摘要
电感耦合等离子体发射光谱法（ICP-AES）在铌钽测定方面获得广泛应用,但灵敏度较低、检出限较高,不能满足矿石和选冶样品中的低含量铌钽的检测要求。本文优化了ICP-AES测试过程中多种有机试剂的增敏效果,结果表明：样品采用氢氟酸-硝酸-硫酸敞开酸溶,选择乙醇作增敏剂,雾化效率最佳,当乙醇浓度为6%时,原子线Nb 292.781 nm、Ta 240.063 nm的灵敏度分别增强了180.5%和265.5%;铌的检出限由不加乙醇的5.85μg/g降低到3.22μg/g,钽的检出限由不加乙醇的10.65μg/g降低到5.03μg/g;Nb2O5回收率为97.7%~101.9%,Ta2O5回收率为96.8%~97.2%;方法精密度（RSD）〈6%。本方法适用于低含量和高含量铌钽的同时测定,尤其有利于选冶流程样品中同一批次的精矿、中矿和尾矿的同时测定,克服了以往分别采用光谱法和质谱法测定所产生的仪器间误差导致回收率吻合程度不好的缺陷。
Inductively Coupled Plasma-Atomic Emission Spectrometry（ ICP-AES） has been widely used in the determination of Nb and Ta,but its low sensitivity and high detection limits cannot meet the analysis requirement of low content Nb and Ta in ores and metallurgical samples. The sensitizing effect of many organic reagents was optimized in the ICP-AES determination. The results show that ethanol is the best sensitizer for determination of Nb and Ta after the samples were decomposed by open acid-solution with HF-HNO3-H2SO4 mixture. When the concentration of ethanol reaches 6%,the sensitivities of Nb（292. 781 nm） and Ta（240. 063 nm） have increases of 180. 5% and 265. 5%,respectively. Moreover,the detection limits of Nb and Ta were reduced from 5. 85 to3. 22 μg / g and from 10. 65 to 5. 03 μg / g,respectively. The recoveries of Nb2O5 and Ta2O5were 97. 7%-101. 9% and 96. 8%-97. 2%,respectively. The precision of this method was less than 6%. The method is suitable for the simultaneous determination of low and high contents of Nb and Ta,and is particularly suitable for determining Nb and Ta in ore concentrates,medium ores and the tailings of metallurgical samples from the same batch,which overcomes the bad agreement of recovery between ICP-AES and Inductively Coupled Plasma-Mass Spectrometry（ ICP-MS）.
出处
《岩矿测试》
CAS
CSCD
北大核心
2015年第2期224-228,共5页
Rock and Mineral Analysis
基金
中国地质调查局地质调查项目(12120113014300)
关键词
矿石
选冶样品
铌
钽
敞开酸溶
乙醇
电感耦合等离子体发射光谱法
ores
metallurgical samples
niobium
tantalum
open acid-solution
ethanol
Inductively Coupled Plasma-Atomic Emission Spectrometry（ICP-AES）
