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Physico-Chemical Analysis of Engineered Nanomaterials

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A special issue of Materials (ISSN 1996-1944). This special issue belongs to the section "Advanced Nanomaterials and Nanotechnology".

Deadline for manuscript submissions: closed (20 May 2023) | Viewed by 35238

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Dr. Erika Andrea Levei

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INCDO-INOE 2000, Research Institute for Analytical Instrumentation, 400293 Cluj-Napoca, Romania
Interests: analytical chemistry; nanocomposites; infrared spectroscopy; sol–gel synthesis; spinel ferrite
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Dr. Oana Cadar

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INCDO-INOE 2000, Research Institute for Analytical Instrumentation, 400293 Cluj-Napoca, Romania
Interests: porous materials; nanomaterials; synthesis; X-ray diffraction; applications
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

In the last few years, the need for raw materials with specific characteristics in industries has sharply increased. To satisfy this demand, research related to the development and characterization of new materials and the identification of new applications for existing materials bloomed. In this sense, engineered nanomaterials have been put in the spotlight as they have outstanding structural and functional features. The characterization of nanomaterials is an important step in determining their structure, properties, and potential applications. The physico-chemical characterization methods are excellent tools to explore the composition, purity, structure, stability, particle shape, size, size distribution, surface properties, chemical and thermal behavior, and dielectric, magnetic, or optical properties. Based on the provided information, the most commonly used techniques for nanomaterial characterization are as follows: (i) structure – X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and atomic force microscopy (AFM); (ii) composition – Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, nuclear magnetic resonance (NMR), energy-dispersion X-ray spectroscopy (EDS), X-ray fluorescence (XRF), X-ray photoelectron spectroscopy (XPS), and inductively coupled plasma optical emission spectrometry (ICP-OES); (iii) thermal behavior –thermogravimetry (TGA), differential thermal analysis (DTA), and differential scanning calorimetry (DSC); (iv) magnetic behavior (Mössbauer spectroscopy and vibrating sample magnetometry (VSM)). This Special Issue will gather information on the application of different physico-chemical characterization methods in the development of new engineered nanomaterials or the identification of new properties of existing materials.

Dr. Erika Andrea Levei
Dr. Oana Cadar
Guest Editors

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Keywords

nanomaterials
physico-chemical methods
structure
composition
thermal behavior
magnetic behavior

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Published Papers (11 papers)

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Research

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13 pages, 4906 KiB

Open AccessArticle

In Vitro Degradation of Mg-Doped ZrO₂ Bioceramics at the Interface with Xerostom^® Saliva Substitute Gel

by Liliana Bizo, Marieta Mureşan-Pop, Réka Barabás, Lucian Barbu-Tudoran and Antonela Berar

Materials 2023, 16(7), 2680; https://doi.org/10.3390/ma16072680 - 28 Mar 2023

Cited by 1 | Viewed by 1700

Abstract

Zirconia-based bioceramics, one of the most important materials used for dental applications, have been intensively studied in recent years due to their excellent mechanical resistance and chemical inertness in the mouth. In this work, the structural, morphological and dissolution properties of the Zr_1−xMg_xO₂ (x = 0.05, 0.1, 0.15, 0.2, 0.25, and 0.3) system, prepared by the conventional ceramic method, were evaluated before and after immersion in saliva substitute gel (Xerostom^®, Biocosmetics Laboratories, Madrid, Spain), one of the most common topical dry mouth products used in dentistry. The X-ray powder diffraction (XRPD), Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy/energy-dispersive X-ray spectroscopy (SEM/EDS) techniques were employed to investigate the phase transformations and morphology of the ceramics during the degradation process in Xerostom^®. In vitro analyses showed overall good stability in the Xerostom^® environment, except for the x = 0.05 composition, where significant t- to m-ZrO₂ transformation occurred. In addition, the strong interconnection of the grains was maintained after immersion, which could allow a high mechanical strength of the ceramics to be obtained. Full article

(This article belongs to the Special Issue Physico-Chemical Analysis of Engineered Nanomaterials)

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14 pages, 1007 KiB

Open AccessArticle

Zeolites Reduce the Transfer of Potentially Toxic Elements from Soil to Leafy Vegetables

by Oana Cadar, Zamfira Stupar, Marin Senila, Levente Levei, Ana Moldovan, Anca Becze, Alexandru Ozunu and Erika Andrea Levei

