电感耦合等离子体质谱及其联用技术基础理论与地质应用研究
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摘要
电感耦合等离子体质谱(ICP-MS)以其灵敏度高、检出限低、精密度好、线性范围宽、干扰少，并可提供同位素比值信息等优势成为不同物质中多元素同时分析的首选技术。各种不同的分离技术(HPLC，GC)与高灵敏的ICP-MS联用已成为元素形态分析的最为有效的研究方法。激光剥蚀固体采样技术与ICP-MS的结合可提供原位(in situ)、实时(real time)的元素与同位素的组成信息而成为一种最具潜力的固体微区分析技术。在这些ICP-MS及其联用技术中，非质谱干扰、有机介质的增敏效应、固体微区分析的定量校正技术等基本的理论与应用研究一直是研究的热点问题。本文通过对电感耦合等离子体质谱及其联用技术基础理论的探讨及其在地质、环境样品中的应用研究，获得如下认识：
一．对于不同岩性的地质样品中痕量超痕量稀土元素的ICP-MS分析中的基体效应、氧化物及多原子离子干扰的研究表明：
1．采用模拟地质样品中天然组成比的基体匹配标准校正溶液，可有效地抑制复杂样品中元素基体效应和样品中稀土元素间含量的差异所带来的基体效应；采用~(115)In-~(103)Rh双内标元素校正技术，可有效地监控和校正分析信号的短期和长期漂移，并对基体效应具有明显的补偿作用。氧化物及氢氧化物的干扰通过对单个稀土元素及钡的氧化物、氢氧化物分析信号强度的测定，计算出等效的干扰浓度，进而可有效地校正稀土元素分析中多原子离子干扰。
2．建立了碳酸岩中超痕量稀土元素ICP-MS的测定方法，研究表明高含量的钙、镁基体对稀土的测定无影响，稀土元素间的干扰可通过匹配的基体标准得以有效的抑制。
3．以P_(507)萃淋树脂为固定相，在酸度为pH 2.6时，可不经淋洗有效的分离地下水中大部分Ca，Mg等基体元素，少量保留在柱上的基体元素用0.02 MHCl洗脱与稀土完全分离。以100mmol的EDTA洗脱，5ml内可淋洗完全。可用于地下水、海水中痕量、超痕量稀土元素及钪、钇的分析。
二．通过对不同有机介质中不同质量数和不同电离能元素的质谱行为及其增敏效应的系统
Inductively coupled plasma-mass spectrometry (ICP-MS) has been a preferred technique for analysis of trace elements in various samples owing to its low limits of detection, high sensitivity, widely dynamic linearity, multi-element determinations and isotope ratio measurement capability. The hyphenated technique of combination of different separation and preconcentration technique with specific detection techniques has become an effective method for element speciation analysis. Laser ablation solid sampling with inductively coupled plasma-mass spectrometry is a most potential solid microanalysis, offering in situ and real time information of elements and isotope ratio. However, the non-mass spectrum interference, enhancement effects of organic reagent and quantitative calibration technique of solid microanalysis are "hot" topic in ICP-MS and LA-ICP-MS. The major contents are described as follows:
1. The studies on the calibration of matrix effects and polyatomic ion for rare earth
elements in variety lithology samples were discussed.
a. Synthetic matrix-matched calibration solution that simulated the composition of natural rocks by statistically calculating the average values of 20 geological samples and normalization was adopted to minimize the matrix effects and inter-elements matrix effects. Two separate internal standards of ~(115)In-~(103)Rh were selected to compensate the drift of analytical signals. Polyatomic ions were calibrated by measuring the oxides (MO~+) and hydroxide (MOH~+) with individual La, Ce, Pr and Ba solution for the ratio of MO~+/M~+ and MOH~+/M~+ and calculating equivalently concentrations.
b. The method for the determination of ultra-trace rare earth elements in carbonate by ICP-MS has been developed. The inter-element matrix effect of REEs was minimized by using matrix-matched calibration solution. The matrix effect of Ca, Mg can be ignored.
c. The most matrix of Ca, Mg in ground water can be removed without elution at pH 2.6 by using P507 resin as the stationary phase . A few matrix retainment on column was eluted with 0.02 HCl. Then the REEs were eluted with 100mmo EDTA as mobile phase in 5ml elution. The proposed method has been applied to the analysis of ultra-trace REEs and Y, Sc in ground water.
