电热蒸发原子光谱/质谱联用技术及痕量分析
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摘要
电感耦合等离子体原子发射光谱/质谱(ICP-AES/MS)具有灵敏度高,线性范围宽,分析速度快和可同时测定多元素等优点,已成为痕量/超痕量分析的主要方法之一,广泛应用于生命、食品、临床、新材料、环境、地质、冶金和核技术等领域。应当指出,从原子光谱到原子质谱标志着分析科学学科发展中的重要突破。
新进样技术研究一直是原子光谱/质谱分析界关注的热点之一。电热蒸发(ETV),作为一种使待测物以气态形式引入ICP-AES/MS的进样技术,具有以下一些突出的优点:(1)进样效率高(～80%),方法的检出限得到显著改善;(2)试样的蒸发和激发(电离)过程分步进行,有利于实验参数的优化和降低基体产生的干扰;(3)耗样量少,微克级或微升级;(4)可直接分析固体试样,省去了样品预处理;(5)利用化学改进剂可进一步提高方法的灵敏度与选择性。
本论文的研究目的是,系统研究和发展ETV-ICP-MS联用新技术,将聚四氟乙烯(PTFE)化学改进剂(氟化剂)引入ETV-ICP-MS体系,探索降低质谱干扰和基体效应的途径,研究其规律性及机理,在此基础上,建立ETV-ICP-MS直接分析固体试样(难熔材料、生物试样)的新方法。此外,研究ETV-ICP-AES/MS与有特色的分离富集前处理技术联用,并将它用于痕量元素成分和形态分析。主要研究内容包括:
(1)建立了氟化电热蒸发(FETV)-ICP-MS直接测定难熔Nb_2O_5固体粉末中的痕量杂质的新方法,试样以悬浮体形式引入(一次分析,所需试样的量仅为0.002mg),无需任何化学前处理。对石墨炉与ICP之间的接口进行了改进,并对影响分析物信号强度的石墨炉载气和辅助载气的流速进行了优化;研究了在不同实验条件下的分析物电热蒸发信号轮廓,及悬浮体中基体总量对分析物信号的影响;用实验方法详细考察了PTFE分解产物可能产生的质谱干扰并对这一干扰的可能性进行了评价。提出了一种用实验手段判断基体效应是否存在的新方法。结果表明,应用FETV-ICP-MS直接测定痕量金属杂质,基体(Nb_2O_5)在悬浮体中的浓度不大于200mg L~(-1)时,不存在基体效应:用标准溶液工作曲线法、标准加入法及常规溶液雾化法所测定的结果一致。
(2)通过对试样的适当稀释和对石墨炉升温程序的有效控制,可以完全消除或显著降低血清试样中主要基体(有机基体和无机基体)产生的影响;详细考察了存在或不存在PTFE的条件下非金属元素Cl、S、P和金属元素Na、K、Ca、Mg在石墨炉中的挥发行为,并优化了实验参数。据此,建立了石墨炉原位分离基体后,用ETV-ICP-MS直接测定生物流体中痕量难熔元素的新方法。该法已成功应用于人血清中痕量V、Cr、Mo、Ba、La、Ce和W的同时/直接测定,无需任何化学前处理,无需基体匹配,灵敏、简单、快速及试样消耗少。
(3)以纳米二氧化钛为吸附材料,考察了在不同pH条件下,纳米二氧化钛对
Inductively coupled plasma atomic emission spectrometry / mass spectrometry (ICP-AES/MS) has several advantages for trace element determination: low detection limits, wide linear dynamic range, multi-element detection capability, and high sample throughput. Therefore, it has a widespread application in an extensive field such as life science, food science, clinical chemistry, material technology, environmental science, geological chemistry, metallurgic chemistry, and nuclear technology. And it is worthy of note that the appearance of ICP-MS is a significant breakthrough in atomic spectrometry.Electrothermal vaporization (ETV), which converts both the solution and the solid samples to the vapor state, is considered to be a useful technique of sample introduction for ICP-AES / MS over conventional pneumatic nebulization. The advantages of ETV can be described as follows: (1) high efficiency of sample introduction (~ 80%), which results in low detection limit; (2) separation processes of vaporization and excitation / ionization of analyte, which is beneficial to the optimization of experimental parameters and alleviation of interferences caused by matrix; (3) small size of sample requirement, which could be applied to the analysis of samples at micro-level; (4) capability of direct solid analysis, which reduces sample pretreatment and gives low risk of contamination and analyte loss; (5) and the sensitivity and selectivity of the method can be promoted further with the usage of chemical modifier.The objective of this dissertation is to study the vaporization behaviors of refractory / carbide forming elements in a graphite furnace with / without the use of polytetrafluoroethylene (PTFE) emulsion as chemical modifier; to explore the possibility of in-situ elimination of spectral interferences and matrix effect in the graphite furnace; and then to develop a new method of fluorination assisted electrothermal vaporization (FETV)-ICP-MS for the direct analysis of micro-amount of refractory solid powder and biological samples. For the analysis of ultra-trace elements and elemental species, some new separation / preconcentration techniques was developed and combined with ETV-ICP-MS. The main interests of this dissertation are summarized as follows:(1) A method of slurry sampling FETV-ICP-MS was developed to directly determine the trace impurities in niobium pentaoxide solid powder in which a PTFE emulsion was used as fluorinating modifier to promote the vaporization of refractory elements from a graphite furnace and to avoid the formation of thermal stable carbides. For one analysis run, only 0.002 mg of Nb_2O_5 sample was required. The electrothermal vaporizer device was connected to the ICP system by a laboratory-built interface, and the flow rates of sample carrier gas and auxiliary carrier gas were optimized experimentally. The
