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Contents Summary 432 I. Introduction 433 II. Preparation of plant samples for X‐ray micro‐analysis 433 III. X‐ray elemental mapping techniques 438 IV. X‐ray data analysis 442 V. Case studies 443 VI. Conclusions 446 Acknowledgements 449 Author contributions 449 References 449

Hyperaccumulators are attractive models for studying metal(loid) homeostasis, and probing the spatial distribution and coordination chemistry of metal(loid)s in their tissues is important for advancing our understanding of their ecophysiology. X‐ray elemental mapping techniques are unique in providing in situ information, and with appropriate sample preparation offer results true to biological conditions of the living plant. The common platform of these techniques is a reliance on characteristic X‐rays of elements present in a sample, excited either by electrons (scanning/transmission electron …