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1.
Talanta ; 246: 123501, 2022 Aug 15.
Artículo en Inglés | MEDLINE | ID: mdl-35525057

RESUMEN

ß-cyclodextrin/graphene oxide (GO-ß-CD) was applied for dispersive micro-solid phase extraction (DMSPE) of uranyl ions (UO22+) from water samples and their determination by energy-dispersive (EDXRF) and total-reflection X-ray fluorescence spectrometry (TXRF). The structure of GO-ß-CD was characterized by X-ray photoelectron spectroscopy, scanning electron microscopy, Fourier transform infrared spectroscopy, and Raman spectroscopy. The results of batch adsorption experiment indicate that the maximum recoveries for UO22+ ions are observed at pH 4.5. The Langmuir isotherm model fits the adsorption data, which stands for the chemisorption mechanism. The obtained adsorption capacity of 87.7 mg g-1 indicates a great potential of the synthesized adsorbent in the UO22+ ions preconcentration. The GO-ß-CD exhibits high resistance to high ionic strength (up to 2 mol L-1), indicating that high salinity samples can be treated with the evaluated preconcentration procedure. The obtained limit of detection values were 0.40 µg L-1 for the EDXRF and only 0.014 µg L-1 for TXRF analysis. The accuracy of the method was verified by analyzing certified reference material (spring water NIST-SRM 1640a) and spiked water samples (mineral, lake, river, and artificial sea water).


Asunto(s)
Grafito , Uranio , beta-Ciclodextrinas , Adsorción , Grafito/química , Agua/química , Rayos X , beta-Ciclodextrinas/química
2.
RSC Adv ; 12(11): 6377-6388, 2022 Feb 22.
Artículo en Inglés | MEDLINE | ID: mdl-35424628

RESUMEN

The 5-aminolevulinic acid (5-ALA) prodrug is widely used in clinical applications, primarily for skin cancer treatments and to visualize brain tumors in neurosurgery. Unfortunately, its applications are limited by unfavorable pharmacological properties, especially low lipophilicity; therefore, efficient nanovehicles are needed. For this purpose, we synthesized and characterized two novel water-soluble fullerene nanomaterials containing 5-ALA and d-glucuronic acid components. Their physicochemical properties were investigated using NMR, XPS, ESI mass spectrometry, as well as TEM and SEM techniques. In addition, HPLC and fluorescence measurements were performed to evaluate the biological activity of the fullerene nanomaterials in 5-ALA delivery and photodynamic therapy (PDT); additional detection of selected mRNA targets was carried out using the qRT-PCR methodology. The cellular response to the [60]fullerene conjugates resulted in increased levels of ABCG2 and PEPT-1 genes, as determined by qRT-PCR analysis. Therefore, we designed a combination PDT approach based on two fullerene materials, C60-ALA and C60-ALA-GA, along with the ABCG2 inhibitor Ko143.

3.
Materials (Basel) ; 14(10)2021 May 12.
Artículo en Inglés | MEDLINE | ID: mdl-34066302

RESUMEN

This paper refers to the structural and magnetic properties of [(Fe80Nb6B14)0.88Dy0.12]1-xZrx (x = 0; 0.01; 0.02; 0.05; 0.1; 0.2; 0.3; 0.5) alloys obtained by the vacuum mold suction casting method. The analysis of the phase contribution indicated a change in the compositions of the alloys. For x < 0.05, occurrence of the dominant Dy2Fe14B phase was observed, while a further increase in the Zr content led to the increasing contribution of the Fe-Zr compounds and, simultaneously, separation of crystalline Dy. The dilution of (Fe80Nb6B14)0.88Dy0.12 in Zr strongly influenced the magnetization processes of the examined alloys. Generally, with the increasing x parameter, we observed a decrease in coercivity; however, the unexpected increase in magnetic saturation and remanence for x = 0.2 and x = 0.3 was shown and discussed.

