Institute of Chemistry, University of Silesia, Szkolna 9, 40-006, Katowice, Poland.
Institute of Low Temperature and Structure Research, Polish Academy of Sciences, P.O. Box 1410, 50-950, Wrocław, Poland.
Anal Bioanal Chem. 2018 Nov;410(29):7793-7802. doi: 10.1007/s00216-018-1397-8. Epub 2018 Oct 5.
Obtaining new nanocomposites with sorption properties towards chromium is highly important not only from the environmental point of view but also for developing eco-friendly methods of chromium determination. The potential use of aluminum oxide-coated nano-graphite (AlO/nano-G) as a new nanosorbent in ultrasound-assisted dispersive micro-solid-phase extraction (DMSPE) for rapid speciation of trace chromium(III) and chromium(VI) ions in natural water was evaluated. In the developed method, the crucial issue is the new nanocomposite synthesized by coating alumina on a nano-graphite surface with sorption properties. Structural researches of the nanocomposite were carried out by scanning electron microscopy (SEM), powder X-ray diffraction (XRD), and Raman spectroscopy. Maximum adsorption capacity of AlO/nano-G towards Cr(III) was 32.8 mg g. The influence of the method's factors like pH, sample volumes, contact time, coexisting ions, and humic acid on the recovery of chromium was examined. The nanocomposites have been found to be stable and effective as a sorbent in water with high concentrations of selected cations and anions present in water as well as in water of various pH. AlO/nano-G is selective for Cr(III) in presence of Cr(VI). Cr(III) was determined by the developed method, total Cr after reduction of Cr(VI) to Cr(III), and Cr(VI) was calculated as the difference between total Cr and Cr(III). After sorption, the nanocomposite with chromium was collected on 5-mm diameter filters and analyzed by energy-dispersive X-ray fluorescence spectrometry (EDXRF) to determine the chromium concentration. The method was characterized by correlation coefficient 0.999, limit of detection (LOD) 0.04 ng mL, and relative standard deviation (RSD) 3.5%. AlO/nano-G combined with proposed DMSPE/EDXRF was verified by analysis of certificate reference material of natural water (NIST 1640a). Graphical abstract ᅟ.
获得对铬具有吸附性能的新型纳米复合材料不仅从环境角度来看非常重要,而且对于开发环保的铬测定方法也很重要。评估了氧化铝涂覆纳米石墨(AlO/nano-G)作为超声辅助分散微固相萃取(DMSPE)中新型纳米吸附剂,用于快速形态分析天然水中痕量铬(III)和铬(VI)离子的潜力。在所开发的方法中,关键问题是在纳米石墨表面涂覆氧化铝而合成的新型纳米复合材料,具有吸附性能。通过扫描电子显微镜(SEM)、粉末 X 射线衍射(XRD)和拉曼光谱对纳米复合材料进行了结构研究。AlO/nano-G 对 Cr(III) 的最大吸附容量为 32.8 mg g。考察了方法的因素,如 pH 值、样品体积、接触时间、共存离子和腐殖酸对铬回收的影响。研究发现,纳米复合材料在存在高浓度所选阳离子和阴离子以及各种 pH 值的水中作为吸附剂是稳定且有效的。AlO/nano-G 对存在的 Cr(VI) 具有选择性。Cr(III) 通过开发的方法测定,Cr(VI) 还原为 Cr(III) 后的总 Cr,Cr(VI) 计算为总 Cr 与 Cr(III) 的差值。吸附后,用 5 毫米直径的过滤器收集含铬的纳米复合材料,并通过能量色散 X 射线荧光光谱法(EDXRF)进行分析,以确定铬浓度。该方法的特征在于相关系数为 0.999、检测限(LOD)为 0.04 ng mL 和相对标准偏差(RSD)为 3.5%。AlO/nano-G 与提议的 DMSPE/EDXRF 结合,通过分析天然水证书参考物质(NIST 1640a)进行了验证。