Magnetic Solid Phase Extraction of Lead (II) and Cadmium (II) From Water Samples Using ZnO@Fe3O4 Nanoparticles Combined With Flame Atomic Absorption Spectrometry Determination

IF 2.8 3区 工程技术 Q2 CHEMISTRY, ANALYTICAL Journal of separation science Pub Date : 2025-03-17 DOI:10.1002/jssc.70115
Şeyma Korkmaz, Elvan Hasanoğlu Özkan, Demet Uzun, Nurdan Kurnaz Yetim, Cemile Özcan
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Abstract

A new magnetic solid phase extraction method was developed utilizing magnetically enhanced zinc oxide (ZnO@Fe3O4) nanoparticles for the separation and enrichment of lead (II) and cadmium (II) before sample determination through flame atomic absorption spectrometry. The ZnO@Fe3O4 nanoparticles synthesized by the hydrothermal method were characterized by x-ray diffraction, scanning electron microscopy, and energy-dispersive x-ray spectroscopy. The experimental factors like pH (6.0), eluent type and concentration (1 M nitric acid for lead (II), 1 M hydrochloric acid for cadmium (II)), adsorbent amount (150 mg for lead (II), and 200 mg for cadmium (II)), sample volume (5 mL), and extraction time (5 min for lead (II), and 10 min for cadmium (II)) were optimized. Under the optimization conditions, limits of detection of 2.36 and 7.86 µg/L for lead (II) and cadmium (II) were obtained with a wide concentration range from 50 to 5000 µg/L, respectively. The presented method was successfully applied to real water samples with spiked recoveries in the range of 99.2%–101% for lead (II) and 99.6%–100% for cadmium (II).

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利用 ZnO@Fe3O4 纳米粒子磁性固相萃取水样中的铅(II)和镉(II)并结合火焰原子吸收光谱法进行测定
在火焰原子吸收光谱法测定样品之前,利用磁性增强氧化锌纳米粒子(ZnO@Fe3O4)建立了一种新的磁性固相萃取方法,用于分离和富集铅(II)和镉(II)。通过x射线衍射、扫描电镜和能量色散x射线能谱对水热法制备的ZnO@Fe3O4纳米粒子进行了表征。优化了pH(6.0)、洗脱液类型和浓度(1 M硝酸对铅(II)、1 M盐酸对镉(II))、吸附剂用量(150 mg铅(II)、200 mg镉(II))、进样量(5 mL)、提取时间(5 min铅(II)、10 min镉(II))等实验因素。在优化条件下,铅(II)和镉(II)在50 ~ 5000µg/L范围内的检出限分别为2.36µg/L和7.86µg/L。该方法成功地应用于实际水样,铅(II)的加标回收率为99.2% ~ 101%,镉(II)的加标回收率为99.6% ~ 100%。
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来源期刊
Journal of separation science
Journal of separation science 化学-分析化学
CiteScore
6.30
自引率
16.10%
发文量
408
审稿时长
1.8 months
期刊介绍: The Journal of Separation Science (JSS) is the most comprehensive source in separation science, since it covers all areas of chromatographic and electrophoretic separation methods in theory and practice, both in the analytical and in the preparative mode, solid phase extraction, sample preparation, and related techniques. Manuscripts on methodological or instrumental developments, including detection aspects, in particular mass spectrometry, as well as on innovative applications will also be published. Manuscripts on hyphenation, automation, and miniaturization are particularly welcome. Pre- and post-separation facets of a total analysis may be covered as well as the underlying logic of the development or application of a method.
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