Abstract:Lithium is one of the well- known strategy metal resources in China. Among various minerals in lithium deposits, spodumene is the major mineral showing great commercial value. For effective estimation of lithium levels and deep investigation of the mining process of lithium deposits, accurate lithium determination is of pivotal significance. In this present work, with spodumene mineral in Kaluan, Dahongliutan and Jingerquan lithium deposits of Xinjiang province as the research subject, we first study the analytical accuracies of ICP- MS and ICP- AES for lithium in detail.Herein, 22 representative spodumene samples from the three lithium mining zones are decomposed using high- pressure closed acidic digestion method and taken for lithium analysis by ICP- MS and ICP- AES.The operating parameters,such as nebulizer gas flow rate, auxiliary gas flow rate and plasma gas flow rate, are well studied.With lithium quantification in the same digestion solution analyzed by both methods, results reveal that there exists systematical error of ICP- MS technique, showing an error coefficient of around 28 to the data that from ICP- AES analytical method.Furthermore, the possible reasons causing the systematic bias of ICP- MS technique are fully discussed,and it can be inferred that ICP- MS solution analysis, which has analytical loss of approximately 648% for lithium in spodumene samples, isn’t recommended in the study of lithium minerals, whilst ICP- AES is an attractive technique with merits of higher accuracy, internal standard free and easier operations.