4.
Front Chem ; 8: 541, 2020.
Artículo en Inglés | MEDLINE | ID: mdl-32695746

RESUMEN

We present an overview of our studies on the hampering effect of heavy water (D2O) on spontaneous oscillatory peptidization of selected proteinogenic α-amino acids. The investigated set of compounds included three endogenous and two exogenous species. The experiments were carried out with use of high-performance liquid chromatography (HPLC), mass spectrometry (MS) and scanning electron microscopy (SEM). These techniques were chosen to demonstrate spontaneous oscillatory peptidization of α-amino acids in an absence of D2O (HPLC) and the hampering effect of D2O on peptidization (HPLC, MS and SEM). The HPLC analyses were carried out at 21 ± 0.5°C with each α-amino acid freshly dissolved in the binary liquid mixture of organic solvent + H2O, 70:30 (v/v) or in pure D2O for several dozen hours or several hours, respectively. The analyses with use of MS and SEM were carried out, respectively, after 7 days and 1 month of sample storage period in the darkness at 21 ± 0.5°C and for these experiments, each α-amino acid was dissolved in the liquid mixture of organic solvent + X, 70:30 (v/v), where X: H2O + D2O in volume proportions from 30:0 to 0:30. The results obtained with use of HPLC, MS and SEM point out to the strong hampering effect of D2O on the oscillations and peptidization yields, yet the dynamics of these processes significantly depends on chemical structure of a given α-amino acid.

5.
ACS Appl Mater Interfaces ; 11(31): 28582-28590, 2019 Aug 07.
Artículo en Inglés | MEDLINE | ID: mdl-31318194

RESUMEN

Graphene oxide (GO) has an excellent adsorption capacity toward metal ions. Therefore, it is widely recognized as an auspicious material for fabrication of membranes applied in metal ion separation. However, GO membranes are not stable in aqueous solution because of electrostatic repulsion between GO nanosheets which are negatively charged. This paper shows that stable GO membranes can be easily obtained by the noncovalent interaction of GO with oxidized carbon nanotubes (CNTs). The experiment also shows that the GO/CNTs membranes can be used for the effective adsorption of metal ions. The kinetic data, adsorption isotherms, competitive adsorption experiment, and X-ray photoelectron spectroscopy indicate that the adsorption of metal ions is based on chemisorption. The membranes are remarkably durable in acidic, neutral, and basic solutions. Although the significant stabilization of the membranes by CNTs is observed, they strongly influence the adsorption process. Our study reveals that even a small amount of CNTs (GO/CNTs in the ratio 8:1) significantly reduces adsorption capacities of the membranes which were as follows: 37, 40, 50, 42, 48, and 98 mg g-1 for Co(II), Ni(II), Cu(II), Zn(II), Cd(II), and Pb(II), respectively. The reduction of the membrane adsorption capacities results from the creation of micro- and nanochannels formed by entangled CNTs. Durability and adsorptive properties of studied membranes indicate their potential use for the removal of metals from water.

6.
Physiol Biochem Zool ; 92(1): 115-124, 2019.
Artículo en Inglés | MEDLINE | ID: mdl-30601104

RESUMEN

Coexistence of organisms and pathogens has resulted in the evolution of efficient antimicrobial defense, especially at the embryonic stage. This investigation aimed to substantiate the hypothesis that the layers of silk in a spider cocoon play a role in the immunity of the embryos against microorganisms present in the external environment. A two-step interdisciplinary attempt has been made. First, the eggs and empty cocoons of the spider Parasteatoda tepidariorum were incubated on lysogeny broth agar media for 3 d. In the samples of eggs, no growth of bacteria was detected. This indicated that the eggs inside cocoons were sterile. Therefore, in the second step, the cocoons and egg surface were analyzed using SEM, TEM, and LM. The obtained images demonstrated that both inner and outer layers of the silk are built of threads of the same diameter, set in an irregular manner, and randomly clustered into groups. The threads in the outer layer were packed more densely than in the inner one. TEM analysis revealed threads of two types of fibrils and their arrangement. The resultant thread tangle of the cocoon, possibly correlated with the ultrastructure of the fibers, seems to be an example of a structure-function relationship playing a crucial ecoimmunological role in spider embryonic development.


