Existing methods for total mercury and methylmercury determination in sedim
ent and porewaters were improved by applying open microwave heating for ext
raction of Hg species from the sample and decomposition of MeHg prior to de
tection as Hg(ll) by CV AFS. It was shown that nitric acid can quantitative
ly leach Hg from sediment, already at a low microwave power (30 W, 5 min).
Methylmercury can be quantitatively leached from sediment by dilute sulphur
ic acid (1 mol/L) at a power of 60 W during 5 minutes, without being decomp
osed. So obtained extract can be further distilled with a reduced possibili
ty for artefactual MeHg formation, as it contains much lower levels of inor
ganic Hg, compared to the original sediment. Microwave-assisted BrCl oxidat
ion was shown to be more effective for decomposition of MeHg and stable org
anomercury complexes in water solutions (sediment distillate and porewater)
, as compared with BrCl oxidation at room-temperature. Therefore, the appli
cation of low-power microwave digestion can significantly improve determina
tion of Hg species in sediment and porewater, both in terms of time and eff
iciency.