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13 pages, 2452 KiB

Open AccessArticle

Fe₃O₄@SiO₂@VAN Nanoadsorbent Followed by GC-MS for the Determination of Polycyclic Aromatic Hydrocarbons at Ultra-Trace Levels in Environmental Water Samples

by Yu Tian, Zhigang Xu, Zhimin Liu, Xiaoxi Si, Fengmei Zhang and Wei Jiang

Nanomaterials 2022, 12(17), 2921; https://doi.org/10.3390/nano12172921 - 24 Aug 2022

Cited by 4 | Viewed by 1429

Abstract

In the present study, silica-coated magnetic nanoparticles functionalized with vancomycin (Fe₃O₄@SiO₂@VAN) were synthesized. The Fe₃O₄@SiO₂@VAN nanocomposite was used as a sorbent for the magnetic solid-phase extraction (MSPE) of polycyclic aromatic hydrocarbons [...] Read more.

In the present study, silica-coated magnetic nanoparticles functionalized with vancomycin (Fe₃O₄@SiO₂@VAN) were synthesized. The Fe₃O₄@SiO₂@VAN nanocomposite was used as a sorbent for the magnetic solid-phase extraction (MSPE) of polycyclic aromatic hydrocarbons (PAHs) from environmental water, followed by GC-MS. The nanocomposite was characterized by Fourier-transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, transmission electron microscopy, vibrating sample magnetometry, and nitrogen sorption. Various experimental parameters were optimized, including extraction condition and desorption condition. Results show that Fe₃O₄@SiO₂@VAN combined the advantages of nanomaterials and magnetic separation technology, showing excellent dispersibility and high selectivity for PAHs in environmental water sample. Under the optimal extraction conditions, an analytical method was established with the sensitive limit of detection (LOD) of 0.03–0.16 μg L⁻¹. The method was successfully applied for the analysis of environmental water samples. The relative standard deviations (%) were in the range of 0.50–12.82%, and the extraction recovery (%) was in the range of 82.48% and 116.32%. MSPE-coupled gas chromatography–mass spectrometry quantification of PAHs is an accurate and repeatable method for the monitoring of PAH accumulation in environmental water samples. It also provides an effective strategy for the tracing and quantification of other environmental pollutants in complex samples. Full article

(This article belongs to the Special Issue Nanomaterials-Based Sample Pretreatment)

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14 pages, 3762 KiB

Open AccessArticle

A Novel Ca-Modified Biochar for Efficient Recovery of Phosphorus from Aqueous Solution and Its Application as a Phosphorus Biofertilizer

by Yue Xu, Huan Liao, Jing Zhang, Haijun Lu, Xinghua He, Yi Zhang, Zhenbin Wu, Hongyu Wang and Minghua Lu

Nanomaterials 2022, 12(16), 2755; https://doi.org/10.3390/nano12162755 - 11 Aug 2022

Cited by 4 | Viewed by 1717

Abstract

Recovery phosphorus (P) from P-contaminated wastewater is an efficient and environmentally friendly mean to prevent water pollution and alleviate the P shortage crisis. In this study, oyster shell as calcium sources and peanut shells as carbon sources (mass ratio 1:1) were used to [...] Read more.

Recovery phosphorus (P) from P-contaminated wastewater is an efficient and environmentally friendly mean to prevent water pollution and alleviate the P shortage crisis. In this study, oyster shell as calcium sources and peanut shells as carbon sources (mass ratio 1:1) were used to prepare a novel Ca-modified biochar (OBC) via co-pyrolysis, and its potential application after P adsorption as a P biofertilizer for soil was also investigated. The results shown that OBC had a remarkable P adsorption capacity from wastewater in a wide range of pH 4–12. The maximum P adsorption capacity of OBC was about 168.2 mg/g with adsorbent dosage 1 g/L, which was about 27.6 times that of the unmodified biochar. The adsorption isotherm and kinetic data were better described by Langmuir isotherm model (R² > 0.986) and the pseudo second-order model (R² > 0.975), respectively. Characterization analysis of OBC before and after P adsorption by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and specific surface area and porosity analyzer (BET) indicated that the remarkable P adsorption capacity of OBC was mainly ascribed to chemical precipitation, electrostatic adsorption, and hydrogen bonding. Pot experiment results showed that OBC after P adsorption could significantly promote the germination and growth of Spinacia, which manifested that OBC after P adsorption exhibited a good ability to be reused as P fertilizer for soil. Full article