Asunto(s)
Bacterias/crecimiento & desarrollo , Seda/ultraestructura , Arañas/embriología , Animales , Embrión no Mamífero/microbiología , Arañas/microbiología , Arañas/ultraestructura
7.
Anal Chim Acta ; 1008: 57-65, 2018 May 30.
Artículo en Inglés | MEDLINE | ID: mdl-29420944

RESUMEN

A simple method for highly selective determination of trace and ultratrace arsenic ions, i.e. arsenite and arsenate, was developed. The method is based on new miniaturized membranes, 5 mm diameter and 4.4 mg weight, which are prepared by synthesis of amorphous silica coating on cellulose fibers followed by the modification with (3-mercaptopropyl)-trimethoxysilane. The batch adsorption experiments show that membranes have high selectivity toward arsenite in the presence of heavy metals and anions that usually exist in natural water. Arsenite can be quantitatively adsorbed at pH 1 from 50 mL sample within 60 min using the miniaturized membrane with maximum adsorption capacity of 60 mg g-1. The excellent adsorptive properties of membranes open the path to simple and selective determination of trace and ultratrace arsenite in water. Moreover, the membranes can be applied in the arsenic speciation due to their selectivity toward arsenite in the presence of arsenate. After adsorption, the arsenite retained onto the membrane is directly measured by energy-dispersive X-ray fluorescence spectrometry, avoiding elution step usually required in other spectroscopy techniques. The method is characterized by excellent enrichment factor of 972, detection limit of 0.045 ng mL-1 and can be successfully applied in analysis of high salinity water, which is difficult to analyze by other spectroscopy techniques. The proposed method is a solvent-free approach based on the use of miniaturized membranes as sorbent followed by the direct measurement using a low-power X-ray spectrometer without either elution step or gas consumption during measurement. It can be considered as environmentally friendly and meets the standards of green analytical chemistry principles.

8.
Mikrochim Acta ; 185(2): 117, 2018.
Artículo en Inglés | MEDLINE | ID: mdl-29386691

RESUMEN

Novel adsorbents are described for the preconcentration of chromium(VI). Graphene oxide (GO) was modified with various amino silanes containing one, two, or three nitrogen atoms in the molecule. These include 3-aminopropyltriethoxysilane (APTES), N-(3-trimethoxysilylpropyl)ethylenediamine (TMSPEDA), and N1-(3-trimethoxysilylpropyl)diethylenetriamine (TMSPDETA). The resulting GO derivatives were characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, and energy-dispersive X-ray fluorescence spectrometry (EDXRF). Adsorption studies show that these GO based sorbents are highly selective for Cr(VI) in the presence of Cr(III) at pH 3.5. Although the amino silanes applied in modification of GO contain different numbers of nitrogen atoms, the maximum adsorption capacities of GO derivatives are very similar (13.3-15.1 mg·g-1). Such results are in accordance with spectroscopy studies which show that the amount of amino silanes attached to GO decreases in the order of APTES > TMSPEDA > TMSPDETA. The APTES-modified GO was applied to selective and sensitive extraction of Cr(VI) ions prior to quantitation by low-power EDXRF using the Cr Kα line. The Cr(VI) ions need not be eluted from the solid adsorbent. The method has a 0.17 ng·mL-1 detection limit, and the recovery is 99.7 ± 2.2% at a spiking level of 10 ng·mL-1. The method was successfully applied to the determination of Cr(VI) in water samples. Graphical abstractGraphene oxide adsorbents modified with various amino silanes are described for the preconcentration and speciation of trace and ultratrace levels of chromium ions.

9.
Protoplasma ; 255(3): 773-784, 2018 May.
Artículo en Inglés | MEDLINE | ID: mdl-29143884

RESUMEN

Vascular plants are able to conduct biomineralization processes and collect synthesized compounds in their internal tissues or to deposit them on their epidermal surfaces. This mechanism protects the plant from fluctuations of nutrient levels caused by different levels of supply and demand for them. The biominerals reflect both the metabolic characteristics of a vascular plant species and the environmental conditions of the plant habitat. The SEM/EDX method was used to examine the surface and cross-sections of the Calamagrostis epigejos and Phragmites australis leaves from post-industrial habitats (coal and zinc spoil heaps). The results from this study have showed the presence of mineral objects on the surfaces of leaves of both grass species. The calcium oxalate crystals, amorphous calcium carbonate spheres, and different silica forms were also found in the inner tissues. The high variety of mineral forms in the individual plants of both species was shown. The waxes observed on the leaves of the studied plants might be the initializing factor for the crystalline forms and structures that are present. For the first time, wide range of crystal forms is presented for C. epigejos. The leaf samples of P. australis from the post-industrial areas showed an increased amount of mineral forms with the presence of sulfur.


