Activated carbon (AC) is an effective sorbent for sequestering dioxin-like compounds, thereby reducing their bioavailability. Consequently, AC amendment is a promising tool for remediating dioxin-polluted soils, but tracking remediation results requires quantification of the dioxins sequestered within ACs. Standard methods for quantifying dioxins in soils are often unable to extract dioxins from AC, so the present study addresses this gap by optimizing an accelerated solvent extraction (ASE) method. The incipient wetness method, based on AC pore volume, was found effective for preparing reproducible, homogeneous, and strong dioxin-AC complexes to test extraction processes, and was validated using