摘要
醋酸酐生产用废铑催化剂样品在密闭消解罐中用HNO3-H2O2于160℃经8 h可消解完全,并避免样品损失。考察了样品处理和不同测定方法对测定结果的影响。结果表明,合适的样品量为0.1～0.3 g;消解液经H2SO4-HClO4发烟处理可以去除样品中有机组分的干扰;氯化亚锡分光光度法和ICP-AES法均可准确测定样品中的铑含量,测定相对标准偏差(RSD)均小于2%,加标回收率分别为97.53%～101.65%和98.19%～102.70%,在实际测定中可根据实验室条件选择合适的测定方法。
The waste rhodium catalyst for production of acetic anhydride was digested by HNO3-H2O2 in a sealed digestion tank at 160℃,and the sample was completely digested without loss after 8 hours.The effect of sample pretreatment and different methods on the determination results was investigated.The results showed that the optimum sample weight was 0.1~0.3 g.The digestion solution was treated by H2SO4-HClO4 to remove the interference of organic matter.Both stannous chloride spectrophotometry and ICP-AES methods can be used for determining the rhodium content in samples.The relative standard deviation was less than 2%,and their recovery rates were 97.53%~101.65%and 98.19%~102.70%,respectively.In actual applications,an appropriate method can be selected according to the available laboratory conditions.
作者
易秉智
陈剑峰
姚田田
张宇辉
暨左成
罗成
YI Bingzhi;CHEN Jianfeng;YAO Tiantian;ZHANG Yuhui;JI Zuocheng;LUO Cheng(Zhejiang Teli Recycling Resources Co.Ltd.,Jiaxing 314300,Zhejiang,China)
出处
《贵金属》
CAS
CSCD
北大核心
2018年第4期70-73,共4页
Precious Metals
