电感耦合等离子体原子发射光谱法测定锆钛砂矿中锆钛铁钍铪

Determination of zirconium,titanium,iron,thorium and hafnium in zirconium-titanium placer by inductively coupled plasma atomic emission spectrometry

为了满足区域资源的调查和研究需要,提出了过氧化钠熔融-电感耦合等离子体原子发射光谱法(ICP-AES)同时测定锆钛砂矿中锆、钛、铁、钍和铪5种元素的分析方法。样品用过氧化钠熔融,水提取熔融物,过滤后沉淀用硝酸溶解,ICP-AES测定。由于过氧化钠与样品的熔融物经水提取和过滤后,大量的钠和大部分干扰元素进入滤液中,而分析元素留在沉淀中,有效消除了高盐效应对测定的影响。方法的检出限为0.010 mg/L(锆)、0.011 mg/L(钛)、0.005 1mg/L(铁)、0.082mg/L(钍)、0.018mg/L(铪),样品中各元素测定结果的相对标准偏差(n=5)小于5%,锆钛砂矿标准样品中各元素的测定值与其认定值一致。

In order to meet the needs of survey and research of regional resources, an inductively cou- pled plasma atomic emission spectrometry （ICP-AES） after sodium peroxide fusion was proposed for simultaneous determination of five elements, namely, zirconium, titanium, iron, thorium and hafni- um in zirconium-titanium placer. The sample was fused with sodium peroxide, the melt was leached with water, and the precipitate after filtration was dissolved in nitric acid and determined by ICP- AES. Because a larger amounts of sodium and most interfering elements remained in the filtrate while the determined elements entered into the precipitate after the melt produced by sodium peroxide and sample was extracted with water and filtered, thus the effect of high salt on the determination was ef- fectively eliminated. The detection limits were 0. 010 mg/L for zirconium, 0. 011 mg/L for titanium, 0. 005 1 mg/L for iron, 0. 082 mg/L for thorium and 0. 018 mg/L for hafnium. The relative standard deviations （n=5） for determination results of elements in sample were less than 5%, and the meas- ured value of each element in the zirconium-titanium placer certified reference materials was consistent with its certified value.