Carrington Nathan A, Thomas George H, Rodman D Lynn, Beach David B, Xue Zi-Ling
Department of Chemistry, The University of Tennessee, Knoxville, TN 37996-1600, USA.
Anal Chim Acta. 2007 Jan 9;581(2):232-40. doi: 10.1016/j.aca.2006.08.032. Epub 2006 Aug 24.
Transparent, pyridine-functionalized sol-gel monoliths have been formed and their use in Cr(VI) sensing applications is demonstrated. The monoliths were immersed in acidic Cr(VI)-containing solutions, and the Cr(VI) uptake was monitored using UV-vis and atomic absorption spectroscopies. At concentrations at the ppm level, the monoliths exhibit a yellow color change characteristic of Cr(VI) uptake, and this can be measured by monitoring the absorption change at about 350 nm using UV-vis spectroscopy. Concentrations at the ppb level are below the limit of detection using this wavelength of 350 nm for measurement. However, by adding a diphenylcarbazide solution to monoliths that have been previously immersed in ppb-level Cr(VI) solutions, a distinct color change takes place within the gels that can be measured at about 540 nm using UV-vis spectroscopy. Concentrations as low as 10 ppb Cr(VI) can be measured using this method. The monoliths can then be regenerated for subsequent sensing cycles by thorough washing with 6.0M HCl. The factors affecting monolith uptake of Cr(VI) have been explored. In addition, the gels have been characterized using X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) measurements.
已制备出透明的、吡啶功能化的溶胶-凝胶整体柱,并展示了其在Cr(VI)传感应用中的用途。将整体柱浸入含酸性Cr(VI)的溶液中,并用紫外-可见光谱和原子吸收光谱监测Cr(VI)的吸收情况。在ppm级浓度下,整体柱呈现出Cr(VI)吸收特有的黄色变化,这可以通过用紫外-可见光谱监测约350 nm处的吸收变化来测量。对于使用350 nm此波长进行测量而言,ppb级浓度低于检测限。然而,通过向先前浸入ppb级Cr(VI)溶液的整体柱中加入二苯卡巴肼溶液,凝胶内部会发生明显的颜色变化,这可以用紫外-可见光谱在约540 nm处进行测量。使用此方法可测量低至10 ppb的Cr(VI)浓度。然后,通过用6.0M HCl彻底洗涤,整体柱可进行再生以用于后续的传感循环。已对影响整体柱对Cr(VI)吸收的因素进行了探索。此外,还使用X射线光电子能谱(XPS)、扫描电子显微镜(SEM)和布鲁诺尔-埃米特-泰勒(BET)测量对凝胶进行了表征。