Determination of 16 rare earth elements in graphite ore by inductively coupled plasma mass spectrometry with microwave digestion
The determination of rare earth elements in graphite ore is of great significance in evaluating re-source value,protecting the environment,and scientific research.In experiments,the samples were trea-ted by high-temperature microwave digestion in HNO3-HF-HClO4-H2 SO4 system.The collision mode was used with helium(He)flow rate of 4-5 mL/min.45Sc,89Y,139La,140Ce,141Pr,146Nd,147Sm,153Eu,157Gd,159Tb,163Dy,165 Ho,166Er,169Tm,172Yb,and 175Lu were selected as the isotopes to be measured.Sc,Y,La,Ce and Pr were corrected using Rh,and Nd,Sm,Eu,Gd,Tb,Dy,Ho,Er,Tm,Yb and Lu were corrected using Re.The multi-atomic ion interference of 157Gd,153Eu,159Tb and 169Tm was corrected by the interference correction equation.The method for the determination of 16 rare earth elements in graphite ore by electrical coupled plasma mass spectrometry(ICP-MS)with microwave digestion was es-tablished.Under the optimized experimental conditions,the linear correlation coefficients of calibration curves of rare earth elements were between 0.999 7 and 1.000 0.The limits of detection were between 0.002 6 and 0.065 μg/g,and the limits of quantification were between 0.008 7 and 0.22 μg/g.The con-tents of 16 rare earth elements in graphite ore standard substances for composition analysis were deter-mined according to the experimental method for 15 times in parallel.The relative standard deviations(RSD,n=15)of determination results were all less than 3.5％.The mixed standard working solution of rare earth elements were added based on 0.5-2 fold of element content for the spiked recovery tests,and the recoveries were between 90％and 105％.16 rare earths in graphite ore sample were analyzed according to the experimental method,and the measurement results were basically consistent with those obtained by ashing-mixed acid dissolution-ICP-MS method.
microwave digestioninductively coupled plasma mass spectrometry(ICP-MS)graphite orerare earth element
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