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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Scalable Enrichment of 48 Ca at the Solid/liquid Interface by Chemical and Electrochemical Methods

This award targets to develop methods to enrich 48 Ca, which is a critical isotope for synthesizing superheavy elements and testing the standard model through neutrinoless double beta decay. The team first tested chemical exchange-based separation between solids and liquids, which is based on the free energy change due to the different vibrational frequencies caused by Ca isotopes in a material. However, the separation factor (alpha), which is defined as the ratio of 40 Ca/ 48 Ca ratios in the two phases, only reach ~1.01. The team then developed liquid centrifugation-based isotope separation, where a Ca salt aqueous solution is centrifuged at a speed of ~60 kRPM, and 48 Ca is enriched at the bottom of a centrifuge tube due to its larger mass. A high α of ~1.2-1.4 is achieved for 40 Ca/ 48 Ca at 40 °C. This method is further approved to be generic for any isotope that can be dissolved in a liquid solution or form liquid chemicals near room temperature. The experimental results also align well with modeling prediction. The team further develop a model to evaluate isotope separation in countercurrent liquid centrifugation. The team found that the countercurrent configuration can also enhance isotope separation in liquids, similar with gas centrifugation, which boost separation for isotopes which are difficult to be gasified near room temperature.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2020

Evolution of collectivity in 118 Xe

A recoil-distance Doppler shift experiment has been performed using the Pd 102 ( F 19 , p 2 n ) reaction at a beam energy of 73 MeV to measure the lifetime of excited states in Xe 118 . Additionally, the differential decay-curve method using γ γ coincidences and a gating procedure that allows to extract the lifetime without feeding assumptions has been employed. The lifetimes obtained for the yrast states up to spin-parity 8 + are compared with interacting boson model calculations and Xe 118 can be classified as a transitional nucleus between the spherical and a deformed shape. Systematics of the B ( E 2 ) values for the 2 + → 0 + and 4 + → 2 + transitions in the isotopic chains of tin, tellurium and xenon are presented. It is proposed that a “critical point” exists at which the B ( E 2 ; 4 + → 2 + ) / B ( E 2 ; 2 + → 0 + ) ratio drops to unity for lower neutron numbers within the isotopic chain. The position of the “critical point” varies with proton number, i.e., it is presumed to be located at the same mass number A = 114 in the Sn, Te, and Xe isotopes.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
NASA NTRS1985

Alfven wave scattering and the secondary to primary ratio

The cosmic ray abundances have traditionally been used to determine the elemental and isotopic nature of galactic ray sources and average measures of propagation conditions. Detailed studies of the physics of propagation are usually paired with relatively straightforward estimates of the secondary-to-primary (S/P) ratios. In the work reported here, calculations of elemental abundances are paired with a more careful treatment of the propagation process. It is shown that the physics of propagation does indeed leave specific traces of Galactic structure in cosmic ray abundances.

Bretthorst, G. L.↗
NASA NTRS1986

The case for a Martian origin of the shergottites. II - Trapped and indigenous gas components in EETA 79001 glass

The isotopic composition of N, Ar, Ne, and He, trapped in an uncrushed sample of the antarctic shergottite EETA 79001, was analyzed by subjecting the evacuated sample to stepped heating in the presence of 100 mtorr of oxygen. The isotopic composition of nitrogen (with the delta-N-15 value of greater than 300 percent) and the elemental ratios Ar-36/N-14 and Ar-40/N-14 were covariant along mixing lines passing through the Martian atmospheric composition. The results of this and previous analyses are consistent with a two-component nitrogen system in which about 84 ppb of trapped Martian atmospheric N is mixed in variable proportions with another, more thermally labile N component during stepped heating. The isotopic Ar-36/Ar-38 ratio of the EETA 79001 is different from that of the earth atmosphere by about 25 percent.

