In situ apatite U-Pb, fission track and (U-Th)/He triple dating using a simple embedding approach
Abstract. Thermo- and geochronology techniques are foundational for many studies in tectonics, petrology, and surface processes. They provide essential information about cooling histories during exhumation or burial, and sediment provenance. Application of these methods has, in the past, primarily focused on applying individual techniques to separate mineral grains. More recently, analytical developments in laser-ablation geochronology have enabled the application of multiple dating techniques to an individual mineral grain (i.e., double or triple dating) to provide enhanced resolution of the mineral’s thermal history or dates and, therefore, the geologic or geomorphic interpretations derived from it. However, applying multiple geochronological methods to individual grains often requires methodological compromises that can restrict their applicability. In this study, we present a simplified and robust technique for embedding apatite grains in Teflon mounts. This approach enables the combined application of U-Pb, apatite fission track, and in-situ (U-Th)/He dating. In addition, this approach preserves the ability to quantify trace-element compositions and radionuclide zoning. The approach enables to significantly increase the number of measurements per sample, thereby opening the door to more robust results required for many applications.
To ensure high data quality from in-situ (U-Th)/He analyses, we introduce a decision matrix based on four key evaluation criteria: laser pit shape, radionuclide zoning, grain geometry, and the pit–grain relationship. We apply this integrated methodology to both the well-characterized Durango apatite standard and a sample from the crystalline basement of the Odenwald, western Germany. Our results demonstrate the robustness and reliability of this approach. Specifically, we obtain in-situ (U-Th)/He ages for Durango apatite (aliquot 1) of 31.04 ± 1.04 Ma (aliquot 1, n=35) and 31.38 ± 2.53 Ma (aliquot 2, n=22), which are in excellent agreement with accepted reference ages. Apatite U-Pb and fission track ages from the same grains, completing the triple dating approach, yield ages of 31.7 ± 1.9 Ma (U-Pb concordia age) and 35.0 ± 4.4 Ma (central AFT age).
The Odenwald sample reveals a complex, multi-phase cooling history consistent with major regional geodynamic events, including Late Cretaceous doming and Eocene exhumation associated with the formation of the Upper Rhine Graben. Importantly, our results confirm that the Teflon mounting procedure, which requires short-term heating to 300 °C, did does not cause measurable helium loss or reduce fission track density and track length in the near F-endmember Durango apatite, a mineral susceptible to annealing. This supports the viability of this approach for high-resolution, multi-system geo- and thermochronology thereby expanding the utility of these techniques to a broader range of geoscience applications.
This is a great paper, showing a really nice integrated methodology for in situ U-Th/He, FT and U-Pb dating of apatite in Teflon mounts. It is going to be a valuable contribution to the field.
I think what would be useful for this manuscript is a figure comprised of a series of schematic panels illustrating all the steps in the triple dating and also explicitly stating the order of the analysis steps in the abstract - mounting, etching, grain selection; FT counting, H measurement, volume estimation and then LA-ICP-MS analysis.
I could not download any of the scripts from the Zenodo repository – were they meant to be visible to the reviewers? It would have been useful if they were.
My only reservation is the U-Pb age calculation. A zircon should not be used as the U-Pb age standard, and Durango is far too young for an accurate correction. McClure Mountain was analysed – it should be the primary. Why was it not used? You also cannot perform a drift correction on the 206Pb/238U ratio because the standards invariably contains variable common Pb – the common Pb correction must be undertaken first, and then you drift correct the common Pb-corrected 206Pb/238U ratio. See Chew et al., 2014 Chemical Geology which discusses all this in detail. Minor edits are listed below.
Best wishes
David Chew
Miinor comments
L46 ‘and expanded’
L51-52 Recent progress in in-situ (U–Th)/He thermochronometry has demonstrated its compatibility with other dating systems, such as U-Pb, Lu-Hf, and fission-track methods (e.g., Carrapa et al., 2009; Bedoya et al., 2024).
I do not get this sentence. Why does compatible mean in this context? Surely the point about in situ (U-Th)/He is that it works (i.e. it reproduces conventional single crystal analyses of age reference materials) and it gives you spatial control.
L61-63 A more recent innovation by Bedoya et al. (2024) involved a sequential analysis of Lu-Hf, U-Pb, and after polishing, the LA-ICP-MS-based fission track dating method was applied to single apatite grains embedded in epoxy mounts.
Emphasize the point here that it does not require extraction from the mount. Is the analysis order correct? It would seem to make sense to count for FT first before the grain is more or less destroyed by the big Lu-Hf spot.
L64 Since epoxy degasses under ultra-high vacuum conditions
Is this true of all epoxy resins? Has anyone tried Petropoxy under a ultra-high vacuum?
L105 1. Initial Setup: A clean glass slide was coated with a thin film of epoxy to fix grains in place during mounting.
Would double-sided tape work – presumably the epoxy will cure at room temperature leaving not much time for grain placement. What epoxy was used?
L164 The zenodo link does not appear to work, and in any case it is not clear what of the following six numbered steps it is used for.
L199, L234,L272, L301 These zenodo links do not appear to be valid either in the DOI system.
L301-312 – see substantive comment.
L322-323 I do not like the term variable common lead composition referring to Durango. I think it is accepted its initial Pb isotopic composition is homogenous (see Paul et al. Chemical Geology 2021); what varies is the amount of common Pbn in each analysis – so refer to variable amounts of common Pb, not variable Pb composition. It is an important difference.
L418 The IM field is a bit broader that – it includes low ASI (non-peraluminous) granites. There is a pre-IOA rhyolite along with pre- and post IOA ignimbrite in Durango, and the the Durango-Mazatlán ignimbrites are true rhyolites in composition that follow a high-potassium calc-alkaline trend (McDowell et al., 2007). So they would likely plot in the IM field.
L449 I would present these data as a lower intercept age on TW concordia – it is very unusual to present 207Pb-corrected data on Wetherill concordia as it makes everything perfectly concordant. Same for sample 22BGE055T in Fig. 4.
L630-631 What inverse thermal history modelling software was used – your own or HeFTy? Needs more detail.