摘要
对目前常用的硝酸-氢氟酸-高氯酸和盐酸-硝酸-氢氟酸-高氯酸两种底泥酸消解体系进行了比较,并对消解过程的温控程序进行了优化。结果表明,两种体系程序升温(起始温度低于180℃)消解方式得到的6种元素(As、Cd、Cr、Cu、Pb和Zn)电感耦合等离子体发射光谱仪同步测定结果精度均高于180℃恒温消解的测定值,特别是As的精确度有明显提高。当消解采用HCl-HNO3-HF-HCl O4体系且控制在80,120℃下逐步消解、180℃下赶酸时,样品的测定结果与标准样品中重金属的含量基本一致,可以达到98.57%~110.42%的回收率,相对标准偏差(RSD)在5%以内。
Two representative systems of sediment acid digestion, HNO3-HF-HC104 and HC1-HNO3-HF- HC104, were investigated by optimizing the temperature profile in digestion process. The results showed that both digestion systems with an initial temperature below 180 ℃ gave higher precision of the metal concentrations (As, Cd, Cr, Cu, Pb and Zn) than those digested at fixed temperature of 180 ℃, as deter- mined by the inductively coupled plasma-atomic emission spectrometry (ICP-AES). Especially, the precision of As concentration was significantly improved. When the sediment sample was gradually digested under 80 ℃ and then 120 ℃ with HCI-HNO3-HF-HC104 system followed by evaporation at 180 ℃ ,the resultant concentrations of target metals were found to be generally consistent with those for the standard sample,with high recovery (98.57% - 110.42% ) and low relative standard deviation ( 〈 5% ).
出处
《应用化工》
CAS
CSCD
北大核心
2015年第8期1546-1549,1555,共5页
Applied Chemical Industry
基金
国家环境保护公益性行业科研专项(201309052)
关键词
底泥
多金属
程序升温
消解
sediment
multi metal elements
programmed temperature
acid digestion