氟化氢铵消解-电感耦合等离子体质谱法测定地球化学调查样品中铌钽锆铪  

Determination of niobium,tantalum,zirconium and hafnium in geochemical survey sample by inductively coupled plasma mass spectrometry with ammonium hydrogen fluoride digestion

作　　者：张元 赵文志 梁中恺 晏福兴 李少文 谢旭 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)

机构地区：[1]中国地质调查局哈尔滨自然资源综合调查中心,黑龙江哈尔滨150086

出　　处：《冶金分析》2023年第7期76-82,共7页Metallurgical Analysis

基　　金：松嫩平原黑河地区黑土地地表基质调查(ZD20220105);自然资源综合调查指挥中心科技创新基金(KC20220022)。

摘　　要：Nb、Ta、Zr、Hf是支撑国家战略发展的关键稀有元素,准确测定地球化学调查样品中这4种元素具有重要意义。采用氟化氢铵消解样品后再用HNO_(3)提取的方法处理样品,以^(93)Nb、^(181)Ta、^(90)Zr、^(178)Hf为待测同位素,建立了电感耦合等离子体质谱法(ICP-MS)测定地球化学调查样品中Nb、Ta、Zr、Hf的方法。对样品前处理条件进行了优化,确定样品与氟化氢铵的质量比为1∶5,消解温度为220℃,消解时间为3 h。各元素校准曲线的线性相关系数均大于0.998,方法检出限在0.014~0.23μg/g之间,定量限在0.047~0.767μg/g之间。按照实验方法、标准方法GB/T 14506.29—2010中的过氧化钠熔融-ICP-MS、GB/T 14506.30—2010中的氢氟酸-硝酸封闭溶解-ICP-MS对地球化学调查样品标准物质平行测定11次,结果表明,3种方法的测定结果均与认定值基本一致,且对数偏差(ΔlgC)均满足要求。将实验方法应用于松嫩平原黑河地区地球化学调查样品中Nb、Ta、Zr、Hf的测定,结果的相对标准偏差(RSD,n=11)均小于10%。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 HNO_(3).^(93)Nb,^(181)Ta,^(90)Zr and ^(178)Hf 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 0.014-0.23μg/g,and the limit of quantification was 0.047-0.767μg/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%.

关 键 词：氟化氢铵消解 铌 钽 锆 铪 电感耦合等离子体质谱法(ICP-MS) 地球化学调查样品 

分 类 号：O657.63[理学—分析化学]