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All sourcesNASA NTRSDOE OSTI
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 OSTI2023

HPLC-Parallel accelerator and molecular mass spectrometry analysis of 14 C-labeled amino acids

Accelerator mass spectrometry (AMS) is the method of choice for quantitation of low amounts of 14 C-labeled biomolecules. Despite exquisite sensitivity, an important limitation of AMS is its inability to provide structural information about the analyte. This limitation is not critical when the labeled compounds are well-characterized prior to AMS analysis. However, analyte identity is important in other experiments where, for example, a compound is metabolized and the structures of its metabolites are not known. We previously described a moving wire interface that enables direct AMS measurement of liquid sample in the form of discrete drops or HPLC eluent without the need for individual fraction collection, termed liquid sample-AMS (LS-AMS). Here, we now report the coupling of LS-AMS with a molecular mass spectrometer, providing parallel accelerator and molecular mass spectrometry (PAMMS) detection of analytes separated by liquid chromatography. The repeatability of the method was examined by performing repeated injections of 14 C-labeled tryptophan, and relative standard deviations of the 14 C peak areas were ≤10.57% after applying a normalization factor based on a standard. Five 14 C-labeled amino acids were separated and detected to provide simultaneous quantitative AMS and structural MS data, and AMS results were compared with solid sample-AMS (SS-AMS) data using Bland-Altman plots. To demonstrate the utility of the workflow, yeast cells were grown in a medium with 14 C-labeled tryptophan. The cell extracts were analyzed by PAMMS, and 14 C was detected in tryptophan and its metabolite kynurenine.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2021

Conversion of the LLNL/CAMS 1 MV biomedical AMS system to a semi-automated natural abundance 14C spectrometer: system optimization and performance evaluation

The Lawrence Livermore National Laboratory – Center for Accelerator Mass Spectrometry compact 1 MV biomedical accelerator mass spectrometer was repurposed and optimized for the semi-automated radiocarbon measurement of natural abundance environmental samples. Here we present results from 15 months of routine system operation and evaluate the system performance based on 30 sample wheels measured with consistent operating conditions over 7 months from August 2019 to March 2020. Additionally, the average measurement precision was 2.7 ± 0.7‰. System accuracy was assessed with measurements of 14 C-free materials, standard materials with 14 C-content spanning 0.5 to 1.5 F 14 C, and by comparison to split samples measured with the 10 MV AMS system. Overall, this system can routinely measure samples as small as 300 µgC and less than 33000 years without the need for size-specific correction protocols.

43 PARTICLE ACCELERATORS↗
DOE OSTI2020

Quantitative Determination of Biomass-derived Renewable Carbon in Fuels from Coprocessing of Bio-oils in Refinery Using a Stable Carbon Isotopic Approach

Increasing renewable carbon incorporation into conventional fuels through coprocessing with vacuum gas oil (VGO, a petroleum refining feedstock) is a critical step in biofuels development, scaling-up, adoption and associated GHG reduction. Optimization of the co-processing parameters maximizes incorporation of the renewable carbon in the fuel products. Quantitative determination of the renewable carbon content in the co-processed products provides direct evaluation of the parameters. The co-processing bio-oil with VGO through hydrocracking (HC) or fluid catalytic cracking (FCC) system resulted in carbon isotopic fractionation that prevented the direct use of the isotope mixing model for quantifying the renewable carbon. Here, we report an algorithm of using a stable carbon isotope approach to quantify the renewable carbon content in co-processing biofuel products through high-precision ?13C analysis. A controlled experiment carried out by blending a fossil diesel (-29.013‰) with a bio-diesel (-30.099‰) at various blending levels up to 98.0/2.0 wt% is presented and has demonstrated the applicability of this approach. The carbon isotope fractionation factors for the bio-oil co-processing were obtained by using a 14C-derived isotope-mixing model. The ?13C method was tested by co-processing 13C-labeled bio-crude and natural woody biomass-derived fast pyrolysis (FP) and catalytic fast pyrolysis (CFP) bio-oils with VGO. The results were verified by 14C accelerator mass spectrometry (AMS) method (ASTM-D6866) and compared with the yield mass balance (YMB) method. Strong agreement between d13C and 14C AMS methods demonstrated the applicability of the ?13C method to quantify renewable carbon content in co-processing fuel products and guide the co-processing optimization

