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Speciation and determination of inorganic arsenic species in water and biological samples by ultrasound assisted-dispersive-micro-solid phase extraction on carboxylated nanoporous graphene coupled with flow injection-hydride generation atomic absorption spectrometry

机译:羧化纳米多孔石墨烯超声辅助分散微固相萃取-流动注射氢化物发生原子吸收光谱法测定水和生物样品中无机砷的形态和测定

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In this paper, the potential use of carboxylated nanoporous graphene (G-COOH) as a nanoadsorbent was evaluated in two types of ultrasound assisted-dispersive micro-solid phase extraction (US-D-mu-SPE) for rapid speciation of trace arsenic(V) and arsenic(III) ions in natural water and human biological samples prior to determination by flow injection-hydride generation atomic absorption spectrometry (FI-HG-AAS). High sample volume-ultrasound assisted-dispersive micro-solid phase extraction (H-US-D-mu-SPE), and low sample volume-ultrasound assisted-dispersive micro-solid phase extraction (L-US-D-mu-SPE) were developed to extract the analyte through two pathways. As(V) ions were quantitatively recovered on G-COOH at pH 3.5, while the recoveries of As(III) were below 5%. Total arsenic content was determined as As(V) after oxidation of As(III) to As(V) using potassium permanganate. Finally, the concentration of As(III) was calculated by subtracting the As(V) content from total arsenic. Carboxylated nanoporous graphene was characterized by XRD, Raman, FT -IR, BET, SEM, TEM, and EDAX analysis. The reusability and adsorption capacity of the nanosorbent were also investigated. Under the optimized conditions, limits of detection and preconcentration factor for As(V) were 0.0021 mu g L-1 and 50.3 in H-US-D-mu-SPE as well as 0.0248 mu g L-1 and 5.1 in L-US-D-mu-SPE. The developed methods were successfully applied for speciation and determination of inorganic arsenic in natural water and human serum/urine samples.
机译:本文在两种类型的超声辅助分散微固相萃取(US-D-mu-SPE)中对痕量砷的快速形态分析评估了羧基化纳米多孔石墨烯(G-COOH)作为纳米吸附剂的潜在用途。在通过流动注射氢化物发生原子吸收光谱法(FI-HG-AAS)测定之前,先在天然水和人体生物样品中添加V)和砷(III)离子。高样品量-超声辅助分散微固相萃取(H-US-D-mu-SPE)和低样品量-超声辅助分散微固相萃取(L-US-D-mu-SPE)开发了通过两种途径提取分析物的方法。在pH 3.5的G-COOH上定量回收了As(V)离子,而As(III)的回收率低于5%。使用高锰酸钾将砷(III)氧化为砷(V)后,将总砷含量确定为砷(V)。最后,通过从总砷中减去As(V)含量来计算As(III)的浓度。羧基化的纳米多孔石墨烯通过XRD,拉曼,FT -IR,BET,SEM,TEM和EDAX分析进行了表征。还研究了纳米吸附剂的可重复使用性和吸附能力。在优化的条件下,H-US-D-mu-SPE中As(V)的检出限和预富集因子分别为0.0021μg L-1和50.3,以及L-US中0.0248μgL-1和5.1 -D-mu-SPE。所开发的方法已成功用于天然水和人血清/尿液样品中无机砷的形态分析和测定。

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