A performance verification demonstration of technologies capable of detecting dioxin and dioxin-like compounds in soil and sediment samples was conducted in April 2004 under the US Environmental Protection Agency’s Superfund Innovative Technology Evaluation (SITE) Monitoring and Measurement Technology (MMT) Program. A demonstration plan was developed with input from the participating technology developers who were part of an advisory panel convened to provide technical guidance for this test. The development of the experimental design began with the framework traditionally used for testing field analytical monitoring technologies under the SITE MMT Program, but various unique aspects of the participating technologies and the expected applications for these technologies necessitated modification of several elements of the traditional design. These critical experimental design considerations are described in this manuscript, along with issues encountered and the remedies that were developed. A summary of the performance data for each technology tested is also presented.