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DOE OSTI2021

Behavior of the Mo, Tl, and U isotope systems during differentiation in the Kilauea Iki lava lake

Stable molybdenum (Mo), thallium (Tl), and uranium (U) isotope ratios were determined in a suite of samples from the 1959 Kilauea eruption and from Kilauea Iki lava lake with the aim of understanding the effects of igneous differentiation on these isotope systems. The samples range from olivine cumulate with MgO up to 27% to internal differentiates with MgO less than 3%, representing a tholeiitic differentiation series. Molybdenum, Tl, and U behave incompatibly during differentiation, and Mo and U isotope ratios do not systematically vary amongst the different samples. δ 98 Mo values range from -0.17 to -0.31‰ and δ 238 U values range from -0.20 to -0.38‰. Most individual analyses for both isotope systems overlap within measurement uncertainty (± ~0.7 and ~ 0.6, respectively). Mean δ 98 Mo and δ238U values are -0.22 ± 0.08‰ (2σ) and - 0.29 ± 0.09‰ (2σ), respectively, which overlap with Pacific mid ocean ridge basalt (MORB). In contrast, Tl isotopes show small but resolvable variations, with ε 205 Tl ranging from +1.20 to -1.38. The most negative ε 205 Tl values are confined to some of the lowest [Tl] samples, but the ε 205 Tl values do not otherwise vary smoothly with MgO or [Tl]. Possible mechanisms for thallium isotope fractionation are considered (e.g., degassing, water leaching, sulfide fractionation) but none are found to be satisfactory. Overall, the lack of resolvable variation in the Mo and U isotope systems and the small magnitude of heterogeneity in the Tl isotope system indicate that differentiation in tholeiitic systems is unlikely to be a major contributor to global variation in these isotope systems.

58 GEOSCIENCES↗

DOE OSTI2025

Consistent $\overline{ν}$ evaluation for minor U isotopes with $\tt{CGMF}$

Following several successful prompt $\overline{ν}$ evaluations using $\tt{CGMF}$, including consistent evaluations for minor Pu isotopes, we detail in this report our efforts to perform a consistent $\overline{ν}$ evaluation for minor U isotopes during FY25. Although we have not yet produced a finalized evaluation, we present the progress that we have made towards such an evaluation for 232,233,234,236,237,239 U prompt $\overline{ν}$. Our milestone explicitly calls out evaluations for 233 U, 234 U, and 236 U, however, to better constrain the model with reliable experimental $\overline{ν}$ data, we also include 235 U and 238 U in the evaluation procedure. Then, we additionally produce evaluations for 232 U, 237 U and 239 U $\overline{ν}$ as a byproduct. Elsewhere, we will report our efforts on a stand-alone 233 U $\overline{ν}$ evaluation. This report is organized in the following manner. In Sec. 2, we briefly outline the updates to CGMF that were needed to be able to calculate all of these minor U fission reactions. The experimental data overview is given in Sec. 3. The evaluation methodology and results are presented in Secs. 4 and 5, respectively. Finally, we conclude and outline work for FY26 in Sec. 6.

07 ISOTOPE AND RADIATION SOURCES↗

DOE OSTI2021

Method Development for Measuring U Isotope Ratios by Laser Ablation MC-ICP-MS. Task 1: Hardware Setup

The aim of this project is to develop methodology to identify and analyze U and Pu containing particles using laser ablation MC-ICP-MS. The final methodology will ultimately be described in a detailed procedural document that will be shared with IAEA-NWAL laboratories. In this report, we describe the Task-1 deliverable; the setup and optimization of hardware required to perform U isotopic analyses by laser ablation MC-ICP-MS.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Characterization of U Isotope Ratios by Laser Ablation MC-ICP-MS for IAEA Safeguards

This project will develop methodology to identify and analyze U and Pu containing particles using laser ablation MC-ICP-MS. The proposed work will involve: i) setup and optimization of the LA-MC-ICP-MS system, ii) testing and validation by analysis of QC standards, iii) designing analytical protocols for single particles, and iv) developing a data processing system. Ultimately, this project will output a detailed operating procedure documenting the experimental techniques and data processing routines required to perform particle identification and analysis by laser ablation MC-ICP-MS, that can be shared with IAEANWAL laboratories.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1993

