室温离子液体在过渡金属及贵金属化学蒸气发生中的应用
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摘要
室温离子液体(Room Temperature Ionic Liquids,RTILs)是一类新型的绿色溶剂,具有许多独特的性质,如液态温度范围宽且具有良好的物理和化学稳定性、不易挥发、对很多无机和有机物质都具有良好的溶解能力、极性可调、电化学稳定性高且具有较高的电导率和较宽的电化学窗口。因此,RTILs在化学和材料科学等诸多领域得到了广泛的应用。在分析化学领域,RTILs已成功地应用于色谱和毛细管电泳的分离介质、萃取溶剂、化学传感介质、基质辅助激光解吸质谱的辅助基质、电化学电解质、荧光光谱和拉曼光谱分析的溶剂。本论文旨在探讨RTILs对过渡金属和贵金属的化学蒸气发生(Chemica VaporGeneration,CVG)的增感作用及其机理,主要内容和创新点如下:
(1)发现了RTILs对过渡金属和贵金属的CVG的增感效应,并采用流动注射(Flow Injection,FI)与原子荧光光谱(Atomic Fluorescence Spectrometry,AFS)联用技术对其增感效应进行了研究。结果表明N-丁基-吡啶四氟硼酸盐([C_4Py][BF_4])不仅使Cu、Ag和Au的CVG效率分别提高了4.8、2.7和3.6倍,而且在一定程度上降低了Zn~(2+)、Fe~(3+)、Co~(2+)、Ni~(2+)、Pb~(2)、Se~Ⅳ和As~Ⅲ对Cu、Ag和Au测定的干扰。据此,发展了以[C_4Py][BF_4]为增感剂的FI-CVG-AFS技术测定痕量Cu、Ag和Au的新方法。在进样量为0.5mL条件下,此方法测定Cu、Ag和Au的检出限分别为19、15和6.3μg L~(-1)。连续11次测定50μg L~(-1)的Cu、Ag和Au的相对标准偏差分别为4.4%、5.2%和4.7%。此方法已成功地应用于六种标准参考物中痕量Cu、Ag和Au含量的测定。
(2)比较系统地研究了八种RTILs对Au的CVG的增感效应,并对其增感机理进行了探讨。这八种RTILs包括[C_4Py][BF_4]、N-丁基吡啶溴盐[C_4Py]Br、1-十六烷基-3-甲基咪唑氯盐[C_(16)mim]Cl、溴化四丁基季铵盐[N_(4444)]Br、1-丁基-3.甲基咪唑溴盐[C_4mim]Br、1-乙基-3-甲基咪唑溴盐[C_2mim]Br、1-痘?3-甲基咪唑四氟硼酸盐[C_4mim][BF_4]和四丁基季铵四氟硼酸盐[N_(4444)][BF_4]。所有这些RTILs均对Au的CVG-AFS检测有增感作用,增感倍数为3～24不等。RTILs的增感效果与其所含阴阳离子的本质有关。含有短链烷基的阳离子的RTILs的增感效果较好,而阳离子的烷基链较长或支链较多的RTILs增感效果不佳。对于含有相同阳离子的RTILs来说,阴离子为Br~-时增感效果最明显。我们认为RTILs的增感机理可能为:RTILs的阳离子与溶液中Au的阴离子通过静电作用形成离子对,而含Br~-的RTILs还会导致Br~-取代[AuCl_4]~-中的Cl~-,以上过程可能改变了参加CVG反应的Au的前驱体的形成,从而改善了Au参加CVG反应的效率;另一方面,RTILs改变了CVG反应环境的物理性质,反应中会产生很多细小均匀的气泡,可以将气态产物与其它物质隔离开而消除它们带来的干扰。结果表明在所研究的RTILs中,[C_4mim]Br的增感效果最佳。据此,发展了以[C_4mim]Br为增感剂的FI-CVG-AFS技术测定Au的新方法。在进样量为0.5 mL条件下,Au的检出限为1.9μg L~(-1)。连续11次测定50μg L~(-1) Au的相对标准偏差为3.1%。此方法已成功地应用于两种标准参考物中痕量Au含量的测定。
(3)发现并详细研究了[C_4mim]Br和二乙基二硫代氨基甲酸钠(DDTC)对以硼氢酸盐为还原剂的Ni的CVG的协同增感效应。结果表明0.02%DDTC和25 mmol L~(-1)[C_4mim]Br共存使FI-CVG-AFS测定Ni的灵敏度提高2400倍。据此,发展了以0.02%DDTC和25 mmol L~(-1)[C_4mim]Br为协同增感剂的FI-CVG-AFS技术测定痕量Ni的新方法。与传统的羰基镍发生的方法相比,此方法不仅毒性低,而且更加有效。在进样量为0.5 mL条件下,Ni的检出限为0.65μg L~(-1)。样品通量为180 h~(-1),连续11次测定20μg L~(-1)Ni的相对标准偏差为3.4%。此方法已成功地应用于四种标准参考物中痕量Ni含量的测定。
Room-temperature ionic liquids(RTILs) have tremendous applications in various fields of chemistry due to their unique properties,such as negligible vapor pressure,good thermal stability,tunable viscosity,miscibility with water and organic solvents,and good extractability for various organic compounds and metal ions. Analytical applications of RTILs are also intriguing regarding the fact that they can be easily handled and used in wide variety of environments.There is a great deal of research on RTIL application as separation media for chromatography and capillary electrophoresis,solvents for extractions,sensing materials for chemosensing, matrices for MALDI-MS,electrolytes for electrochemistry and also as solvents for analytical spectroscopy,such as near infrared spectroscopy,fluorescence spectrometry and Raman spectroscopy.In this dissertation the exploitation of RTILs for the chemical vapor generation(CVG) of transition and noble metals,the mechanism of the enhancement effect of RTILs,and its application to flow injection-CVG-atomic fluorescence spectrometry(FI-CVG-AFS) for the determination of trace Au,Cu,Ag,and Ni are described.
