Determination of niobium,tantalum,zirconium and hafnium in geochemical survey sample by inductively coupled plasma mass spectrometry with ammonium hydrogen fluoride digestion
ZHANG Yuan, ZHAO Wenzhi*, LIANG Zhongkai, YAN Fuxing, LI Shaowen, XIE Xu
Center for Harbin Natural Resources Comprehensive Survey,China Geological Survey,Harbin 150086,China
Abstract：Nb,Ta,Zr and Hf are the key rare elements that support the development of national strategy.It is of great significance to accurately determine these four elements in geochemical survey samples.The sample was digested with ammonium hydrogen fluoride followed by leaching with HNO3.93Nb,181Ta,90Zr and 178Hf were selected as isotopes to be measured.A method for the determination of Nb,Ta,Zr and Hf in geochemical survey samples by inductively coupled plasma mass spectrometry(ICP-MS) was established.The pretreatment conditions of sample were optimized:the mass ratio of sample and ammonium hydrogen fluoride was 1∶5,the digestion temperature was 220 ℃,and the digestion time was 3 h.The linear correlation coefficients of calibration curves were all higher than 0.998.The limit of detection was 0.014-0.23 μg/g, and the limit of quantification was 0.047-0.767 μg/g.The certified reference materials of geochemical survey sample were determined parallelly for 11 times according to the experimental method,sodium peroxide fusion-ICP-MS in GB/T 14506.29-2010,and hydrofluoric acid-nitric acid closed dissolution-ICP-MS in GB/T 14506.30-2010.The results showed that the determination results of three methods were basically consistent with the certified values,and the logarithm deviations (ΔlgC) were met the requirements.The proposed method was applied for the determination of Nb,Ta,Zr and Hf in geochemical survey samples from Heihe area in Songnen plain.The relative standard deviations (RSD, n=11) of determination results were all below 10%.
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