Wiens, R. C.↗
NASA NTRS1995

Stable isotope analysis at the molecular level: A new approach for determining the origins of amino acids in the Murchison meteorite

A combined gas chromatography/isotope ratio mass spectrometry (GC/IRMS) method has been developed that permits the direct stable carbon isotope analysis of N(O)-trifluoroacetyl-isopropyl esters of individual amino acids and their respective enantiomers at nanomole abundances. Calculation of the original delta C-13 values of the amino acids is accomplished via a correction for the carbon introduced during the derivatization process. Previous GC/IRMS analyses of individual amino acids in the non-hydrolyzed water extract of an interior sample of a Murchison meteorite stone revealed an enrichment in C-13 relative to terrestrial organic matter, in agreement with previous findings for bulk extracts. The range of amino acid delta C-13 values (+5 to +30 per mill, PDB) suggests possible kinetic effects during synthesis. In this study, an apparent kinetic isotope effect was also observed for the amino acid products of a spark discharge experiment. These preliminary resutls are supportive of a similar mechanism for the abiotic synthesis of amino acids in the Murchison meteorite.

Engel, M. H.↗
NASA NTRS1989

Sr isotopic variations in Upper Proterozoic carbonates from Svalbard and East Greenland

Precambrian Sr isotope stratigraphy was investigated by determining variations in Sr-87/Sr-86 ratios in the Upper Proterozoic carbonate succession from Svalbard and East Greenland. Data from this study were combined with those from literature to construct a curve of Sr-87/Sr-86 versus time for Upper Proterozoic seawater. The curve for the Upper Riphean-Vandian showed that the isotopic composition of Sr in seawater was low (Delta Sr-87 of about -500) between 900 and 650 Ma but rose rapidly to about +30 by 600 Ma (this range of long-term variation exceeds the total Phanerozoic variation). The very low values of Delta Sr-87 inferred for the Riphean require that, for this time, the submarine hydrothermal water flux was a large fraction of the Sr input to the oceans, while the rise in Delta Sr-87 in the Upper Proterozoic seawater reflects both a change in the ratio of hydrothermal and continental fluxes of Sr to the oceans, and a change in the isotopic composition of Sr from continental sources.

Derry, Louis A.↗
NASA NTRS2006

Carbon-rich Chondritic Clast PV1 from the Plainview H-chondrite Regolith Formation from H3 Chondrite Material by Possible Cometary Impact

Chondritic clast PV1 from the Plainview H-chondrite regolith breccia is a subrounded, 5-mm diameter unequilibrated chondritic fragment that contains 13 wt% C occurring mainly within irregularly shaped 30-400-micron-size opaque patches. The clast formed from H3 chondrite material as indicated by the mean apparent chondrule diameter (310 micron vs. approximately 300 micron in H3 chondrites), the mean Mg-normalized refractory lithophile abundance ratio (1.00 +/- 0.09 XH), the previously determined 0-isotopic composition (Delta O-17 = 0.66% vs. 0.68 +/- 0.04%0 in H3 chondrites and 0.73 +/- 0.09% in H4-6 chondrites), the heterogeneous olivine compositions in grain cores (with a minimum range of Fal-19), and the presence of glass in some chondrules. Although the clast lacks the fine-grained, ferroan silicate matrix material present in type 3 ordinary chondrites, PV1 contains objects that appear to be recrystallized clumps of matrix material. Similarly, the apparent dearth of radial pyroxene and cryptocrystalline chondrules in PV1 is accounted for by the presence of some recrystallized fragments of these chondrule textural types. All of the chondrules in PV1 are interfused indicating that temperatures must have briefly reached approximately 1100C (the approximate solidus temperature of H-chondrite silicate). The most likely source of this heating was by an impact. Some metal was lost during impact heating as indicated by the moderately low abundance of metallic Fe-Ni in PV1 (approximately 14 wt%) compared to that in mean H chondrites (approximately 18 wt%). The carbon enrichment of the clast may have resulted from a second impact event, one involving a cometary projectile, possibly a Jupiter-family comet. As the clast cooled, it experienced hydrothermal alteration at low water/rock ratios as evidenced by the thick rims of ferroan olivine around low-FeO olivine cores. The C-rich chondritic clast was later incorporated into the H-chondrite parent-body regolith and extensively fractured and faulted.

