研究了用高效液相色谱法测定电镀用氰化亚金钾中的杂质元素。电镀用氰化亚金钾样品用微波消解.然后用甲基异丁基酮(MIBK)萃取分离金。镍、铜、铰、铅、镉、汞6种杂质元素用四-(对二甲氨基苯基)-卟啉(T4-DMAPP)柱前衍生,然后用甲醇和四氢呋喃为流动相,ZORBAX Stable Bound(4.6mm×50mm,1.8μm)快速分离柱为固定相分离,6种杂质元素的配合物在2.0min内可达到分离;用二极管矩阵检测器检测,镍、铜、铁、铅、镉、汞的检测限分别为:40ng/L、30ng/L、50ng/L、40ng/L、20ng/L和40ng/L。该方法相对标准偏差为1.8%~3.4%,标准加入回收率为92%~106%。该方法用于测定电镀用氰化亚金钾样品中的痕量镍、铜、铁、铅、镉、汞,结果令人满意。
A new method for the determination of copper, nickel, iron, lead, cadmium and mercury in potassium aurous cyanide was studied. The samples were digested with microwave digestion. The copper, nickel, iron, lead, cadmium and mercury ions were pre-column derived by Tera- (4-dimethylaminophenyl) -porphine ( T4 - DMAPP) to form stable chelates. These chelates were separated on a ZORBAX Stable Bound (4.6mm×50mm, 1.8μm) by gradient elution with methanol and THF as mobile phase at a flow rate of 2.0ml/min and detected with photodiode array detector from 350 - 600nm. The detection limits of nickel, copper, iron, lead, cadmium, and mercury are 40ng/L, 30rig/L, 50ng/L, 40ng/L, 20ng/L and 40ng/L respectively. The results show that most of the relative standard deviations of these ions were 1.8% - 3.4%. The standard recoveries were in the range of 92% - 106%. This method was applied to the determination of nickel, copper, iron, lead, cadmium, and mercury in potassium aurous cyanide with good results.