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Ionic liquid-modified Fe3O4 nanoparticle combined with central composite design for rapid preconcentration and determination of palladium ions

机译:离子液体改性的Fe3O4纳米颗粒与中心复合设计相结合,用于快速预富集和测定钯离子

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In this work, magnetic Fe3O4 nanoparticles (NPs) were synthesized by ultrasonic chemical co-precipitation method. Then hydrophobic ionic liquid (IL), as a green coating agent, was deposited on the surface of synthesized NPs in order to improve their extraction capability toward Pd(II) ions as diethyldithiocarbamate (DDTC) complex. Scanning electron microscopy, thermogravimetric analysis, X-ray diffraction (XRD), vibrating sample magnetometer (VSM), and Fourier transformed infrared (FTIR) techniques were used for characterization of the adsorbent. The adsorption rate was fast and the equilibrium time was achieved within 4min due to the strong interaction of Pd-DDTC complex with the IL and the absence of internal diffusion resistance. The separation of the adsorbent from aqueous bulk was achieved after about 2min by a magnet, so no centrifugation or filtration was required. The effective parameters such as pH, concentration of ligand, amount of adsorbent, and the extraction time were inspected by using a central composite design in order to identify the most important parameters and their interactions. Under optimum conditions, the detection limit was 0.82ngmL(-1) and the relative standard deviation (n=10) was 2.8% for 100ngmL(-1) of Pd(II). The proposed method was applied for the preconcentration of Pd(II) from road dust, liver, and water samples, and it was found that the amounts of palladium ions in dust and liver samples were 104 and 8.7ngmL(-1), respectively.
机译:在这项工作中,通过超声化学共沉淀法合成了磁性Fe3O4纳米颗粒(NPs)。然后,将疏水性离子液体(IL)作为绿色涂层剂沉积在合成NP的表面上,以提高其对二乙基二硫代氨基甲酸酯(DDTC)络合物对Pd(II)离子的萃取能力。扫描电子显微镜,热重分析,X射线衍射(XRD),振动样品磁力计(VSM)和傅立叶变换红外(FTIR)技术用于表征吸附剂。由于Pd-DDTC络合物与IL的强相互作用以及不存在内部扩散阻力,因此吸附速率很快,并且在4分钟内达到了平衡时间。约2分钟后,用磁铁将吸附剂从含水主体中分离出来,因此无需离心或过滤。通过使用中央复合设计检查了有效参数,例如pH,配体的浓度,吸附剂的量和提取时间,以确定最重要的参数及其相互作用。在最佳条件下,对于100ngmL(-1)的Pd(II),检出限为0.82ngmL(-1),相对标准偏差(n = 10)为2.8%。将该方法应用于道路扬尘,肝脏和水样中Pd(II)的富集,发现灰尘和肝脏中钯离子的含量分别为104和8.7ngmL(-1)。

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