【摘要】 详细研究了以大孔硅胶为基质,一步合成8羟-基喹啉(8-HQ)型金属螯合色谱填料的方法,采用正交试验对合成方法进行了优化。与传统合成方法所得的填料进行了比较,从理化指标等方面来看,新的合成方法为佳。将该法用作微柱流动注射(FIA)在线分离、富集和电感耦合等离子体质谱(ICP-MS)分析流程中的固定相,对大洋海水中的痕量铅进行了在线分析,得到了较满意的结果。更多还原

【Abstract】 A new method for the synthesis of 8-hydroxyquinoline（8-HQ） bonded silica（SHQ） for metal chelation applications has been developed.The new synthetic route has been compared with the conventional one reported in the literature in terms of reaction yield,product performance and operational ease.The new method is based on a one-step Mannich reaction,and an orthogonal experimental design has been used for process optimization.The 8-HQ bonded silica product obtained has been characterized by diffuse reflectance infrared Fourier transform（DRIFT） spectroscopy,and the presence of a strong absorption band of the phenol-OH near 1380 cm^-1 indicates the successful bonding of 8-HQ on silica surface.The concentration of 8-HQ bonded to the silica surface quantified by ultroaviolet-visible spectroscopy is 542 μmol/g,much higher than the product obtained by the conventional synthetic route,which is 117 μmol/g.The dynamic binding capacities of the two SHQs towards copper（Ⅱ） has been measured and compared by inductively coupled plasma mass spectrometry（ICP-MS）,and the results are 347 μmol/g for the new SHQ and 76 μmol/g for the（conventional） one.The results demonstrate that the new method is not only simpler and more convenient operationally,but also produced product with better performance.The SHQ synthesized has been used for（measuring） trace lead in（seawater） and estuary water samples using on-line flow injection（FIA）-ICP-MS.The（detection） limit of the method is about 10 ng/L,and the relative standard deviation（s_r） is 9.1%.Using CASS-4 standard seawater samples spiked with Pb standard,the recovery of Pb from the process is about 140%.The high recovery observed is likely due to the contamination of Pb in the high purity nitric cid used in the experiments.更多还原