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本文报导了采用ICP-AES摄谱法同时测定地质样品中微量Nb、Ta、Zr、Hf的分析方法。样品经Na_2O_2熔融、浸提过滤、酸化,以732型阳离子交换树脂静态交换吸附杂质,制备成清液定容后上机测定。本法精密度(RSD)在1.5-6.2%之间,检出限为0.021-0.16微克/毫升,适用于测定地质样品中1ppm以上的Nb、Zr和几个ppm以上的Hf、Ta。一、实验部分(一)仪器装置及工作条件PGS2二米光栅光谱仪,光栅刻线1302条/毫米,中心波长290纳米,狭缝宽度12微米,单透镜(f=150)照明,1∶1成像。光源:它激式高频等离子发生器(石家庄电子加工技术研究所制)频率27.12兆赫,输出功率1.0千瓦。石英炬管端视安装。冷却氩气流量10升/分,等离子气0.5升/分,载样气流量1升/分。进样系统:A型同心玻璃雾化器,小型雾室,蠕动泵进样,溶液提升速度2
This paper reports a method for the simultaneous determination of trace amounts of Nb, Ta, Zr and Hf in geological samples by ICP-AES spectroscopy. Samples were Na 2 O 2 melted, leached and filtered, acidified, and 732 type cation exchange resin was used for static exchange adsorption of impurities to prepare a clear solution for volume determination. The method has a detection limit (RSD) of 1.5-6.2% with a detection limit of 0.021-0.16 μg / ml. This method is suitable for the determination of Nb, Zr and Hf, Ta in excess of 1 ppm in geological samples. First, the experimental part (A) of the instrument apparatus and working conditions PGS2 two grating spectrometer grating line 1302 / mm, the central wavelength of 290 nm, the slit width of 12 microns, single lens (f = 150) illumination, 1: 1 imaging . Light source: It excited high-frequency plasma generator (Shijiazhuang Institute of Electronics Technology) frequency 27.12 MHz, the output power of 1.0 kilowatts. Quartz torch end installation. Cooling argon gas flow rate of 10 liters / min, plasma gas 0.5 liters / min, sample gas flow rate of 1 l / min. Injection System: A concentric glass nebulizer, small fog chamber, peristaltic pump injection, solution lift speed 2