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航空发动机用高温合金中共存W、Mo、Ti、Ta、Zr、Hf合金元素,同时测定该合金中的Zr、Hf一直是国内外研究的重点课题,至今尚无可靠的方法。本文通过测定11个元素在阴离子交换树脂与HCl—H_2C_2O_4溶液间的分配系数,拟定了一种使Zr、Hf与高温合金中共存元素完全分离的阴离子交换法,Zr、Hf的回收率均超过99％。测定了9种离子在H_2SO_4溶液与阴离子交换树脂YSG—R_4NCl(200～400目)间的分配系数,并用作者自己组装的强制流动离子交换系统作了各元素的淋洗曲线,选定了Zr、Hf的最佳分离条件。研究了共存离子的干扰情况。根据以上实验事实,建立了一种快速、简便、准确并同时测定航空发动机用高温合金中Zr、Hf的预分离柱—强制流动离子交换色谱法。给出了合成样品及不含Zr、Hf的高温合金标准样品中Zr、Hf的标准回收结果,并测定了仿美材料Renel 125中Zr、Hf含量。结果令人满意。
The coexistence of W, Mo, Ti, Ta, Zr and Hf alloying elements in the aeroengine superalloy and the determination of Zr and Hf in the alloy at the same time have always been the focus of the research at home and abroad. So far there is no reliable method. In this paper, an anion exchange method was developed for the complete separation of the coexisting elements in Zr, Hf and superalloy by determining the partition coefficients of 11 elements between the anion exchange resin and HCl-H 2 C 2 O 4 solution. The recoveries of Zr and Hf exceeded 99 %. The partition coefficient of 9 ions between H_2SO_4 solution and anion exchange resin YSG-R_4NCl (200 ~ 400 mesh) was measured and the elution curve of each element was established by the forced flow ion exchange system assembled by the authors. Zr, Hf the best separation conditions. The interference of coexisting ions was studied. Based on the above experimental facts, a fast, simple, accurate and simultaneous determination of Zr, Hf pre-separation column-forced flow ion exchange chromatography for aero-engine superalloys was established. The standard recovery results of Zr and Hf in the standard samples of high temperature alloys without Zr and Hf were given. The contents of Zr and Hf in the Renel 125 were also determined. The result is satisfactory.