The control of the normal and safe performance during the operation of nuclear fuel reprocessing is one of the most important security key in the nuclear fuel reprocessing. Traditionally, this control has been performed by sampling the streams for the ex situ analysis. In addition to the consuming time of this protocol, it should be considered the difficulties and the risk of operation with such radioactive and hazardous material. A solution of this problem can be achieved by monitoring on line the content of relevant species in the streams during the separation processes. The feasibility of the Raman spectroscopy technique has been already proven for this propose. However, more studies have to be performed for each molecule and under the conditions of the investigated process (such as pH, concentration, temperature and radiation), in order obtain the right interpretation and assignation of the spectroscopic signals and the determination of the detection and quantification limits. In that sense, in this work we explore the Raman capability for measure the acetohydroxamic acid concentrations (AHA), one of the molecules involved in some proposed nuclear reprocessing processes.