Asunto(s)
Ecosistema , Industrias , Minerales/química , Poaceae/química , Ceras/química , Carbonato de Calcio/química , Oxalato de Calcio/química , Cristalización , Hojas de la Planta/química , Haz Vascular de Plantas/química , Dióxido de Silicio/química , Espectrometría por Rayos X
10.
Nanomaterials (Basel) ; 7(8)2017 Jul 26.
Artículo en Inglés | MEDLINE | ID: mdl-28933732

RESUMEN

Titania nanotube (TNT) coatings were produced using low-potential anodic oxidation of Ti6Al4V substrates in the potential range 3-20 V. They were analysed by X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). The wettability was estimated by measuring the contact angle when applying water droplets. The bioactivity of the TNT coatings was established on the basis of the biointegration assay (L929 murine fibroblasts adhesion and proliferation) and antibacterial tests against Staphylococcus aureus (ATCC 29213). The photocatalytic efficiency of the TNT films was studied by the degradation of methylene blue under UV irradiation. Among the studied coatings, the TiO2 nanotubes obtained with the use of 5 V potential (TNT5) were found to be the most appropriate for medical applications. The TNT5 sample possessed antibiofilm properties without enriching it by additional antimicrobial agent. Furthermore, it was characterized by optimal biocompatibility, performing better than pure Ti6Al4V alloy. Moreover, the same sample was the most photocatalytically active and exhibited the potential for the sterilization of implants with the use of UV light and for other environmental applications.

11.
Nanomaterials (Basel) ; 7(9)2017 Sep 15.
Artículo en Inglés | MEDLINE | ID: mdl-28914821

RESUMEN

Bioactivity investigations of titania nanotube (TNT) coatings enriched with silver nanograins (TNT/Ag) have been carried out. TNT/Ag nanocomposite materials were produced by combining the electrochemical anodization and chemical vapor deposition methods. Fabricated coatings were characterized by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy. The release effect of silver ions from TNT/Ag composites immersed in bodily fluids, has been studied using inductively coupled plasma mass spectrometry (ICP-MS). The metabolic activity assay (MTT) was applied to determine the L929 murine fibroblasts adhesion and proliferation on the surface of TNT/Ag coatings. Moreover, the results of immunoassays (using peripheral blood mononuclear cells-PBMCs isolated from rats) allowed the estimation of the immunological activity of TNT/Ag surface materials. Antibacterial activity of TNT/Ag coatings with different morphological and structural features was estimated against two Staphylococcus aureus strains (ATCC 29213 and H9). The TNT/Ag nanocomposite layers produced revealed a good biocompatibility promoting the fibroblast adhesion and proliferation. A desirable anti-biofilm activity against the S. aureus reference strain was mainly noticed for these TiO2 nanotube coatings, which contain dispersed Ag nanograins deposited on their surface.

12.
Nanomaterials (Basel) ; 7(7)2017 Jul 24.
Artículo en Inglés | MEDLINE | ID: mdl-28737725

RESUMEN

Plasma enhanced atomic layer deposition (PEALD) of silver nanoparticles on the surface of 1-D titania coatings, such as nanotubes (TNT) and nanoneedles (TNN), has been carried out. The formation of TNT and TNN layers enriched with dispersed silver particles of strictly defined sizes and the estimation of their bioactivity was the aim of our investigations. The structure and the morphology of produced materials were determined using X-ray photoelectron spectroscopy (XPS) and scanning electron miscroscopy (SEM). Their bioactivity and potential usefulness in the modification of implants surface have been estimated on the basis of the fibroblasts adhesion and proliferation assays, and on the basis of the determination of their antibacterial activity. The cumulative silver release profiles have been checked with the use of inductively coupled plasma-mass spectrometry (ICPMS), in order to exclude potential cytotoxicity of silver decorated systems. Among the studied nanocomposite samples, TNT coatings, prepared at 3, 10, 12 V and enriched with silver nanoparticles produced during 25 cycles of PEALD, revealed suitable biointegration properties and may actively counteract the formation of bacterial biofilm.

