A novel carboxyl-functionalized hybrid monolithic column was developed based on "thiol-ene" click reaction via "one-pot" by choosing mercaptosuccinic acid, γ-methyl methacrylate trimethoxysilane and tetramethoxysilane as reaction monomers. The design of the hybrid monolithic column was assisted by the comparison in computational simulation with existing carboxyl-functionalized materials. The characterization by scanning electron microscopy, energy dispersive X-ray spectroscopy, N2 adsorption-desorption measurement, Fourier-transform infrared spectroscopy and elemental analysis showed that the carboxyl-functionalized material has the advantages of good permeability and high mechanical strength. Then, we used the prepared carboxyl-hybrid monolith column as solid phase microextraction adsorbent for separation of trace inorganic chromium species. Under pH 4.5, the hybrid monolith column can selectively enrich Cr(III) without adsorbing Cr(VI) and afterwards, Cr(III) can be eluted by 1.0 mol L-1 HCl. The chromium speciation separation method based on carboxyl-hybrid monolith column followed by inductively coupled plasma-mass spectrometry possessed the merits of facile preparation, low cost, simple and mild extraction condition, and sensitive detection, which has been successfully applied to the separation, enrichment and detection of inorganic chromium in environmental waters.

中文翻译：

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通过“硫醇 - 烯”点击反应制备的羧基功能化杂化整体柱用于采用电感耦合等离子体质谱法对铬进行无创形态分析

以巯基丁二酸、γ-甲基丙烯酸甲酯三甲氧基硅烷和四甲氧基硅烷为反应单体，基于“硫醇-烯”点击反应“一锅法”开发了一种新型羧基功能化杂化整体柱。通过与现有羧基官能化材料的计算模拟比较，有助于混合整体柱的设计。扫描电子显微镜、能量色散X射线光谱、N2吸脱附测量、傅里叶变换红外光谱和元素分析的表征表明，羧基功能化材料具有良好的渗透性和较高的机械强度。然后，我们使用制备的羧基杂化整体柱作为固相微萃取吸附剂来分离痕量无机铬物种。在 pH 4.5 下，混合整体柱可以在不吸附 Cr(VI) 的情况下选择性地富集 Cr(III)，之后 Cr(III) 可以被 1.0 mol L-1 HCl 洗脱。基于羧基杂化整体柱-电感耦合等离子体质谱法的铬形态分离方法具有制备简便、成本低、提取条件简单温和、检测灵敏等优点，已成功应用于分离、富集环境水体中无机铬的检测。