Abstract: With the inductively coupled plasma atomic emission spectrometry, the HF-HNO3-HClO4-H3PO4 dissolving samples were employed to determine B in carbonate formations. The method lies in adding an appropriate amount of H3PO4 in the sample dissolution system to avoid the loss of the volatile elements B and testing the optimum amount of H3PO4. The accuracy and precision of the method are demonstrated by analyzing the National Standard Reference Materials, and it is proved that the precision (RSD) is less than 6.44%, and the RE (ΔlgC) is less than 0.087. The method can also determine such elements as Be, Ba, Cr, Cu, Co, Ni, Pb, Mo, V, Mn, Li, Zn and Ga at the same time. The method can determine B and various other elements in soil, rock and stream sediment samples. The method was used to determine B, Co, Ni, Cu, Zn, Pb and Ba in carbonate formation of Karaqi area in southeast Tianshan Mountains, and its geological significance was discussed in this paper.