This thesis focuses on developing a new method to measure trace tellurium (Te) in different environmental samples such as lake waters, mine tailings and sediments. The developed technique is based on Hydride Generation Atomic Fluorescence Spectroscopy (HG-AFS), a technique that can measure low concentration of Te and also allows for Te speciation at low cost and high efficiency in various environmental samples. To validate the method that could be used to determine Te speciation in various types of environmental samples, a series of tests has been designed for finding the best conditions to measure Te(IV) using HG-AFS and obtain accurate and reliable results. Those tests include the stability of the signal, the acidity of the solution, the volatility of Te after digestion of solids, the reduction from Te(VI) to Te(IV), the detection limit of the technique, and the validity of two digestion methods under the optimum (HG-AFS) instrumental settings. An interference study including the most common elements in the Earth’s crust such as (Ni, Fe, Pb, Cr, Cu, Co, Zn, Mn and Mo) was also performed. The results of this study showed that Cu(II) can severely interfere with Te quantification decreasing the Te signal to almost zero. Therefore, different masking agents such as 8-hydroxyquinoline, 1,10-phenanthroline, urea and thiourea were tested to reduce and eliminate this interference.