Grains in Lunar Impact-Melt Breccias

Lunar impact-melt breccias contain metal grains from the meteorites that formed the breccias. Because the breccias contain clastic material that may derive from older breccias, metal grains from earlier impacts may be present, too. The large subset of moderately mafic (8 - 12% FeO), KREEP-rich ("LKFM") melt breccias is particularly important because: (1) these are the melt breccias most likely to have been produced in basin-forming impacts, (2) it is from these breccias that many of the approx. 3.9 Gyr ages that are so common in lunar samples derive, (3) the breccias contain large proportions of FeNi metal, more than 1% in some types of Apollo 16 breccias, and (4) the metal potentially provides information about the impactors causing the apparent cataclysm at 3.9 Gyr.

Korotev, R. L.↗
NASA NTRS2005

LA-ICP-MS Study of Trace Elements in the Chanuskij Metal

This progress report covers work done during the second year of the 3-year proposal. During this year we resolved many issues relevant to the analytical technique developed by us for measuring trace elements in meteoritic metals. This technique was used to measure concentrations of Fe, Ni, Co, Cr, Cu, Ga, Ge, As, Mo, Ru, Rh, Pd, Sb, W, Re, Os, Ir, Pt, and Au in eight large (120 - 160 microns) metal grains from both "igneous" and "metamorphic" lithologies of the Chanuskij silicate inclusions. The first application of OUT technique to metal grains from thin sections showed some limitations. Small thickness of metal grains in the thin section limited the signal to 3-4 time-slices instead of 10- 1 1 ones in polished sections of iron meteorites studied before.

Petaev, Michail I.↗