Abolhasani Jafar, Behbahani Mohammad
Department of Chemistry, Faculty of Science, Tabriz Branch, Islamic Azad University, Tabriz, Iran,
Environ Monit Assess. 2015 Jan;187(1):4176. doi: 10.1007/s10661-014-4176-9. Epub 2014 Dec 12.
Solid-phase extraction is one the most useful and efficient techniques for sample preparation, purification, cleanup, preconcentration, and determination of heavy metals at trace levels. In this paper, functionalized MCM-48 nanoporous silica with 1-(2-pyridylazo)-2-naphthol was applied for trace determination of copper, lead, cadmium, and nickel in water and seafood samples. The experimental conditions such as pH, sample and eluent flow rate, type, concentration and volume of the eluent, breakthrough volume, and effect of coexisting ions were optimized for efficient solid-phase extraction of trace heavy metals in different water and seafood samples. The content of solutions containing the mentioned heavy metals was determined by flame atomic absorption spectrometry (FAAS), and the limits of detection were 0.3, 0.4, 0.6, and 0.9 ng mL(-1) for cadmium, copper, nickel, and lead, respectively. Recoveries and precisions were >98.0 and <4%, respectively. The adsorption capacity of the modified nanoporous silica was 178 mg g(-1) for cadmium, 110 mg g(-1) for copper, 98 mg g(-1) for nickel, and 210 mg g(-1) for lead, respectively. The functionalized MCM-48 nanoporous silica with 1-(2-pyridylazo)-2-naphthol was characterized by thermogravimetry analysis (TGA), differential thermal analysis (DTA), transmission electron microscopy (TEM), Fourier transform infrared spectrometry (FT-IR), X-ray diffraction (XRD), elemental analysis (CHN), and N2 adsorption surface area measurement.
固相萃取是用于样品制备、纯化、净化、预浓缩以及痕量重金属测定的最有用且高效的技术之一。本文中,将带有1-(2-吡啶偶氮)-2-萘酚的功能化MCM-48纳米多孔二氧化硅应用于水和海鲜样品中铜、铅、镉和镍的痕量测定。对诸如pH、样品和洗脱液流速、洗脱液的类型、浓度和体积、穿透体积以及共存离子的影响等实验条件进行了优化,以实现不同水和海鲜样品中痕量重金属的高效固相萃取。采用火焰原子吸收光谱法(FAAS)测定含有上述重金属的溶液的含量,镉、铜、镍和铅的检测限分别为0.3、0.4、0.6和0.9 ng mL⁻¹。回收率和精密度分别>98.0%和<4%。改性纳米多孔二氧化硅对镉、铜、镍和铅的吸附容量分别为178 mg g⁻¹、110 mg g⁻¹、98 mg g⁻¹和210 mg g⁻¹。通过热重分析(TGA)、差示热分析(DTA)、透射电子显微镜(TEM)、傅里叶变换红外光谱法(FT-IR)、X射线衍射(XRD)、元素分析(CHN)以及N₂吸附表面积测量对带有1-(2-吡啶偶氮)-2-萘酚的功能化MCM-48纳米多孔二氧化硅进行了表征。