Dioxins, such as polychlorinated dibenzo-p-dioxins
and polychlorinated dibenzofurans (PCDD/Fs), are among the most toxic
unintentionally produced persistent organic pollutants, and their
emission is of great concern. Herein, we discovered abundant dioxin
formation in soil and various organic carbon-containing matrices after
digestion with aqua regia. Σ17PCDD/Fs concentrations
were in the range of 66.6–142,834 pg/g dw (5.6–17,021
pg WHO2005-TEQ/g dw) in 19 soil samples after digestion
with aqua regia for 6 h. Σ17PCDD/Fs concentration
was significantly and positively correlated with soil organic carbon
content (R
2 = 0.89; p < 0.01). Compared with cellulose and lignin, humic acid served
as an important organic matter component that was converted to PCDD/Fs
during soil digestion. Strong oxidation and production of reactive
chlorine by aqua regia may be the key factors in the formation of
PCDD/Fs. The yearly emission of PCDD/Fs due to digestion with strong
acids by the inspection and testing industry was estimated to be 83.8
g TEQ in China in 2021 based on the highest level, which was ∼0.9%
of the total dioxin inventory in China. Great attention should be
paid to unexpected dioxin formation during digestion processes considering
the potential risk of release from laboratories and enterprises.