Li, Zhenghua↗
NASA NTRS1991

Determination of the isotopic composition of atmospheric methane and its application in the Antarctic

A procedure for establishing the C-13/C-12 ratio and the C-14 abundance in the atmospheric methane is discussed. The method involves air sample collection, measurement of the methane mixing ratio by gas chromotography followed by quantitative conversion of the methane in the air samples to CO2 and H2O, and analysis of the resulting CO2 for the C-13/C-12 ratio by stable isotope ratio mass spectrometry and measurement of C-14 content by accelerator mass spectrometry. The carbon isotropic composition of methane in air collected at Baring Head, New Zealand, and in air collected on aircraft flights between New Zealand and Antarctica is determined by the method, and no gradient in the composition between Baring Head and the South Pole station is found. As the technique is refined, and more data is gathered, small seasonal and long-term variations in C-13 are expected to be resolved.

Lowe, David C.↗
DOE OSTI2026

Bio-distribution and deposition of wildfire smoke chemicals into olfactory bulb and brain of rats after intranasal instillation

Epidemiological and experimental studies suggest wildfire smoke is a potential contributor to neurological dysfunction and associated with neuroinflammation. Using doses comparable to those encountered during intense wildfire events (200-300 μg/m 3 ), we explore the absorption, distribution, metabolism, and elimination (ADME) and pharmacokinetics of representative members of major chemical classes (acid, phenol, PAH, aldehyde) in inhaled wood smoke condensates. Male Sprague Dawley rats were intranasally instilled with smoldering eucalyptus woodsmoke extract (WSE) reconstituted in saline spiked with 14 C-labeled palmitic acid (PA), benzo[a]pyrene (B[a]P), catechol (CAT) or benzaldehyde (BZ). Serum was collected from 5 min to 2 weeks after exposure and tissues were collected at 0.5, 2, 4, 24 h and 2 weeks after exposure. Urine was collected over the 24 h exposure. Tissues were collected, rinsed in PBS and analyzed by accelerator mass spectrometry (AMS) for 14C-labeled chemicals. PA and B[a]P entered circulation slowly, reached maximum concentration (C max ) near 15 ng/mL at 2 h, and had circulating concentrations near 1/3 C max 24 h after exposure. CAT and BZ rapidly entered circulation and were mostly cleared at 2 h. Excess 14 C from all four chemicals was detected in olfactory bulb and brain over the first 24 h but only PA (or its metabolites) was retained in olfactory bulb, brain and kidney at 2 weeks post exposure. All excess 14 C was cleared from the lung at 2 weeks. Metabolite analysis of urine (CAT, BZ and B(a)P) dosed samples did not detect any parent compound. CAT and BZ were rapidly cleared. The slower uptake and clearance of PA or B[a]P or their reactive metabolites when dosed with WSE in brain and olfactory bulb potentially provide greater opportunity for inflammatory response. This study suggests that wildfire smoke chemicals can enter the brain directly from the nasal cavity to the olfactory bulb and via systemic circulation.

63 RADIATION, THERMAL, AND OTHER ENVIRON. POLLUTAN↗
DOE OSTI2023

10 Be at iThemba LABS using a silicon nitride membrane stack as absorber for isobar suppression

10 Be is an important isotope for accelerator mass spectrometry (AMS) because of the demand for cosmogenic radionuclide dating methods in the earth science and paleo-sciences community. At the iThemba Laboratory for Accelerator Based Science (iThemba LABS) we implemented full suppression of the interfering isobar 10 B using a silicon nitride foil-stack, utilizing the 2+ charge state for high efficiency. We demonstrate the performance of this newly established AMS system using standards and test samples. Here we further present the results of an inter-comparison between iThemba LABS and the Center for Accelerator Mass Spectrometry/Lawrence Livermore National Laboratory, on AMS samples prepared from purified quartz at the University of Vermont. The results for 10 Be from the laboratories are in close agreement, fully consistent with cross-calibration between them. AMS results for 26 Al are in similarly good agreement, demonstrating the performance and accuracy of iThemba LABS for the most commonly measured in situ produced cosmogenic nuclides.

