In this study, the suspension-assisted total-reflection X-ray fluorescence analysis of ores was improved using the wet grinding procedure to produce ultra-fine suspended powder mixed with internal standard solution in aqueous media. The advantages of the proposed technique were demonstrated by the example of the determination of S, Fe, Ni, and Cu in sulfide copper‑nickel ores containing various ratios of sulfide and silicate minerals. We showed that the powerful mixing of 100 mg of ore powder and 4 mL of ultra-pure water as a dispersing medium with 20 g of grinding balls of 1 mm in diameter leads to the preparation of homogeneous suspension with monomodal particle size distribution having 90% of the particle size <6 μm. The suspension after wet grinding was diluted up to 50 mL with ultra-pure water to obtain a final concentration of the suspended powder of 2 mg/mL. Relative precision of the described sample preparation technique calculated from duplicate pairs of suspensions was 16% for S, 9% for Fe, 15% for Ni and 10% for Cu. Three spectral data processing techniques were further compared with respect to the quantification accuracy of target elements: internal standard, univariate and multivariate regressions. It was shown that the two latter methods can be used to improve the trueness of the internal standard method, especially for Cu and Fe.