Characterization of industrially important nanophosphors such as ZnS:Mn²⁺, SrAl₂O₄:Eu²⁺, Dy³⁺ and Gd₂O₂S:Pr³⁺ was undertaken with a view to optimize their synthesis methods. To investigate the crystallinity, particle size, efficiency and homogeneity in doping of Mn in ZnS; Eu and Dy in SrAl₂O₄ and Pr in Gd₂O₂S, analytical techniques such as XRD, TEM, PL, TOF-SIMS and laser-SNMS were employed. The XRD and TEM studies revealed the average particle sizes to be between 2 and 15 nm. Photoluminescence (PL) studies carried out for the nanophosphors confirm the effectiveness of doping in the host lattices. TOF-SIMS spectral analysis showed the formation of the crystal (host lattice) with the presence of different dopants. The chemical imaging mode of TOF-SIMS suggested homogeneous doping in ZnS:Mn²⁺ nanophosphor while in the case of SrAl₂O₄:Eu²⁺, Dy³⁺ the degree of homogeneity of doping was found to be considerably less. The broad band of PL in SrAl₂O₄:Eu²⁺, Dy³⁺ nanophosphor may be attributed to such an inhomogeneity to some extent. In the case of Gd₂O₂S:Pr³⁺, the PL was found to be brightest at the higher energy region. But because of very low level doping of Pr³⁺ in the Gd₂O₂S lattice, additional laser-SNMS studies were carried out for analysing the doping distribution using chemical imaging data, which indicated a high degree of homogeneity.