[en] The present work summarizes preliminary experiments dealing with the analysis of the main organophosphorus extracting agents TBP, DEHPA and TOPO widely used in hydrometallurgy and particulary in uranium one treatment. In order to ovoid the thermodegraduation processes of such compounds, an adequate combination of vaporization temperature and the carrier gas flow, i,e, the time contact of the compounds in column must be made. In this context, the present work was justly achieved in order to elaborate a only the separation but also the accurate determination of the compounds dealt with. One can remark that maintaining constant the temperature and slightly varying the flow velocity of the carrier gas, the peaks of TBP and butanol were better separated. Nevertheless, a limitation may appear when nitrogen flow is raised up to 30m1/mn. This is essentially due to the lose polarity and their analogous chemical behaviours. Thus one can conclude that such compounds can be easily determined in the ranges of 0-60% for D2EHPA, for TOPO and 24% for TBP. The determination accuracy for all compounds varies between 0.005 and 0.12%. Thus, one can conclude that the organophosphorus extracting agents such as TBP, D2EHPA and TOPO can be easily determined without previous purification. The isothermal conditions are strongly recommemded in this case because of the quickness of the technique. The secondary products resulting from the synthesis process do not affect greatly the determinations of such compounds and their accuracies