U-Pb isotopic systematics of ferroan anorthosite 60025

Preliminary U-Pb isotopic data from separates of ferroan anorthosite 60025 confirm its antiquity at approximately 4.42 Ga. Three Pb-Pb isochron ages involving different sets of mineral separates vary by only 20 million years, but indicate derivation of the sets from isotopically distinct magma sources. If this anorthosite was a monomict cumulate product formed during the Moon's early primary differentiation stage, then residual liquids of crystallizing magmas were evolving isotopically, even at the cm-scale, over the duration of the crystallization period. Another explanation is that this sample is simply a polymict breccia and that the Pb isotopic results are a result of subsequent mechanical mixing of mineral assemblages from various cumulate piles formed coevally at approximately 4.42 Ga from isotopically distinct magma sources. In our ongoing search for early lunar Pb isotopic compositions, we have analyzed Apollo 16 anorthosites 67075 and 62337 and Apollo 17 high-Mg suite cumulates (troctolite 76535, norite 78235, and dunite 72415). The U-Pb isotopic systematics have been better behaved in the high-Mg suite rocks than in the anorthosites that have shown evidence of mineral assemblages of mixed parentage. Our aim in analyzing anorthosite 60025 was to avoid or minimize this problem as it had been considered essentially monomict, although recent work has shown that not only is 60025 polymict, but shows textual evidence of at least two episodes of deformation. Of five splits studied by James, Lindstrom and McGee, the four mineral splits appeared monomict, whereas the whole-rock split was considered polymict. Previous isotopic work indicate that this anorthosite was quite primitive, a claim that was apparently confirmed by the U-Pb isotopic age of 4.51 +/- .01 Ga on three plagioclase separates. However, a Sm-Nd internal isochron age of 4.44 +/- 0.02 Ga was determined using plagioclase, olivine, and mafic mineral separates, creating some doubt about the anorthosite's true age. It was pointed out that the use of slightly evolved initial Pb values (corresponding to a source-micron value of approximately 35) to correct the U-Pb data can result in an U-Pb age of 4.44 Ga. The need to resolve the age and isotopic nature of this anorthosite is paramount to furthering our understanding of processes of ferroan anorthosite formation as well as the magmatic history of the early Moon.

Premo, W. R.↗

DOE OSTI2023

Spatially Resolved Characterisation of Low Mass Fraction Uranium Glass Working Reference Materials

Here, we present the results of a study to generate reference glasses that reflect an environment analogous to historic nuclear fallout samples of interest for post-detonation nuclear forensics. The glasses were generated by melting and then quenching SiO 2 , Al 2 O 3 and CaCO 3 powders. Two suites of glasses with three distinct U isotopic ratios were successfully made with enrichments in the 235 U isotope (~ natural [0.72%], ~ 53% and 94%), but the bulk elemental data showed heterogeneity (~ 10% RSD) with U mass fractions ranging from 331.47 to 373.63 μg g -1 . Spatially resolved U isotopic measurements were performed using three mass spectrometry techniques (secondary ion mass spectrometry-single stage accelerator mass spectrometry [SIMS-SSAMS], large geometry [LG] - SIMS, and laser ablation-inductively coupled plasma-mass spectrometry [LA-ICP-MS]) across five National Laboratories. The results showed good agreement with the bulk U isotopic data for the low, medium, and high U mass fractions. We conclude that despite elemental heterogeneity, these samples can serve as useful working reference materials for spatially resolved nuclear fallout analyses, as well as for other related spatially resolved analyses.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Precision Local Burnup Assessment Through Dynamic Peak Fitting in Atom Probe Tomography for Depleted, Enriched, and Irradiated Metallic and Ceramic Fuels

Abstract Burnup estimation in nuclear fuels is vital for evaluating fuel performance, transportation, and safe fuel storage. Accurate assessments of burnup from service period and spent fuels involve tracking the consumption of fissile isotopes of uranium (U) offering a direct insight into energy changes within the fuels especially for thermal spectrum reactors. In current approach, mass spectroscopic technique in atom probe tomography (APT) is utilized for accurate quantification of U isotopes. Quantification of U peaks in mass spectrum is performed on asymmetric shapes due to delayed signals, known as thermal tails, particularly for poorly conducting samples analyzed in laser mode. In this study, we introduce a novel quantification tool for isotopic analysis from APT datasets by developing a fitting algorithm based on shapes of the peaks. A MATLAB-based dynamic peak fitting toolbox is developed and designed to adapt to various peak shapes, ensuring accurate quantification of U isotopes. The effectiveness of this approach is demonstrated in standard Ni-Cr sample, depleted and enriched U samples, and U-based fuels with different burnup levels. The viability of this approach for isotopic quantification is demonstrated on both metallic and ceramic fuels.

