Pure nano-Al 13 and aggregates at various concentrations were prepared to examine the particle size effect of coagulation with inorganic polymer flocculant. The property and stability of various species formed were characterized using Infrared, 27 Al-NMR, photo correlation spectroscopy (PCS), and Ferron assay. Results showed that concentration and temperature exhibited different roles on the stability of Al 13 . The quantity of Al b species analyzed by ferron assay in the initial aging period corresponded well with that of Al 13 , which has been confirmed in a dimension range of 1-2 nm by PCS. Al 13 solutions at high concentrations (0.5-2.11 mol/L) were observed to undergo further aggregation with aging. The aggregates with a wide particle size distribution would contribute to the disappeared/decreased Al 13 basis on the 27 Al-NMR spectrum, whereas a part of Al 13 would still remain as Al b . At low concentrations, Al 13 solution was quite stable at normal temperature, but lost its stability quickly when heating to 90°C.