Rubin, Alan E.↗
DOE OSTI2023

A decay database of coincident γ–γ and γ–X -ray branching ratios for in-field spectroscopy applications

Current fieldable spectroscopy techniques often use single detector systems heavily impacted by interferences from intense background radiation fields. These effects result in low-confidence measurements that can lead to misinterpretation of the collected spectrum. To help improve interpretation of the fission products and short-lived radionuclides produced in a composite sample, a coincidence-database is being developed in support of a robust portable and X-ray coincidence detector system concurrently under development at the Pacific Northwest National Laboratory for in-field deployment. Hitherto, no database exists containing coincident γ–γ and γ–X-ray branching-ratio intensities on an absolute scale that will greatly enhance isotopic identification for in-field applications. As part of this project, software has been developed to parse all radioactive-decay data sets from the Evaluated Nuclear Structure Data File (ENSDF) archive to enable translation into a more useful JavaScript Object Notation (JSON) formats that more readily supports query-based data manipulation. The coincident database described in this work is the first of its kind and contains coincidence γ–γ and γ–X-ray intensities and their corresponding uncertainties, together with auxiliary metadata associated with each decay data set. The new JSON format provides a convenient and portable means of data storage that can be imported into analysis frameworks with relatively low overhead allowing for meaningful comparison with measured data.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
NASA NTRS1978

Nitrogen isotope systematics of two Apollo 12 soils

Soils 12023 and 12037 were analyzed for nitrogen by step-wise heating. Helium contents, Ar-40/Ar-36 ratios and spallation N-15 ages were determined in addition to nitrogen contents and isotopic compositions. The results for 12023 show it to be a typical lunar soil similar to many Apollo 16 and 17 soils in its nitrogen content and delta N-15 value, with a complex history. Soil 12037 appears to have had a simple, two-stage surface exposure history; one exposure occurring recently for about 10-20 m.y. and the other between about 3 to 4 b.y. ago. The delta N-15 value of nitrogen implanted in the earlier exposure was -125%. This nitrogen may reside in the minor components of 12037 such as the KREEP. If it should reside in the basaltic component of 12037, however, then the variation in the delta N-15 of implanted nitrogen with time probably has been more complex than previously considered.

Becker, R. H.↗
DOE OSTI2026

Depth of nutrient uptake by deep-rooted plants is regulated by water availability

The capacity of some plants to access water and nutrients at depths greater than one meter is a critical functional trait that confers resistance to drought and impacts both belowground and shallow soil processes. Here, we report water and strontium isotopic data from an alpine meadow transect showing the correlation between water and nutrient acquisition depths. The isotopic compositions of Sr ( 87 Sr/ 86 Sr ratio) and water in rock and soil, and in plant leaf tissues, reveal that deeper-rooted plants acquire a higher proportion of water, Sr, and cation nutrients that are derived from the saprolite, a zone of silicate weathering, than shallow-rooted grass. A three-decade dendrochemical record reveals that reductions of wet precipitation drive deep-rooted plants to acquire cation nutrients from deeper saprolite or bedrock regions. Thus, the depth of cation nutrient acquisition by deep-rooted plant species at this site is tightly coupled with, and likely determined by, water availability in soil, saprolite, and bedrock. The enhanced uptake of cations as well as water from deeper saprolite zones could impact the rate of bedrock weathering and watershed chemistry during drought.

biogeochemistry↗
NASA NTRS2013

Radiogenic Ingrowth of 40CA from Decay of 40K Provides a Powerful Tracer for Understanding the Origins of Felsic Magmas