Materials 2022, 15(16), 5657; https://doi.org/10.3390/ma15165657 - 17 Aug 2022

Cited by 6 | Viewed by 1789

Abstract

The ability of natural zeolite amendment to reduce the uptake of potentially toxic elements (PTEs) by lettuce, spinach and parsley was evaluated using pot experiments. PTE concentrations in roots and shoots, as well as the pseudo total (PT), water soluble (WS) and bioavailable (BA) PTE fractions in the amended soils, were assessed. Although the PT PTE concentration was high, the WS fraction was very low (<0.4%), while the BA fraction varied widely (<5% for Cr, Mn and Co, <15% for Ni, Pb and Zn, >20% for Cd and Cu). PTE concentration decreased in both roots and shoots of all leafy vegetables grown on zeolite amended soils, especially at high amendment dose (10%). The uptake of PTEs mainly depended on plant species, PTE type and amendment dose. With the exception of Zn in spinach, the bioaccumulation factor for roots was higher than for shoots. Generally, lettuce displayed the highest PTE bioaccumulation capacity, followed by spinach and parsley. Except for Zn in spinach, the transfer factors were below 1 for all PTEs, all plant species and all amendment doses. Our results showed that the natural zeolites are promising candidates in the reclamation of contaminated soils due to their ability to immobilize PTEs. Full article

(This article belongs to the Special Issue Physico-Chemical Analysis of Engineered Nanomaterials)

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18 pages, 3832 KiB

Open AccessArticle

The Potential Application of Natural Clinoptilolite-Rich Zeolite as Support for Bacterial Community Formation for Wastewater Treatment

by Lacrimioara Senila, Alexandra Hoaghia, Ana Moldovan, Iulia Anamaria Török, Dalma Kovacs, Dorina Simedru, Calin Horea Tomoiag and Marin Senila

Materials 2022, 15(10), 3685; https://doi.org/10.3390/ma15103685 - 20 May 2022

Cited by 17 | Viewed by 2885

Abstract

The aim of this study was to investigate the use of natural zeolite as support for microbial community formation during wastewater treatment. Scanning electron microscopy (SEM), thermal decomposition and differential thermogravimetric curves (TGA/DGT) techniques were used for the physicochemical and structural characterization of zeolites. The chemical characterization of wastewater was performed before and after treatment, after 30 days of using stationary zeolite as support. The chemical composition of wastewater was evaluated in terms of the products of nitrification/denitrification processes. The greatest ammonium (NH₄⁺) adsorption was obtained for wastewater contaminated with different concentrations of ammonium, nitrate and nitrite. The wastewater quality index (WWQI) was determined to assess the effluent quality and the efficiency of the treatment plant used, showing a maximum of 71% quality improvement, thus suggesting that the treated wastewater could be discharged into aquatic environments. After 30 days, NH₄⁺ demonstrated a high removal efficiency (higher than 98%), while NO₃⁺ and NO₂⁺ had a removal efficiency of 70% and 54%, respectively. The removal efficiency for metals was observed as follows (%): Mn > Cd > Cr > Zn > Fe > Ni > Co > Cu > Ba > Pb > Sr. Analysis of the microbial diversity in the zeolite samples indicated that the bacteria are formed due to the existence of nutrients in wastewater which favor their formation. In addition, the zeolite was characterized by SEM and the results indicated that the zeolite acts as an adsorbent for the pollutants and, moreover, as a support material for microbial community formation under optimal conditions. Comparing the two studied zeolites, NZ1 (particle size 1–3 mm) was found to be more suitable for wastewater treatment. Overall, the natural zeolite demonstrated high potential for pollutant removal and biomass support for bacteria community growth in wastewater treatment. Full article

(This article belongs to the Special Issue Physico-Chemical Analysis of Engineered Nanomaterials)

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16 pages, 4514 KiB

Open AccessArticle

Preparation and Characterization of Doxycycline-Loaded Electrospun PLA/HAP Nanofibers as a Drug Delivery System

by Noémi-Izabella Farkas, Laura Marincaș, Réka Barabás, Liliana Bizo, Aranka Ilea, Graziella Liana Turdean, Monica Toșa, Oana Cadar and Lucian Barbu-Tudoran

