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The Rhodope Metamorphic Complex (RMC) is a high-grade crystalline massif located at the northern margin of the Aegean region. Numerous scenarios have been proposed for the evolution of the RMC during Alpine times. A debated issue is whether there has been a single protracted orogenic cycle since around the mid-Mesozoic or whether Alpine orogeny involved distinct episodes of subduction and crustal accretion. We describe a key outcrop located on the Nestos Shear Zone (NSZ), a major NNE-dipping top-to-SW shear zone characterized by an inverted metamorphic sequence. Structural and petrological data document the existence of two anatectic events. The first event, best preserved in decametric structural lenses, is pre-kinematic with respect to top-to-SW shearing and involved high-temperature “dry” melting. Zircon and monazite LA-ICPMS U-Th-Pb data indicate that this event occurred at ∼140 Ma. The second event is syn-kinematic with respect to top-to-SW shearing and involved lower-temperature water-assisted melting. Zircon and rutile LA-ICPMS U-Pb data indicate that this second event occurred at ∼40 Ma. During ongoing top-to-SW shearing and as late as ∼36 Ma, the rocks from the outcrop were at higher temperatures than the peak temperatures experienced by lower levels of the NSZ. This confirms the existence of the inverted metamorphic sequence and demonstrates that the NSZ was a major thrust at 36–40 Ma. The ∼100 Myr time laps between the two anatectic events encompasses the period from ∼115 to ∼70 Ma characterized by a gap in the geochronological record on the scale of the RMC (the Eastern Rhodope excluded). This ∼45 Myr gap likely reflects a period of tectonic quiescence between the mid-Mesozoic orogen and the Cenozoic one, attesting for polycyclic Alpine orogeny in the RMC. Unlike assumed in several geodynamic scenarios, the Alpine evolution of the RMC did not consist of a single orogenic cycle of Mesozoic age followed by Cenozoic crustal-scale extension triggered by mantle delamination. Polycyclic orogeny has resulted in a two-loop P-T-t path for the hangingwall unit of the NSZ. The Cenozoic P-T paths of this unit and the footwall unit merged while both units were being exhumed, a feature attributed to syn-thrusting extensional spreading of the main mass of the hangingwall unit above the NSZ.

High spatial resolution, quantitative chemical imaging is of importance to various scientific communities, however high spatial resolution and robust quantification are not trivial to attain at the same time. In order to achieve microscopic chemical imaging with enhanced quantification capabilities, the current study links the independent and complementary advantages of two micro-analytical techniques – Synchrotron Radiation-based micro X-ray Fluorescence (SR-microXRF) and Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICPMS). A cross-calibration approach is established between these two techniques and validated by one experimental demonstration. In the presented test case, the diffusion pattern of trace level Cs migrating into a heterogeneous geological medium is imaged quantitatively with high spatial resolution. The one-dimensional line scans and the two-dimensional chemical images reveal two distinct types of geochemical domains: calcium carbonate rich domains and clay rich domains. During the diffusion, Cs shows a much higher interfacial reactivity within the clay rich domain, and turns out to be nearly non-reactive in the calcium carbonate domains. Such information obtained on the micrometer scale improves our chemical knowledge concerning reactive solute transport mechanism in heterogeneous media. Related to the chosen demonstration study, the outcome of the quantitative, microscopic chemical imaging contributes to a refined safety assessment of potential host rock materials for deep-geological nuclear waste storage repositories.