Absorption of organic pollutants from industrial effluents is necessary to prevent the spread of environmental contaminants. Phenols and other aromatic compounds are common pollutants that are often found in the wastewater refineries and petrochemical industries. Tetracyclines are also the second most widely used anti-microbial antibiotic in the world. Adsorption is more widely used, due to its simplicity, flexibility and speed of adsorption. High porosity, high surface area, presence of active surfactant groups, and the ability to separate adsorbent from the properties of a suitable absorbent, chitosan have the characteristics of a suitable adsorbent. The purpose of this research is to produce and characterize chitosan/PVA/Fe 3 O 4 nanoparticles by electrospinning method to separate phenol and tetracycline from water. Due to the fundamental problem of chitosan electrospinning, poly (vinyl alcohol) was used as a polymer in the production of nanofibers. For this purpose, firstly, the effective electrical process factors on the production of chitosan/poly (vinyl alcohol) nanofibers were investigated. Then, for adsorbent, the effective factors on adsorption were investigated. Statgraphics software used to optimize electrospinning and adsorption factors. At first, the electrospinning factors such as flow intensity (1.5-2 mL h -1 ), voltage (15-30 kV), distance (10-20 cm), as well as volume ratio of chitosan polymers to poly (Vinyl alcohol) with ratios (25:75-50:50-75:25) were optimized for both phenol and tetracycline pollutants separately. The SEM analysis showed that the adsorbent produced in this study had a mean diameter of 95-105 nm. The presence of pixels related to the functional groups of the compounds in the produced adsorbent was demonstrated by FTIR spectroscopy analysis of composite nanofibers. XRD analysis of the samples shows that the combination of two polymers of chitosan and poly (vinyl alcohol) causes the peaks to be broadened and the adsorbent shape changes from crystalline to amorphous. The result of the TGA test shows that absorbent degradation began at a temperature of 200°C and completely degraded at 500°C. In the second part of the study, for phenol adsorption, the pH value was in the range of 6 to 12, the initial concentration of phenol was 10 to 50 mg/L and the adsorbent content was 0.75 to 1 g/l. The equilibrium time for adsorbing phenol was 3 hours and the adsorbing capacity was 41 mg/g. On the other hand, to determine adsorption of tetracycline, the pH value was between 6 and 12, the initial concentration of tetracycline was 50 to 150 mg/L, and the amount of adsorbent for tetracycline was 5 to 25 g/L. The results of adsorption showed that the equilibrium time for the tetracycline adsorption process was 48 hours and the adsorption capacity of tetracycline was 102 mg/g. The Results showed that phenol adsorption follows by Langmuir and Freundlich isotherms and tetracycline adsorption was followed by only Langmuir isotherm. A second-order polynomial model was obtained using the Statgraphics software for adsorption of both phenol and tetracycline pollutants. Also, the process of adsorption of phenol follows from pseudo-second order kinetics equation and the kinetic of tetracycline were fitted to pseudo-first-order equation. Results of phenol and tetracycline adsorption factors by chitosan/poly (vinyl alcohol) nanofibers showed that phenol and tetracycline adsorption decreases with decreasing pH. The highest removal percent for phenol were achieved at pH=6, initial concentration of the contaminant equal to 10 mg/L and amount of adsorbent is 1 g/L, respectively and for tetracycline pH=6, initial concentration of the contaminant is equal to 100 mg/L and the adsorbent amount is respectively 25 g/L gained the highest absorption capacity. The presence of Fe 3 O 4 nanoparticles used in chitosan/poly(vinyl alcohol) nanofibers was investigated by FESEM and EDAX tests. Also, the VSM test was used to calculate the magnetic strength of nanofibres, which obtained 44 and 5.8 emu/g for pure iron oxide nanoparticles and magnetic nanofibers respectively