Materials 2022, 15(6), 2105; https://doi.org/10.3390/ma15062105 - 12 Mar 2022

Cited by 29 | Viewed by 4824

Abstract

The present study aimed to prepare nanofibers by electrospinning in the system polylactic acid-hydroxyapatite-doxycycline (PLA-HAP-Doxy) to be used as a drug delivery vehicle. Two different routes were employed for the preparation of Doxy-containing nanofibers: Immobilization on the electrospun mat’s surface and encapsulation in the fiber structure. The nanofibers obtained by Doxy encapsulation were characterized using Fourier transform infrared (FTIR) spectroscopy, thermogravimetric (TG) and differential thermal analyses (DTA) and scanning electron microscopy (SEM). The adsorption properties of pure PLA and PLA-HAP nanofibers were investigated for solutions with different Doxy concentrations (3, 7 and 12 wt%). Moreover, the desorption properties of the active substance were tested in two different fluids, simulated body fluid (SBF) and phosphate buffer solution (PBS), to evidence the drug release properties. In vitro drug release studies were performed and different drug release kinetics were assessed to confirm the use of these nanofiber materials as efficient drug delivery vehicles. The obtained results indicate that the PLA-HAP-Doxy is a promising system for biomedical applications, the samples with 3 and 7 wt% of Doxy-loaded PLA-HAP nanofibers prepared by physical adsorption are the most acceptable membranes to provide prolonged release in PBS/SBF rather than an immediate release of Doxy. Full article

(This article belongs to the Special Issue Physico-Chemical Analysis of Engineered Nanomaterials)

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13 pages, 1183 KiB

Open AccessArticle

Assessment of Lithium, Macro- and Microelements in Water, Soil and Plant Samples from Karst Areas in Romania

by Anamaria Iulia Török, Ana Moldovan, Erika Andrea Levei, Oana Cadar, Claudiu Tănăselia and Oana Teodora Moldovan

Materials 2021, 14(14), 4002; https://doi.org/10.3390/ma14144002 - 17 Jul 2021

Cited by 18 | Viewed by 2985

Abstract

Lithium is a critical element for the modern society due to its uses in various industrial sectors. Despite its unequal distribution in the environment, Li occurrence in Romania was scarcely studied. In this study a versatile measurement method using ICP-MS technique was optimized for the determination of Li from various matrixes. Water, soil, and plant samples were collected from two important karst areas in the Dobrogea and Banat regions, Romania. The Li content was analyzed together with other macro- and microelement contents to find the relationship between the concentration of elements and their effect on the plants’ Li uptake. In Dobrogea region, half of the studied waters had high Li concentration, ranging between 3.00 and 12.2 μg/L in the case of water and between 0.88 and 11.1 mg/kg DW in the case of plants, while the Li content in the soil samples were slightly comparable (from 9.85 to 11.3 mg/kg DW). In the Banat region, the concentration of Li was lower than in Dobrogea (1.40–1.46 μg/L in water, 6.50–9.12 mg/kg DW in soil, and 0.19–0.45 mg/kg DW in plants). Despite the high Li contents in soil, the Li was mostly unavailable for plants uptake and bioaccumulation. Full article

(This article belongs to the Special Issue Physico-Chemical Analysis of Engineered Nanomaterials)

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15 pages, 2242 KiB

Open AccessArticle

Immobilization of Potentially Toxic Elements in Contaminated Soils Using Thermally Treated Natural Zeolite

by Oana Cadar, Zamfira Dinca, Marin Senila, Anamaria Iulia Torok, Florin Todor and Erika Andrea Levei

