摘要
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.
出处
《冶金分析》
CAS
CSCD
北大核心
2016年第9期77-81,共5页
Metallurgical Analysis
基金
国家自然科学基金(20961012)
关键词
MCI-GEL树脂
二苯胍
固相萃取
钯
富集
MCI-GEL resin
1
3-diphenylguanidine
solid phase extraction
palladium
enrichment