We report the first application of an RTIL in the CVG of transition and noble metals following reduction of acidified analyte solution with KBH_4.Copper,silver and gold were selected as model analytes,and N-butylpyridinium tetrafluoroborate ([C_4Py][BF_4]) was used as a model RTIL.The RTIL-enhanced CVG of copper,silver and gold was evaluated by FI-CVG-AFS.The addition of[C_4Py][BF_4]leads to a 4.8-, 2.7- and 3.6-times improvement in the CVG efficiencies for copper,silver and gold, respectively.Interference from Zn~(2+),Fe~(3+),Co~(2+),Ni~(2+),Pb~(2+),Se~Ⅳand As~Ⅲwas also reduced in the presence of[C_4Py][BF_4].The role of the RTIL was supposed to be inhibition of further coalescence of the metal nanoparticles which may constitute the volatile metal species leaving the solution and/or reaching the atomizer,and hence prevention of the loss of volatile metal species.With the consumption of a 0.5 mL sample solution,the detection limits(3σ) for Cu,Ag and Au are 19,15 and 6.3μg L~(-1), respectively.The precisions(RSD,n=11) for eleven replicate measurements of the standard solution containing 50μg L~(-1) Cu,Ag and Au were 4.4%,5.2%and 4.7%, respectively.The developed RTIL-enhanced FI-CVG-AFS method was successfully applied to determination of trace Cu,Ag and Au in several certified biological and geological reference materials.
To get insight into the mechanism of the effect of RTILs on the CVG of noble metals,gold was taken as a model element,and eight RTILs were examined. FI-CVG-AFS was selected for detecting Au,and UV-vis spectrophotometry was used to elucidate the interactions of RTILs and the analyte.The RTILs involved include [C_4Py][BF_4],[C_4Py]Br,[C_(16)mim]Cl,[N_(4444)]Br,[C_4mim]Br,[C_2mim]Br,[C_4mim][BF_4] and[N_(4444)][BF_4].All the RTILs resulted in 3-24 times improvement in sensitivity for Au,depending on their nature.For the RTILs with identical anion,the RTILs with the cations of short chain exhibited better enhancement effect than those with long alkyl chain length or complex branch chain.For the RTILs with identical cation,the RTILs with Br~- gave the best enhancement effect.The formation of ion pairs between the cation of RTILs and the anion species of gold via electrostatic interaction,and/or the substitution of the Cl~- in the anion species of gold by the anion of RTILs likely enabled amore effective CVG reaction to occur.The RTILs also facilitated the generation of small bubbles and provided an electrostatic stabilization to protect the unstable volatile gold species and to help fast isolation of volatile gold species from the reaction mixture.[C_4mim]Br gave the best improvement in the sensitivity(24 times) among the RTILs studied,and also reduced the interferences from common transition and other noble metals.Based on the enhancement effect of[C_4mim]Br,a novel FI-CVG-AFS a detection limit(3σ) of 1.9μg L~(-1) and a precision of 3.1%(50μg L~(-1),RSD,n=11) was developed for the determination of trace gold in geological samples.