Materials 2021, 14(14), 3777; https://doi.org/10.3390/ma14143777 - 6 Jul 2021

Cited by 13 | Viewed by 2286

Abstract

Rehabilitation of contaminated soils is a complex and time-consuming procedure. One of the most cost-effective and easy-to-use soil remediation approaches is the use of amendments that stabilize the potential toxic elements (PTE) in soil by reducing their mobility and bioavailability. The stabilization of Cu, Pb, Zn, Cd, Co, Cr, Ni in a contaminated soil using 5% and 10% amendment with thermally treated natural zeolite was investigated using a sequential extraction procedure, contamination and environmental risk factors. The results showed that after amendment, the PTE concentration decreased in the exchangeable and reducible fractions and increased in the oxidizable and residual fractions. The highest immobilization effect, consisting in the decrease of exchangeable fractions with 69% was obtained in case of 10% zeolite amendment and 90 days of equilibration time for Pb; also, more than half of the mobile fraction was immobilized in case of Zn, Cu, and Co and about one third in case of Ni, Cr, and Cd. Generally, the immobilization effect of the 5% and 10% amendment is comparable, but a higher equilibration time enhanced the immobilization effect, especially in the case of Cd, Co, Cu, Pb, and Zn. Full article

(This article belongs to the Special Issue Physico-Chemical Analysis of Engineered Nanomaterials)

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16 pages, 5244 KiB

Open AccessArticle

Evaluation of the Impact of Different Natural Zeolite Treatments on the Capacity of Eliminating/Reducing Odors and Toxic Compounds

by Vanda Liliana Babalau Fuss, Gabriel Bruj, Lucian Dordai, Marius Roman, Oana Cadar and Anca Becze

Materials 2021, 14(13), 3724; https://doi.org/10.3390/ma14133724 - 2 Jul 2021

Cited by 15 | Viewed by 3072

Abstract

Unlike odorants that mask odors, natural zeolite acts as a molecular sieve that captures and eliminates odors. Different treatment methods can be applied to influence the properties of the natural zeolites. To enhance the odor adsorption capacities of the natural zeolite two types of treatment methods were applied: chemical (acid, basic) and thermal. The initial natural zeolites and the activated one were characterized using X-ray diffraction (XRD) and scanning electron microscope (SEM-EDX). Two experiments were performed to establish the odor adsorption capacity of the activated natural zeolites. The best zeolite for the adsorption of humidity, ammonia and hydrogen sulfide was the 1–3 mm zeolite activated through thermal treatment. For the adsorption of PAHs, the best zeolite was the one activated through basic treatment, with an adsorption capacity of 89.6 ng/g. Full article

(This article belongs to the Special Issue Physico-Chemical Analysis of Engineered Nanomaterials)

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15 pages, 1927 KiB

Open AccessArticle

Formation, Structure and Magnetic Properties of MFe₂O₄@SiO₂ (M = Co, Mn, Zn, Ni, Cu) Nanocomposites

by Thomas Dippong, Erika Andrea Levei and Oana Cadar

Materials 2021, 14(5), 1139; https://doi.org/10.3390/ma14051139 - 28 Feb 2021

Cited by 83 | Viewed by 3505

Abstract

The formation, structure, and thermal and magnetic properties of MFe₂O₄@SiO₂ (M = Co, Mn, Zn, Ni, Cu) (60% MFe₂O₄/40% SiO₂) nanocomposites produced by a modified sol-gel method, followed by annealing at 300, 600, 900 and 1200 °C, were studied. The thermal analysis and Fourier transform infrared spectroscopy showed the formation of metal-glyoxylates below 210 °C and their decomposition into the corresponding ferrite around 300 °C. The evolution of crystalline phases and variation of crystallite sizes differs from ferrite to ferrite and depends on the annealing temperature. The magnetic measurements revealed the dependence of saturation and remanent magnetization, coercivity, and anisotropy on ferrite type, annealing temperature, and particle size. By annealing the nanocomposites (NCs) at 1200 °C paramagnetic MnFe₂O₄, CoFe₂O₄, NiFe₂O₄ and CuFe₂O₄ and antiferromagnetic ZnFe₂O₄ are obtained. Full article

(This article belongs to the Special Issue Physico-Chemical Analysis of Engineered Nanomaterials)

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13 pages, 453 KiB

Open AccessArticle

Performance Parameters of Inductively Coupled Plasma Optical Emission Spectrometry and Graphite Furnace Atomic Absorption Spectrometry Techniques for Pd and Pt Determination in Automotive Catalysts

by Marin Senila, Oana Cadar, Lacrimioara Senila, Sarah Böringer, Karine Seaudeau-Pirouley, Andrea Ruiu and Patrick Lacroix-Desmazes

