针对电感耦合等离子体质谱法(ICP-MS)测定汞元素时存在汞记忆效应严重,且消除时前处理过程复杂的问题,提出了此项研究。取样品0.5000 g置于聚四氟乙烯消解罐中,加入5 m L硝酸和1 m L 30%(质量分数)过氧化氢溶液,置于100℃恒温消解仪中加...针对电感耦合等离子体质谱法(ICP-MS)测定汞元素时存在汞记忆效应严重,且消除时前处理过程复杂的问题,提出了此项研究。取样品0.5000 g置于聚四氟乙烯消解罐中,加入5 m L硝酸和1 m L 30%(质量分数)过氧化氢溶液,置于100℃恒温消解仪中加热30 min,冷却,将消解罐密封置于微波消解仪中,消解后冷却,打开消解罐,置于100℃恒温消解仪中15 min,将消解溶液转移至25 m L容量瓶中,用水洗涤消解罐数次,清洗液与消解溶液合并,用水定容至25 m L,与清洗试剂[2 mg·L^(-1)金元素标准使用液或2%(质量分数,下同)L-半胱氨酸溶液]配制的20μg·L^(-1)186Re内标溶液在线混匀后,采用ICP-MS进行测定。结果表明,清洗试剂可消除0.5~5μg·L^(-1)汞元素标准溶液的汞记忆效应,对下一个样品的测定结果不产生影响。汞元素的质量浓度在0.5~5μg·L^(-1)内与所对应的信号强度与内标元素信号强度比呈线性关系,采用2 mg·L^(-1)金元素标准使用液配制内标溶液时,检出限(3s)为0.0010 mg·kg^(-1),采用2%L-半胱氨酸溶液配制内标溶液时,检出限(3s)为0.0012 mg·kg^(-1)。按照标准加入法进行回收试验,回收率为90.2%~104%,测定值的相对标准偏差(n=6)均小于9.0%。方法用于3种市售化妆品分析,使用2种清洗试剂配制的内标溶液得到的检出量一致,为0.0080~0.13 mg·kg^(-1)。展开更多
A method of analysis trace element chloride in cleaning products by Inductively Coupled Plasma-Mass Sepctrometry (ICPMS) was studied. It has good precision (RSD<5%). The LOD is 0.06 μg/L (n=7). The recovery is 93....A method of analysis trace element chloride in cleaning products by Inductively Coupled Plasma-Mass Sepctrometry (ICPMS) was studied. It has good precision (RSD<5%). The LOD is 0.06 μg/L (n=7). The recovery is 93.7%-110.0%.展开更多
In this paper,the determination of six heavy metal ions (arsenic,lead,cadmium,chromium,mercury and nickel) in the Chinese Herb by inductively coupled plasma-mass spectrometry (ICP-MS) was studied.The samples were dige...In this paper,the determination of six heavy metal ions (arsenic,lead,cadmium,chromium,mercury and nickel) in the Chinese Herb by inductively coupled plasma-mass spectrometry (ICP-MS) was studied.The samples were digested by nitric acid and hydrogen peroxide in a microwave oven.The Sc,Y,In,Bi were added as internal standards to eliminate the matrix interferences.The results show that most of the relative standard deviations of these trace elements were below 3.5%,the standard recoveries of these elements were in the range of 91%-107%,and the detection limits were in the range of 0.001-0.006 μg·L-1. This method is accurate,rapid,convenience,and can be applied to the determination of arsenic,lead,cadmium,chromium,mercury and nickel in Chinese Herb with good results.展开更多
文摘针对电感耦合等离子体质谱法(ICP-MS)测定汞元素时存在汞记忆效应严重,且消除时前处理过程复杂的问题,提出了此项研究。取样品0.5000 g置于聚四氟乙烯消解罐中,加入5 m L硝酸和1 m L 30%(质量分数)过氧化氢溶液,置于100℃恒温消解仪中加热30 min,冷却,将消解罐密封置于微波消解仪中,消解后冷却,打开消解罐,置于100℃恒温消解仪中15 min,将消解溶液转移至25 m L容量瓶中,用水洗涤消解罐数次,清洗液与消解溶液合并,用水定容至25 m L,与清洗试剂[2 mg·L^(-1)金元素标准使用液或2%(质量分数,下同)L-半胱氨酸溶液]配制的20μg·L^(-1)186Re内标溶液在线混匀后,采用ICP-MS进行测定。结果表明,清洗试剂可消除0.5~5μg·L^(-1)汞元素标准溶液的汞记忆效应,对下一个样品的测定结果不产生影响。汞元素的质量浓度在0.5~5μg·L^(-1)内与所对应的信号强度与内标元素信号强度比呈线性关系,采用2 mg·L^(-1)金元素标准使用液配制内标溶液时,检出限(3s)为0.0010 mg·kg^(-1),采用2%L-半胱氨酸溶液配制内标溶液时,检出限(3s)为0.0012 mg·kg^(-1)。按照标准加入法进行回收试验,回收率为90.2%~104%,测定值的相对标准偏差(n=6)均小于9.0%。方法用于3种市售化妆品分析,使用2种清洗试剂配制的内标溶液得到的检出量一致,为0.0080~0.13 mg·kg^(-1)。
文摘A method of analysis trace element chloride in cleaning products by Inductively Coupled Plasma-Mass Sepctrometry (ICPMS) was studied. It has good precision (RSD<5%). The LOD is 0.06 μg/L (n=7). The recovery is 93.7%-110.0%.
文摘In this paper,the determination of six heavy metal ions (arsenic,lead,cadmium,chromium,mercury and nickel) in the Chinese Herb by inductively coupled plasma-mass spectrometry (ICP-MS) was studied.The samples were digested by nitric acid and hydrogen peroxide in a microwave oven.The Sc,Y,In,Bi were added as internal standards to eliminate the matrix interferences.The results show that most of the relative standard deviations of these trace elements were below 3.5%,the standard recoveries of these elements were in the range of 91%-107%,and the detection limits were in the range of 0.001-0.006 μg·L-1. This method is accurate,rapid,convenience,and can be applied to the determination of arsenic,lead,cadmium,chromium,mercury and nickel in Chinese Herb with good results.
