新型吸附材料的制备及其对溶液样品中痕量元素吸附性能的研究
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摘要
随着经济的快速发展，由重金属元素造成的污染与日俱增，成为影响我国人民健康水平和社会经济发展的一个重要因素。因此如何准确测定地质、生物和环境样品中的痕量元素成为分析化学中一项十分重要并具有挑战性的工作；尤其是环境水样中重金属离子的含量需做常规的监测。尽管目前仪器分析方法的大发展已经可以达到痕量甚至超痕量水平的准确度，然而对于复杂样品，由于基体效应和干扰物质的存在，直接分析仍然很困难。在分析实践中，往往需要经过样品的预处理—富集分离以后才能进行准确的测定。因此，选用选择性高、吸附容量大的各种吸附材料和运用合适的分离方法从基体中分离和预富集痕量元素显得十分必要。
本论文以建立痕量组分的富集分离及分析为目的，合成了几种新型的吸附材料，并对合成条件以及材料的选择吸附性能开展了系统研究，主要进行了以下几方面的创新性研究工作：
1．以γ-氨丙基三乙氧基硅烷(APS)为硅烷偶联剂，用乙酰水杨酸、姜黄素和氧氟沙星成功修饰了纳米SiO_2和硅胶，将合成的新型固相萃取吸附剂用来富集分离溶液中痕量Cr(Ⅲ)、Cu(Ⅱ)、Fe(Ⅲ)、Pb(Ⅱ)、Ni(Ⅱ)和Zn(Ⅱ)离子，用电感耦合等离子体原子发射光谱(ICP-AES)进行测定。详细研究了富集酸度、洗脱酸度和体积、流速、抗干扰能力、精密度和准确度等富集分离的条件和性能并建立了相应的分析方法，应用于生物样品和水样中痕量金属离子的测定，分析结果满意。
2．用谷氨酸负载活性炭，合成了新型固相萃取吸附剂，用来富集分离溶液中痕量Pb(Ⅱ)和Hg(Ⅱ)离子，用ICP-AES进行测定。详细研究了富集分离的条件和性能并建立了相应的分析方法，应用于水样中痕量金属离子的测定，分析结果满意。
3．应用硅胶表面修饰技术，首次将Pb(Ⅱ)作为印迹离子合成了Pb(Ⅱ)印迹聚合物，研究了离子印迹聚合物和非印迹聚合物对Pb(Ⅱ)的分离富集特性，建立了分离富集测定Pb(Ⅱ)的新方法。对照了印迹聚合物和非印迹聚合物对模板离子的吸附选择性，结果表明印迹聚合物对模板离子具有较高的亲和性和选择吸附性能。
4．以N，N′-二环己基碳二亚胺为缩合剂，用二乙烯三胺成功修饰了多壁碳纳米管，将其用来富集分离溶液中的Cr(Ⅲ)、Fe(Ⅲ)、Mn(Ⅱ)和Pb(Ⅱ)离子，用ICP-AES进行测定，详细研究了富集分离的条件和性能并建立了相应的分析方法，应用于水样中痕量金属离子的测定，分析结果满意。
With the rapid development of economy, the pollution caused by heavy metalsbecomes more severe, which is also a dominant factor for jeopardizing the publichealth and preventing social economical development of our country. The accuratedetermination of trace element in geological, biological and environmental samples isan important and challenging task in analytical chemistry; especially heavy metals areoften routinely monitored in environmental water. Although many instrument analysismethods have been developed recently and reached trace level or super trace levelsensitivity, the direct analysis is still difficult because of the high complexity ofsamples and severe interference caused by matrix effects. For this reason, thepreliminary separation and preconcentration of trace elements from matrix using highselectivity and adsorption capacity with suitable method is often required.