Burnup↗

DOE OSTI2022

Corrosion of U233-Doped Uranium Oxide using Microfluidics Methods

The aim of work this year has been to investigate the role of alpha (α)-radiation and hydrogen (H 2 ) on the corrosion of uranium oxide (UO 2 ) using a microfluidic device. The microfluidic device, termed the Particle-Attached Microfluidic Electrochemical Cell, (PAMEC), enables monitoring of the UO 2 electrochemical corrosion potential (E corr ) under different environments, including de-aerated conditions and in the presence of dissolved H 2 . The Si 3 N 4 window allows us to study morphological and chemical changes under an electron microscope. We have previously demonstrated that the PAMEC matches the results from bulk electrochemical tests with UO 2 [1]. We used the high specific activity uranium (U) isotope, 233 U, (t 1/2 = 160,000 years) incorporated into UO 2 , to generate a localized a-field. The objective of the experiments were to mimic the radiation environment that would be experience at the surface of aged spent nuclear fuel (SNF) during long-term geologic disposal under anoxic conditions. Wittman et al. [2] predicted that in the presence of a pure a-radiation field and under H 2 conditions, the concentration of the radiolytic oxidant H 2 O 2 would be suppressed or even eliminated. In a UO 2 corrosion experiment this would be exhibited through a lowering of the measured UO 2 corrosion potential compared to identical conditions in the absence of dissolved H 2 . We found that the predictions of Wittman and co-workers were supported and that the corrosion potential of the 233 U-doped UO 2 in solution lowered with presence of H 2 gas and increased in the absence of H 2 , when under anoxic conditions. The PAMEC experiments indicate that H 2 O 2 has been eliminated in a solution sparged with H 2 while exposed to an a-radiation field. The corrosion potential of the a-doped 233 U(10%)- 238 UO 2 in a solution sparged with Ar/H 2 matched the corrosion potential of 238 UO 2 in solution sparged with air. This clearly demonstrated that the H 2 O 2 had been eliminated and that the only oxidant present was O 2 in this system in complete agreement with the modeling results of Wittman et al. These results point to the need to improve the Fuel Matrix Degradation (FMD) Process Model training data set that is being used in the FMD surrogate model that is being developed for the repository program. The incorporation of realistic radiation chemistry will improve the scientific basis for the FMD Model.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASA NTRS1992

U-Pb isotopic results for single shocked and polycrystalline zircons record 550-65.5-Ma ages for a K-T target site and 2700-1850-Ma ages for the Sudbury impact event

The refractory mineral zircon develops distinct morphological features during shock metamorphism and retains these features under conditions that would anneal them in other minerals. In addition, weakly shocked zircon grains give primary ages for the impact site, while highly reconstituted (polycrystalline) single grains give ages that approach the age of the impact event. Data for a series of originally coeval grains will define a mixing line that gives both of these ages providing that no subsequent geological disturbances have overprinted the isotopic systematics. In this study, we have shown that the three zircon grain types described by Bohor, from both K-T distal ejecta (Fireball layer, Raton Basin, Colorado) and the Onaping Formation, represent a progressive increase in impact-related morphological change that coincides with a progressive increase in isotopic resetting in zircons from the ejecta and basement rocks. Unshocked grains are least affected by isotopic resetting while polycrystalline grains are most affected. U-Pb isotopic results for 12 of 14 single zircon grains from the Fireball layer plot on or close to a line recording a primary age of 550 +/- 10 Ma and a secondary age of 65.5 +/- 3 Ma. Data for the least and most shocked grains plot closest to the primary and secondary ages respectively. The two other grains each give ages between 300 and 350 Ma. This implies that the target ejecta was dominated by 550-Ma rocks and that the recrystallization features of the zircon were superimposed during the impact event at 65.5 Ma. A predominant age of 550 Ma for zircons from the Fireball layer provides an excellent opportunity to identify the impact site and to test the hypothesis that multiple impacts occurred at this time. A volcanic origin for the Fireball layer is ruled out by shock-related morphological changes in zircon and the fact that the least shocked grains are old. Basement Levack gneisses north of the Sudbury structure have a primary age of 2711 Ma. Data for three single zircons from this rock, which record a progressive increase in shock features, are displaced 24, 36, and 45 percent along a Pb-loss line toward the 1850 +/- 1 Ma minimum age for the impact as defined by the age of the norite. Southeast of the structure three shocked grains from the Murray granite record a primary age of 2468 Ma and are displaced 24, 41, and 56 percent toward the 1853 +/- 4 Ma even as defined by coexisting titanite.

