共查询到19条相似文献,搜索用时 140 毫秒
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采用正交设计实验方法,研究了从环境模拟样品中超临界流体萃取多环芳烃的最佳萃取条件。着重考察了超临界流体的压力、温度和用量等对萃取效率的影响。 相似文献
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采用正交设计实验方法,研究了从环境模拟样品中超临界流体萃取(SFE)多环芳烃(PAH)的最佳萃取条件。着重考察了超临界流体的压力、温度和用量等对萃取效率的影响。结果表明,压力的影响居第一位,温度影响次之,超临界CO2的用量的影响居第三位。建立了选择超临界流体萃取条件的简单方法 相似文献
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固体和液体中的金属离子能在含有有机螯合剂的超临界二氧化碳(SC-CO2)流体中被有效地萃取出来。超临界流体萃取(SFE)金属离子的效率取决于下列因素:螯合剂在SC-CO2中的稳定性和溶解性、金属络合物在SC-CO2中的溶解度、水、pH值、压力、温度及金属离子的化学形式和基质的性质等。 相似文献
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土壤中烃类污染物的超临界流体萃取 总被引:7,自引:0,他引:7
采用超临界流体萃取技术提取环境样品中的烃类污染物,以色谱-质谱联用仪测定了萃取物的化学成分,考察了影响萃取效率的主要因素。比传统的索氏萃取能更有效地从复杂环境样品中萃取分析物。 相似文献
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金属检测中新型前处理技术研究进展及应用 总被引:1,自引:0,他引:1
精准检测环境和食品中金属含量对环境保护和人体健康至关重要.样品的准备环节是造成样品损失和二次污染的关键步骤, 因此合适的前处理方法可以提高金属分析的选择性和灵敏度.从液相萃取和非液相萃取新技术两方面综述了浊点萃取、离子液体、超分子溶剂-分散液液微萃取、顶空固相微萃取技术、超临界流体萃取特点及在复杂样品前处理中的应用和研究进展, 并对其未来发展方向进行了展望. 相似文献
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综述高效液相色谱样品处理技术.液–液萃取在常温常压下开展,处理能力强,回收率高;固相萃取所需样品量少,耗费溶剂少,操作简单,重复性好;固相微萃取在固相萃取的基础上,简化样品制备与分析过程;微波辅助萃取则利用高频电磁波的穿透和电磁场作用缩短萃取时间,提高萃取效率;超临界流体萃取凭借超临界流体萃取剂的惰性、低毒、纯净、无残留,实现样品处理的高效、环保、节能;加速溶剂萃取通过提高温度和增大压力,提升萃取效率,减少溶剂用量;浊点萃取利用加入表面活性剂后产生的增溶和浊点现象实现提取,安全低毒,操作简便,富集倍数高.这些前处理技术在食品、药品、环境、生物等领域得到了广泛的应用.在保证待测组分选择性好、回收率高的前提下,使用绿色、环保、经济的设备及试剂减少引入误差、简化处理过程、提高处理效率是现代高效液相色谱分析样品处理技术的发展方向. 相似文献
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The use of four dithiocarbamates and three fluorinated β-diketones as potential chelating agents for three transition metal ions (Cd2+, Pb2+, and Hg2+) extracted from spiked sand and filter paper samples by supercritical fluid extraction (SFE) was investigated. The extractions were performed at 45°C and 250 atm for spiked sand samples and at 60°C and 200 atm for filter paper samples using supercritical carbon dioxide modified with 5% methanol. At 250 atm and using carbon dioxide modified with 5% methanol, the recoveries of Cd2+, Pb2+, and Hg2+ ions from spiked sand samples were 95% with lithium bis(trifluoroethyl)dithiocarbamate (LiFDDC) as the chelating agent; they ranged from 83–97% with diethylammonium diethyldithiocarbamate and from 87–97% with sodium di-ethyldithiocarbamate as chelating agents, and from 68–96% with trifluoracetylacetone, hexafluoroacetylacetone, and thenoylfluoroacetone as chelating agents. Ammonium pyrrolidinedithiocarbamate was not effective in the chelation SFE of Cd2+, Pb2+, and Hg2+ ions from either spiked sand or spiked filter paper samples under the extraction conditions used. Supercritical carbon dioxide alone gave consistently lower analyte recoveries than supercritical carbon dioxide modified with 5% methanol. The results suggest that the solubility of the metal chelate in the supercritical fluid plays a more important role than the solubility of the chelating agent in the supercritical fluid, as long as sufficient chelating agent is present in the fluid phase. Fluorination of the chelating agent, as in the case of LiFDDC, increases the solubility of the metal chelate, and subsequently enhances the extraction efficiency for the metal ions. 相似文献
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J.D. Glennon S. Hutchinson A. Walker S.J. Harris C.C. McSweeney 《Journal of chromatography. A》1997,770(1-2):85-91
Research to date on the supercritical fluid extraction (SFE) of metal ions has focused on the use of dithiocarbamates and β-diketones. Hydroxamic acids are well known as effective chelating agents for a broad range of transition metal ions. Much attention has centred in inorganic chemistry on the effect of N-substitution on metal chelate stability and selectivity, and in analytical chemistry on the immobilisation of the chelating agents to the chosen solid supports such as silica. In this paper, the synthesis of selected fluorinated mono hydroxamic acids and their N-substituted derivatives is reported. The new reagents are applied in the SFE of metal ions in