Tokalıoğlu Şerife, Yavuz Emre, Şahan Halil, Çolak Süleyman Gökhan, Ocakoğlu Kasım, Kaçer Mehmet, Patat Şaban
Erciyes University, Faculty of Science, Chemistry Department, TR-38039 Kayseri, Turkey.
Erciyes University, Faculty of Science, Chemistry Department, TR-38039 Kayseri, Turkey.
Talanta. 2016 Oct 1;159:222-230. doi: 10.1016/j.talanta.2016.06.022. Epub 2016 Jun 16.
In this study a new adsorbent, ionic liquid (1,8-naphthalene monoimide bearing imidazolium salt) coated carbon nanospheres, was synthesized for the first time and it was used for the solid phase extraction of copper and lead from various samples prior to determination by flame atomic absorption spectrometry. The ionic liquid, carbon nanospheres and ionic liquid coated carbon nanospheres were characterized by using Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, (1)H NMR and (13)C NMR, Brunauer, Emmett and Teller surface area and zeta potential measurements. Various parameters for method optimization such as pH, adsorption and elution contact times, eluent volume, type and concentration, centrifuge time, sample volume, adsorption capacity and possible interfering ion effects were tested. The optimum pH was 6. The preconcentration factor, detection limits, adsorption capacity and precision (as RSD%) of the method were found to be 300-fold, 0.30µgL(-1), 60mgg(-1) and 1.1% for copper and 300-fold, 1.76µgL(-1); 50.3mgg(-1) and 2.2%, for lead, respectively. The effect of contact time results showed that copper and lead were adsorbed and desorbed from the adsorbent without vortexing. The equilibrium between analyte and adsorbent is reached very quickly. The method was rather selective for matrix ions in high concentrations. The accuracy of the developed method was confirmed by analyzing certified reference materials (LGC6016 Estuarine Water, Reference Material 8704 Buffalo River Sediment, and BCR-482 Lichen) and by spiking sea water, wastewater, street dust and spice samples.
在本研究中,首次合成了一种新型吸附剂,即离子液体(含咪唑盐的1,8-萘二甲酰亚胺)包覆的碳纳米球,并将其用于在火焰原子吸收光谱法测定之前从各种样品中固相萃取铜和铅。通过傅里叶变换红外光谱、X射线衍射、扫描电子显微镜、(1)H NMR和(13)C NMR、布鲁诺尔-埃米特-泰勒表面积和zeta电位测量对离子液体、碳纳米球和离子液体包覆的碳纳米球进行了表征。测试了方法优化的各种参数,如pH值、吸附和洗脱接触时间、洗脱剂体积、类型和浓度、离心时间、样品体积、吸附容量以及可能的干扰离子效应。最佳pH值为6。该方法对铜的预富集因子、检测限、吸附容量和精密度(以相对标准偏差%计)分别为300倍、0.30µgL(-1)、60mgg(-1)和1.1%,对铅分别为300倍、1.76µgL(-1)、50.3mgg(-1)和2.2%。接触时间结果表明,铜和铅在不涡旋的情况下从吸附剂上吸附和解吸。分析物与吸附剂之间的平衡很快达到。该方法对高浓度基体离子具有较高的选择性。通过分析有证标准物质(LGC6016河口海水、标准物质8704布法罗河沉积物和BCR-482地衣)以及对海水、废水、街道灰尘和香料样品进行加标,证实了所开发方法的准确性。