Dissolved organic matter (DOM) can be originated from autochthonous or allochthonous sources, where allochthonous DOM can be from pedogenic sources (humic substances-HSs) or anthropogenicsources (wastewater). The analysis of fluorescence emission, excitation, synchronous or excitation-emission matrix (EEM) have been used to identify the main source or probable contribution of dissolved compounds, such as humic acids (HA), fulvic acids (FA) and dissolved organic carbon (DOC) from sewage, but does not quantify. Fluorescence emission is a powerful technique to detect and qualify organic dissolved compounds but fails in quantitative aspects. In this work, we propose an in situ method for direct determination of DOC using synchronous fluorescence spectra with independent component analysis (ICA). Well known standard solutions were used for method development and validation. In this work, we show that it is possible to predict the number of independent contributions using an unsupervised method based on iterative Principal Component Analysis and Independent Component Analysis (PCA-ICA) approach over combined matrix results. Within these results it's also possible to see that with a very small amount of independent compo-