In this research paper, several new adsorption materials are synthesized in orderto pre-concentration and separation of trace components. Their adsorption andselectivity characteristics for trace components have been investigated systematically.The more detailed novelty of this research can be categorized as following:
1. Nanometer SiO_2 and silica gel was modified with acetylsalicylic acid (aspirin),curcnmin and ofloxacin under the silane coupling agent (APS) and used forpreconcentration and separation of trace amounts of Cr(Ⅲ), Cu(Ⅱ), Fe(Ⅲ), Pb(Ⅱ),Ni(Ⅱ) and Zn(Ⅱ) from solution samples prior to their determination by inductivelycoupled plasma optical emission spectrometry (ICP-AES). The separation/preconcentration conditions of analytes, which include the effects of the pH, thesample flow rate and volume, the elution condition, detection limits and precision andthe interfering ions on the recovery of the analytes were investigated in detail. Theaccuracy of the proposed each method was checked by analyzing standard referencematerial with satisfactory results.
2. The new adsorbent was prepared using glutamic acid (GA) impregnatedactivated carbon (AC) followed by activating agent of NaOH. The modified activatedcarbon with glutamic acid (AC-GA) was used as an adsorbent for the solid-phaseextraction (SPE) of trace amounts of Pb(Ⅱ) and Hg(Ⅱ) from solution samples prior totheir determination by inductively coupled plasma optical emission spectrometry (ICP-AES). The separation/pre-concentration conditions of analytes were investigatedin detail. This sorbent was used in analysis of water samples and the results aresatisfactory.
3. The imprinted and non-imprinted polymers for Pb(Ⅱ) were obtained by a surfaceimprinting technique for selective solid-phase extraction (SPE) of Pb(Ⅱ) and prior toits determination by ICP-AES. The separation/pre-concentration conditions ofanalytes were investigated in detail with reliable and satisfactory results. The substrateselectivity of imprinted polymer and non-imprinted polymer was investigated. Theresults showed that the imprinted polymer exhibited much higher affinity for Pb(Ⅱ).
4. Multi-wall carbon nanotubes were modified with diethylenetriamine(DETA)under the condensation agent of N,N'-dicyclohexylcarbodiimide and used forpreconcentration and separation of trace amounts of Cr(Ⅲ), Fe(Ⅲ), Pb(Ⅱ) and Mn(Ⅱ)from solution samples prior to their determination by inductively coupled plasmaoptical emission spectrometry (ICP-AES). The separation/preconcentration conditionsof analytes were investigated in detail. This sorbent was used in analysis of watersamples and the results are satisfactory.
本论文以建立痕量组分的富集分离及分析为目的，合成了几种新型的吸附材料，并对合成条件以及材料的选择吸附性能开展了系统研究，主要进行了以下几方面的创新性研究工作：
1．以γ-氨丙基三乙氧基硅烷(APS)为硅烷偶联剂，用乙酰水杨酸、姜黄素和氧氟沙星成功修饰了纳米SiO_2和硅胶，将合成的新型固相萃取吸附剂用来富集分离溶液中痕量Cr(Ⅲ)、Cu(Ⅱ)、Fe(Ⅲ)、Pb(Ⅱ)、Ni(Ⅱ)和Zn(Ⅱ)离子，用电感耦合等离子体原子发射光谱(ICP-AES)进行测定。详细研究了富集酸度、洗脱酸度和体积、流速、抗干扰能力、精密度和准确度等富集分离的条件和性能并建立了相应的分析方法，应用于生物样品和水样中痕量金属离子的测定，分析结果满意。
2．用谷氨酸负载活性炭，合成了新型固相萃取吸附剂，用来富集分离溶液中痕量Pb(Ⅱ)和Hg(Ⅱ)离子，用ICP-AES进行测定。详细研究了富集分离的条件和性能并建立了相应的分析方法，应用于水样中痕量金属离子的测定，分析结果满意。
3．应用硅胶表面修饰技术，首次将Pb(Ⅱ)作为印迹离子合成了Pb(Ⅱ)印迹聚合物，研究了离子印迹聚合物和非印迹聚合物对Pb(Ⅱ)的分离富集特性，建立了分离富集测定Pb(Ⅱ)的新方法。对照了印迹聚合物和非印迹聚合物对模板离子的吸附选择性，结果表明印迹聚合物对模板离子具有较高的亲和性和选择吸附性能。
4．以N，N′-二环己基碳二亚胺为缩合剂，用二乙烯三胺成功修饰了多壁碳纳米管，将其用来富集分离溶液中的Cr(Ⅲ)、Fe(Ⅲ)、Mn(Ⅱ)和Pb(Ⅱ)离子，用ICP-AES进行测定，详细研究了富集分离的条件和性能并建立了相应的分析方法，应用于水样中痕量金属离子的测定，分析结果满意。
