Abstract: As strategic emerging mineral resources supported by the state, niobium and tantalum are the functional and structural materials needed for the development of emerging industries. Therefore, conducting research on the determination of niobium and tantalum in related materials is of great significance. Unfortunately, niobium and tantalum have similar physical and chemical properties, making it difficult to separate them. However, they are easy to hydrate. Geological samples are difficult to be decomposed, thus the determination of niobium and tantalum has always been a difficult issue. Sample pre-treatment technology and modern analytical techniques are reviewed in this paper. Sample pre-treatment is the key step for niobium and tantalum analysis, therefore a suitable sample digestion and preconcentration method combined with analytical methods and sample characteristics is the premise of accurate determination of niobium and tantalum. Instrument analysis is the mainstream of modern analytical technology. Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) and Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) are the most widely used methods for the determination of niobium and tantalum, but it is necessary to solve problems such as coexisting component interference, matrix effects and salt influence. Laser Ablation (LA), X-ray Fluorescence Spectrometry (XRF), and Neutron Activation Analysis (NAA) are the development direction of tantalum and niobium analysis, due to the fact that they avoid the complicated sample pre-treatment and addition of impurities by solid sample introduction.