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锆是钢铁材料中重要微量合金元素之一,少量锆能提高合金的强度。随着微合金材料研究工作的日益开展,对分析方法灵敏度提出了新的要求。常用测定锆的偶氮胂Ⅲ分光光度法,虽灵敏度较高,但在实际分析工作中,测定钢中<0.005％Zr有一定困难,且分离手续繁琐、有毒。极谱法是一种灵敏度较高的测试手段,但因锆几乎为电不活性,用极谱法很难测定。迄今尚未见到能定量测定微量锆的极谱法报导。作者试用金属有机染料络合吸附电流,以探索极谱法测定锆的途径。经大量试验研究得到成功。本文结合强酸性阳离子交换树脂一次分离,建立了示波极谱法测定钢铁和合金中微量锆的新方法,操作简便,无毒。检测下限20ppbZr(Ⅳ)、测定<0.005％Zr(Ⅳ),相对标准偏差<6％。
Zirconium is one of the important microalloying elements in steel. A small amount of zirconium can improve the strength of the alloy. With the development of microalloyed materials research, new requirements are put forward for the sensitivity of analytical methods. Commonly used in the determination of zirconium arsenazo Ⅲ spectrophotometry, although the sensitivity is high, but in the actual analysis, the determination of steel <0.005% Zr have some difficulties, and the separation procedures cumbersome and toxic. Polarographic method is a high sensitivity test method, but because of zirconium is almost electrically inactive, polarography is difficult to determine. To date, no polarographic method has been reported for the quantitative determination of trace zirconium. The authors try to metal-organic dye complex adsorption current to explore the polarographic determination of zirconium pathway. After a large number of experimental research has been successful. In this paper, a new method for the determination of trace zirconium in steel and alloy by oscillopolarographic method was established by one-time separation of strong acid cation exchange resin. The method is simple, nontoxic. The detection limit of 20ppbZr (Ⅳ), the determination of <0.005% Zr (Ⅳ), the relative standard deviation <6%.