RTIL in combination with sodium diethyldithiocarbamate(DDTC) were used to synergetically improve the CVG of nickel.Volatile species of nickel were effectively generated through reduction of acidified analyte solution with KBH_4 in the presence of 0.02%DDTC and 25 mmol L~(-1)[C_4mim]Br at room temperature.Thus,a new FI-CVG-AFS method was developed for determination of nickel.The combination of [C_4mim]Br with DDTC gave an enhancement factor of 2400.With consumption of 0.5 mL sample solution,a detection limit of 0.65μg L~(-1)(3σ) and a sampling frequency of 180 h~(-1) were obtained.The relative standard deviation for eleven replicate determinations of 20μg L~(-1) Ni was 3.4%.The developed FI-CVG-AFS method was successfully applied to determination of trace Ni in several certified biological reference materials.
(1)发现了RTILs对过渡金属和贵金属的CVG的增感效应,并采用流动注射(Flow Injection,FI)与原子荧光光谱(Atomic Fluorescence Spectrometry,AFS)联用技术对其增感效应进行了研究。结果表明N-丁基-吡啶四氟硼酸盐([C_4Py][BF_4])不仅使Cu、Ag和Au的CVG效率分别提高了4.8、2.7和3.6倍,而且在一定程度上降低了Zn~(2+)、Fe~(3+)、Co~(2+)、Ni~(2+)、Pb~(2)、Se~Ⅳ和As~Ⅲ对Cu、Ag和Au测定的干扰。据此,发展了以[C_4Py][BF_4]为增感剂的FI-CVG-AFS技术测定痕量Cu、Ag和Au的新方法。在进样量为0.5mL条件下,此方法测定Cu、Ag和Au的检出限分别为19、15和6.3μg L~(-1)。连续11次测定50μg L~(-1)的Cu、Ag和Au的相对标准偏差分别为4.4%、5.2%和4.7%。此方法已成功地应用于六种标准参考物中痕量Cu、Ag和Au含量的测定。
(2)比较系统地研究了八种RTILs对Au的CVG的增感效应,并对其增感机理进行了探讨。这八种RTILs包括[C_4Py][BF_4]、N-丁基吡啶溴盐[C_4Py]Br、1-十六烷基-3-甲基咪唑氯盐[C_(16)mim]Cl、溴化四丁基季铵盐[N_(4444)]Br、1-丁基-3.甲基咪唑溴盐[C_4mim]Br、1-乙基-3-甲基咪唑溴盐[C_2mim]Br、1-痘?3-甲基咪唑四氟硼酸盐[C_4mim][BF_4]和四丁基季铵四氟硼酸盐[N_(4444)][BF_4]。所有这些RTILs均对Au的CVG-AFS检测有增感作用,增感倍数为3～24不等。RTILs的增感效果与其所含阴阳离子的本质有关。含有短链烷基的阳离子的RTILs的增感效果较好,而阳离子的烷基链较长或支链较多的RTILs增感效果不佳。对于含有相同阳离子的RTILs来说,阴离子为Br~-时增感效果最明显。我们认为RTILs的增感机理可能为:RTILs的阳离子与溶液中Au的阴离子通过静电作用形成离子对,而含Br~-的RTILs还会导致Br~-取代[AuCl_4]~-中的Cl~-,以上过程可能改变了参加CVG反应的Au的前驱体的形成,从而改善了Au参加CVG反应的效率;另一方面,RTILs改变了CVG反应环境的物理性质,反应中会产生很多细小均匀的气泡,可以将气态产物与其它物质隔离开而消除它们带来的干扰。结果表明在所研究的RTILs中,[C_4mim]Br的增感效果最佳。据此,发展了以[C_4mim]Br为增感剂的FI-CVG-AFS技术测定Au的新方法。在进样量为0.5 mL条件下,Au的检出限为1.9μg L~(-1)。连续11次测定50μg L~(-1) Au的相对标准偏差为3.1%。此方法已成功地应用于两种标准参考物中痕量Au含量的测定。
(3)发现并详细研究了[C_4mim]Br和二乙基二硫代氨基甲酸钠(DDTC)对以硼氢酸盐为还原剂的Ni的CVG的协同增感效应。结果表明0.02%DDTC和25 mmol L~(-1)[C_4mim]Br共存使FI-CVG-AFS测定Ni的灵敏度提高2400倍。据此,发展了以0.02%DDTC和25 mmol L~(-1)[C_4mim]Br为协同增感剂的FI-CVG-AFS技术测定痕量Ni的新方法。与传统的羰基镍发生的方法相比,此方法不仅毒性低,而且更加有效。在进样量为0.5 mL条件下,Ni的检出限为0.65μg L~(-1)。样品通量为180 h~(-1),连续11次测定20μg L~(-1)Ni的相对标准偏差为3.4%。此方法已成功地应用于四种标准参考物中痕量Ni含量的测定。
Room-temperature ionic liquids(RTILs) have tremendous applications in various fields of chemistry due to their unique properties,such as negligible vapor pressure,good thermal stability,tunable viscosity,miscibility with water and organic solvents,and good extractability for various organic compounds and metal ions. Analytical applications of RTILs are also intriguing regarding the fact that they can be easily handled and used in wide variety of environments.There is a great deal of research on RTIL application as separation media for chromatography and capillary electrophoresis,solvents for extractions,sensing materials for chemosensing, matrices for MALDI-MS,electrolytes for electrochemistry and also as solvents for analytical spectroscopy,such as near infrared spectroscopy,fluorescence spectrometry and Raman spectroscopy.In this dissertation the exploitation of RTILs for the chemical vapor generation(CVG) of transition and noble metals,the mechanism of the enhancement effect of RTILs,and its application to flow injection-CVG-atomic fluorescence spectrometry(FI-CVG-AFS) for the determination of trace Au,Cu,Ag,and Ni are described.
