In forensics, 18 O mapping in materials can be instrumental for tracing geographical origins of animals and humans. [17] Among the different methods used to study the oxidation mechanisms in solid materials, in situ environmental transmission electron microscopy (TEM) and in situ scanning tunneling microscopy are powerful for studying the atomic-scale structural changes associated with the early stages of oxidation. [1,3,5,18,19] However, these in situ techniques lack the sensitivity to distinguish individual oxygen isotopes. At the same time, nanosecondary ion mass spectrometry (SIMS) and other massspectrometry-based techniques, which are highly sensitive for oxygen isotopes, lack 3D sub-nanometer-scale spatial resolutions. [14,17,20,21] Recently, ex situ atom probe tomography (APT) studies validated the ability of APT to achieve sub-nanometerscale spatially resolved mapping of 18 O isotope distribution in materials. [10,[22][23][24][25] However, expanding this ability of APT in mapping 18 O quantitatively at sub-nanometer scale spatial resolution toward in situ oxidation studies is yet to be demonstrated.Here, we demonstrate for the first time in situ APT analysis of oxygen diffusion in a model Fe-18 wt% Cr-14 wt% Ni model alloy (from here on called as Fe18Cr14Ni) using an 18 O isotopic Understanding the early stages of interactions between oxygen and material surfaces-especially at very high spatial resolutions-is highly beneficial for fields ranging from materials degradation, corrosion, geological sciences, forensics, and catalysis. The ability of in situ atom probe tomography (APT) is demonstrated to track the diffusion of oxygen and metal ions at nanoscale spatial resolution during the early stages of oxidation of a model Fe-Cr-Ni alloy. Using 18 O isotope tracers in these in situ APT experiments and complementary ex situ multimodal microscopy, spectroscopy, and computational simulations allows to precisely analyze the kinetics of oxidation and determine that outward cation diffusion to oxide/air interface is the primary mechanism for intragranular oxide growth in this alloy at 300 °C. This unique in situ isotopic tracer APT approach and the insights gained can be highly beneficial for studying early stages of gas-surface reactions in a broad array of materials.