(This article belongs to the Special Issue Nanomaterials-Based Sample Pretreatment)

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16 pages, 2964 KiB

Open AccessArticle

Development of Eggshell-Based Orange Peel Activated Carbon Film for Synergetic Adsorption of Cadmium (II) Ion

by Joseph Merillyn Vonnie, Chua Shek Li, Kana Husna Erna, Koh Wee Yin, Wen Xia Ling Felicia, Md Nasir Nur’ Aqilah and Kobun Rovina

Nanomaterials 2022, 12(16), 2750; https://doi.org/10.3390/nano12162750 - 11 Aug 2022

Cited by 3 | Viewed by 2029

Abstract

Heavy metal contamination has spread around the world, particularly in emerging countries. This study aimed to assess the effectiveness of starch/eggshell/orange peel-activated carbon-based composite films in removing cadmium (II) ions from water samples. X-ray diffraction and scanning electron microscopy were used to characterize [...] Read more.

Heavy metal contamination has spread around the world, particularly in emerging countries. This study aimed to assess the effectiveness of starch/eggshell/orange peel-activated carbon-based composite films in removing cadmium (II) ions from water samples. X-ray diffraction and scanning electron microscopy were used to characterize the composite films. The effect of Cd²⁺ was studied using a UV-Vis spectrophotometer and atomic absorption spectroscopy. The morphology of the composite film reveals a highly porous and rough surface with more open channels and a non-uniform honeycomb, indicating that the film has a high potential to adsorb Cd²⁺. The diffraction peaks for this film were found to be at 13.74°, 17.45°, 18.4°, and 23.6°, indicating a typical crystalline A-type packing arrangement within the starch granules. The results indicate that crystalline structure was unaffected by the addition of eggshell powder and orange peel-activated carbon. In 0.5 mg L⁻¹ and 1.0 mg L⁻¹ Cd²⁺ ions, the composite film removed 100% and 99.7% of the Cd²⁺, respectively, while the maximum removal efficiency for methylene blue was 93.75%. Thus, the current study shows that starch/eggshell/orange peel activated carbon film has a high potential for commercial activated carbon as a low-cost adsorbent. Full article

(This article belongs to the Special Issue Nanomaterials-Based Sample Pretreatment)

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13 pages, 4848 KiB

Open AccessArticle

Covalent Organic Framework/Polyacrylonitrile Electrospun Nanofiber for Dispersive Solid-Phase Extraction of Trace Quinolones in Food Samples

by Jinghui Zhou, An Chen, Hongying Guo, Yijun Li, Xiwen He, Langxing Chen and Yukui Zhang

Nanomaterials 2022, 12(14), 2482; https://doi.org/10.3390/nano12142482 - 20 Jul 2022

Cited by 11 | Viewed by 1958

Abstract

The extraction of quinolone antibiotics (QAs) is crucial for the environment and human health. In this work, polyacrylonitrile (PAN)/covalent organic framework TpPa–1 nanofiber was prepared by an electrospinning technique and used as an adsorbent for dispersive solid-phase extraction (dSPE) of five QAs in [...] Read more.

The extraction of quinolone antibiotics (QAs) is crucial for the environment and human health. In this work, polyacrylonitrile (PAN)/covalent organic framework TpPa–1 nanofiber was prepared by an electrospinning technique and used as an adsorbent for dispersive solid-phase extraction (dSPE) of five QAs in the honey and pork. The morphology and structure of the adsorbent were characterized, and the extraction and desorption conditions for the targeted analytes were optimized. Under the optimal conditions, a sensitive method was developed by using PAN/TpPa–1 nanofiber as an adsorbent coupled with high-performance liquid chromatography (HPLC) for five QAs detection. It offered good linearity in the ranges of 0.5–200 ng·mL⁻¹ for pefloxacin, enrofloxacin, and orbifloxacin, and of 1–200 ng·mL⁻¹ for norfloxacin and sarafloxacin with correlation coefficients above 0.9946. The limits of detection (S/N = 3) of five QAs ranged from 0.03 to 0.133 ng·mL⁻¹. The intra-day and inter-day relative standard deviations of the five QAs with the spiked concentration of 50 ng·mL⁻¹ were 2.8–4.0 and 3.0–8.8, respectively. The recoveries of five QAs in the honey and pork samples were 81.6–119.7%, which proved that the proposed method has great potential for the efficient extraction and determination of QAs in complex samples. Full article