particular Fe(III) using unmodified supercritical CO2. Metal extraction is monitored using atomic absorption spectroscopy and visible spectrophotometry. The extraction efficiencies were determined as a function of pressure and temperature. The new ligands synthesised and applied were perfluorooctanohydroxamic acid (PFOHA), heptafluorobutyrichydroxamic acid (HFBHA) and their N-methylhydroxamic acid derivatives. Of the synthesised reagents, PFOHA was the most soluble and effective extractant of Fe(III) from spiked filter paper, reaching 97% extraction of the metal ion under optimised conditions. The selectivity of this ligand for Fe(III) in the presence of Cu(II), Ni(II), Pb(II) and Zn(II) is also demonstrated. 相似文献
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Extraction of heavy metal ions from solid matrix by means of an incorporation of chelating agents with supercritical carbon dioxide(scCO2) was investigated experimentally. Four commercially available chelating agents, diethylammonium diethyldithiocarbamate(Et2NH2DDC), trifluoroacetylacetone(TFA), hexafluoroacetylacetone(HFA) and thenoyltrifluoroacetone(TTA) were tested. The extraction experiments were conducted at 50 °C and 1.39×107― 2.80×107 Pa. According to the experimental results, for the extraction of Cu2+, all the chelating agents investigated here are effective. For other metal ions, such as Pb2+, Ni2+ and Cd2+, Et2NH2DDC exhibited a better extraction result, while other chelating agents were less effective. This investigation is expected to provide a tentative evaluation on the scCO2-based metal extraction from solid media. 相似文献
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Wendy C. Andersen 《Analytica chimica acta》2003,485(1):1-8
Supercritical fluid extraction (SFE) of aqueous solutions is often limited by poor mass transport. The performance of a new gas-liquid entraining device was investigated to improve mass transport and thereby increase extraction efficiency. As a test system, iron(III) was extracted from water with a β-diketone chelating agent (HL) and supercritical fluid carbon dioxide. Metal β-diketonate complexes with sufficient solubility in supercritical fluid CO2 are often poorly extracted from aqueous solutions due to limited mass transport between the water-soluble metal ion and the CO2-soluble chelating agent. The new entraining device maximizes contact between the ligand-rich CO2 phase and the metal ion-rich aqueous phase. Iron(III) was extracted from water with the chelating agent 2,2,7-trimethyl-3,5-octanedione (H(tod)) and supercritical fluid CO2 at 60 °C and 20.8 MPa. With entrainment, 79% of the iron was removed from the aqueous phase. This represents a three-fold increase in iron extraction efficiency over that of a static system. 相似文献
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4,4'-Bis(dihexylaminocarbonyl)-2,2'-bipyridine (BDC-Bipy) was synthesized and studied systematically as a chelating reagent for metal ions extraction in supercritical CO(2). The compound showed high extraction efficiency for Co(2+) (100%), Cu(2+) (100%), Cd(2+) (98.2%), and Zn(2+) (100%) ions and good extraction efficiency for Sr(2+) (79.4%) and Pb(2+) (89.8%) when the extraction was performed in supercritical CO(2) at 313 K and 25 MPa with the system of BDC-Bipy, deionized water and perfluoro-1-octanesulfonic acid tetraethylammonium salt. The recoveries of mixed metal ions were also measured; unfortunately, the system of extraction has no selectivity for the metal ions. 相似文献
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Metal Ions Extraction with Glucose Derivatives as Chelating Reagents in Supercritical Carbon Dioxide
Guo Chen YANG Hai Jian YANG 《中国化学快报》2006,17(11):1489-1492
A series of glucose derivatives have been used as chelating reagents to extract metal ions in supercritical carbon dioxide. With perfluoro-1-octanesulfonic acid tetraethylammonium salt as additive, glucose derivatives were selective for Sr2 and Pb2 extraction in supercritical carbon dioxide. 相似文献