10-Be↗
DOE OSTI2024

Quantifying replication through repeated analysis of UVM-A, a liquid reference material for cosmogenic 10 Be and 26 Al studies

In this study, in-situ produced cosmogenic nuclide sample preparation and analysis is a complicated, multi-step process with numerous possible sources of error, many of which have not been robustly quantified. Here, we use a liquid reference material (UVM-A) to test whether the analytic precision associated with individual isotopic ratios (n = 96) measured at two Accelerator Mass Spectrometry facilities (Lawrence Livermore National Laboratory and Purdue Rare Isotope Measurement Laboratory) accurately represents the range of values determined for aliquots prepared in a single laboratory over a period of five years. We find that 10 Be/ 9 Be ratios measured at the different accelerator facilities (n = 26 and n = 70) have statistically indistinguishable central tendencies, matching to within 0.1 %. Based on this large dataset, we suggest preliminary consensus values for UVM-A of 1.45 ± 0.06 x 10 -13 for 10 Be/ 9 Be (mean, one standard deviation, n = 96) and 4.47 ± 0.22 x 10 -13 for 26 Al/ 27 Al (mean, one standard deviation, n = 27). For both 10 Be/ 9 Be and 26 Al/ 27 Al, the relative standard deviations of the measured ratios are similar to the reported analytic uncertainties of sample measurement, suggesting that sample preparation introduced little if any additional scatter beyond the uncertainty of isotopic analysis. This dataset demonstrates that robust sample preparation and measurement can generate isotope ratio data reproducible at the level of counting statistics.

58 GEOSCIENCES↗
DOE OSTI2025

DNA adducts form in mouse lung and liver after oral naphthalene exposure

Naphthalene is a ubiquitous combustion product and environmental contaminant with known human exposure. Chronic exposure to naphthalene vapor leads to respiratory tumor formation in rodents. Naphthalene forms DNA adducts (precursors to genotoxicity) in tissue explants but it is unclear if this occurs in vivo. Wild-type C57BL/6 mice were orally exposed to 50 mg/kg 14 C-naphthalene. Naphthalene-DNA adducts were detected by accelerator mass spectrometry at 2- to 72-h post-exposure in both lung and liver, with decreasing abundance over time. Adducts persisted even at 72-h after exposure, which indicates possible evasion of DNA repair and potential to contribute to mutagenesis.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2025

The development and evolution of biological AMS at Livermore: a perspective

Biological accelerator mass spectrometry (AMS) provides ultrasensitive carbon-14 isotopic analysis enabling a deeper understanding of human health concerns by enabling quantification of pharmacokinetics and other molecular endpoints directly in humans. It enables environmentally and human relevant studies of metabolic pathways through the use of very low concentrations of labeled metabolic substrates in cells and organisms. Here, we discuss why AMS is an important tool for the biosciences, the development and evolution of biological AMS at Livermore and discuss technical refinements that will improve the efficiency of operation for the measurement of ultra-trace levels of 14 C, which, long term, will enable greater ease of use and sample throughput.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

Oxaliplatin–DNA Adducts as Predictive Biomarkers of FOLFOX Response in Colorectal Cancer: A Potential Treatment Optimization Strategy

FOLFOX is one of the most effective treatments for advanced colorectal cancer (CRC). However, cumulative oxaliplatin neurotoxicity often results in halting the therapy. Oxaliplatin functions predominantly via the formation of toxic covalent drug-DNA adducts. We hypothesize that oxaliplatin-DNA adduct levels formed in vivo in peripheral blood mononuclear cells (PBMC) are proportional to tumor shrinkage caused by FOLFOX therapy. We further hypothesize that adducts induced by sub-therapeutic "diagnostic microdoses" are proportional to those induced by therapeutic doses and are also predictive of response to FOLFOX therapy. These hypotheses were tested in CRC cell lines and a pilot clinical study. Four CRC cell lines were cultured with therapeutically relevant (100 µM) or diagnostic microdose (1 µM) concentrations of [ 14 C]oxaliplatin. The C-14 label enabled quantification of oxaliplatin-DNA adduct level with accelerator mass spectrometry (AMS). Oxaliplatin-DNA adduct formation was correlated with oxaliplatin cytotoxicity for each cell line as measured by the MTT viability assay. Six CRC patients received by IV a diagnostic microdose containing [ 14 C]oxaliplatin prior to treatment, as well as a second [ 14 C]oxaliplatin dose during FOLFOX chemotherapy, termed a "therapeutic dose." Oxaliplatin-DNA adduct levels from PBMC correlated significantly to mean tumor volume change of evaluable target lesions (5 of the 6 patients had measurable disease). Finally, oxaliplatin-DNA adduct levels were linearly proportional between microdose and therapeutically relevant concentrations in cell culture experiments and patient samples, as was plasma pharmacokinetics, indicating potential utility of diagnostic microdosing.