(This article belongs to the Special Issue Nanomaterials-Based Sample Pretreatment)

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12 pages, 3439 KiB

Open AccessArticle

Selective Detection of Nucleotides in Infant Formula Using an N-Rich Covalent Triazine Porous Polymer

by Yafei Hou, Xiaodan Pei, Yuancheng Wang, Luyuan Zhang, Xiaohui Wei, Hongyan Mao, Wuduo Zhao, Shusheng Zhang and Wenfen Zhang

Nanomaterials 2022, 12(13), 2213; https://doi.org/10.3390/nano12132213 - 28 Jun 2022

Cited by 3 | Viewed by 1375

Abstract

The aromatic structure and the rich nitrogen content of polymers based on covalent triazine-based frameworks (CTF) and their unique hydrophilic-lipophilic-balanced adsorption properties make them promising candidates for an adsorbent that can be used for sample pretreatment. Herein, a new covalent triazine-based framework (CTF-DBF) [...] Read more.

The aromatic structure and the rich nitrogen content of polymers based on covalent triazine-based frameworks (CTF) and their unique hydrophilic-lipophilic-balanced adsorption properties make them promising candidates for an adsorbent that can be used for sample pretreatment. Herein, a new covalent triazine-based framework (CTF-DBF) synthesized by a Friedel–Crafts reaction was used for the determination of the content of nucleotides in commercial infant formula. It was shown that the synthetic materials had an amorphous microporous structure, a BET surface area of up to 595.59 m²/g, and 0.39 nm and 0.54 nm micropores. The versatile adsorption properties of this material were evaluated by quantum chemistry theory calculations and batch adsorption experiments using five nucleotides as probes. The quantum chemistry results demonstrated that CTF-DBF can participate in multiple interactions with nucleotides. All the analyses performed present good linearity with R² > 0.9993. The detection limits of targets ranged from 0.3 to 0.5 mg/kg, the spiked recoveries were between 85.8 and 105.3% and the relative standard deviations (RSD, n = 6) were between 1.1 and 4.5%. All these results suggest that this versatile CTF-DBF has great potential for sample pretreatment. Full article

(This article belongs to the Special Issue Nanomaterials-Based Sample Pretreatment)

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16 pages, 4385 KiB

Open AccessArticle

Porous Hexagonal Boron Nitride as Solid-Phase Microextraction Coating Material for Extraction and Preconcentration of Polycyclic Aromatic Hydrocarbons from Soil Sample

by Dan Li, Mengyuan Li, Shiping Zhu, Yanmei Gao, Mengyao Mu, Ning Zhang, Youmei Wang and Minghua Lu

Nanomaterials 2022, 12(11), 1860; https://doi.org/10.3390/nano12111860 - 29 May 2022

Cited by 2 | Viewed by 1861

Abstract

Sample pretreatment plays important role in the analysis and detection of trace pollutants in complex matrices, such as environmental and biological samples. The adsorption materials of sample pretreatment receive considerable attention, which has a significant effect on the sensitivity and selectivity of the [...] Read more.

