Azizi Parastou, Golshekan Mostafa, Shariati Shahab, Rahchamani Jalal
Young Researchers and Elite Club, Lahijan Branch, Islamic Azad University, Lahijan, Iran.
Environ Monit Assess. 2015 Apr;187(4):185. doi: 10.1007/s10661-015-4419-4. Epub 2015 Mar 18.
In the present study, silica magnetite mesoporous nanoparticles functionalized with a new chelating agent were synthesized and introduced as a magnetic solid phase for preconcentration of trace amounts of Cu2+, Ni2+, and Co2+ ions from aqueous solutions. Briefly, MCM-41 mesoporous-coated magnetite nano-particles (MMNPs) with particle size lower than 15 nm were synthesized via chemical co-precipitation methods. Then, N-(4-methoxysalicylidene)-4,5-dinitro-1,2-phenylenediamine (HL) as a new chelating agent was synthesized and used for surface modification of mesoporous magnetic solid phase by dispersive liquid-liquid functionalization (DLLF) as a new rapid method to form HL functionalized mesoporous magnetite nanoparticles (MMNPs─HL). The structure and morphology of prepared sorbent were characterized by FT-IR, XRD, VSM, and TEM. Finally, the prepared nanoparticles were utilized for preconcentration of Cu2+, Ni2+, and Co2+ ions prior to determination by atomic absorption spectrophotometery. The calibration graph was obtained under the optimized conditions with linear dynamic range of 1.0-300 μg L(-1) and correlation coefficient (r2) of 0.998. The detection limits of this method for cobalt, nickel, and copper ions were 0.03, 0.03, and 0.04 ng/mL, respectively. Finally, the method was successfully applied to the extraction and determination of the analyte ions in natural waters and reference plant samples.
在本研究中,合成了一种用新型螯合剂功能化的二氧化硅磁铁矿介孔纳米颗粒,并将其作为磁性固相,用于从水溶液中预富集痕量的Cu2+、Ni2+和Co2+离子。简要地说,通过化学共沉淀法合成了粒径小于15 nm的MCM-41介孔包覆磁铁矿纳米颗粒(MMNPs)。然后,合成了新型螯合剂N-(4-甲氧基亚水杨基)-4,5-二硝基-1,2-苯二胺(HL),并采用分散液-液功能化(DLLF)这一新型快速方法对介孔磁性固相进行表面改性,以形成HL功能化介孔磁铁矿纳米颗粒(MMNPs─HL)。通过傅里叶变换红外光谱(FT-IR)、X射线衍射(XRD)、振动样品磁强计(VSM)和透射电子显微镜(TEM)对制备的吸附剂的结构和形貌进行了表征。最后,将制备的纳米颗粒用于在原子吸收分光光度法测定之前对Cu2+、Ni2+和Co2+离子进行预富集。在优化条件下获得了校准曲线,线性动态范围为1.0 - 300 μg L(-1),相关系数(r2)为0.998。该方法对钴、镍和铜离子的检测限分别为0.03、0.03和0.04 ng/mL。最后,该方法成功应用于天然水和参考植物样品中分析物离子的萃取和测定。