Beryllium metal and beryllium oxide are important industrial materials used in a variety of applications in the electronics, nuclear energy, and aerospace industries. These materials are highly toxic, they must be disposed of with care, and exposed workers need to be protected. Recently, a new analytical method was developed that uses dilute ammonium bifluoride for extraction of beryllium and a high quantum yield optical fluorescence reagent to determine trace amounts of beryllium in airborne and surface samples. The sample preparation and analysis procedure was published by both ASTM International and the National Institute for Occupational Safety and Health (NIOSH). The main advantages of this method are its sensitivity, simplicity, use of lower toxicity materials, and low capital costs. Use of the technique for analyzing soils has been initiated to help meet a need at several of the U.S. Department of Energy legacy sites. So far this work has mainly concentrated on developing a dissolution protocol for effectively extracting beryllium from a variety of soils and sediments so that these can be analyzed by optical fluorescence. Certified reference materials (CRM) of crushed rock and soils were analyzed for beryllium content using fluorescence, and results agree quantitatively with reference values.