With the rapid development of economy, the pollution caused by heavy metalsbecomes more severe, which is also a dominant factor for jeopardizing the publichealth and preventing social economical development of our country. The accuratedetermination of trace element in geological, biological and environmental samples isan important and challenging task in analytical chemistry; especially heavy metals areoften routinely monitored in environmental water. Although many instrument analysismethods have been developed recently and reached trace level or super trace levelsensitivity, the direct analysis is still difficult because of the high complexity ofsamples and severe interference caused by matrix effects. For this reason, thepreliminary separation and preconcentration of trace elements from matrix using highselectivity and adsorption capacity with suitable method is often required.
In this research paper, several new adsorption materials are synthesized in orderto pre-concentration and separation of trace components. Their adsorption andselectivity characteristics for trace components have been investigated systematically.The more detailed novelty of this research can be categorized as following:
1. Nanometer SiO_2 and silica gel was modified with acetylsalicylic acid (aspirin),curcnmin and ofloxacin under the silane coupling agent (APS) and used forpreconcentration and separation of trace amounts of Cr(Ⅲ), Cu(Ⅱ), Fe(Ⅲ), Pb(Ⅱ),Ni(Ⅱ) and Zn(Ⅱ) from solution samples prior to their determination by inductivelycoupled plasma optical emission spectrometry (ICP-AES). The separation/preconcentration conditions of analytes, which include the effects of the pH, thesample flow rate and volume, the elution condition, detection limits and precision andthe interfering ions on the recovery of the analytes were investigated in detail. Theaccuracy of the proposed each method was checked by analyzing standard referencematerial with satisfactory results.
2. The new adsorbent was prepared using glutamic acid (GA) impregnatedactivated carbon (AC) followed by activating agent of NaOH. The modified activatedcarbon with glutamic acid (AC-GA) was used as an adsorbent for the solid-phaseextraction (SPE) of trace amounts of Pb(Ⅱ) and Hg(Ⅱ) from solution samples prior totheir determination by inductively coupled plasma optical emission spectrometry (ICP-AES). The separation/pre-concentration conditions of analytes were investigatedin detail. This sorbent was used in analysis of water samples and the results aresatisfactory.
3. The imprinted and non-imprinted polymers for Pb(Ⅱ) were obtained by a surfaceimprinting technique for selective solid-phase extraction (SPE) of Pb(Ⅱ) and prior toits determination by ICP-AES. The separation/pre-concentration conditions ofanalytes were investigated in detail with reliable and satisfactory results. The substrateselectivity of imprinted polymer and non-imprinted polymer was investigated. Theresults showed that the imprinted polymer exhibited much higher affinity for Pb(Ⅱ).
4. Multi-wall carbon nanotubes were modified with diethylenetriamine(DETA)under the condensation agent of N,N'-dicyclohexylcarbodiimide and used forpreconcentration and separation of trace amounts of Cr(Ⅲ), Fe(Ⅲ), Pb(Ⅱ) and Mn(Ⅱ)from solution samples prior to their determination by inductively coupled plasmaoptical emission spectrometry (ICP-AES). The separation/preconcentration conditionsof analytes were investigated in detail. This sorbent was used in analysis of watersamples and the results are satisfactory.
引文
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