基于Pd(Ⅱ)与二苯胍(DPG)形成的络合物能够被MCI-GEL树脂固相萃取柱萃取、富集,建立了一种固相萃取钯的方法。经过实验发现:当溶液中nDPG∶nPd(Ⅱ)=0.5,盐酸介质浓度为0.05mol/L,过柱流速为10mL/min,Pd(Ⅱ)的萃取率可达99%;通过流出曲线测定出MCIGEL树脂固相小柱的萃取容量为4.86mg/g;筛选出最佳洗脱液为酸性硫脲溶液,且3.0mL20g/L的酸性硫脲溶液以1.0mL/min的洗脱速度能完全洗脱4.86mg/g钯。在0.05~2.0mol/L盐酸介质中,利用MCI-GEL树脂固相小柱对合成试样溶液中Pd(Ⅱ)进行分离和测定,通过计算分离系数,证明在0.05mol/L盐酸介质中,Pd(Ⅱ)可与Pt(Ⅳ)、Fe(Ⅲ)、Ni(Ⅱ)、Cu(Ⅱ)、Zn(Ⅱ)离子定量分离。
The complex formed by Pd(Ⅱ) and diphenylguanidine(DPG)could be extracted and enriched by solid phase extraction column of MCI-GEL resin.Based on this,a solid phase extraction method of palladium was established.The results showed that the extraction rate of Pd(Ⅱ) could be up to 99 % under the following conditions:the mole ratio of DPG and Pd(Ⅱ)in solution was nDPG︰nPd(Ⅱ)=0.5;the concentration of hydrochloric acid medium was 0.05mol/L;the flow rate passing through column was 10mL/min.The extraction capacity of MCI-GEL resin solid phase column was measured by elution curve method,and the result was 4.86mg/g.The optimal elution solution was acid thiocarbamide solution.Moreover,4.86mg/g of palladium could be fully eluted when the elution rate of 3mL of 20g/L acid thiocarbamide solution was 1.0mL/min.The MCI-GEL resin solid phase column was used to separate and determine Pd(Ⅱ)in synthetic sample in 0.05-2.0mol/L hydrochloric acid medium,and it proved that in 0.05mol/L hydrochloric acid medium,Pd(Ⅱ) could be quantitatively separated from Pt(Ⅳ),Fe(Ⅲ),Ni(Ⅱ),Cu(Ⅱ) and Zn(Ⅱ) by calculating the separation coefficient.