Calcination,potentionmetric titration and compleximetry titration methods are used to determine the contents of CaCO3 in three cigarette papers,the results indicate that the measuring results by calcination are evidently influenced by the calcining heat and calcining time,which has adverse effect for the accuracy.Fiber in the papers are oxidized totally when the cigarette papers are calcined in the condition of 900 ℃ for 2 h .The measuring results by potentionmetric titration and compleximetry titration are rather stable,while the metallic oxides and carbonates in the cigarette papers bring errors for the measuring results by potentionmetric titration method.The impurity ions in the cigarette papers are sheltered by covering reagent in compleximetry titration,so the accuracy of the measuring results is high.The XPS analyzing results show that the CaO is the main component in the ashes of three cigarette papers,and the other chemical compounds such as C,Na2CO3,Na2SiO3,Na3PO4,CaSiO3,Ca3(PO4)2 are also checke.The SEM analyzing results show that the CaCO3 distribute in the fibres exhibits spindle-shaped microcrystallite and spheric cluster.This study presents an accurate method to determine the content of CaCO3 in paper.