Historically, measurement of technetium-99 in environmental matrices has been carried out by radiometric methods such as liquid scintillation counting and gas flow proportional counting. This work evaluates the use of ¹⁸⁵Re-enriched rhenium as a yield monitor, and presents a simple microwave digestion of wet sample, coupled with TEVA resin extraction and ICP-MS measurement for the rapid determination of Tc-99 in soil, silt and sediment samples.