电感耦合等离子体原子发射光谱法测定海绵铪中8种杂质元素

海绵铪对杂质元素的种类及含量要求严格,现有检测方法难以快速、准确地测定海绵铪中钨、镍、锰、钛、钒、钼,钴、铜等8种杂质元素。实验采用硝酸、氢氟酸溶解样品,采用基体匹配法绘制校准曲线并消除基体效应的影响,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定海绵铪中钨、镍、锰、钛、钒、钼、钴、铜,方法可以测定海绵铪中0.001%～0.010%(质量分数,下同)钨、镍、锰、钛、钒、钼、钴、铜。各元素质量浓度在0.10～3.00 μg/mL范围内与其发射光谱强度呈良好的线性关系,线性相关系数大于0.999;各元素检出限不大于0.000 5%,定量限不大于0.001 5%。按照实验方法测定海绵铪中8种杂质元素,结果的相对标准偏差(RSD,n=8)为4.3%～9.8%,测定结果与电感耦合等离子体质谱法(ICP-MS)一致。

Determination of eight impurity elements in sponge hafnium by inductively coupled plasma atomic emission spectrometry

Sponge hafnium has strict requirements to the type and content of impurity element. The current detection methods are difficult to determine eight impurity elements (including tungsten, nickel, manganese, titanium, vanadium, molybdenum, cobalt, and copper) rapidly and accurately in sponge hafnium. In experiments, the sample was dissolved with nitric acid and hydrofluoric acid. The calibration curves were prepared by matrix matching method to eliminate the influence of matrix effect. The contents of tungsten, nickel, manganese, titanium, vanadium, molybdenum, cobalt, and copper in sponge hafnium were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The proposed method enabled to determine tungsten, nickel, manganese, titanium, vanadium, molybdenum, cobalt, and copper in sponge hafnium with content in range of 0.001%-0.010% (mass fraction, similarly hereinafter). The mass concentration of elements in range of 0.10-3.00 μg/mL had good linear relationship with the corresponding intensity of emission spectrum, and the linear correlation coefficients were greater than 0.999. The limits of detection for each elements were not more than 0.000 5%, and the limits of quantification were not more than 0.001 5%. Eight impurity elements in sponge hafnium were determined according to the experimental method. The relative standard deviations (RSD, n=8) of determination results were between 4.3% and 9.8%. The found results were consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS).