Analytical Spectroscopy Research Laboratory, Department of Chemistry, Faculty of Sciences, Azarbaijan Shahid Madani University, 35 Km Tabriz-Marageh Road, P.O. Box 53714-161, Tabriz, 5375171379, Iran.
Mikrochim Acta. 2018 Jun 28;185(7):343. doi: 10.1007/s00604-018-2874-7.
Magnesium(II)-doped nickel ferrite (Mg-NiFeO) nanoparticles are introduced as a new adsorbent for magnetic solid phase extraction of lead(II) ions from aqueous solutions. The structure and morphology of the adsorbent was characterized by FTIR, X-ray diffraction and scanning electron microscopy. The effects of pH value, amount of adsorbent, type, concentration and volume of the eluent and adsorption/desorption time on the extraction efficiency were studied. Following elution with hydrochloric acid, Pb(II) ions were quantified by flame atomic absorption spectrometry. Under optimized conditions, the calibration graph is linear in the 0.5-125 ng mL Pb(II) ion concentration range. Other figures of merit include (a) a 0.2 ng mL limit of detection, (b) an enrichment factor of 200, (c) an intra-day relative standard deviation (for n = 6 at 50 ng mL) of 1.6%, and (d) an inter-day precision of 3.8%. The method was validated by the analysis of the certified reference material, NIST SRM 1566b. It was successfully applied to the determination of Pb(II) ion in spiked water samples, industrial wastewater and acidic lead battery waters. Graphical abstract Schematic of the synthesis of Mg(II)-doped NiFeO nanoparticles and their application as a magnetic sorbent for solid-phase extraction of a Pb(II) ions prior to determination by flame atomic absorption spectrometry (FAAS).
镁掺杂镍铁氧体 (Mg-NiFeO) 纳米粒子被引入作为一种从水溶液中磁性固相萃取铅 (II) 离子的新型吸附剂。通过傅里叶变换红外光谱 (FTIR)、X 射线衍射和扫描电子显微镜对吸附剂的结构和形态进行了表征。研究了 pH 值、吸附剂用量、洗脱剂类型、浓度和体积以及吸附/解吸时间对萃取效率的影响。用盐酸洗脱后,用火焰原子吸收光谱法定量测定 Pb(II) 离子。在优化条件下,校准曲线在 0.5-125ngmL Pb(II) 离子浓度范围内呈线性。其他优点包括 (a) 0.2ngmL 的检测限,(b) 200 的富集因子,(c) 50ngmL 时 6 次重复测定的日内相对标准偏差为 1.6%,以及 (d) 3.8%的日间精密度。该方法通过对 NIST SRM 1566b 认证参考物质的分析进行了验证。该方法成功应用于测定加标水样、工业废水和酸性铅电池水中的 Pb(II) 离子。