the Creative Commons Attribution 4.0 License.
the Creative Commons Attribution 4.0 License.
Infrared-radiofluorescence in feldspar: grain-scale mineralogy and its effect on dose response curves and apparent saturation
Abstract. Infrared radiofluorescence (IR-RF) dating of K-feldspar is commonly performed on multi-grain aliquots, implicitly treating the IR-RF dose response curve (DRC) and its apparent saturation behavior as properties of a sample. Here, we test the alternative hypothesis that bulk DRC curvature and plateau dose can emerge from mixtures of grains with contrasting mineralogy and luminescence behavior. We combine (i) single-grain, multi-spectral RF measurements (710, 850, 880 nm) on feldspar reference materials spanning the ternary diagram, (ii) controlled mixed-grain aliquot experiments using a detection window centered at 850 nm, (iii) spatially resolved IR-RF (SR IR-RF) imaging of natural samples (X7363, X7368) using an RF70 style protocol and grain-scale DRC classification, and (iv) synchrotron-based µ-XRF mapping at 10 keV to assess grain-scale chemistry and evaluate surface versus interior controls.
Reference measurements confirm strong dependence of IR-RF behavior on feldspar type and polymorph. Albite and microcline commonly show high initial intensities and decaying DRCs at 850–880 nm, whereas Ca-rich feldspars are weak and near-flat, and sanidine exhibits variable, sometimes increasing DRCs. Mixing experiments demonstrate that adding a small number of grains with contrasting behavior measurably shifts microcline DRC curvature and reduces apparent saturation. SR IR-RF reveals that both natural samples tested contain grains with decreasing, increasing, and near-flat regenerative DRCs, and that polishing produces minimal change in DRC shape, arguing against a purely surface-controlled origin for anomalous behavior. Qualitative 10 keV µ-XRF maps show that grain-scale elemental detections and spatial patterns do not uniquely predict the DRC category, implying that IR-RF behavior is not controlled by composition alone. For dating purposes, these results imply that saturation limits and equivalent dose estimates should not be inferred from averaged signals in heterogeneous samples, particularly those of volcanic origin. We propose a practical two-step screening workflow that combines DRC-shape classification with the dose corresponding to 95 % of the fitted asymptotic level (D95) to prioritize high-capacity grains. This approach now requires validation on independently well-dated and/or stratigraphically constrained sequences.
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Status: final response (author comments only)
- RC1: 'Comment on egusphere-2026-2868', Anonymous Referee #1, 07 Jul 2026
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RC2: 'Comment on egusphere-2026-2868', Anonymous Referee #2, 30 Jul 2026
General comments:
The manuscript by Grandfield et al. investigates the production of feldspar Infrared-radiofluorescence (IR-RF) signals and their relationship to grain-specified mineralogy, which is essential for IR-stimulated luminescence dating of feldspars. The authors show highly variable IR-RF dose-response behaviors among different grains within a single sample using multi-spectral single-grain RF measurements, controlled artificial mixing experiments, and spatially resolved IR-RF imaging (SR IR-RF). These characteristics are not solely dependent upon the chemical composition of the grains, which are revealed by synchrotron-based XRF mapping. Based upon these observations, the authors proposed a two-step screening strategy by combining DRC shape and 95% saturation to pick out feldspar grains suitable for dating. The manuscript is clear, well-structured, and it will be a valuable contribution to Geochronology. However, some points and figures need to be clarified before its formal acceptance for publication; a mild to major revision referring to the comments below is therefore encouraged.
Major comments
- The synchrotron uXRF mapping is the key support of the conclusion drawn by this study, although it, to some extent, denies the main role of chemical composition on IR-RF behavior. It’s better to state clearly the analytical constraints and detection limits by using 10 keV XRF and the accuracy and precision in determining the content of key elements, e.g., Fe, Mn, Ti, that may affect the luminescence production. Including the analysis of a standard sample is highly encouraged. Meanwhile, the authors need to bear in mind that the minor role of major element chemistry does not necessarily deny the contribution from the subtle roles of trace elements in forming recombination centers or altering the configuration of the crystal lattice.
- The authors proposed to use the dose corresponding to 95% of the fitted asymptotic saturation level to screen out grains for IR-RF dating. It is better to have a sensitivity test using different functions to fit the dose response. In addition, I strongly encourage the authors to include two samples with independent age control, one fully bleached and the other not fully bleached, to show how the grain-level IR-RF characteristics would affect the dating accuracy.
Minor comments
- In general, when I read through the m/s, I feel strongly that the authors need to balance the details of different sections. On one hand, the illustration of experimental results needs to be more accurate and concise. For instance, lines 273 to 284 are too descriptive; what do “sharp” increase or decrease mean exactly? I may suggest the authors adopt a more systematic way and simply claim whether the IR-RF DRCs are negative, positive, or not dependent upon the radiation doses. The use of a parameter, decay constant or growth constant to quantify such dependence is highly encouraged. In my opinion, it’s better to avoid a long description of the curves. On the other hand, more details about the experiment and how you made the measurements need to be more detailed.
- For Fig. 1, it is not clear whether the elements are mineral-limited or detection-limited. It’s better to include both the consensus of the elements expected to be observed for different mineralogy and the actually detected elements. Fig 3 lacks the spatial scale for the u-XRF images, and there are also no labels for the X and Y axes. Fig 4a, the Y-axis should also be IR-RF? I may suggest you integrate Fig. 4, 5, 6, and 8 into one figure to make the m/s more compact. For the spatially resolved measurements, all data are shown in supplementary figures (Fig. S10 and S11), and no spatial information could be identified. I may suggest some attempt to align the IR-RF emission/characteristic maps with the u-XRF elemental maps and show the figure in the main text.
- For the mixing experiment, it would be better to specify more experimental details when synthesizing the DRC from individual grain curves.
Citation: https://doi.org/10.5194/egusphere-2026-2868-RC2
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General comments
Taylor Grandfield and her co-authors investigated the IR-RF dose saturation behaviour of single sediment grains containing different types of K-feldspar. In a series of intriguing experiments, they demonstrated the inter-grain IR-RF signal decay heterogeneity and its impact on combined multi-grain signals. Using the D95 fitting value, they introduced a new measure of single-grain dose saturation. However, they were unable to correlate the observed IR-RF curve behaviours with µ-XRF element mappings, but explained why.
The manuscript is well written, following a scientific narrative that makes it easy to read and understand. However, it is rather weak regarding rigour and attention to detail. In my opinion, some obvious issues should have been spotted during internal group reviews before submission. The µ-XRF part of the manuscript is especially problematic. It contains misinterpretations of the data and shortcomings in the documentation itself. If that part were the main scientific contribution of the manuscript, I would recommend rejection. Fortunately, the more important IR-RF section of the manuscript is scientifically sound, although not without issues.
Overall, this manuscript makes an important contribution to research on K-feldspar IR-RF as a new dating method and is thus well within the scope of Geochronology. For this reason, I recommend accepting the manuscript for publication, but only after a major revision.
For specific and technical comments, please see the attached PDF file.