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稀有难熔金属铌铪合金、铌钽钨合金及锆钨钼化合物 (ZrW1 -x MoxO8)等材料具有特有的高熔点 ,高强度 ,高硬度特点 ,应用于航天航空等领域 ,其成分及难熔金属杂质分析是化学分析中难度较大的课题 ,在实际分析中令分析工作者感到棘手[1 ] 。对锆铪分析通常不仅需与共存元素分离 ,而且要进行锆与铪的分离。由于锆铪受镧系收缩效应的影响 ,其化学性质极为相似 ,要将二者分离完全相当困难 ,常用离子交换色谱分离[2 ] ,手续繁杂 ,时间冗长。为此本报告以纸上色谱法分离钽铌进行预处理 ,采用电感耦合等离子体发射光谱法 (ICP_AES)测定 ,建立稀有难熔金属合金中Zr、Hf测定的新方法 ,测定范围 :0 0x %——— 1 0 0 0 %。方法能同时得到Zr、Hf的分析结果 ,相对标准偏差 1 0 %的Hf为 0 97% ,0 5%的Zr为 8 2 8%。方法简便 ,准确度在实样分析中取得满意的结果。
Rare refractory metal niobium hafnium alloy, niobium tantalum tungsten alloy and zirconium tungsten molybdenum compound (ZrW1-x MoxO8) and other materials with unique high melting point, high strength, high hardness, used in aerospace and other fields, the composition and refractory Analysis of metal impurities is a more difficult chemical analysis of the subject, in fact, analysts feel thorny [1]. Analysis of zirconium and hafnium usually not only with the separation of coexisting elements, but also for zirconium and hafnium separation. Due to the zirconium and hafnium by lanthanide contraction effect, its chemical properties are very similar, to separate the two completely quite difficult, commonly used ion exchange chromatography [2], complicated procedures, time-length. To this end, the paper pretreated with tantalum and niobium by paper chromatography and determined by inductively coupled plasma atomic emission spectrometry (ICP_AES) to establish a new method for the determination of Zr and Hf in rare refractory metal alloys. The measuring range is: 0 × 0% --- 1 0 0 0%. The analytical results of Zr and Hf can be obtained at the same time. The relative standard deviation (Hf) of 10% is 0 97% and that of 0 5% is 8 2 8%. The method is simple and accurate, with satisfactory results obtained in real sample analysis.