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Most agricultural soils in semi-arid regions present a deficiency of organic matter (SOM). In order to improve this soil, wastewater is used due to its high organic carbon content. The objective of the present work was to characterize the dissolved organic matter in five residual water samples and ten soil samples from the agricultural area of the municipality of San Luis Potosi by 3D fluorescence spectroscopy. The changes in some physical and chemical properties of the soil were also analyzed. The soil samples were collected at different depths to observe the anthropogenic organic matter presence, their retention in the soil profile, their fluorescence intensity changes and their migration into the aquifer. Temperature, electrical conductivity, dissolved oxygen, oxidation-reduction potential and total dissolved solids were determined in situ. The major anions and cations: Na+, K+, Mg2+, Ca2+, PO43-, SO42-, NO3-, NO2-, were analysed in laboratory. The results show the great contribution of organic matter (> 2020 mg/L) in the residual water used for irrigation, as well as, the low content of SOM. The physical and chemical results indicate that the high electrical conductivity of the water, represents a risk of salinization for soils, but not of short term sodicity. The 3D fluorescence spectra of the soil profile, shows the presence of humic and fulvic acids, aromatic proteins and products of microbial degradation. The latter observed in that depth where there is a greater percentage of clay.