Abstract：A method of microwave digestion-inductively coupled plasma atomic emission spectrometry(ICP-AES) for 0.003%-0.100% boron and bismuth in vanadium pentoxide was established in coupled with high pressure enclosed microwave heating method and mixed acid of HNO3 and HCl (VHNO3∶VHCl=1∶2) dissolution. It was found that vanadium did not produce spectral overlapping interference with boron and bismuth, but the matrix effect of high concentration vanadium had reduced the detection signal intensity of boron and bismuth; the continuous background overlapping of vanadium matrix had induced the enhancement of background baseline signal intensity; some of the sensitive spectral lines of boron and bismuth was disturbed with the spectral line of coexisting impurities such as chromium and iron. The matrix effect was removed by means of vanadium matrix matching together with synchronous background correction. Spectral lines with high sensitivity and free of coexisting components effect were selected as analytical lines, and appropriate detection integration and background correction zone were selected, so that the detection performance of trace boron and bismuth was improved. The limit of quantification for boron and bismuth were 0.001 1% and 0.002 3% (both were mass fraction). The background equivalent concentration were 0.000 4% and 0.001 8% (both were mass fraction). The relative standard deviations for determination of vanadium pentoxide actual sample were less than 8.0% (RSD,n=8). The standard addition recoveries were 93%-110%. The determination results of actual samples by proposed method were in good agreement with those obtained by inductively coupled plasma mass spectrometry(ICP-AMS).