potentially polyatomic interferences resulting from the pyrolysates of PTFE were evaluated. A new method by stepwise diluting the sample matrix is proposed for investigating the matrix effect and the results showed that no obvious matrix effect was observed with the sample matrix (Nb2O5) concentration of less than 200 mg I/1. The proposed method has been applied to determine the trace impurities in M^Os powder, and both the results obtained from the external calibration curves and the standard addition curves were in a good agreement with those obtained by conventional nebulization ICP-MS.(2) A method of in situ removal of matrix was proposed for direct determination of the trace refractory elements in human serum by ETV-ICP-MS with the use of PTFE as fluorinating reagent. Attention has been paid to investigating the vaporization behaviors of both refractory elements of interest and matrix elements (Na, K, Ca, Mg, Cl, S, P) in a graphite furnace with the PTFE modifier presence or not. It was shown that the potential interferences of the organic and inorganic matrices in serum sample could be eliminated or reduced to a neglectable level with properly diluting the human serum and deliberately optimizing the ETV temperature program. The proposed method has been applied to the direct simultaneous determination of V, Cr, Mo, Ba, La, Ce and W in human serum.(3) Anew method for the determination of La3+ and La complexes in solution using a nanometer-sized titanium dioxide as solid-phase extractant and fiuorination assisted electrothermal vaporization (FETV)-ICP-AES as sensitive detector has been developed. The effect of pH on the adsorption characteristics of nanometer TiC>2 for La3+ and La-complexes of citric acid, 2-hydroxyisobutyric acid, and humic acid has been investigated and optimized. Based on the difference in volatility between fluorides of analyte (lanthanum) and matrix (titanium), an in-situ removal of the adsorbent matrix (TiCb) from a graphite furnace was realized. Therefore, the La3+ in solution and La-complexes absorbed on nanometer-sized titanium dioxide could be determined respectively by FETV-ICP-AES without any chemical pretreatment. The proposed method has been applied for the determination of free La3+ and La-complexes in synthetic solutions and soil extracts with satisfactory results.(4) Anew method is described for single-drop microextraction of trace rare earth elements La, Y and Yb with l-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) / benzene solution as organic phase. ETV-ICP-MS was used to determine the analyte in post-extraction organic drop. Several parameters, which influence the microextraction behavior of analyte, such as sample flow rate, microdroplet volume, solvent and extraction time, were investigated and the optimized experimental conditions were established, hi order to explore the process of microextraction, the conventional pneumatic nebulization ICP-MS was used for on-line monitoring the analyte concentration change in the aqueous phase. Based on the obtained experimental results, a dynamic model for continuous-flow