Over time high K/Ca continental crust produces a unique Ca isotopic reservoir, with measurable 40Ca excesses compared to Earth's mantle (ɛCa=0). Thus, values of ɛCai > 1 indicate a significant crustal contribution to a magma. Values of ɛCai (<1) indistinguishable from mantle Ca indicate that the Ca in those magmas is either directly from the mantle, or is from partial melting of newly formed crust. So, whereas 40Ca excesses clearly define crustal contributions, mantle-like 40Ca/44Ca ratios are not as definitive. Here we present Ca isotopic measurements of intermediate to felsic igneous rocks from the western United States, and two crustal xenoliths found within the Fish Canyon Tuff (FCT). The two crustal xenoliths found within the 28.2 Ma FCT of the southern Rocky Mountain volcanic field (SRMVF) yield ɛCa values of ~4 and ~7.5, respectively. The 40Ca excesses of these possible source rocks are due to long-term in situ 40K decay and suggest that they are Precambrian in age. However, the FCT (ɛCai ~0.3) is within uncertainty of the mantle 40Ca/44Ca. Together, these data indicate that little Precambrian crust was involved in the petrogenesis of the FCT. Nd isotopic analyses of the FCT imply that it was generated from 10- 75% of an enriched component, and the Ca isotopic data appear to restrict that component to newly formed lower crust, or enriched mantle. However, the Ca isotopic data do permit assimilation of some crust with low Ca/Nd; decreasing the 143Nd/144Nd without adding much excess 40Ca to the FCT. Several other large tuffs from the SRMVF and from Yellowstone have ɛCai indistinguishable from the mantle. However, a few large tuffs from the SRMVF show significant 40Ca excesses. These tuffs (Wall Mountain, Blue Mesa, and Grizzly Peak) are likely sourced from near, or within the Colorado Mineral Belt. New isotopic measurements of Mesozoic and Tertiary granites from across the northern Great Basin show a range of ɛCai from 0 to ~3. In these samples ɛCai is generally correlated with ɛSri and is broadly negatively correlated with ɛNdi. However, for granites with similar ɛNdi at a given general location ɛCai can vary significantly (1 to 2 epsilon units). In rocks where low ɛNdi could also be due to melting from enriched reservoirs in the mantle lithosphere, the combination of high ɛCai with low ɛNdi clearly identifies crustal melts.

Mills, Ryan D.↗
NASA NTRS1991

Petrogenesis of Challis volcanics from central and southwestern Idaho - Trace element and Pb isotopic evidence

An analysis of the lava flows and ash-flow tuffs in Idaho is conducted to determine the composition of the volcanics in terms of major and trace elements and Pb isotopic substances. Al2O3 is found to be low, MgO content is high, and the concentration of K2O is higher or equal to that of Na2O with respect to the lavas of mafic to intermediate composition. Trace elements and element ratios are compatible with the crustal component, and the Pb isotopic compositions suggest a lack of assimilation during crystallization. The evidence does not support the notion of a magma system related to subduction, and the data regarding Pb isotopes and trace elements point to a connection with the lithosphere. A model is proposed for the Challis volcanics in which they resulted from completely melting within the lithosphere and then extending during the late Mesozoic and early Cenozoic compression.

Norman, Marc D.↗
DOE OSTI2023

Full-Field Strain Measurement Integrated with Two Dimension Regression Analysis to Evaluate the Bi-Modulus Elastic Properties of Isotropic and Transversely Isotropic Materials

Background: Measuring the physical properties of shale is critical for optimizing engineering activities such as geothermal energy generation and hydraulic fracturing. Shale is a transversely isotropic material. Furthermore, this material can also include micro and macro cracks at different locations and orientations that cause it to behave differently under tensile or compressive loading. Objective: In this work, a combined experimental–numerical approach is proposed to evaluate the bi-modulus elastic properties of isotropic and transversely isotropic materials. Methods: Full-field strain measurements for a circular disk under diametral compression are integrated with a regression analysis technique to evaluate the elastic properties of bi-modulus materials subjected to tensile and compressive loads using two loading configurations on the same specimen. Digital Image Correlation (DIC) is used to measure the full-field strains. Subsequently, in the case of an isotropic material, a linear least-squares approach is utilized to process the experimentally determined strains in conjunction with analytical expressions of the stress fields (in terms of far-field loading) to determine the elastic modulus E, the shear modulus G, and the Poisson’s ratio $v$. In the case of a transversely isotopic material, such as shale, a finite element model is implemented to determine the stress fields (again in terms of far-field loading), which is followed by repeating the previous regression analysis in an iterative process to estimate the elastic parameters. Results: The results show that the proposed technique successfully provides a complete set of elastic properties as a function of both the loading condition and the principal material directions. The technique is validated by measurements on a known isotropic material and then applied to determine the properties of shale. Conclusion: In this work, the proposed approach is successfully used to calculate the bi-modulus elastic response of poly(methyl meth- acrylate) (PMMA) and shale. As expected, PMMA exhibits an isotropic response with no bi-modulus effect, however, shale exhibits both transverse isotropy and a bi-modulus effect. Therefore, this approach holds promise for investigating the elastic properties of materials like rocks and fiber-reinforced composite laminates as functions of the principal material directions and the loading conditions.

