Naturally occurring radioactive materials (NORMs) are abundant in the environment and create important causes of anthropological exposure to ionizing radiation. Industrial activities such as mining, oil and gas exploration, fertilizer production, and mineral processing can increase the concentration and redistribution of these radionuclides, thereby increasing potential environmental and health risks. Consequently, reliable analytical methods and techniques are essential for the detection, identification, quantification, and monitoring of NORMs in environmental and industrial samples. This review examines the major methods and techniques employed in NORM analysis, with emphasis on their principles, applications, advantages, and limitations. Gamma-ray spectrometry, particularly using Sodium Iodide [NaI(Tl)] and High-Purity Germanium (HPGe) detectors, remains the most widely utilized technique because of its non-destructive nature, high detection capability, and simultaneous multi-radionuclide analysis. Other important techniques reviewed include alpha spectrometry, liquid scintillation counting, neutron activation analysis, inductively coupled plasma mass spectrometry (ICP–MS), radon monitoring methods, X-ray fluorescence, and autoradiography. The review further compares these techniques based on sensitivity, accuracy, operational requirements, and suitability for different sample matrices. Findings indicate that no single analytical method is universally applicable for all NORM investigations; rather, the selection of a technique depends on the radionuclides of interest, sample characteristics, detection limits, and research objectives. The integration of complementary analytical techniques therefore provides more reliable and comprehensive radiological assessments. This review contributes to the understanding of current methodologies in NORM studies and highlights the importance of advanced analytical approaches in environmental radiation monitoring and radiological protection.