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采用氧化石墨烯负载氧化铝测定和形态分析痕量砷和铬形态。

Determination and speciation of ultratrace arsenic and chromium species using aluminium oxide supported on graphene oxide.

机构信息

University of Silesia, Institute of Chemistry, 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.

出版信息

Talanta. 2018 Aug 1;185:264-274. doi: 10.1016/j.talanta.2018.03.090. Epub 2018 Mar 28.

Abstract

Alumina supported on graphene oxide (AlO/GO) nanocomposite as new nanosorbent in dispersive micro-solid phase extraction (DMSPE) for As(V) and Cr(III) preconcentration is described. The crucial issue of the study is synthesis of novel nanocomposite suitable for sorption of selected species of arsenic and chromium. AlO/GO demonstrates selectivity toward arsenates in the presence of arsenites at pH 5 and chromium(III) ions in the presence of chromate anions at pH 6. The AlO/GO nanocomposite was characterized by scanning electron microscopy (SEM) transmission electron microscopy (TEM), powder X-ray diffraction (XRD) and the Raman spectroscopy. The maximum adsorption capacity calculated based on the Langmuir adsorption model were 43.9 mg g and 53.9 mg g for As(V) and Cr(III), respectively. The nanocomposite was used as solid sorbent in preconcentration of As(V) and Cr(III)_ions from water samples and their determination using energy dispersive X-ray fluorescence spectrometry (EDXRF). The As(V) and Cr(III) ions can be quantitatively preconcentrated from 25 to 100 mL aqueous samples within 5 min using DMSPE procedure and 1 mg of AlO/GO. The nanocomposite was also used for preparation of AlO/GO membrane. Then, As(V) and Cr(III)_ions can be retained under flow condition by passing analyzed solution through AlO/GO membrane. Under the optimized conditions, As(V) and Cr(III) ions can be determined with very good recovery (92-108%), precision (RSD 2.7-4.0%) and excellent limit of detection (0.02 ng mL As and 0.11 ng mL Cr). The accuracy of the method was studied by analyzing certified reference materials (NIST 1640a) and spiked real water samples.

摘要

氧化铝负载在氧化石墨烯(AlO/GO)纳米复合材料上作为一种新型纳米吸附剂,用于分散固相微萃取(DMSPE)中砷(V)和铬(III)的预浓缩。该研究的关键问题是合成适合于吸附砷和铬特定物种的新型纳米复合材料。在 pH 值为 5 时,AlO/GO 对砷酸盐表现出选择性,而在 pH 值为 6 时,对铬酸盐阴离子存在下的铬(III)离子也表现出选择性。AlO/GO 纳米复合材料采用扫描电子显微镜(SEM)、透射电子显微镜(TEM)、粉末 X 射线衍射(XRD)和拉曼光谱进行了表征。基于 Langmuir 吸附模型计算的最大吸附容量分别为 43.9mg/g 和 53.9mg/g,用于砷(V)和铬(III)。该纳米复合材料被用作固相吸附剂,用于从水样中预浓缩砷(V)和铬(III)离子,并使用能量色散 X 射线荧光光谱法(EDXRF)进行测定。通过 DMSPE 程序,在 5 分钟内,可从 25 至 100mL 水样中定量预浓缩砷(V)和铬(III)离子,使用 1mg AlO/GO。该纳米复合材料还用于制备 AlO/GO 膜。然后,通过将分析溶液通过 AlO/GO 膜,在流动条件下可以保留砷(V)和铬(III)离子。在优化条件下,砷(V)和铬(III)离子可以以非常好的回收率(92-108%)、精密度(RSD 2.7-4.0%)和优异的检出限(0.02ng/mL 砷和 0.11ng/mL 铬)进行测定。通过分析认证参考物质(NIST 1640a)和加标实际水样来研究该方法的准确性。

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