microextraction of inorganic elements has been supposed. Under the selected experimental conditions, the preconcentration factors with a 25 min cycle-flow microextraction of a 1 mL sample were 233, 242 and 244 for La, Y and Yb, respectively. The proposed method was applied to the analysis of biological materials (GBW07605 Tea leaves and GBW07601 Human hair), and the results obtained were in good agreement with the certified values.(5) A procedure for copper, zinc and manganese determination in food samples by slurry sampling graphite furnace atomic absorption spectrometry (GFAAS) is proposed. The analysis results of food reference materials (NIST SRM1567, 1568) agreed with the reference value and the spiked recoveries of real samples were in the range of 95% -106%.(6) The mechanism of vaporization / atomization of Cr, Ni, Zr, Nb and Yb has been studied using ETV-ICP-MS and GFAAS. The behavior of vaporization / atomization of Cr, Ni, Zr, Nb and Yb in a graphite furnace with and without chemical modifiers (Pd, Mg, PTFE) were compared. The effect of some operation parameters such as atomization temperature and ICP power on the signal intensities and the signal profiles of Cr, Ni, Zr, Nb and Yb in ETV-ICP-MS were investigated. It was found that: (1) Pd and Mg have no obvious modification on the behavior of vaporization and atomization of Cr, Ni, Zr, Nb and Yb in the graphite furnace. (2) In the presence of PTFE, the behavior of vaporization of Cr, Ni, Zr, Nb and Yb were remarkably changed, the formation of refractory carbides were successfully circumvented, and the vaporization temperatures were decreased significantly; the signal intensities of Cr and Ni in GFAAS were enhanced in some extent, however, those of Yb, Nb and Zr were restrained greatly. It was attributed to the high bond dissociation energies of the fluorides of Yb, Nb and Zr, which caused ineffective dissociation / atomization of analytes in the graphite furnace.
新进样技术研究一直是原子光谱/质谱分析界关注的热点之一。电热蒸发(ETV),作为一种使待测物以气态形式引入ICP-AES/MS的进样技术,具有以下一些突出的优点:(1)进样效率高(～80%),方法的检出限得到显著改善;(2)试样的蒸发和激发(电离)过程分步进行,有利于实验参数的优化和降低基体产生的干扰;(3)耗样量少,微克级或微升级;(4)可直接分析固体试样,省去了样品预处理;(5)利用化学改进剂可进一步提高方法的灵敏度与选择性。
本论文的研究目的是,系统研究和发展ETV-ICP-MS联用新技术,将聚四氟乙烯(PTFE)化学改进剂(氟化剂)引入ETV-ICP-MS体系,探索降低质谱干扰和基体效应的途径,研究其规律性及机理,在此基础上,建立ETV-ICP-MS直接分析固体试样(难熔材料、生物试样)的新方法。此外,研究ETV-ICP-AES/MS与有特色的分离富集前处理技术联用,并将它用于痕量元素成分和形态分析。主要研究内容包括:
(1)建立了氟化电热蒸发(FETV)-ICP-MS直接测定难熔Nb_2O_5固体粉末中的痕量杂质的新方法,试样以悬浮体形式引入(一次分析,所需试样的量仅为0.002mg),无需任何化学前处理。对石墨炉与ICP之间的接口进行了改进,并对影响分析物信号强度的石墨炉载气和辅助载气的流速进行了优化;研究了在不同实验条件下的分析物电热蒸发信号轮廓,及悬浮体中基体总量对分析物信号的影响;用实验方法详细考察了PTFE分解产物可能产生的质谱干扰并对这一干扰的可能性进行了评价。提出了一种用实验手段判断基体效应是否存在的新方法。结果表明,应用FETV-ICP-MS直接测定痕量金属杂质,基体(Nb_2O_5)在悬浮体中的浓度不大于200mg L~(-1)时,不存在基体效应:用标准溶液工作曲线法、标准加入法及常规溶液雾化法所测定的结果一致。
(2)通过对试样的适当稀释和对石墨炉升温程序的有效控制,可以完全消除或显著降低血清试样中主要基体(有机基体和无机基体)产生的影响;详细考察了存在或不存在PTFE的条件下非金属元素Cl、S、P和金属元素Na、K、Ca、Mg在石墨炉中的挥发行为,并优化了实验参数。据此,建立了石墨炉原位分离基体后,用ETV-ICP-MS直接测定生物流体中痕量难熔元素的新方法。该法已成功应用于人血清中痕量V、Cr、Mo、Ba、La、Ce和W的同时/直接测定,无需任何化学前处理,无需基体匹配,灵敏、简单、快速及试样消耗少。
(3)以纳米二氧化钛为吸附材料,考察了在不同pH条件下,纳米二氧化钛对
Inductively coupled plasma atomic emission spectrometry / mass spectrometry (ICP-AES/MS) has several advantages for trace element determination: low detection limits, wide linear dynamic range, multi-element detection capability, and high sample throughput. Therefore, it has a widespread application in an extensive field such as life science, food science, clinical chemistry, material technology, environmental science, geological chemistry, metallurgic chemistry, and nuclear technology. And it is worthy of note that the appearance of ICP-MS is a significant breakthrough in atomic spectrometry.Electrothermal vaporization (ETV), which converts both the solution and