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基于磁性纳米材料Fe3O4/C吸附测定水样中痕量结晶紫的方法

肖 芳1,郭 岚1,2,*,柳英霞2,鄢爱平2,万益群1,2   

  1. 1.南昌大学化学学院,江西 南昌 330031;2.南昌大学分析测试中心,江西 南昌 330047
  • 出版日期:2016-03-25 发布日期:2016-03-18

Preparation of Fe3O4/C Magnetic Nanomaterial and Its Application in Detection of Trace Crystal Violet in Water

XIAO Fang1, GUO Lan1,2,*, LIU Yingxia2, YAN Aiping2, WAN Yiqun1,2   

  1. 1. College of Chemistry, Nanchang University, Nanchang 330031, China;
    2. Center of Analysis and Testing, Nanchang University, Nanchang 330047, China
  • Online:2016-03-25 Published:2016-03-18

摘要:

采用溶剂热/水热法合成了磁性纳米粒子Fe3O4/C,利用透射电镜、傅里叶变换红外光谱、X射线衍射等对其进行表征。将该材料用作磁性固相萃取吸附剂萃取富集水中的痕量结晶紫,之后用紫外分光光度法测定,建立了一种分离富集和检测结晶紫的方法。考察水样酸度、搅拌时间和吸附温度对结晶紫吸附率的影响。结果显示,在pH 8.0、搅拌时间10 min、吸附温度25 ℃条件下,该材料对结晶紫具有良好的吸附性,用乙醇-0.5 mol/L对甲苯磺酸(9∶1,V/V)可以很好地解吸。在优化实验条件下,方法对结晶紫的检出限为0.024 mg/L。对赣江水样品中的结晶紫进行检测,加标回收率为105.8%~108.4%,相对标准偏差为3.6%~6.1%。

关键词: 磁性纳米材料, 结晶紫, 富集, 水样

Abstract:

A magnetic nanoparticle Fe3O4/C was prepared by solvothermal/hydrothermal method and characterized by
transmission electron microscope, Fourier transform infrared spectroscopy and X-ray diffraction. Using the material as a
magnetic solid phase extraction sorbent, a new method for the detection of trace crystal violet (CV) in water was established
by UV spectrophotometry. Effects of several factors including sample pH stirring time, and adsorption temperature on
the percent adsorption of CV were investigated. The optimum adsorption conditions were determined as follows: pH,
8.0; stirring time, 10 min; and temperature, 25 ℃, and high desorption efficiency was achieved using ethanol-0.5 mol/L
p-toluenesulfonic acid (9:1, V/V) as the eluent. Under the optimum conditions, the limit of detection (LOD) of this method
was 0.024 mg/L. The proposed method was applied to the determination of CV in Ganjiang river water with spiked
recoveries of 105.8%–108.4% and relative standard deviation (RSD) of 3.6%–6.1%, respectively.

Key words: magnetic nanomaterials, crystal violet, enrichment, water sample

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