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USGS2025

RioM-1: A new calcite reference material for U-Pb LA-ICP-MS geochronology

Determining absolute ages of carbonate diagenesis, faulting, fossil formation, speleothem growth, carbonate-hosted hydrocarbon deposits, vein mineralisation and hydrothermal alteration has become increasingly accessible through LA-ICP-MS U-Pb dating of calcite, complementing traditional isotope dilution methods still applicable to certain materials (e.g., speleothems via micro-drilling). However, well-calibrated reference materials for LA-ICP-MS calcite geochronology remain scarce. Here, we characterise the Rio Maior calcite, designated ‘RioM-1’, as a potential reference material for U-Pb dating by LA-ICP-MS. Fragments (0.1 to 1 cm 3 ) from a single scalenohedral crystal were analysed by ID-TIMS (U-Pb), LA-ICP-MS (U-Pb and 87 Sr/ 86 Sr), and SIMS (O isotopes). RioM-1 displays high U mass fraction and low, though variable, proportions of common Pb. Combined ID-TIMS analyses from two independent laboratories yielded a Tera-Wasserburg lower intercept date of 63.93 ± 0.11 Ma (2 s , MSWD = 1.3, n = 16). LA-ICP-MS U-Pb data from three independent laboratories are concordant with the TIMS age, producing a pooled date of 64.10 ± 0.12/1.2 Ma (2 s , MSWD = 7.7, n = 708) and an initial 207 Pb/ 206 Pb ratio of 0.85 ± 0.01. Other calcite reference materials, when normalised to RioM-1, yielded dates within uncertainty of their published values. SIMS measurements returned a mean 18 O/ 16 O of 0.002044450 ± 181 (1 s ) and δ 18 O SMOW of 19.57 ± 0.92‰ (1 s ), while LA-ICP-MS strontium isotope measurement yielded a mean 87 Sr/ 86 Sr of 0.708177 ± 9 (2 s ).

Geostandards and Geoanalytical Research↗
USGS2025

Using peak geometry and shifts in the x-ray spectrum of carbon from electron probe microanalysis to determine thermal maturity of organic matter

During the burial of mudstones, the associated organic matter undergoes gradual thermal maturation, a key process that can influence the reactivity of organic matter during catagenesis, the formation of hydrocarbon deposits and the chemical weathering of mudstones. Conventional methods for assessing the thermal maturity of organic matter often fail to reflect the geochemical heterogeneity between individual organic phases in mudstone samples. Here, we report an alternative, non-destructive, surficial and micro-scale (analytical spot size of ~ 300 nm with about 4 μm diffusion depth for micrometre-size organic grains) method to evaluate the thermal maturity of organic matter in mudstones using the carbon K α X-ray spectrum measured by field emission-electron probe microanalyser (FE-EPMA). Using this method, we observed correlations between parameter values derived from FE-EPMA spectra, including the peak position, the peak area and the intra-sample heterogeneity of these measurements, and independently measured vitrinite/solid bitumen reflectance for a suite of mudstones, representing different age, geological context and burial depth. With the increased values in peak area and position, we identified an increase in the carbon mass fraction of organic matter and the mean nominal oxidation state of carbon approaching zero. These trends, which are consistent with aromatisation and graphitisation, provide the rationale for using FE-EPMA to estimate the thermal maturity of organic matter. To explore some of these trends in more detail, we employed time-of-flight secondary ionisation mass spectrometry, X-ray photoelectron spectroscopy and optical reflectance measurements on a subset of samples.

Geostandards and Geoanalytical Research↗