In this article we report about the synthesis of superparamagnetic bare Fe 3 O 4 nanostructures and core/shell (Fe 3 O 4 /alginate) nanocomposites by simple low-temperature based method at pH values 5, 9, and 14. The structural morphology and magnetic behavior of Fe 3 O 4 nanostructures and core/shell (Fe 3 O 4 /alginate) nanocomposites (Fe 3 O 4 /alg NCs) have been investigated by X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy (RS), ultraviolet–visible (UV–vis) spectroscopy, transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX) and vibrating sample magnetometer (VSM). The particle size was calculated by TEM measurements and it turns out to be ∼10nm and ∼14nm for bare Fe 3 O 4 nanoparticle and Fe 3 O 4 /alg NCs with core/shell structure, respectively. The magnetic properties of the synthesized products were found to be function of pH at which the synthesis has been done. The synthesized Fe 3 O 4 nanoparticle and Fe 3 O 4 /alg NCs were found to be superparmagnetic in nature at room temperature. We observed that the value of saturation magnetization in case of Fe 3 O 4 /alg NCs decreases by increasing the pH value.