纸上层析分离-ICP-AES测定稀有金属矿中的铌钽
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摘要
采用HF、HNO_3溶解样品,纸上层析分离富集铌、钽,焦硫酸钾分解铌钽氧化物,酒石酸浸取,ICP-AES测定稀有金属矿中铌钽。研究了溶样用酸、色层分离展开剂比例及展开温度、焦硫酸钾用量、酒石酸浓度等对测定结果的影响,结果表明,采用纸上层析法可使铌钽与其他干扰元素彻底分离,焦硫酸钾熔融后,用酒石酸浸取使铌、钽完全进入溶液,以电感耦合等离子体光谱仪(ICP-AES)进行测定。在20 g/L的酒石酸介质中,ICP-AES测定铌钽的线性范围为0~50μg/mL,检出限为铌0.14μg/mL,钽0.16μg/mL;相对误差小于8%,精密度(RSD)小于6%,可测定矿石中0.001%~40%的Nb_2O_5,Ta_2O_5。该方法可同时测定稀有金属矿中铌钽原矿、精矿及尾矿中铌钽的含量,适合基体复杂、含量差别大的批量样品的检测。
An analytical method for the determination of niobium and tantalum in rare metal ores by paper chromatography-inductively coupled plasma spectrometry was developed.The Nb and Ta of samples which were dissolved by hydrofluoric acid and nitric acid were separated and enriched by paper chromatography.The Nb and Ta in the chromatography paper could be determined by ICP directly after they were melted by potassium pyrophosphate and dissolved by tartaric acid.The article discussed the influences of dissolved acids,the ratio of chromatography developer,temperature,the amount of potassium pyrophosphate and the concentration of tartaric acid.The results showed that Nb and Ta could be completely separated from other interference elements by paper chromatography.In the tartaric acid medium of 20 g/L,the linear range of Nb and Ta by ICP-AES is 0~50 μg/mL.The limits of detection of Nb and Ta are 0.14 μg/mL and 0.16 μg/mL,respectively.The relative error is less than 8% and the precision(RSD) is less than 6%.The method has wide detection range and is suitable for the simultaneous determination of niobium and tantalum in raw ore with low content and high content of niobium and tantalum.It can meet the determination requirements of samples with complex matrix,large variation range of niobium and tantalum content and large sample.
An analytical method for the determination of niobium and tantalum in rare metal ores by paper chromatography-inductively coupled plasma spectrometry was developed.The Nb and Ta of samples which were dissolved by hydrofluoric acid and nitric acid were separated and enriched by paper chromatography.The Nb and Ta in the chromatography paper could be determined by ICP directly after they were melted by potassium pyrophosphate and dissolved by tartaric acid.The article discussed the influences of dissolved acids,the ratio of chromatography developer,temperature,the amount of potassium pyrophosphate and the concentration of tartaric acid.The results showed that Nb and Ta could be completely separated from other interference elements by paper chromatography.In the tartaric acid medium of 20 g/L,the linear range of Nb and Ta by ICP-AES is 0~50 μg/mL.The limits of detection of Nb and Ta are 0.14 μg/mL and 0.16 μg/mL,respectively.The relative error is less than 8% and the precision(RSD) is less than 6%.The method has wide detection range and is suitable for the simultaneous determination of niobium and tantalum in raw ore with low content and high content of niobium and tantalum.It can meet the determination requirements of samples with complex matrix,large variation range of niobium and tantalum content and large sample.
引文
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[3]He H L,Li B,Han L R,et al.Chin J Anal Lab,2002,21(5):8何红蓼,李冰,韩丽荣,等.分析试验室,2002,21(5):8
[4]Du M,Xu T.Phys Tesing Cherm Anal Part B,2014,50(3):317杜梅,许涛.理化检验化学分册,2014,50(3):317
[5]Cui A R,Zhang H Q.Chin Rare Earths,2009,30(6):71崔爱瑞,张弘强.稀土,2009,30(6):71
[6]Liu Y B,Wang J R.Yun Nan Metal,2013,42(1):58刘英波,王劲榕,云南冶金,2013,42(1):58
[7]Jin T S,Wu A P,Chen Y J,et al.J.Nanjing Univ.,1995,31(3):524金同顺,吴爱萍,陈逸君,等.南京大学学报,1995,31(3):524
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[9]Xu T,Cui A R,Du M,et al.J Anal Sci,2007,23(3):346许涛,崔爱端,杜梅,等.分析科学学报,2007,23(3):346
[10]Fu J S.Hunan Nonferrous Met,2010,26(2):66伏军胜.湖南有色金属,2010,26(2):66
[11]Yan H L,Lai X Z,Wang L,et al.Global Geology,2011,30(3):493闫红玲,来新泽,王琳,等.世界地质,2011,30(3):493
[12]Cheng Y.Metall Anal,2015,35(9):32成勇.冶金分析,2015,35(9):32
[13]Li S M,Wang G Z,Zhao J,et al.Metall Anal,2012,32(3):48李韶梅,王国增,赵军,等.冶金分析,2012,32(3):48
[14]Yin X F,Cui J,Dong Y L.Metall Anal,2003,23(5):74殷学峰,崔军,董玉兰,冶金分析,2003,23(5):74
[15]Wang Z H.Metallurgical analysis of niobium and tantalum.Beijing:Metallurgical Industry Press,1986王兆海.铌和钽的冶金分析.北京:冶金工业出版社,1986