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微量镁的存在可以大大改善高温合金的许多性能。但现有高温合金中微量镁测定方法的灵敏度及准确度还不能满足要求。本文提出以镁(Ⅱ)—铬兰黑R配合物极谱波测定镁(Ⅱ)的方法。线性范围1.7 × 10~(-7)～2.5 × 10~(-5) mol·dm~(-3),检测下限5.5 × 10~(-8) mol·dm~(-3)借助于乙酰丙酮一氯仿,铜试剂—氯仿,萃取剂(Ⅱ)一氯仿联合萃取,稀盐酸反萃的分离方法测定了镍盐及GH33高温合金中微量镁结果满意,并探讨了配合物电极反应机理。
The presence of trace amounts of magnesium can greatly improve many properties of superalloys. However, the sensitivity and accuracy of the existing trace magnesium determination methods in superalloys can not meet the requirements. In this paper, a method of polarographic determination of magnesium (Ⅱ) with magnesium (Ⅱ) -chromium-black-black R complex has been proposed. The linear range was 1.7 × 10 -7 ~ 2.5 × 10 -5 mol · dm -3 and the detection limit was 5.5 × 10 -8 mol · dm -3 with the aid of acetylacetone The results of the determination of trace magnesium in nickel salt and GH33 superalloy by the separation method of chloroform, copper reagent - chloroform and extractant (Ⅱ) combined with chloroform and back-extraction with dilute hydrochloric acid were satisfactory. The reaction mechanism of the complex electrode was also discussed.