60 APPLIED LIFE SCIENCES↗
NASA NTRS1984

Radioactivities in returned lunar materials and in meteorites

Carbon 14 terrestial ages were determined with low level minicomputers and accelerator mass spectrometry on 1 Yamato and 18 Allan Hills and nearby sited meteorites. Techniques for an accelerator mass spectrometer which make C(14) measurements on small samples were developed. Also Be(10) concentrations were measured in Byrd core and Allan Hills ice samples.

Fireman, E. L.↗
DOE OSTI2023

Benzo[$\mathcal{a}$]pyrene toxicokinetics in humans following dietary supplementation with 3,3'-diindolylmethane (DIM) or Brussels sprouts

Utilizing the atto-zeptomole sensitivity of UPLC-accelerator mass spectrometry (UPLC-AMS), we previously demonstrated significant first-pass metabolism following escalating (25–250 ng) oral micro-dosing in humans of [ 14 C]-benzo[a]pyrene ([ 14 C]-BaP). The present study examines the potential for supplementation with Brussels sprouts (BS) or 3,3' -diindolylmethane (DIM) to alter plasma levels of [ 14 C]-BaP and metabolites over a 48-h period following micro-dosing with 50 ng (5.4 nCi) [ 14 C]-BaP. Volunteers were dosed with [ 14 C]-BaP following fourteen days on a cruciferous vegetable restricted diet, or the same diet supplemented for seven days with 50 g of BS or 300 mg of BR-DIM ® prior to dosing. BS or DIM reduced total [ 14 C] recovered from plasma by 56–67% relative to nonintervention. Dietary supplementation with DIM markedly increased T max and reduced C max for [ 14 C]-BaP indicative of slower absorption. Further, both dietary treatments significantly reduced C max values of four downstream BaP metabolites, consistent with delaying BaP absorption. Dietary treatments also appeared to reduce the T 1/2 and the plasma AUC( 0,$\infty$ ) for Unknown Metabolite C, indicating some effect in accelerating clearance of this metabolite. Toxicokinetic constants for other metabolites followed the pattern for [ 14 C]-BaP (metabolite profiles remained relatively consistent) and non-compartmental analysis did not indicate other significant alterations. Significant amounts of metabolites in plasma were at the bay region of [ 14 C]-BaP irrespective of treatment. Although the number of subjects and large interindividual variation are limitations of this study, it represents the first human trial showing dietary intervention altering toxicokinetics of a defined dose of a known human carcinogen.

3,3'-diindolylmethane↗
DOE OSTI2025

First experimental determination of the ⁴⁰Ar(𝑛, 2𝑛)³⁹Ar reaction cross section and ³⁹Ar production in Earth’s atmosphere

The cosmogenic ³⁹Ar(t1∕2 = 268 years) isotope of argon is used for geophysical dating and tracing of underground and ocean water, as well as ice owing to its appropriate half-life and chemical inertness as a noble gas; ³⁹Ar serves also in nuclear weapon test monitoring. We measured for the first time the total cross section of the main ³⁹Ar cosmogenic production reaction in the atmosphere, namely ⁴⁰Ar(𝑛, 2𝑛)39 Ar, using 14.8 ± 0.3 MeV neutrons. The neutrons, produced by a deuterium-tritium generator, impinged on a stainless steel sphere filled with Ar gas highly enriched in the ⁴⁰Ar isotope and were monitored by a stack of fast-neutron activation foils. The reaction yield was measured by atom counting of long-lived ³⁹Ar with noble gas accelerator mass spectrometry and, independently, by decay counting relative to atmospheric argon (³⁹Ar/Ar= 8.12 × 10−16 ). A total ⁴⁰Ar(𝑛, 2𝑛)39 Ar cross section of 610 ± 100 mb was determined at 14.8 ± 0.3 MeV incident neutron energy. This result serves as a benchmark for recent theoretical calculations and evaluations, found to reproduce well the experimental total cross section. We use these energy-dependent theoretical cross sections together with experimental spectra of cosmogenic neutrons at different altitudes to calculate the global average rate of neutron-induced ³⁹Ar atmospheric production, resulting in 770 ± 240 39 Ar atoms/cm²/day. The secular equilibrium between the ³⁹Ar calculated production rate and radioactive decay rate leads to a partial isotopic abundance ³⁹Ar/Ar = (5.9 ± 1.8) × 10−16 , showing that ≈73% of atmospheric ³⁹Ar is produced by cosmogenic neutrons, the remaining part believed to be induced by muons and high-energy 𝛾 rays. The ⁴⁰Ar(𝑛, 2𝑛)³⁹Ar cross section at 14 MeV is also a key parameter for quantifying the anthropogenic contribution to atmospheric 39 Ar produced during the thermonuclear tests of the 1960s. We estimate that anthropogenic ³⁹Ar accounts for roughly 20% of the present atmospheric inventory.