13.
J Chromatogr Sci ; 54(8): 1301-9, 2016 Sep.
Artículo en Inglés | MEDLINE | ID: mdl-27190310

RESUMEN

We report observations of pulsating peptide formation and depeptidization in 70% aqueous acetonitrile solutions of l-Pro-l-Phe and l-Cys, resulting in the oscillatory appearance and disappearance of solid masses of microfibers and microspheres, respectively. We monitor the concentration changes of the monomeric amino acids by high-performance liquid chromatography. The concentration of all amino acid solutions used is 1.0 mg mL(-1), due to solubility limitations in 70% aqueous acetonitrile. The nonlinear concentration changes of l-Pro, l-Phe and l-Cys, and the amounts of the main peptidization products observed within our monitoring periods (for l-Pro-l-Phe, 250 h, and for l-Cys, 70 h) are typically from several to 20% of the original monomer concentrations. We follow the formation and decay of the insoluble peptides by turbidimetry. We also investigate the materials formed using scanning electron microscopy and mass spectrometry. We carry out numerical simulations on a simple model that reflects the main features of spontaneous pulsation of peptide fiber or sphere formation in this abiotic liquid system.


Asunto(s)
Aminoácidos/análisis , Péptidos/química , Acetonitrilos/química , Secuencia de Aminoácidos , Cromatografía Líquida de Alta Presión , Simulación por Computador , Espectrometría de Masas , Microscopía Electrónica de Rastreo , Modelos Químicos , Agua/química
14.
Mikrochim Acta ; 183: 231-240, 2016.
Artículo en Inglés | MEDLINE | ID: mdl-26766877

RESUMEN

We describe a novel solid phase sorbent that was synthesized by coupling graphene oxide (GO) to ethylenediamine (EDA). This nanomaterial (referred to as GO-EDA) is capable of adsorbing the ions of iron, cobalt, nickel, copper, zinc and lead. The ethylenediamine-modified graphene oxide was characterized by X-ray photoelectron spectroscopy, scanning electron microscopy and Fourier transform infrared spectroscopy. The analytical procedure relies on (a) sorption of metal ions on GO-EDA dispersed in aqueous samples; (b) filtering, and (c) direct submission of the filter paper to energy-dispersive X-ray fluorescence spectrometry. This kind of dispersive micro-solid phase extraction was optimized with respect to pH values, concentration of GO-EDA, contact time, and the effects of interfering ions and humic acid on recovery of determined elements. Under optimized conditions, the recoveries of spiked samples range from 90 to 98 %. The detection limits are 0.07, 0.10, 0.07, 0.08, 0.06 and 0.10 ng mL-1 for Fe(III), Co(II), Ni(II), Cu(II), Zn(II) and Pb(II), respectively. The method has a relative standard deviation of <6 %, and its accuracy was verified by analysis of two standard reference materials [LGC6016 (estuarine water) and BCR-610 (groundwater)]. It was successfully applied to the determination of trace amounts of these metal ions in water samples. Graphical AbstractGraphene oxide was coupled to ethylenediamine in order to obtain an effective sorbent (GO-EDA) for preconcentration of Fe(III), Co(II), Ni(II), Cu(II), Zn(II) and Pb(II) from environmental water samples.

15.
Curr Protein Pept Sci ; 17(2): 106-16, 2016.
Artículo en Inglés | MEDLINE | ID: mdl-26521956

RESUMEN

Earlier, we have collected an experimental evidence showing that low molecular weight chiral carboxylic acids (amino acids included) can spontaneously undergo an oscillatory chiral conversion and an oscillatory condensation in abiotic aqueous and non-aqueous liquid systems, stored for certain amount of time under mild external conditions. These earlier findings are summarized in the introductory part of this study. In the second part, a preliminary report is given on spontaneous pulsation of peptide microfibers in the aged proline-phenylalanine (Pro-Phe) solution in 70% aqueous acetonitrile. The experimental evidence originates from a number of advanced analytical techniques. In view of our earlier and present findings, a presumption is made that the mechanism of spontaneous pulsation (formation and decay) of Pro-Phe microfibers is directly related to the oscillatory chiral conversion and oscillatory peptidization. The entity of the discussed results pointing out to spontaneous and uncontrolled instability of peptide structures might be a bad prognostic for employing such structures in nanobiotechnology.