the solid samples to the vapor state, is considered to be a useful technique of sample introduction for ICP-AES / MS over conventional pneumatic nebulization. The advantages of ETV can be described as follows: (1) high efficiency of sample introduction (~ 80%), which results in low detection limit; (2) separation processes of vaporization and excitation / ionization of analyte, which is beneficial to the optimization of experimental parameters and alleviation of interferences caused by matrix; (3) small size of sample requirement, which could be applied to the analysis of samples at micro-level; (4) capability of direct solid analysis, which reduces sample pretreatment and gives low risk of contamination and analyte loss; (5) and the sensitivity and selectivity of the method can be promoted further with the usage of chemical modifier.The objective of this dissertation is to study the vaporization behaviors of refractory / carbide forming elements in a graphite furnace with / without the use of polytetrafluoroethylene (PTFE) emulsion as chemical modifier; to explore the possibility of in-situ elimination of spectral interferences and matrix effect in the graphite furnace; and then to develop a new method of fluorination assisted electrothermal vaporization (FETV)-ICP-MS for the direct analysis of micro-amount of refractory solid powder and biological samples. For the analysis of ultra-trace elements and elemental species, some new separation / preconcentration techniques was developed and combined with ETV-ICP-MS. The main interests of this dissertation are summarized as follows:(1) A method of slurry sampling FETV-ICP-MS was developed to directly determine the trace impurities in niobium pentaoxide solid powder in which a PTFE emulsion was used as fluorinating modifier to promote the vaporization of refractory elements from a graphite furnace and to avoid the formation of thermal stable carbides. For one analysis run, only 0.002 mg of Nb_2O_5 sample was required. The electrothermal vaporizer device was connected to the ICP system by a laboratory-built interface, and the flow rates of sample carrier gas and auxiliary carrier gas were optimized experimentally. The
potentially polyatomic interferences resulting from the pyrolysates of PTFE were evaluated. A new method by stepwise diluting the sample matrix is proposed for investigating the matrix effect and the results showed that no obvious matrix effect was observed with the sample matrix (Nb2O5) concentration of less than 200 mg I/1. The proposed method has been applied to determine the trace impurities in M^Os powder, and both the results obtained from the external calibration curves and the standard addition curves were in a good agreement with those obtained by conventional nebulization ICP-MS.(2) A method of in situ removal of matrix was proposed for direct determination of the trace refractory elements in human serum by ETV-ICP-MS with the use of PTFE as fluorinating reagent. Attention has been paid to investigating the vaporization behaviors of both refractory elements of interest and matrix elements (Na, K, Ca, Mg, Cl, S, P) in a graphite furnace with the PTFE modifier presence or not. It was shown that the potential interferences of the organic and inorganic matrices in serum sample could be eliminated or reduced to a neglectable level with properly diluting the human serum and deliberately optimizing the ETV temperature program. The proposed method has been applied to the direct simultaneous determination of V, Cr, Mo, Ba, La, Ce and W in human serum.