AbstractSodium aluminosilicate scaling in evaporators during alkali recovery is often associated with the concentration of aluminum and silicon in black liquor. The scaling problems are widespread during the utilization of non-wood raw materials. This study established a fast, reliable, and precise method to determine the aluminum concentration in bamboo black liquor by inductively coupled plasma-atomic emission spectrometry (ICP-AES). Prior to ICP-AES measurements, black liquor samples were digested in an automatic electric heating assisted digestion system. After optimizing the digestion, ICP-AES testing showed that the recovery of the element was 96.2% to 99.9% and the relative standard deviation (RSD) was 0.07% to 0.52%. Additionally, comparative data for the concentration of analytes was obtained by flame atomic absorption spectrometry (FAAS). This technique will be useful for assessing the scaling properties of black liquor in the alkali recovery phase.