Asunto(s)
Péptidos/química , Fenilalanina/química , Prolina/química , Ácidos Carboxílicos/química , Nanofibras/química
16.
Anal Chem ; 87(6): 3535-42, 2015 Mar 17.
Artículo en Inglés | MEDLINE | ID: mdl-25707847

RESUMEN

A new method based on dispersive microsolid phase extraction (DMSPE) and total-reflection X-ray fluorescence spectrometry (TXRF) is proposed for multielemental ultratrace determination of heavy metal ions and arsenic species. In the developed methodology, the crucial issue is a novel adsorbent synthesized by grafting 3-mercaptopropyl trimethoxysilane on a graphene oxide (GO) surface. Mercapto-modified graphene oxide (GO-SH) can be applied in quantitative adsorption of cobalt, nickel, copper, cadmium, and lead ions. Moreover, GO-SH demonstrates selectivity toward arsenite in the presence of arsenate. Due to such features of GO-SH nanosheets as wrinkled structure and excellent dispersibility in water, GO-SH seems to be ideal for fast and simple preconcentration and determination of heavy metal ions using methodology based on DMSPE and TXRF measurement. The suspension of GO-SH was injected into an analyzed water sample; after filtration, the GO-SH nanosheets with adsorbed metal ions were redispersed in a small volume of internal standard solution and deposited onto a quartz reflector. The high enrichment factor of 150 allows obtaining detection limits of 0.11, 0.078, 0.079, 0.064, 0.054, and 0.083 ng mL(-1) for Co(II), Ni(II), Cu(II), As(III), Cd(II), and Pb(II), respectively. Such low detection limits can be obtained using a benchtop TXRF system without cooling media and gas consumption. The method is suitable for the analysis of water, including high salinity samples difficult to analyze using other spectroscopy techniques. Moreover, GO-SH can be applied to the arsenic speciation due to its selectivity toward arsenite.

17.
ACS Appl Mater Interfaces ; 6(22): 20144-53, 2014 Nov 26.
Artículo en Inglés | MEDLINE | ID: mdl-25329565

RESUMEN

The aminosilanized graphene oxide (GO-NH2) was prepared for selective adsorption of Pb(II) ions. Graphene oxide (GO) and GO-NH2 prepared through the amino-silanization of GO with 3-aminopropyltriethoxysilane were characterized by scanning electron microscopy, powder X-ray diffraction, X-ray photoelectron spectroscopy, and Raman spectroscopy. The batch experiments show that GO-NH2 is characterized by high selectivity toward Pb(II) ions. Adsorption isotherms suggest that sorption of Pb(II) on GO-NH2 nanosheets is monolayer coverage, and adsorption is controlled by a chemical process involving the surface complexation of Pb(II) ions with the nitrogen-containing groups on the surface of GO-NH2. Pb(II) ions can be quantitatively adsorbed at pH 6 with maximum adsorption capacity of 96 mg g(-1). The GO-NH2 was used for selective and sensitive determination of Pb(II) ions by electrothermal atomic absorption spectrometry (ET-AAS). The preconcentration of Pb(II) ions is based on dispersive micro solid-phase extraction in which the suspended GO-NH2 is rapidly injected into analyzed water sample. Such features of GO-NH2 nanosheets as wrinkled structure, softness, flexibility, and excellent dispersibility in water allow achieving very good contact with analyzed solution, and adsorption of Pb(II) ions is very fast. The experiment shows that after separation of the solid phase, the suspension of GO-NH2 with adsorbed Pb(II) ions can be directly injected into the graphite tube and analyzed by ET-AAS. The GO-NH2 is characterized by high selectivity toward Pb(II) ions and can be successfully used for analysis of various water samples with excellent enrichment factors of 100 and detection limits of 9.4 ng L(-1).