We report the first application of an RTIL in the CVG of transition and noble metals following reduction of acidified analyte solution with KBH_4.Copper,silver and gold were selected as model analytes,and N-butylpyridinium tetrafluoroborate ([C_4Py][BF_4]) was used as a model RTIL.The RTIL-enhanced CVG of copper,silver and gold was evaluated by FI-CVG-AFS.The addition of[C_4Py][BF_4]leads to a 4.8-, 2.7- and 3.6-times improvement in the CVG efficiencies for copper,silver and gold, respectively.Interference from Zn~(2+),Fe~(3+),Co~(2+),Ni~(2+),Pb~(2+),Se~Ⅳand As~Ⅲwas also reduced in the presence of[C_4Py][BF_4].The role of the RTIL was supposed to be inhibition of further coalescence of the metal nanoparticles which may constitute the volatile metal species leaving the solution and/or reaching the atomizer,and hence prevention of the loss of volatile metal species.With the consumption of a 0.5 mL sample solution,the detection limits(3σ) for Cu,Ag and Au are 19,15 and 6.3μg L~(-1), respectively.The precisions(RSD,n=11) for eleven replicate measurements of the standard solution containing 50μg L~(-1) Cu,Ag and Au were 4.4%,5.2%and 4.7%, respectively.The developed RTIL-enhanced FI-CVG-AFS method was successfully applied to determination of trace Cu,Ag and Au in several certified biological and geological reference materials.
To get insight into the mechanism of the effect of RTILs on the CVG of noble metals,gold was taken as a model element,and eight RTILs were examined. FI-CVG-AFS was selected for detecting Au,and UV-vis spectrophotometry was used to elucidate the interactions of RTILs and the analyte.The RTILs involved include [C_4Py][BF_4],[C_4Py]Br,[C_(16)mim]Cl,[N_(4444)]Br,[C_4mim]Br,[C_2mim]Br,[C_4mim][BF_4] and[N_(4444)][BF_4].All the RTILs resulted in 3-24 times improvement in sensitivity for Au,depending on their nature.For the RTILs with identical anion,the RTILs with the cations of short chain exhibited better enhancement effect than those with long alkyl chain length or complex branch chain.For the RTILs with identical cation,the RTILs with Br~- gave the best enhancement effect.The formation of ion pairs between the cation of RTILs and the anion species of gold via electrostatic interaction,and/or the substitution of the Cl~- in the anion species of gold by the anion of RTILs likely enabled amore effective CVG reaction to occur.The RTILs also facilitated the generation of small bubbles and provided an electrostatic stabilization to protect the unstable volatile gold species and to help fast isolation of volatile gold species from the reaction mixture.[C_4mim]Br gave the best improvement in the sensitivity(24 times) among the RTILs studied,and also reduced the interferences from common transition and other noble metals.Based on the enhancement effect of[C_4mim]Br,a novel FI-CVG-AFS a detection limit(3σ) of 1.9μg L~(-1) and a precision of 3.1%(50μg L~(-1),RSD,n=11) was developed for the determination of trace gold in geological samples.
RTIL in combination with sodium diethyldithiocarbamate(DDTC) were used to synergetically improve the CVG of nickel.Volatile species of nickel were effectively generated through reduction of acidified analyte solution with KBH_4 in the presence of 0.02%DDTC and 25 mmol L~(-1)[C_4mim]Br at room temperature.Thus,a new FI-CVG-AFS method was developed for determination of nickel.The combination of [C_4mim]Br with DDTC gave an enhancement factor of 2400.With consumption of 0.5 mL sample solution,a detection limit of 0.65μg L~(-1)(3σ) and a sampling frequency of 180 h~(-1) were obtained.The relative standard deviation for eleven replicate determinations of 20μg L~(-1) Ni was 3.4%.The developed FI-CVG-AFS method was successfully applied to determination of trace Ni in several certified biological reference materials.
引文
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