Sample pretreatment plays important role in the analysis and detection of trace pollutants in complex matrices, such as environmental and biological samples. The adsorption materials of sample pretreatment receive considerable attention, which has a significant effect on the sensitivity and selectivity of the analytical method. In this work, the porous hexagonal boron nitride (h-BN) was utilized as a coating material of solid-phase microextraction (SPME) to extract and preconcentrate polycyclic aromatic hydrocarbons (PAHs) prior to separation and detection with GC-FID. Attributed to the multiple interactions including hydrophobicity, hydrogen bonding and strong π–π interaction, the h-BN coating showed excellent extraction performance for PAHs. Under the optimal conditions, the method showed the linear relationship in the range of 0.1–50 ng mL⁻¹ for acenaphthene, 0.05–50 ng mL⁻¹ for pyrene, and 0.02–50 ng mL⁻¹ for fluorene, phenanthrene and anthracene with a correlation coefficient (R²) not lower than 0.9910. The enrichment factors were achieved between 1526 and 4398 for PAHs with h-BN as SPME fiber coating. The detection limits were obtained in the range of 0.004–0.033 ng mL⁻¹, which corresponds to 0.08–0.66 ng g⁻¹ for soil. The method was successfully applied to analysis of real soil samples. The recoveries were determined between 78.0 and 120.0% for two soil samples. The results showed that h-BN material provided a promising alternative in sample pretreatment and analysis. Full article

(This article belongs to the Special Issue Nanomaterials-Based Sample Pretreatment)

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10 pages, 5632 KiB

Open AccessArticle

Silica Aerogel Hybridized with Melamine-Terephthalaldehyde Polymer for In-Tube Solid-Phase Microextraction of Polycyclic Aromatic Hydrocarbons from Environment Water

by Qiong Jiang, Shuwu Zhang, Juanjuan Feng and Min Sun

Nanomaterials 2022, 12(10), 1766; https://doi.org/10.3390/nano12101766 - 22 May 2022

Viewed by 1686

Abstract

To improve the extraction performance of the silica aerogel, a melamine-terephthalaldehyde polymer was used to hybridize silica aerogel, and the hybridized aerogel was coated on the surface of stainless steel wire to prepare a fiber-filled extraction tube through placing four wires into a [...] Read more.

To improve the extraction performance of the silica aerogel, a melamine-terephthalaldehyde polymer was used to hybridize silica aerogel, and the hybridized aerogel was coated on the surface of stainless steel wire to prepare a fiber-filled extraction tube through placing four wires into a polyetheretherketone tube. The tube was combined with high-performance liquid chromatography, then the online extraction and detection were established. Several polycyclic aromatic hydrocarbons (PAHs) were selected as the target analytes. Under the optimum extraction and desorption conditions, the limit of detection was as low as 3.0 ng L⁻¹, and the linear range was 0.01–20.0 μg L⁻¹. The enrichment factors of PAHs were in the range of 1724–2393. Three environmental water samples of mineral water, tap water and river water were analyzed by this method, and the recoveries that spiked at 1.0–10.0 μg L⁻¹ were between 80.5–126%. It showed many advantages compared with other methods, such as better sensitivity, faster detection and online analysis. Full article

(This article belongs to the Special Issue Nanomaterials-Based Sample Pretreatment)

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14 pages, 2212 KiB

Open AccessArticle

A Sustainable Strategy for Solid-Phase Extraction of Antiviral Drug from Environmental Waters by Immobilized Hydrogen Bond Acceptor

by Hongrui Yang, Chen Wang, Wenjuan Zhu, Xia Zhang, Tiemei Li and Jing Fan

Nanomaterials 2022, 12(8), 1287; https://doi.org/10.3390/nano12081287 - 10 Apr 2022

Cited by 3 | Viewed by 1370

Abstract

Deep eutectic solvents are a new generation of green solvents composed of hydrogen bond acceptors and donors. However, when used as extractants in liquid–liquid separation, they are difficult to recycle and easy to lose. In order to solve these problems, herein, immobilized hydrogen [...] Read more.

Deep eutectic solvents are a new generation of green solvents composed of hydrogen bond acceptors and donors. However, when used as extractants in liquid–liquid separation, they are difficult to recycle and easy to lose. In order to solve these problems, herein, immobilized hydrogen bond acceptor adsorbent material was prepared for the separation and enrichment of antiviral drug arbidol from seven kinds of environmental water samples by in situ formation of hydrophobic deep eutectic solvents. The structure, morphology and thermal stability of the adsorbents were characterized, the separation and enrichment conditions for the targeted analyte were optimized, and the adsorption thermodynamics and kinetics were investigated. It was found that the adsorbent material could effectively enrich trace arbidol with the recovery more than 95% at the concentration above 7.5 ng/mL, and the enrichment factor was as high as 634.7. Coexisting substances, such as NaCl, KCl, CaCl₂ and MgCl₂, did not interfere with the adsorption of arbidol, even if their concentration was high, up to 1.0 mol/L, and the relative recovery for real samples was in the range from 92.5% to 100.3%. Furthermore, the immobilized hydrogen bond acceptor could be recycled and reused, and the recovery of arbidol was still above 95% after 12 adsorption–desorption cycles. The mechanism study demonstrates that the synergistic effect of hydrogen bonding and π-π stacking is the primary factor for the high adsorption efficiency. Full article