Krogh, T. E.↗

DOE OSTI2022

Characterization and Optimization of a Spectral Window for Direct Gaseous Uranium Hexafluoride Enrichment Assay Using Laser-Induced Breakdown Spectroscopy

Through a systematic scanning of 235 U and 238 U emission lines between 280 nm and 745 nm, the optimal emission line for direct gaseous uranium hexafluoride (UF 6 ) enrichment assay using laser-induced breakdown spectroscopy (LIBS) was found. Screening for spectral features that are potentially useful for U isotopic analysis was gauged from the magnitude of the 235 U– 238 U isotopic shift and the signal-to-background ratio of the emission line through a parameter termed ΔSBR 235U–238U . The ΔSBR spectrum shows peaks at wavelength positions where there are strong lines with significant 235 U– 238 U shifts. The screening identified 13 spectral-window candidates, which were down selected based on their overall accuracy in predicting the 235 U enrichment of three UF 6 samples of natural (0.720 atom% 235 U) and low-enriched (4.675 atom% and 9.157 atom% 235 U) grades. The U(I) 646.498 nm emission line, with a determined 235 U– 238 U isotopic shift of -17.7 pm, was found to be the optimal spectral window for direct UF 6 enrichment assay. The root mean square error for enrichment assays on the three natural and low-enriched UF 6 samples, with each sample measured in six replicates, was 0.31% in absolute 235 U content. Each measurement comprised LIBS signals accumulated from 3000 laser shots. In conclusion, the analytical bias and precision were better than 0.5% and 0.3%, respectively, in absolute [ 235 U/( 235 U + 238 U)] ratios. Specific for the two low-enriched UF 6 samples, the relative standard deviations from six replicated measurements were around 2%.

47 OTHER INSTRUMENTATION↗

NASA NTRS1993

U-Pb isotopic ages and characteristics of ancient (greater than 4.0 Ga) lunar highland rocks

A review of the present (and certainly sparse) U-Pb isotopic database for ancient (greater than 4.0 Ga) lunar highland rocks indicates that both early-forming anorthosites and high-Mg suite rocks were formed from sources with a wide variety of U-238/Pb-204(mu) values as early as 4.44 Ga. The U-Pb data from Apollo 16 anorthosites 67075, 60025, and 62337 indicate source-mu values between approximately 55 and approximately 350; whereas values for high-Mg suite rocks are tentatively considered to be over 500, similar to KREEP sources. At present, I interpret the data to indicate that either early cumulates were formed slowly in a magma environment that allowed isotopic reequilibration or mixing over a long period of crystallization, or these cumulates formed from rapidly-evolving (both geochemically and isotopically) residual liquids. It is possible that an early bombardment period played a role in the mixing process.

Premo, W. R.↗

DOE OSTI2024

A preliminary investigation into the feasibility of laser ablation U–Pb isotope ratio measurement via all‐faraday cup detection with 10 11 ‐ and 10 13 ‐Ω amplifiers on the Neoma multicollector‐inductively coupled plasma‐mass spectrometer

Rationale Signal detection for uranium–lead (U–Pb) dating of zircon is typically performed via ion counters. Here, we develop a preliminary understanding of the strengths and limitations of faraday‐cup‐based detection. Methods A suite of zircon reference materials and the NIST‐610 glass were sampled using laser ablation followed by U–Pb isotope ratio measurement on a Neoma multicollector‐inductively coupled plasma‐mass spectrometer. Results We were able to produce geologically accurate 207 Pb/ 206 Pb, 206 Pb/ 238 U, and 207 Pb/ 235 U ratios for the NIST‐610 glass and the zircon standards, with ages ranging from ~2.5 Ga to ~337 Ma (TanBrown A, Oracle, 91550, Mud Tank, Temora, and Plešovice). Two of the younger zircon standards examined (94‐35, ~55.6 Ma, and Fish Canyon, 28.6 Ma) yielded accurate 206 Pb/ 238 U but not 207 Pb/ 235 U or 207 Pb/ 206 Pb ratios, whereas the youngest zircon standard (Penglai, ~4.4 Ma) failed for all three ratios of interest. The accuracy and precision of the all‐faraday method are directly tied to signal intensity, with reliable data capable of being produced even when both isotopes in a ratio have signals below ~0.001 V (equivalent to ~62 500 cps on an ion counter). Conclusion The all‐faraday cup multicollection method provides sufficient sensitivity to obtain geologically meaningful U–Pb data, with possible advantages being that laser pit depth‐dependent changes in the observed interelemental fractionation behavior may be easier to correct using a static collector configuration compared to when the ion beam is swept across a single detector while also removing the need for an interdetector‐type calibration. Further work is needed to refine the all‐faraday cup method (e.g., application of background subtraction and common Pb corrections, outlier removal, and interelement as well as down‐hole fractionation corrections), but our initial results demonstrate that the faraday detector method has sufficient sensitivity to warrant further study.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2022

