化学学报 ›› 2013, Vol. 71 ›› Issue (09): 1287-1292.DOI: 10.6023/A13030328 上一篇    下一篇

研究论文

FePO4包覆Fe3O4磁性纳米微粒的合成及其在Cr(III)富集分离中的应用

王都留a, 杨建东a, 杨升宏b, 郭锦秀b   

  1. a 陇南师范高等专科学校生化系 成县 742500;
    b 兰州大学化学化工学院 兰州 730000
  • 收稿日期:2013-04-04 出版日期:2013-09-14 发布日期:2013-07-19
  • 通讯作者: 王都留,E-mail:lsshxwdl@163.com;Tel.:0939-3203519 E-mail:lsshxwdl@163.com
  • 基金资助:

    项目受陇南师专2012校级重点科研项目(Nos. 2012LSZK01001, 2012LSZK01003)资助.

Synthesis of Iron Phosphate Coated Nano-Fe3O4 Particles and Its Application in the Enrichment of Chromium(III) from Aqueous Solutions

Wang Duliua, Yang Jiandonga, Yang Shenghongb, Guo Jinxiub   

  1. a Department of Biology & Chemistry, Longnan Normal College, Chengxian 742500;
    b College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000
  • Received:2013-04-04 Online:2013-09-14 Published:2013-07-19
  • Supported by:

    Project supported by the key research projects of the Longnan Normal College (Nos. 2012LSZK01001, 2012LSZK01003).

采用液相沉积的方法将磷酸铁包覆在纳米Fe3O4颗粒表面, 成功制备了具有超顺磁性的吸附剂, 并用于水中微量Cr(III)的富集. 通过振动样品磁强计、X射线衍射、扫描电子显微镜、透射电子显微镜、X射线光电子能谱、Zeta电势和激光动态光散射等对Fe3O4磁性纳米粒子进行了形貌表征, 研究了该吸附剂在不同的pH值、吸附时间及溶液体积对Cr(III)的吸附效率. 结果表明在pH=5.3温度为25 ℃时, 0.0200 g吸附剂可使体积为20.0 mL 20.0 μg•L-1 Cr(III)定量吸附, 吸附等温线符合Freundlich模型, 吸附动力学过程符合假二级动力学方程. 该吸附剂适合大体积试样中极微量Cr(III)的富集, 对800 mL浓度为0.5 μg•L-1的Cr(III)吸附率可达80%以上, 富集倍数可达1125倍, 可以满足痕量分析的要求. 该吸附剂可以回收使用, 重复使用10次, 吸附率仍能达到95%.

关键词: 磷酸铁, 纳米四氧化三铁, 富集, 石墨炉原子吸收, 铬(III)

Magnetic separation has been proved to be superior to the traditional column separation or filtration especially when nanosized adsorbents are used. In this work, iron phosphate coated nano-Fe3O4 particles (Fe3O4@FePO4) were synthesized in aqueous solution through deposition of Fe(III) and phosphate ions onto the superparamagnetic nano-Fe3O4 particles that were prepared by coprecipitation. The synthesized nano-particles were applied to the enrichment of trace amounts of Cr(III) for its determination by graphite furnace atomic absorption spectrometry (GF-AAS). The magnetic property and morphology of Fe3O4@FePO4 were characterized by vibrating sample magnetometer (VSM), scanning electron microscope (SEM), transmission electron microscope (TEM). The results indicated that the adsorbent was superparamagnetic. Its saturated intensity of magnetization was 23.0 emu•g-1. This value implied that the prepared Fe3O4@FePO4 could be efficiently separated from the solutions by magnetic fields. The diameters of the particles evaluated from TEM images were in a range of 2~9 nm, which were consistent with that obtained from dynamic light scattering. X-ray photoelectron spectroscopy (XPS) and Zeta potential measurement were used for determining the composition and surface charge of the adsorbent. Based on XPS results, the amount of FePO4 in Fe3O4@FePO4 was 33.8%. Cr was found in Fe3O4@FePO4 after Cr adsorption. Zeta potential measurement indicated that the surface of Fe3O4@FePO4 carried positive charge at pH<4 and negative charge at pH>4. The influence of pH, adsorption time and sample volume on the rate of adsorption were systematically investigated. At pH 5.3, 0.0200 g of Fe3O4@FePO4 could quantitatively adsorb Cr(III) from 20.0 mL of sample within 20 min. Freundlich isotherm and pseudo second order adsorption kinetics were observed. Adsorbed Cr(III) could be desorbed with 0.3 mol•L-1 NH3-1% (V/V) H2O2 for direct GF-AAS analysis. The adsorbent was also used for the enrichment of Cr(III) from large volume samples. After stirring for 2 h, more than 80% of Cr(III) in 800 mL (0.5 μg•L-1) of aqueous solution could be adsorbed and an enrichment factor of 1125 was attained, which confirmed its suitability for the analysis of trace amounts of Cr(III). The adsorbent was successfully used for the real sample analysis and could be re-used 10 times after proper washing and drying.

Key words: iron phosphate, Fe3O4 nanoparticle, enrichment, GF-AAS, chromium (III)