(This article belongs to the Special Issue Nanomaterials-Based Sample Pretreatment)

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16 pages, 4985 KiB

Open AccessArticle

Rapid Determination of Vitamin D₃ in Aquatic Products by Polypyrrole-Coated Magnetic Nanoparticles Extraction Coupled with High-Performance Liquid Chromatography Detection

by Xinyan Liu, Ru Song and Rongbian Wei

Nanomaterials 2022, 12(7), 1226; https://doi.org/10.3390/nano12071226 - 06 Apr 2022

Cited by 7 | Viewed by 1960

Abstract

A method using polypyrrole-coated Fe₃O₄ (Fe₃O₄@PPy composites) based extraction coupled with high performance liquid chromatography was developed for adsorption and detection of trace vitamin D₃ (VD₃) in aquatic products. The fabricated Fe₃ [...] Read more.

A method using polypyrrole-coated Fe₃O₄ (Fe₃O₄@PPy composites) based extraction coupled with high performance liquid chromatography was developed for adsorption and detection of trace vitamin D₃ (VD₃) in aquatic products. The fabricated Fe₃O₄@PPy composites were characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Fourier transform infrared spectroscopy, and thermogravimetric analysis. Fe₃O₄@PPy composites showed efficient adsorption of VD₃ at pH 9.0 and 25 °C with a dose of 25 mg per 10 mL of sample solution and an adsorption time of 11 min. Methanol was selected as the desorption solvent to recover VD₃ from Fe₃O₄@PPy composites after 3 min of static treatment. Fe₃O₄@PPy composites can be used for VD₃ adsorption at least two times. The developed method showed a good linearity for VD₃ determination in the range of 0.1–10 μg/mL with a correlation coefficient of 0.9989. The limits of detection and quantification were 10 ng/mL and 33 ng/mL, respectively. The recovery of VD₃ in a spiking test was 97.72% with a relative standard deviation value of 1.78%. The content of VD₃ in nine aquatic products was determined with this method. Our results show that Fe₃O₄@PPy composites provide a convenient method for the adsorption and determination of VD₃ from the complex matrix of aquatic products. Full article

(This article belongs to the Special Issue Nanomaterials-Based Sample Pretreatment)

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12 pages, 1548 KiB

Open AccessArticle

Carbon Dot-Decorated Graphite Carbon Nitride Composites for Enhanced Solid-Phase Microextraction of Chlorobenzenes from Water

by Shengrui Xu, Hailin Liu, Anying Long, Huimin Li, Changpo Chen, Suling Feng and Jing Fan

Nanomaterials 2022, 12(3), 335; https://doi.org/10.3390/nano12030335 - 21 Jan 2022

Cited by 10 | Viewed by 1836

Abstract

In this work, carbon dot-decorated graphite carbon nitride composites (CDs/g-C₃N₄) were synthesized and innovatively used as a SPME coating for the sensitive determination of chlorobenzenes (CBs) from water samples, coupled with gas chromatography–mass spectrometry. The CDs/g-C₃N₄ [...] Read more.

In this work, carbon dot-decorated graphite carbon nitride composites (CDs/g-C₃N₄) were synthesized and innovatively used as a SPME coating for the sensitive determination of chlorobenzenes (CBs) from water samples, coupled with gas chromatography–mass spectrometry. The CDs/g-C₃N₄ coating presented superior extraction performance in comparison to pristine g-C₃N₄, owing to the enhancement of active groups by CDs. The extraction capacities of as-prepared SPME coatings are higher than those of commercial coatings due to the functions of nitrogen-containing and oxygen-containing group binding, π–π stacking, and hydrophobic interactions. Under optimized conditions, the proposed method exhibits a wide linearity range (0.25–2500 ng L⁻¹), extremely low detection of limits (0.002–0.086 ng L⁻¹), and excellent precision, with relative standard deviations of 5.3–9.7% for a single fiber and 7.5–12.6% for five fibers. Finally, the proposed method was successfully applied for the analysis of CBs from real river water samples, with spiked recoveries ranging from 73.4 to 109.1%. This study developed a novel and efficient SPME coating material for extracting organic pollutants from environmental samples. Full article