39 Ar atmospheric production↗
DOE OSTI2026

Naphthalene-DNA Adduct Formation in a Lung Airway Explant Model: The Role of Bioactivation and Naphthalene Metabolites

Humans are widely exposed to naphthalene. Once inhaled or ingested, naphthalene is metabolized by cytochrome P450 and other enzymes to form toxic metabolites known to harm lung epithelial cells. Naphthalene metabolites circulate in the blood. Chronic naphthalene inhalation promotes lesions in the epithelium of the mouse lung and rat nose. Oral naphthalene exposure leads to DNA adduct formation in mouse lung, but the contributions of different enzymatic pathways and the metabolites they generate are not fully understood. This study explores the influence of naphthalene metabolites on DNA adduct formation in the lungs of two species (mice and primates). To isolate the lung response, conducting airway explants containing Club cells, a target for pulmonary naphthalene toxicity, were microdissected from live lung tissue and incubated with 14 C-naphthalene or its metabolites: 14 C-1,2-naphthoquinone or 14 C-naphthalene-1,2-dihydrodiol. Explants were incubated for 1 h, then processed immediately (T1), or were transferred to clean media for the remainder of the 24 h (T24), to monitor 14 C in DNA over time. Accelerator mass spectrometry analysis revealed the formation of DNA adducts by all three radiolabeled compounds by T24. Our results support the notion that P450 enzymes of the Cyp2abfgs subfamily contribute to naphthalene-induced DNA adduct formation (approximately 4-fold reduction in male mice lacking the Cyp2abfgs genes, P < 0.01). The finding that naphthalene-1,2-dihydrodiol, a stable metabolite, formed DNA adducts (102–117 adducts/10 8 nucleotides) at 24 h following addition to the culture media validates the concern that circulating naphthalene metabolites can contribute to DNA adduct formation in the lung. DNA adducts persisted to 24 h after exposure in both mouse and primate airways and at comparable levels between species (77.8 vs 129 adducts/10 8 nucleotides, respectively). Together, these results support the importance of a potential genotoxic mechanism of naphthalene and its metabolites in vivo in both mice and nonhuman primates, and possibly also in humans.

Biological and medical sciences↗
DOE OSTI2021

Benzo[a]pyrene (BaP) metabolites predominant in human plasma following escalating oral micro-dosing with [ 14 C]-BaP