Analysis of solid uranium particulates on cotton swipes with an automated microextraction-ICP-MS system

Here, an automated microextraction method coupled to an inductively coupled plasma – mass spectrometer (ICP-MS) was developed for the direct analysis of solid uranium particulates on the surface of cotton swipes. The microextraction probe extracts particulates from the sample surface, in a flowing solvent, and directs the removed analyte to an ICP-MS for isotopic determination. The automated system utilizes a mechanical XY stage that is software controlled with the capability of saving and returning to specific locations and a camera focused to the swipe surface for optimal viewing of the extracted locations (i.e., material present). Here, particulates (n = 135) were extracted and measured by ICP-MS, including 35 depleted uranyl nitrate hexahydrate (UN) (used for mass bias corrections), 50 uranyl fluoride (UO 2 F 2 ), and 50 uranyl acetate (UAc) particulates. Blank extractions were performed on the cotton swipes between triplicate sample analyses. Between each swipe extraction, the probe was sent between two wells containing 10% and 5% HNO 3 to clean the probe head and to eliminate any analyte carryover between particulates. The measured 235 U/ 238 U and 234 U/ 238 U isotope ratios for the UO 2 F 2 particulates were 0.00725(8) and 0.000054(4), a percent relative difference (% RD) of –0.041% and –1.7% from the reference isotope ratios determined in-lab through multi-collector ICP-MS analysis of dissolved aliquots of the U material. The UAc samples had a measured 235 U/ 238 U isotope ratio of 0.00206(7), a –0.96% relative difference from the reference value of 0.00208(1). The 234 U/ 238 U and 236 U/ 238 U isotope ratios were 0.000008(1) and 0.000031(4), –5.1% RD and –4.3% RD, respectively. The automated sample stage enabled seamless and rapid particle analysis, leading to a significant increase in throughput versus what was previously possible. Additionally, the saved location capability reduced user sampling error as sampling locations were easily stored and recalled. Analysis of U particles on the swipe surface – including blanks, mass bias, and triplicate extractions – was completed in less than an hour without any sample preparation necessary.

47 OTHER INSTRUMENTATION↗

DOE OSTI2021

Isotopic Heterogeneity Imaged in a Uranium Fuel Pellet with Extreme Ultraviolet Laser Ablation and Ionization Time-of-Flight Mass Spectrometry

We use extreme ultraviolet laser ablation and ionization time-of-flight mass spectrometry (EUV TOF) to map uranium isotopic heterogeneity at the nanoscale (=100 nm). Using low-enriched uranium fuel pellets that were made by blending two isotopically distinct feedstocks, we show that EUV TOF can map the 235U/238U content in 100 nm-sized pixels. The two-dimensional (2D) isotope maps reveal U ratio variations in sub-microscale to =1 µm areas of the pellet that had not been fully exposed by microscale or bulk mass spectrometry analyses. Compared to the ratio distribution measured in a homogeneous U reference material, the ratios in the enriched pellet follow a ~3× wider distribution. These results indicate U heterogeneity in the fuel pellet from incomplete blending of the different source materials. EUV TOF results agree well with those obtained on the same enriched pellets by nanoscale secondary ionization mass spectrometry (NanoSIMS), which reveals a comparable U isotope ratio distribution at the same spatial scale. EUV TOF’s ability to assess and map isotopic heterogeneity at the nanoscale makes it a promising tool in fields such as nuclear forensics, geochemistry, and biology that could benefit from uncovering sub-microscale sources of chemical modifications.

