摘要
采用微波消解-电感耦合等离子体-原子发射光谱法(ICP-AES),通过分析回收率,着重研究消解用无机酸(盐酸、硝酸和过氧化氢)对油墨中铅含量测定的影响。盐酸的加入对ICP-AES分析影响较小,但会与铅形成二氯化铅,造成微量损失,回收率下降。硝酸对ICP—AES分析有酸效应,过量硝酸会影响仪器精准性。当过氧化氢用量为1.0-2.0mL时,对回收率基本没有影响。结果表明,6mL硝酸和1mL过氧化氢就可使1.5g油墨消解完全,此时铅的加标回收率为100.7%。实验优化了前处理方法,使结果更加准确可靠。
A method for determination of lead(Pb) in printing ink was studied by microwave digestion and inductively coupled plasma-atomic emission spectrometry(ICP-AES).Effects of contents of inorganic acids(chlorhydric acid,nitric acid and hydrogen peroxide) were mainly investigated through investigating the recovery of Pb.Effects of chlorhydric acid on ICP-AES were little,but it can form lead dichloride with Pb,which lead to small loss of Pb and decrease the recovery.Too much nitric acid resulted in the acid effects of ICP-AES.Hydrogen peroxide had little influences on determination of Pb,when the added content of hydrogen peroxide was 1.0—2.0mL.The results showed that,l.5g printing ink can be completely digested,when 6mL nitric acid and lmL hydrogen peroxide were used. The recovery of Pb was 100.7%.The pre-treating method was optimized and it was suitable for determination of Pb in printing ink with its simplicity and accuracy.
出处
《光谱实验室》
CAS
CSCD
2012年第1期423-426,共4页
Chinese Journal of Spectroscopy Laboratory