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Pollution caused by heavy metal ions has become a global issue owing to their severe threat to the ecological environment and human health. However, it remains a considerable challenge to detect heavy metal ions in an efficient, selective, and high signal‐to‐noise ratio way. Herein, a portable and sensitive method is presented to probe Hg2+ by using an ultralong afterglow dispersion. The in situ encapsulation of phosphorescent carbon dots (CDs) within rigid hydrogen‐bonded organic frameworks (HOFs) leads to ultralong room temperature phosphorescence (RTP) in water with a maximum lifetime of up to 974.86 ms. Moreover, the resultant CDs@HOFs material exhibits robust and long‐term RTP emission with enhanced performance under strongly acidic or alkaline conditions, which contributes to the practical detection of Hg2+ in water. As such, an efficient and sensitive afterglow probe is facilely fabricated by integrating CDs@HOFs with a Hg2+ probe Rhodamine B derivative (RhBTh), demonstrating selective sensing of Hg2+ with greatly improved signal‐to‐noise ratios based on the triplet‐singlet Förster resonance energy transfer system (TS‐FRET). This work not only provides a reliable and versatile method for realizing robust RTP emission in water, but also expands the applications of afterglow materials in the field of optical sensing of toxic analytes. [ABSTRACT FROM AUTHOR]