Enhancing Trace Metal Extraction from Wastewater: Magnetic Activated Carbon as a High-Performance Sorbent for Inductively Coupled Plasma Optical Emission Spectrometry Analysis

IF 2.5 4区工程技术 Q3 CHEMISTRY, ANALYTICAL

Separations Pub Date : 2023-11-10 DOI:10.3390/separations10110563

Sergio J. Abellán-Martín, David Villalgordo-Hernández, Miguel Ángel Aguirre, Enrique V. Ramos-Fernández, Javier Narciso, Antonio Canals

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引用次数: 0

Abstract

A new fast, sensitive, and environmentally friendly analytical method has been developed for the simultaneous determination of Ba, Be, Cd, Cr, Cu, Fe, Hg, Mn, Ni, Pb, and Zn in wastewater samples using inductively coupled plasma optical emission spectroscopy (ICP OES). A preconcentration step using a magnetic dispersive solid-phase extraction (MDSPE) technique with a new magnetic sorbent was performed. The new sorbent material was a carbon containing magnetic cobalt and nitrogen groups. This material was synthetized using controlled pyrolysis of a zeolitic imidazolate framework (i.e., ZIF-67). In order to optimize the experimental parameters that affect the MDSPE procedure, a multivariate optimization strategy, using Plackett–Burman and circumscribed central composite designs (CCD), was used. The method has been evaluated employing optimized experimental conditions (i.e., sample weight, 10 g; sample pH, 7.6; amount of sorbent, 10 mg; dispersive agent, vortex; complexing agent concentration, 0.5%; ionic concentration, 0%; eluent, HCl; eluent concentration, 0.5 M; eluent volume, 300 μL; elution time, 3 min and extraction time, 3 min) using external calibration. Limits of detection (LODs) in a range from 0.073 to 1.3 μg L−1 were obtained, and the repeatability was evaluated at two different levels, resulting in relative standard deviations below 8% for both levels (n = 5). An increase in the sensitivity was observed due to the high enrichment factors (i.e., 3.2 to 13) obtained compared with direct ICP OES analysis. The method was also validated through carrying out recovery studies that employed a real wastewater sample and through the analysis of a certified reference material (ERM®-CA713). The recovery values obtained with the real wastewater were between 94 and 108% and between 90 and 109% for the analysis of ERM®-CA713, showing negligible matrix effects.

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提高废水中痕量金属的提取:磁性活性炭作为电感耦合等离子体发射光谱分析的高性能吸附剂

建立了一种快速、灵敏、环保的废水样品中Ba、Be、Cd、Cr、Cu、Fe、Hg、Mn、Ni、Pb、Zn的电感耦合等离子体发射光谱(ICP OES)同时测定方法。采用新型磁性吸附剂进行了磁分散固相萃取(MDSPE)预富集。这种新型吸附材料是一种含有磁性钴和氮基团的碳。该材料采用沸石咪唑酯骨架(即ZIF-67)的受控热解合成。为了优化影响MDSPE过程的实验参数，采用了Plackett-Burman和限制性中心复合设计(CCD)的多元优化策略。采用优化的实验条件(即样品质量为10 g;样品pH, 7.6;吸附剂用量:10mg;分散剂，旋涡;络合剂浓度，0.5%;离子浓度，0%;盐酸洗脱液;洗脱液浓度，0.5 M;洗脱液体积，300 μL;洗脱时间，3分钟，提取时间，3分钟)使用外部校准。检测限(lod)在0.073 ~ 1.3 μg L−1范围内，并在两个不同的水平上进行了重复性评估，两个水平的相对标准偏差均低于8% (n = 5)。与直接ICP OES分析相比，由于获得了较高的富集因子(即3.2 ~ 13)，观察到灵敏度的提高。该方法还通过使用实际废水样品进行回收研究并通过认证标准物质(ERM®-CA713)分析进行验证。实际废水的回收率在94 ~ 108%之间，ERM®-CA713的回收率在90 ~ 109%之间，基质效应可以忽略不计。

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来源期刊

Separations Chemistry-Analytical Chemistry

CiteScore

3.00

自引率

15.40%

发文量

342

审稿时长

12 weeks

期刊介绍： Separations (formerly Chromatography, ISSN 2227-9075, CODEN: CHROBV) provides an advanced forum for separation and purification science and technology in all areas of chemical, biological and physical science. It publishes reviews, regular research papers and communications. Our aim is to encourage scientists to publish their experimental and theoretical results in as much detail as possible. There is no restriction on the length of the papers. The full experimental details must be provided so that the results can be reproduced. There are, in addition, unique features of this journal: Manuscripts regarding research proposals and research ideas will be particularly welcomed. Electronic files and software regarding the full details of the calculation and experimental procedure, if unable to be published in a normal way, can be deposited as supplementary material. Manuscripts concerning summaries and surveys on research cooperation and projects (that are funded by national governments) to give information for a broad field of users. The scope of the journal includes but is not limited to: Theory and methodology (theory of separation methods, sample preparation, instrumental and column developments, new separation methodologies, etc.) Equipment and techniques, novel hyphenated analytical solutions (significantly extended by their combination with spectroscopic methods and in particular, mass spectrometry) Novel analysis approaches and applications to solve analytical challenges which utilize chromatographic separations as a key step in the overall solution Computational modelling of separations for the purpose of fundamental understanding and/or chromatographic optimization