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应用阳离子交换树脂色层分离法使锆合金(锆锡铁铬镍合金)中锆与铝、钡、铜、镍、钛、钒等6种元素分离,以电感耦合等离子体原子发射光谱法测定6种微量元素。通过选择不同浓度的硝酸作淋洗液,可使吸附于阳离子色层柱上的锆和6种微量元素分别洗脱(先用0.010 mol/L硝酸洗脱锆,然后用2.0 mol/L硝酸洗脱待测元素),达到了锆与待测元素分离的目的。与待测元素同时洗脱下来的锡、铬、铁对已选定的分析线没有显著的光谱干扰。各元素的检出限在0.008~0.015μg/mL之间,测定下限为0.10μg/mL。对样品进行加标回收率和精密度试验,得到回收率和相对标准偏差分别为93.2%~108%和3.3%~8.2%。
The separation of zirconium from aluminum, barium, copper, nickel, titanium and vanadium in zirconium alloy (zirconium-tin-iron-chromium-nickel alloy) was determined by cation exchange resin chromatography with inductively coupled plasma atomic emission spectrometry Trace elements By choosing different concentrations of nitric acid as eluent, the adsorbed zirconium and six kinds of trace elements on the chromatographic column can be eluted respectively (zirconium is first eluted with 0.010 mol / L nitric acid and then with 2.0 mol / L nitric acid Off test element), to achieve the purpose of separation of zirconium and the element to be tested. The tin, chromium and iron eluted simultaneously with the analyte did not show any significant spectral interference on the selected analytical line. The detection limits of each element ranged from 0.008 to 0.015 μg / mL with the lower limit of determination of 0.10 μg / mL. The recoveries and relative standard deviations (RSDs) of the samples were 93.2% -108% and 3.3% -8.2%, respectively.