Institute of Chemistry, University of Silesia, Szkolna 9, 40-006, Katowice, Poland.
Institute of Chemistry, University of Silesia, Szkolna 9, 40-006, Katowice, Poland.
Talanta. 2022 Aug 15;246:123501. doi: 10.1016/j.talanta.2022.123501. Epub 2022 Apr 25.
β-cyclodextrin/graphene oxide (GO-β-CD) was applied for dispersive micro-solid phase extraction (DMSPE) of uranyl ions (UO) from water samples and their determination by energy-dispersive (EDXRF) and total-reflection X-ray fluorescence spectrometry (TXRF). The structure of GO-β-CD was characterized by X-ray photoelectron spectroscopy, scanning electron microscopy, Fourier transform infrared spectroscopy, and Raman spectroscopy. The results of batch adsorption experiment indicate that the maximum recoveries for UO ions are observed at pH 4.5. The Langmuir isotherm model fits the adsorption data, which stands for the chemisorption mechanism. The obtained adsorption capacity of 87.7 mg g indicates a great potential of the synthesized adsorbent in the UO ions preconcentration. The GO-β-CD exhibits high resistance to high ionic strength (up to 2 mol L), indicating that high salinity samples can be treated with the evaluated preconcentration procedure. The obtained limit of detection values were 0.40 μg L for the EDXRF and only 0.014 μg L for TXRF analysis. The accuracy of the method was verified by analyzing certified reference material (spring water NIST-SRM 1640a) and spiked water samples (mineral, lake, river, and artificial sea water).
β-环糊精/氧化石墨烯（GO-β-CD）被应用于分散固相微萃取（DMSPE）水样中的铀酰离子（UO），并通过能量色散 X 射线荧光光谱（EDXRF）和全反射 X 射线荧光光谱（TXRF）进行测定。GO-β-CD 的结构通过 X 射线光电子能谱、扫描电子显微镜、傅里叶变换红外光谱和拉曼光谱进行了表征。批量吸附实验的结果表明，UO 离子的最大回收率出现在 pH 4.5。Langmuir 等温吸附模型拟合吸附数据，表明吸附机制为化学吸附。得到的吸附容量为 87.7 mg g，表明合成吸附剂在 UO 离子预浓缩方面具有很大的潜力。GO-β-CD 具有高抗高离子强度（高达 2 mol L）的特性，表明可以用评估的预浓缩程序处理高盐度样品。对于 EDXRF 分析，得到的检出限为 0.40 μg L，而对于 TXRF 分析，检出限仅为 0.014 μg L。该方法的准确性通过分析认证参考物质（泉水 NIST-SRM 1640a）和加标水样（矿泉水、湖水、河水和人工海水）得到了验证。