2. The enhancement effects of organic reagent in ICP-MS were investigated in detail. The
一．对于不同岩性的地质样品中痕量超痕量稀土元素的ICP-MS分析中的基体效应、氧化物及多原子离子干扰的研究表明：
1．采用模拟地质样品中天然组成比的基体匹配标准校正溶液，可有效地抑制复杂样品中元素基体效应和样品中稀土元素间含量的差异所带来的基体效应；采用~(115)In-~(103)Rh双内标元素校正技术，可有效地监控和校正分析信号的短期和长期漂移，并对基体效应具有明显的补偿作用。氧化物及氢氧化物的干扰通过对单个稀土元素及钡的氧化物、氢氧化物分析信号强度的测定，计算出等效的干扰浓度，进而可有效地校正稀土元素分析中多原子离子干扰。
2．建立了碳酸岩中超痕量稀土元素ICP-MS的测定方法，研究表明高含量的钙、镁基体对稀土的测定无影响，稀土元素间的干扰可通过匹配的基体标准得以有效的抑制。
3．以P_(507)萃淋树脂为固定相，在酸度为pH 2.6时，可不经淋洗有效的分离地下水中大部分Ca，Mg等基体元素，少量保留在柱上的基体元素用0.02 MHCl洗脱与稀土完全分离。以100mmol的EDTA洗脱，5ml内可淋洗完全。可用于地下水、海水中痕量、超痕量稀土元素及钪、钇的分析。
二．通过对不同有机介质中不同质量数和不同电离能元素的质谱行为及其增敏效应的系统
Inductively coupled plasma-mass spectrometry (ICP-MS) has been a preferred technique for analysis of trace elements in various samples owing to its low limits of detection, high sensitivity, widely dynamic linearity, multi-element determinations and isotope ratio measurement capability. The hyphenated technique of combination of different separation and preconcentration technique with specific detection techniques has become an effective method for element speciation analysis. Laser ablation solid sampling with inductively coupled plasma-mass spectrometry is a most potential solid microanalysis, offering in situ and real time information of elements and isotope ratio. However, the non-mass spectrum interference, enhancement effects of organic reagent and quantitative calibration technique of solid microanalysis are "hot" topic in ICP-MS and LA-ICP-MS. The major contents are described as follows:
1. The studies on the calibration of matrix effects and polyatomic ion for rare earth
elements in variety lithology samples were discussed.
a. Synthetic matrix-matched calibration solution that simulated the composition of natural rocks by statistically calculating the average values of 20 geological samples and normalization was adopted to minimize the matrix effects and inter-elements matrix effects. Two separate internal standards of ~(115)In-~(103)Rh were selected to compensate the drift of analytical signals. Polyatomic ions were calibrated by measuring the oxides (MO~+) and hydroxide (MOH~+) with individual La, Ce, Pr and Ba solution for the ratio of MO~+/M~+ and MOH~+/M~+ and calculating equivalently concentrations.
b. The method for the determination of ultra-trace rare earth elements in carbonate by ICP-MS has been developed. The inter-element matrix effect of REEs was minimized by using matrix-matched calibration solution. The matrix effect of Ca, Mg can be ignored.
c. The most matrix of Ca, Mg in ground water can be removed without elution at pH 2.6 by using P507 resin as the stationary phase . A few matrix retainment on column was eluted with 0.02 HCl. Then the REEs were eluted with 100mmo EDTA as mobile phase in 5ml elution. The proposed method has been applied to the analysis of ultra-trace REEs and Y, Sc in ground water.
2. The enhancement effects of organic reagent in ICP-MS were investigated in detail. The
引文
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