The potential risk of various silver-containing nanoparticles (AgCNPs) in soils is related to the concentration, size, and speciation, but their determination remains a great challenge. Herein, we developed an effective method for determining the particle number, size, and species of dominant AgCNPs in soils, including nanoparticles of silver (Ag NPs), silver chloride (AgCl NPs), and silver sulfide (Ag 2 S NPs). By ultrasonication wand-assisted tetrasodium pyrophosphate extraction, these AgCNPs were extracted efficiently from soils. Then, multistep selective dissolution of Ag NPs, AgCl NPs, and whole Ag NPs/AgCl NPs/Ag 2 S NPs was achieved by 1% (v/v) H 2 O 2 , 5% (v/v) NH 3 •H 2 O, and 10 mM thiourea in 2% (v/v) acetic acid, respectively. Finally, the particle number concentration and size distribution of AgCNPs in the extracts and the remaining AgCNP particle number concentration after each dissolution were determined by single-particle inductively coupled plasma mass spectroscopy for speciation of the dominant AgCNPs. AgCNPs were detected in all five soil samples with the concentrations of 0.23−8.00 × 10 7 particles/g and sizes of 16−110 nm. Ag 2 S NPs were the main form of AgCNPs in the examined soils with the percentage range of 53.98−69.19%, followed by AgCl NPs (11.42−23.31%) and Ag NPs (7.78−16.19%). Our method offers a new approach for evaluating the occurrence and potential risk of AgCNPs in environmental soils.