Benzo[a]pyrene (BaP) is formed by incomplete combustion of organic materials (petroleum, coal, tobacco, etc.). BaP is designated by the International Agency for Research on Cancer as a group 1 known human carcinogen; a classification supported by numerous studies in preclinical models and epidemiology studies of exposed populations. Risk assessment relies on toxicokinetic and cancer studies in rodents at doses 5–6 orders of magnitude greater than average human uptake. Using a dose–response design at environmentally relevant concentrations, this study follows uptake, metabolism, and elimination of [ 14 C]-BaP in human plasma by employing UPLC - accelerator mass spectrometry (UPLC-AMS). Volunteers were administered 25, 50, 100, and 250 ng (2.7–27 nCi) of [ 14 C]-BaP (with interceding minimum 3-week washout periods) with quantification of parent [ 14 C]-BaP and metabolites in plasma measured over 48 h. [ 14 C]-BaP median T max was 30 min with C max and area under the curve (AUC) approximating dose-dependency. Marked inter-individual variability in plasma pharmacokinetics following a 250 ng dose was seen with 7 volunteers as measured by the C max (8.99 ± 7.08 ng × mL -1 ) and AUC0-48hr (68.6 ± 64.0 fg × hr -1 × mL -1 ). Approximately 3–6% of the [ 14 C] recovered (AUC 0-48 hr ) was parent compound, demonstrating extensive metabolism following oral dosing. Metabolite profiles showed that, even at the earliest time-point (30 min), a substantial percentage of [ 14 C] in plasma was polar BaP metabolites. The best fit modeling approach identified non-compartmental apparent volume of distribution of BaP as significantly increasing as a function of dose (p = 0.004). Bay region tetrols and dihydrodiols predominated, suggesting not only was there extensive first pass metabolism but also potentially bioactivation. AMS enables the study of environmental carcinogens in humans with de minimus risk, allowing for important testing and validation of physiologically based pharmacokinetic models derived from animal data, risk assessment, and the interpretation of data from high-risk occupationally exposed populations.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2026

Queen bees offload pesticide burden to eggs when social buffering is overwhelmed

Honey bee colonies pollinate about one-third of the world’s food crops, and their rapid decline directly threatens agricultural productivity and ecosystem stability. Understanding how colony-level social defenses influence pesticide fate and the circumstances under which they fail is therefore a crucial question in pollinator biology. We used biological accelerator mass spectrometry (BioAMS), a sensitive radiotracer technique, to track the movement of a model pesticide through a small honey bee colony under laboratory conditions. We tested the hypothesis that social buffering protects honey bees from toxic accumulation and that this protection can be overcome, leading to maternal offloading of the pesticide to developing eggs. Consistent with this hypothesis, our results identified three key mechanisms governing chemical movement within a social insect colony: (1) worker bees initially decrease dietary pesticide levels by 95% through diet filtering and deposition in honeycombs, though this declines to 86% by day 10; (2) queen bees maintain markedly lower pesticide levels than workers but, over time, they accumulate the pesticide in their ovaries and transfer it into developing eggs, revealing a previously undocumented protective mechanism in reproductive individuals; and (3) the presence of a queen bee shifts colony-wide chemical distribution by concentrating worker exposure and increasing pesticide deposition in wax. Our findings show that honey bee colonies function as integrated detoxification networks, in which chemical fate depends on complex social behaviors and caste-specific physiology. When social buffering is overwhelmed, reproductive queens may survive by transferring their chemical burden to their offspring.

Biological and medical sciences↗
DOE OSTI2022

Clean quartz matters for cosmogenic nuclide analyses: An exploration of the importance of sample purity using the CRONUS-N reference material

We report reference materials are key for assessing inter-laboratory variability and measurement quality, and for placing analytical uncertainty bounds on sample analyses. Here, we investigate four years of data resulting from repeated processing of the CRONUS-N reference material for cosmogenic 10 Be and 26 Al analyses. At University of Vermont, we prepared a CRONUS-N aliquot with most of our sample batches from 2013 to 2017; these reference material samples were then distributed to four different accelerator mass spectrometry facilities, yielding 73 10 Be analyses and 58 26 Al analyses. We determine CRONUS-N 10 Be concentrations of (2.26 ± 0.14) x 10 5 atoms g -1 (n = 73, mean, 1 SD) and 26 Al concentrations of (1.00 ± 0.08) x 10 6 atoms g -1 (n = 58, mean, 1 SD). We find a reproducibility of 6.3% for 10 Be and 7.7% for 26 Al (relative standard deviations). We also document highly variable 27 Al and Mg concentrations and a 10 Be dispersion twice as large as the mean AMS analytic uncertainty. Analyses of the CRONUS-N material with and without density separation demonstrate that non-quartz minerals are present in the material and have a large impact on measured concentrations of 27 Al, 10 Be, and impurities; these non-quartz minerals represent only a very small portion of the total mass (0.6–0.8%) but have a disproportionally large effect on the resulting data. Our results highlight the importance of completely removing all non-quartz mineral phases from samples prior to Be/Al extraction for the determination of in situ cosmogenic 10 Be and 26 Al concentrations.

58 GEOSCIENCES↗