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In both nature and synthetic experiments, the common iron oxide haematite (α‐Fe2O3) can incorporate significant amounts of U into its crystal structure and retain radiogenic Pb over geological time. Haematite is a ubiquitous component of many ore deposit types and, therefore, represents a valuable hydrothermal mineral geochronometer, allowing direct constraints to be placed on the timing of ore formation and upgrading. However, to date, no suitable natural haematite reference material has been identified. Here, a synthetic haematite U‐Pb reference material (MR‐HFO) is characterised using LA‐ICP‐MS and ID‐TIMS. Centimetre‐scale ‘chips’ of synthesised α‐Fe2O3 were randomly microsampled via laser ablation‐extraction and analysed using ID‐TIMS. Reproducible U/Pb and Pb/Pb measurements were obtained across four separate chips (n = 13). Subsequently, an evaluation of the suitability MR‐HFO in constraining U‐Pb data via LA‐ICP‐MS is presented using a selection of natural samples ranging from Cenozoic to Proterozoic in age. The MR‐HFO normalised U‐Pb ratios are more concordant and ages more accurate versus the same LA‐ICP‐MS spot analyses normalised to zircon reference material, when compared with independently acquired ID‐TIMS data from the same natural haematite grains. Results establish MR‐HFO as a suitable reference material for LA‐ICP‐MS haematite U‐Pb geochronology.

Establishing timescales for iron oxide copper-gold (IOCG) deposit formation and the temporal relationships between ores and the magmatic rocks from which hydrothermal, metal-rich fluids are sourced is often dependent on low-precision data, particularly for deposits that formed during the Proterozoic. Unlike accessory minerals routinely used to track hydrothermal mineralization, iron oxides are dominant components of IOCG systems and are therefore pivotal to understanding deposit evolution. The presence of ubiquitous, magmatic-hydrothermal U-(Pb)-W-Sn-Mo–bearing zoned hematite resolves a range of geochronological issues concerning formation of the ~1.6 Ga Olympic Dam IOCG deposit, South Australia, at up to ~0.05% precision (207Pb/206Pb weighted mean; 2σ) using isotope dilution-thermal ionization mass spectrometry (ID-TIMS). Coupled with chemical abrasion-ID-TIMS zircon dates from host granite and volcanic rocks within and enclosing the ore-body, a confident magmatic-hydrothermal chronology is defined. The youngest zircon date from the granite intrusion hosting Olympic Dam indicates magmatism was occurring up until 1593.28 ± 0.26 Ma. The orebody was principally formed during a major mineralizing event following granite uplift and during cupola collapse, whereby the hematite with the oldest age is recorded in the outer shell of the deposit at 1591.27 ± 0.89 Ma, ~2 m.y. later than the youngest documented magmatic zircon. Hematite dates captured throughout major lithologies, different ore zones, and the ~2-km vertical extent of the deposit support ~2 m.y. of hydrothermal activity. New age constraints on the spatial-temporal evolution of the formation of Olympic Dam are considered with respect to a mantle to crustal continuum model. Cyclical tapping of magma reservoirs to maintain crystal mushes for extended time periods and incremental building of batholiths on the million-year scale prior to main mineralization pulses can explain the ~2-m.y. temporal window temporal win

In both nature and synthetic experiments, the common iron oxide haematite (α‐Fe2O3) can incorporate significant amounts of U into its crystal structure and retain radiogenic Pb over geological time. Haematite is a ubiquitous component of many ore deposit types and, therefore, represents a valuable hydrothermal mineral geochronometer, allowing direct constraints to be placed on the timing of ore formation and upgrading. However, to date, no suitable natural haematite reference material has been identified. Here, a synthetic haematite U‐Pb reference material (MR‐HFO) is characterised using LA‐ICP‐MS and ID‐TIMS. Centimetre‐scale ‘chips’ of synthesised α‐Fe2O3 were randomly microsampled via laser ablation‐extraction and analysed using ID‐TIMS. Reproducible U/Pb and Pb/Pb measurements were obtained across four separate chips (n = 13). Subsequently, an evaluation of the suitability MR‐HFO in constraining U‐Pb data via LA‐ICP‐MS is presented using a selection of natural samples ranging from Cenozoic to Proterozoic in age. The MR‐HFO normalised U‐Pb ratios are more concordant and ages more accurate versus the same LA‐ICP‐MS spot analyses normalised to zircon reference material, when compared with independently acquired ID‐TIMS data from the same natural haematite grains. Results establish MR‐HFO as a suitable reference material for LA‐ICP‐MS haematite U‐Pb geochronology.

Hematite (α-Fe2O3) is a common iron-oxide mineral known to incorporate U into its crystal lattice at up to wt% concentrations and has been previously used to date ore formation within iron-oxide copper gold and banded iron formation deposits. However, there has been no detailed evaluation of the potential challenges this novel mineral geochronometer may present for accurate temporal interpretation. We report a multi-technique UPb geochronological study comprising laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS), sensitive high-resolution ion microprobe (SHRIMP) and the first isotope dilution-thermal ionization mass spectrometry (ID-TIMS) procedure and analyses using an in-situ grain micro-sampling technique. We assess intra- and inter-sample data reproducibility, and examine the compatibility of spatial and analytical resolutions to texturally and compositionally diverse samples. Five samples of hydrothermal, primary, oscillatory-zoned hematite were analysed from distinct lithologies throughout the ~1.59 Ga Olympic Dam Cu-U-Au-Ag deposit, with typical U concentrations ranging between ~20 and 1000 ppm. LA-ICP-MS mapping of isotope distributions across mm-sized grains allows pinpointing of U-rich and relatively U/Pb isotopically ‘homogeneous’ domains. Micro-domains were extracted via laser-cut square shaped trenches (100 × 100 μm). UPb datum range in complexity, with concordant age domains measured by ID-TIMS indicating that hematite can retain a near-closed UPb system over ~1.6 Ga, while also demonstrating that younger Pb-loss events may be recorded. Significant reverse discordance is common in the data, likely to be a real feature due to both internal decoupling and mobility of Pb within a single grain and UPb fractionation during microbeam analysis. These effects will obscure the interpretation of real ages for Proterozoic samples where non-zero age Pb-loss events occur, and restricts the evaluation of common Pb mixing components. As a result