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The results of the synthesis of PAN(polyacrylonitrile)-magnetite composite fibers using the electrospinning method are presented. The electrospinning installation included a rotating drum collector for collecting fibers. Magnetite nanoparticles were synthesized using chemical condensation from an iron chloride solution. It was shown that homogeneous Fe3O4 magnetite nanoparticles with particle sizes of 6–16 nm could be synthesized using this method. Magnetite nanoparticles were investigated using X-ray diffraction analyses and transmission electron microscopy. Based on magnetite nanoparticles, composite PAN/magnetite fibers were obtained through electrospinning. The obtained composite fibers were investigated using scanning electron microscopy, X-ray diffraction analyses, and elemental analyses. It was shown that the magnetite nanoparticles were uniformly distributed on the surface of the fibers. A comparison of PAN fibers without any added magnetite to PAN/magnetite fibers showed that the addition of magnetite led to a decrease in the value of the fiber diameter at the same polymer concentration and under the same electrospinning process conditions.