42 ENGINEERING↗
DOE OSTI2023

Developing a peptide concatemer (PepCon) as a process control for LC-MS based proteomics

Quantitative concatenated peptide (QconCAT) technology is currently used for the absolute quantification of proteins of interest in a biological sample. It relies on artificially created proteins that are concatenations of different, isotopically labeled peptides. Because these isotopically labeled peptides are at a 1:1 ratio and correspond to naturally occurring peptides in the biological sample, each peptide can be used as a standard for the absolute quantitation of all proteins of interest at once. Although the QconCAT technology has utility for quantitation of known peptides in a mixture, it is not helpful for scientists who need a proteomics standard (1) that can be spiked into a protein mixture at an extremely low level, (2) that can be co-purified during sample fractionation, and (3) that is optimized for ESI used in mass spectrometry. Thus, there exists a need for an ideal standard protein that is large enough to behave as a protein but consists of multiple, concatenated copies of the same peptide, which, upon digestion, amplifies (e.g., >10-fold) into a detectable peptide species. Here, this technical report describes the development of “PepCon”, a peptide concatemer that fulfills this unmet need.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2022

The calculation of light element impurity (α, n) yield curves in a PuO 2 matrix and associated specific yield coefficients: Influence of the reaction cross sections

Most of the Pu separated from irradiated commercial nuclear fuel is stored as PuO 2 . The primary quantitative nondestructive measurement technique used to verify the amount of Pu in storage containers is passive neutron correlation counting. An important physical property of the oxide material is the ratio, α, of the rate of (α, n) neutrons produced inside the item to the rate of neutrons produced by spontaneous fission. This ratio influences the precision of the correlated counting method and affects the interpretation of the data because of how it changes both the primary total neutron production rate and the rate of induced fission events taking place inside the item. In addition to the main O(α, n) contribution, additional contributions come from α-particle interactions with light element impurities that are inevitably present. In this work, we calculate specific (α, n) yield coefficients, expressed in units of neutrons per second per gram of α-emitting nuclide per part per million by mass of the specified impurity element distributed in a pure PuO 2 matrix, for some key α-emitting actinides commonly present in reprocessed Pu ( 238–242 Pu+ 241 Am). These coefficients are directly applicable to nuclear safeguards verification work in which the α ratio is often calculated from the Pu-isotopic composition and chemical information obtained by other means. Further, they also provide a convenient up-to-date reference set against which values generated by other methods can be compared. Results are presented for impurities with atomic number from 3 to 17 inclusive, plus K and Fe. In most cases, these coefficients are not expected to change by more than 5%–10% at any time in the future. However, as new data become available, changes as large as 20% may be needed for some targets (e.g., F). The present yield calculations are limited by the general shortage of quality experimental total (α, n) reaction cross section data, which, together with unexplained variation between determinations, means that an objective and coherent evaluation is not possible. The situation is even less satisfactory for the partial differential cross section needed to calculate neutron spectra.

(𝛼, n) reactions↗
DOE OSTI2021

Measuring Signatures of Fuel Irradiation in Large Particle Samples

Understanding the operating history of a nuclear facility is one of the key goals in nuclear safeguards, enabling the verification of declared activities. This is accomplished via a number of mechanisms, including the analysis of samples collected at the facility. The best metrics for understanding and verifying the history of nuclear fuel are (1) actinide isotopic content and (2) actinide inter-element ratios. While techniques have long existed for measuring these values with high accuracy and precision in bulk samples, as samples become smaller – such as may be collected in environmental collection – new methods are required both for clean processing of pure samples, and for analysis of these small samples. This study describes a new extraction chromatography technique for recovering U, Pu, and Am from single small aliquots, and advanced mass spectrometry methods for high-precision and high-accuracy analysis of trace and ultra-trace levels of actinides. These techniques are applied to particle samples cut from fuel from a historic nuclear reactor. Ages calculated from Pu–Am chronometry of particles are in excellent agreement with the known operating history of the reactor.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