The radiological dispersal device (RDD) is a weapon of great concern to those agencies responsible for protecting the public from the modern age of terrorism. In order to effectively respond to an RDD event, these agencies need to possess the capability to rapidly identify the radiological agents involved in the incident and assess the uptake of each individual victim. Since medical treatment for internal radiation poisoning is radionuclide-specific, it is critical to identify and quantify the radiological uptake of each individual victim. This dissertation describes the development of automated analytical components that could be used to determine and quantify multiple radionuclides in human urine bioassays. This is accomplished through the use of extraction chromatography that is plumbed in-line with one of a variety of detection instruments. Flow scintillation analysis is used for ⁹⁰Sr and ²¹⁰Po determination, flow gamma analysis is used assess ⁶⁰Co and ¹³⁷Cs, and inductively coupled plasma mass spectrometry is used to determine actinides. Detection limits for these analytes were determined for the appropriate technique and related to their implications for health physics.