18.
Anal Chim Acta ; 834: 22-9, 2014 Jun 27.
Artículo en Inglés | MEDLINE | ID: mdl-24928241

RESUMEN

Graphene oxide (GO) is a novel material with excellent adsorptive properties. However, the very small particles of GO can cause serious problems is solid-phase extraction (SPE) such as the high pressure in SPE system and the adsorbent loss through pores of frit. These problems can be overcome by covalently binding GO nanosheets to a support. In this paper, GO was covalently bonded to spherical silica by coupling the amino groups of spherical aminosilica and the carboxyl groups of GO (GO@SiO2). The successful immobilization of GO nanosheets on the aminosilica was confirmed by scanning electron microscopy and X-ray photoelectron spectroscopy. The spherical particle covered by GO with crumpled silk wave-like carbon sheets are an ideal sorbent for SPE of metal ions. The wrinkled structure of the coating results in large surface area and a high extractive capacity. The adsorption bath experiment shows that Cu(II) and Pb(II) can be quantitatively adsorbed at pH 5.5 with maximum adsorption capacity of 6.0 and 13.6 mg g(-1), respectively. Such features of GO nanosheets as softness and flexibility allow achieving excellent contact with analyzed solution in flow-rate conditions. In consequence, the metal ions can be quantitatively preconcentrated from high volume of aqueous samples with excellent flow-rate. SPE column is very stable and several adsorption-elution cycles can be performed without any loss of adsorptive properties. The GO@SiO2 was used for analysis of various water samples by flame atomic absorption spectrometry with excellent enrichment factors (200-250) and detection limits (0.084 and 0.27 ng mL(-1) for Cu(II) and Pb(II), respectively).

19.
Dalton Trans ; 42(16): 5682-9, 2013 Apr 28.
Artículo en Inglés | MEDLINE | ID: mdl-23443993

RESUMEN

The adsorptive properties of graphene oxide (GO) towards divalent metal ions (copper, zinc, cadmium and lead) were investigated. GO prepared through the oxidation of graphite using potassium dichromate was characterized by scanning electron microscopy (SEM), powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and infrared spectroscopy (FT-IR). The results of batch experiments and measurements by flame atomic absorption spectrometry (F-AAS) indicate that maximum adsorption can be achieved in broad pH ranges: 3-7 for Cu(II), 5-8 for Zn(II), 4-8 for Cd(II), 3-7 for Pb(II). The maximum adsorption capacities of Cu(II), Zn(II), Cd(II) and Pb(II) on GO at pH = 5 are 294, 345, 530, 1119 mg g(-1), respectively. The competitive adsorption experiments showed the affinity in the order of Pb(II) > Cu(II) ≫ Cd(II) > Zn(II). Adsorption isotherms and kinetic studies suggest that sorption of metal ions on GO nanosheets is monolayer coverage and adsorption is controlled by chemical adsorption involving the strong surface complexation of metal ions with the oxygen-containing groups on the surface of GO. Chemisorption was confirmed by XPS (binding energy and shape of O1s and C1s peaks) of GO with adsorbed metal ions. The adsorption experiments show that the dispersibility of GO in water changes remarkably after complexation of metal ions. After adsorption, the tendency to agglomerate and precipitate is observed. Excellent dispersibility of GO and strong tendency of GO-Me(II) to precipitate open the path to removal of heavy metals from water solution. Potential application of GO in analytical chemistry as a solid sorbent for preconcentration of trace elements and in heavy metal ion pollution cleanup results from its maximum adsorption capacities that are much higher than those of any of the currently reported sorbents.

20.
Bull Environ Contam Toxicol ; 88(2): 255-9, 2012 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-22072273

RESUMEN

Mass size distributions of ambient aerosol were measured in Zabrze, a heavily industrialized city of Poland, during a summer and a winter season. The chemical analyses of the surface layer of PM(10), PM(2.5) and PM(1) in this area were also performed by X-ray photoelectron spectroscopy (XPS). Results suggested that the influence of an atmospheric aerosol on the health condition of Zabrze residents can be distinctly stronger in winter than in summer because of both: higher concentration level of particulate matter (PM) and higher contribution of fine particles in winter season compared to summer. In Zabrze in June (summer) PM(10) and PM(2.5) reached about 20 and 14 µg/m(3), respectively, while in December (winter) 57 and 51 µg/m(3), respectively. The XPS analysis showed that elemental carbon is the major surface component of studied airborne particles representing about 78%-80% (atomic mass) of all detected elements.


Asunto(s)
Aerosoles/análisis , Contaminantes Atmosféricos/análisis , Contaminación del Aire/estadística & datos numéricos , Material Particulado/análisis , Aerosoles/química , Contaminantes Atmosféricos/química , Ciudades/estadística & datos numéricos , Monitoreo del Ambiente , Tamaño de la Partícula , Material Particulado/química , Polonia , Estaciones del Año
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