(3) Anew method for the determination of La3+ and La complexes in solution using a nanometer-sized titanium dioxide as solid-phase extractant and fiuorination assisted electrothermal vaporization (FETV)-ICP-AES as sensitive detector has been developed. The effect of pH on the adsorption characteristics of nanometer TiC>2 for La3+ and La-complexes of citric acid, 2-hydroxyisobutyric acid, and humic acid has been investigated and optimized. Based on the difference in volatility between fluorides of analyte (lanthanum) and matrix (titanium), an in-situ removal of the adsorbent matrix (TiCb) from a graphite furnace was realized. Therefore, the La3+ in solution and La-complexes absorbed on nanometer-sized titanium dioxide could be determined respectively by FETV-ICP-AES without any chemical pretreatment. The proposed method has been applied for the determination of free La3+ and La-complexes in synthetic solutions and soil extracts with satisfactory results.(4) Anew method is described for single-drop microextraction of trace rare earth elements La, Y and Yb with l-phenyl-3-methyl-4-benzoyl-5-pyrazolone (PMBP) / benzene solution as organic phase. ETV-ICP-MS was used to determine the analyte in post-extraction organic drop. Several parameters, which influence the microextraction behavior of analyte, such as sample flow rate, microdroplet volume, solvent and extraction time, were investigated and the optimized experimental conditions were established, hi order to explore the process of microextraction, the conventional pneumatic nebulization ICP-MS was used for on-line monitoring the analyte concentration change in the aqueous phase. Based on the obtained experimental results, a dynamic model for continuous-flow
microextraction of inorganic elements has been supposed. Under the selected experimental conditions, the preconcentration factors with a 25 min cycle-flow microextraction of a 1 mL sample were 233, 242 and 244 for La, Y and Yb, respectively. The proposed method was applied to the analysis of biological materials (GBW07605 Tea leaves and GBW07601 Human hair), and the results obtained were in good agreement with the certified values.(5) A procedure for copper, zinc and manganese determination in food samples by slurry sampling graphite furnace atomic absorption spectrometry (GFAAS) is proposed. The analysis results of food reference materials (NIST SRM1567, 1568) agreed with the reference value and the spiked recoveries of real samples were in the range of 95% -106%.(6) The mechanism of vaporization / atomization of Cr, Ni, Zr, Nb and Yb has been studied using ETV-ICP-MS and GFAAS. The behavior of vaporization / atomization of Cr, Ni, Zr, Nb and Yb in a graphite furnace with and without chemical modifiers (Pd, Mg, PTFE) were compared. The effect of some operation parameters such as atomization temperature and ICP power on the signal intensities and the signal profiles of Cr, Ni, Zr, Nb and Yb in ETV-ICP-MS were investigated. It was found that: (1) Pd and Mg have no obvious modification on the behavior of vaporization and atomization of Cr, Ni, Zr, Nb and Yb in the graphite furnace. (2) In the presence of PTFE, the behavior of vaporization of Cr, Ni, Zr, Nb and Yb were remarkably changed, the formation of refractory carbides were successfully circumvented, and the vaporization temperatures were decreased significantly; the signal intensities of Cr and Ni in GFAAS were enhanced in some extent, however, those of Yb, Nb and Zr were restrained greatly. It was attributed to the high bond dissociation energies of the fluorides of Yb, Nb and Zr, which caused ineffective dissociation / atomization of analytes in the graphite furnace.
引文
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