(This article belongs to the Special Issue Nanomaterials-Based Sample Pretreatment)

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Review

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26 pages, 8353 KiB

Open AccessReview

Nanomaterials with Excellent Adsorption Characteristics for Sample Pretreatment: A Review

by Wen-Xin Liu, Shuang Song, Ming-Li Ye, Yan Zhu, Yong-Gang Zhao and Yin Lu

Nanomaterials 2022, 12(11), 1845; https://doi.org/10.3390/nano12111845 - 27 May 2022

Cited by 15 | Viewed by 2483

Abstract

Sample pretreatment in analytical chemistry is critical, and the selection of materials for sample pretreatment is a key factor for high enrichment ability, good practicality, and satisfactory recoveries. In this review, the recent progress of the sample pretreatment methods based on various nanomaterials [...] Read more.

Sample pretreatment in analytical chemistry is critical, and the selection of materials for sample pretreatment is a key factor for high enrichment ability, good practicality, and satisfactory recoveries. In this review, the recent progress of the sample pretreatment methods based on various nanomaterials (i.e., carbon nanomaterials, porous nanomaterials, and magnetic nanomaterials) with excellent adsorption efficiency, selectivity, and reproducibility, as well as their applications, are presented. Due to the unique nanoscale physical–chemical properties, magnetic nanomaterials have been used for the extraction of target analytes by easy-to-handle magnetic separation under a magnetic field, which can avoid cumbersome centrifugation and filtration steps. This review also highlights the preparation process and reaction mechanism of nanomaterials used in the sample pretreatment methods, which have been applied for the extraction organophosphorus pesticides, fluoroquinolone antibiotics, phenoxy carboxylic acids, tetracycline antibiotics, hazardous metal ions, and rosmarinic acid. In addition, the remaining challenges and future directions for nanomaterials used as sorbents in the sample pretreatment are discussed. Full article

(This article belongs to the Special Issue Nanomaterials-Based Sample Pretreatment)

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18 pages, 2074 KiB

Open AccessReview

The Adsorption of Heavy Metal Ions by Poly (Amidoamine) Dendrimer-Functionalized Nanomaterials: A Review

by Dandan Guo, Shaohua Huang and Yan Zhu

Nanomaterials 2022, 12(11), 1831; https://doi.org/10.3390/nano12111831 - 27 May 2022

Cited by 10 | Viewed by 1991

Abstract

Rapid industrialization has resulted in serious heavy metal pollution. The removal of heavy metal ions from solutions is very important for environmental safety and human health. Poly (amidoamine) (PAMAM) dendrimers are artificial macromolecular materials with unique physical and chemical properties. Abundant amide bonds [...] Read more.

Rapid industrialization has resulted in serious heavy metal pollution. The removal of heavy metal ions from solutions is very important for environmental safety and human health. Poly (amidoamine) (PAMAM) dendrimers are artificial macromolecular materials with unique physical and chemical properties. Abundant amide bonds and amino functional groups provide them with a high affinity for heavy metal ions. Herein, PAMAM-functionalized adsorbents are reviewed in terms of different nanomaterial substrates. Approaches in which PAMAM is grafted onto the surfaces of substrates are described in detail. The adsorption isotherms and kinetics of these adsorbents are also discussed. The effects of PAMAM generation, pH, adsorbent dosage, adsorption time, thermodynamics, and ionic strength on adsorption performance are summarized. Adsorption mechanisms and the further functionalization of PAMAM-grafted adsorbents are reviewed. In addition to the positive results, existing problems are also put forward in order to provide a reference for the optimization of PAMAM-grafted adsorbents of heavy metal ions. Full article

(This article belongs to the Special Issue Nanomaterials-Based Sample Pretreatment)

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