Investigating the magnetic nanoparticle size and the effective magnetic interactions that form the magnetic domain can lead us to nanoparticles with targeted applications, such as targeted drug delivery and higher resolution MRI imaging. In this study magnetic susceptibility and coercive field properties, and the structure size range of single-domain magnetic capsules with high magnetization were obtained by structural analysis of volumetric DLS properties. In this regard, the role of exchange, anisotropy, and magnetostatic interaction was investigated in the structure of a magnetic capsule containing Fe3O4 nanoparticles (MCap-NPs). The stable capsules were synthesized in an emulsion solution with magnetic surfactants M(AOT)2 (M = Co, Ni). Vibrating Sample Magnetometer (VSM) and capsule relative volume (CRV) of Dynamic Light Scattering (DLS) were used to determine the magnetic properties of the single-domain (SD) structure. The produced emulsion samples were found to have superparamagnetic properties property with saturation magnetization in the range of 2–6 × 10−3emu/g for NiCap-NPs, and 5-13 × 10−3emu/g for CoCap-NPs. The results show that nanoparticles have the most significant effect on magnetization. The coercive field, the anisotropy energy values, and the SD of M(AOT)2 were determined using magnetic susceptibility distribution. The outcome results show that the surface of the magnetic capsule plays an essential role in forming a single-domain structure. It was also found that the saturation magnetization of the samples in the emulsion solution is proportional to the nanoparticle density and not to the mass of nanoparticles. All produced samples have distinct peaks in CRV versus capsule size, and each peak follows a log-normal distribution. For both samples, except for the samples with molar ratios ω of 23 (Co3 and Ni4 samples), the positions of the second and third relative volume peaks were constant at 269 ± 3 nm and 424±6 nm, respectively. The behavior of the CRV function normalized to the peak size showed a proportionality between the coercive field and the CRV.