Rush, Lydia A.↗

DOE OSTI2025

Real-Time Screening for Uranium Enrichment by Paper Spray Ionization Mass Spectrometry for Field Applications

A rapid isotope ratio screening technique for uranium enrichment is demonstrated by utilizing paper spray ionization (PSI) high-resolution mass spectrometry (HRMS). Measurements were conducted using an ambient ionization mass spectrometer coupled to a custom-made JEOL PSI attachment apparatus, with de minimus sample preparation requirements. The current method detection limit for individual isotopes (e.g., 235 U and 238 U) is approximately 50 pg, with subsequent optimization expected to further improve U isotopic sensitivity. The PSI analytical method described herein can support rapid analysis (both in-field and in-lab screening) of isotopes-of-interest, as demonstrated by empirical differentiation of depleted uranium (DU) and low enriched uranium (LEU) analytical aliquots. Furthermore, this analytical workflow holds promise for applications in nuclear forensics, international nuclear safeguards, and nonproliferation missions.

Anions↗

DOE OSTI2021

Application of saturation absorption spectroscopy to study the hyperfine structure of 235U and accurate 235U/238U isotope ratio determinations at 861.031 nm

The uranium transition 5f 3 6d7s 2 ( 5 L 6 ) → 5f 3 7s 2 7p ( 5 K 5 ) at 861.031 nm was studied using saturation absorption spectroscopy. The hyperfine structure of the 235 U isotope was determined by measuring the Doppler-suppressed absorption spectrum, and the hyperfine structure constants were obtained by employing transition-specific line strength theory and spectral fitting. The magnetic-dipole and electric-quadrupole constants were determined to be A = -3.2887 ± 0.1957 mK and B = 31.8712 ± 8.0789 mK for the upper state 5f 3 7s 2 7p ( 5 K 5 ). A theoretical calculation for the hyperfine structure constants of the 235 U isotope was also carried out by the relativistic configuration-interaction (RCI) method, and the obtained values were found to be in agreement with the measured values. In addition, the line profile of 238 U was experimentally investigated for different excitation intensities and modeled using the RCI method for estimating the transition probability and oscillator strength, with various residual broadening mechanisms considered beyond the radiative decay. Finally, we show that these results allow us to make improvements on the precision of spectral measurements using our previously developed technique for isotope ratio determinations in atomic beams.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Forensics, Instruments, Turtles & Hot Sauce: The Role of an Isotope Geochemist at LANL [Slides]

Measurable quantities of U in Turtle and Tortoise scute. Turtle samples from areas of known history of radionuclide releases found to have non-natural U isotope signatures. These signatures match what we know about the release of uranium radionuclides at each site. Able to determine quantifiable changes in the U concentration and isotope composition along individual layers of growth (representing seven years of life). Possible correlations with historical releases of U from Oak Ridge site.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2014

Preliminary Report on U-Th-Pb Isotope Systematics of the Olivine-Phyric Shergottite Tissint

Geochemical studies of shergottites suggest that their parental magmas reflect mixtures between at least two distinct geochemical source reservoirs, producing correlations between radiogenic isotope compositions, and trace element abundances.. These correlations have been interpreted as indicating the presence of a reduced, incompatible-element- depleted reservoir and an oxidized, incompatible-element-rich reservoir. The former is clearly a depleted mantle source, but there has been a long debate regarding the origin of the enriched reservoir. Two contrasting models have been proposed regarding the location and mixing process of the two geochemical source reservoirs: (1) assimilation of oxidized crust by mantle derived, reduced magmas, or (2) mixing of two distinct mantle reservoirs during melting. The former clearly requires the ancient martian crust to be the enriched source (crustal assimilation), whereas the latter requires a long-lived enriched mantle domain that probably originated from residual melts formed during solidification of a magma ocean (heterogeneous mantle model). This study conducts Pb isotope and U-Th-Pb concentration analyses of the olivine-phyric shergottite Tissint because U-Th-Pb isotope systematics have been intensively used as a powerful radiogenic tracer to characterize old crust/sediment components in mantle- derived, terrestrial oceanic island basalts. The U-Th-Pb analyses are applied to sequential acid leaching fractions obtained from Tissint whole-rock powder in order to search for Pb isotopic source components in Tissint magma. Here we report preliminary results of the U-Th-Pb analyses of acid leachates and a residue, and propose the possibility that Tissint would have experienced minor assimilation of old martian crust.

Moriwaki, R.↗