A microdistillation technique has been developed to isolate methylmercury f
rom various environmental sample matrices. The new design eliminates methyl
mercury contamination from the distillation equipment. It does not require
the use of a stripping gas and is less tedious and time-consuming than prev
iously used techniques. Because of miniaturization the unit is particularly
useful when the sample size is limited. Certified reference materials were
analyzed applying speciated isotope dilution ICP-MS. No statistical differ
ences between certified and measured values were detected. Distillation tim
e and temperature as well as the type of collecting solution were optimized
. As little as 10 pg of methylmercury was successfully distilled from water
samples. The method was further used to isolate methylmercury from insect
larvae weighing less than 2 mg (dry weight).