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本文以色谱理论,离子交换和溶液平衡理论为指导,结合少量实验确定了一个分离Cu~(2+)、Ni~(2+)、Zn~(2-)、Pb~(2-)、Co~(2-)、Cd~(2+)的较好三元络合洗脱液:酒石酸钠、柠檬酸钠,氯化钠。分别用正交设计和单纯形最优化两种方法选出了洗脱液的最佳组成(以,作为优化目标函数),用国产填料和仪器,23分钟之内成功地分离了上述六种重金属离子,各相邻峰间的分离度均达1.1以上。 在前人工作的基础上,自行设计并使用了富集柱在pH=1～1.5的HCl介质条件下富集重金属,并同时分离基体贵金属,然后用六通阀切换以测定重金属的连续操作流程。考察了富集液流速、酸度,NaNO_3用量等因素对富集效率的影响和共存其他金属的干扰,选出了合适的富集和测定条件。 用所建立的方法测定了实际样品铂、钯、铱中的痕量重金属杂质(含量<0.0025％)。变异系数小于3.3％,相对误差小于±6.0％,加标回收率大于97％。
Under the guidance of chromatographic theory, ion exchange and solution equilibrium theory, a small amount of experiments were carried out to determine the effect of separation of Cu2 +, Ni2 +, Zn2-, Pb2-, Co ~ (2 -), Cd ~ (2+) better ternary complex eluent: sodium tartrate, sodium citrate, sodium chloride. The optimal composition of the eluate was selected by orthogonal design and simplex optimization (respectively, as the objective function of optimization). With the domestic fillers and instruments, the above six heavy metals were successfully separated within 23 minutes Ions, the resolution between adjacent peaks reached 1.1 or more. Based on the previous work, the enrichment column was designed and used to enrich the heavy metals under the condition of pH = 1 ~ 1.5 HCl medium and separate the matrix precious metals at the same time, and then use the six-way valve to switch to determine the continuous operation flow of heavy metals . The effect of enrichment liquid flow rate, acidity, NaNO 3 dosage and other factors on the enrichment efficiency and the coexistence of other metals were investigated. The suitable enrichment and determination conditions were selected. The trace amounts of heavy metal impurities (content <0.0025%) in the actual samples platinum, palladium and iridium were determined by the established method. The coefficient of variation is less than 3.3%, the relative error is less than ± 6.0%, and the recovery of standard addition is more than 97%.