Materials 2020, 13(22), 5136; https://doi.org/10.3390/ma13225136 - 14 Nov 2020

Cited by 15 | Viewed by 3203

Abstract

Palladium (Pd) and platinum (Pt) are extensively used as catalysts in the petrochemical and automotive industries, and due to high demand for them on the market, their recycling from spent supported catalysts is clearly needed. To assess the content of Pd and Pt in catalysts in order to establish their commercial value or to evaluate the recovery efficiency of technologies used for recycling, reliable analytical methods for determination of these elements are required. Spectrometric methods, such as inductively coupled plasma optical emission spectrometry (ICP-OES) and graphite furnace atomic absorption spectrometry (GFAAS) are powerful tools that can be employed for the determination of Pd and Pt in various sample matrices. However, these methods allow only the injection of liquid samples. In this regard, the digestion of solid sample by microwave-assisted acid extraction procedures at high pressures and temperatures is often used. In this study, a microwave acid digestion method was optimized for the extraction of Pd and Pt from spent catalysts, using a four-step program, at a maximum 200 °C. The resulting solutions were analyzed using ICP-OES, at two different wavelengths for each metal (Pd at 340.458 and 363.470 nm, and Pt at 265.945 and 214.423 nm, respectively) and using GFAAS (Pd at 247.64 nm, Pt at 265.94 nm). Five types of spent catalyst were analyzed and the standard deviations of repeatability for five parallel samples were less than predicted relative standard deviations (PRSD%) calculated using Horvitz’s equation for all the analyzed samples. Full article

(This article belongs to the Special Issue Physico-Chemical Analysis of Engineered Nanomaterials)

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Review

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23 pages, 2261 KiB

Open AccessReview

Recent Trends in Hydroxyapatite Supplementation for Osteoregenerative Purposes

by Ana Zastulka, Simona Clichici, Maria Tomoaia-Cotisel, Aurora Mocanu, Cecilia Roman, Cristian-Doru Olteanu, Bogdan Culic and Teodora Mocan

Materials 2023, 16(3), 1303; https://doi.org/10.3390/ma16031303 - 3 Feb 2023

Cited by 29 | Viewed by 3786

Abstract

Bone regeneration has gained attention in the biomedical field, which has led to the development of materials and synthesis methods meant to improve osseointegration and cellular bone activity. The properties of hydroxyapatite, a type of calcium phosphate, have been researched to determine its advantages for bone tissue engineering, particularly its biocompatibility and ability to interact with bone cells. Recently, the advantages of utilizing nanomolecules of hydroxyapatite, combined with various substances, in order to enhance and combine their characteristics, have been reported in the literature. This review will outline the cellular and molecular roles of hydroxypatite, its interactions with bone cells, and its nano-combinations with various ions and natural products and their effects on bone growth, development, and bone repair. Full article

(This article belongs to the Special Issue Physico-Chemical Analysis of Engineered Nanomaterials)

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17 pages, 1667 KiB

Open AccessReview

Biomarkers in Pancreatic Cancer as Analytic Targets for Nanomediated Imaging and Therapy

by Cristiana Maria Grapa, Lucian Mocan, Dana Crisan, Mira Florea and Teodora Mocan

Materials 2021, 14(11), 3083; https://doi.org/10.3390/ma14113083 - 4 Jun 2021

Cited by 5 | Viewed by 2999

Abstract

As the increase in therapeutic and imaging technologies is swiftly improving survival chances for cancer patients, pancreatic cancer (PC) still has a grim prognosis and a rising incidence. Practically everything distinguishing for this type of malignancy makes it challenging to treat: no approved method for early detection, extended asymptomatic state, limited treatment options, poor chemotherapy response and dense tumor stroma that impedes drug delivery. We provide a narrative review of our main findings in the field of nanoparticle directed treatment for PC, with a focus on biomarker targeted delivery. By reducing drug toxicity, increasing their tumor accumulation, ability to modulate tumor microenvironment and even improve imaging contrast, it seems that nanotechnology may one day give hope for better outcome in pancreatic cancer. Further conjugating nanoparticles with biomarkers that are overexpressed amplifies the benefits mentioned, with potential increase in survival and treatment response. Full article

(This article belongs to the Special Issue Physico-Chemical Analysis of Engineered Nanomaterials)

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