Biosynthesis of palladium nanoparticles using Saccharomyces cerevisiae extract and its photocatalytic degradation behaviour

NASA Astrophysics Data System (ADS)

Sriramulu, Mohana; Sumathi, Shanmugam

2018-06-01

In this article, we have discussed the biosynthesis of palladium nanoparticles (PdNPs) using aqueous Saccharomyces cerevisiae extract and its photocatalytic application. The biosynthesised PdNPs were characterised by UV-Vis spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FTIR), x-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDX) and Atomic force microscopy (AFM). The formation of PdNPs was confirmed from the disappearance of the peak at 405 nm in the UV-Vis spectrum. Agglomerated and hexagonal shaped PdNPs were noted by SEM. FTIR was performed to identify the biomolecules responsible for the synthesis of PdNPs. Bioactive compounds in the yeast extract acted as secondary metabolites which facilitated the formation of PdNPs. The yeast synthesised PdNPs degraded 98% of direct blue 71 dye photochemically within 60 min under UV light.

One-dimensional nanoferroic rods; synthesis and characterization

NASA Astrophysics Data System (ADS)

Ahmed, M. A.; Seddik, U.; Okasha, N.; Imam, N. G.

2015-11-01

One-dimensional nanoferroic rods of BaTiO3 were synthesized by improved citrate auto-combustion technology using tetrabutyl titanate. X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), transmission electron microscopy (TEM), atomic force microscopy (AFM) and Fourier transform infrared spectroscopy (FTIR) have been used to characterize the prepared sample. The results indicated that the crystal structure of BaTiO3 is tetragonal phase with an average crystallite size of 47 nm. SEM image gives a cauliflower-like morphology of the agglomerated nanorods. The stoichiometry of the chemical composition of the BaTiO3 ceramic was confirmed by EDX. TEM micrograph exhibited that BaTiO3 nanoparticles have rod-like shape with an average length of 120 nm and width of 43 nm. AFM was used to investigate the surface topography and its roughness. The topography image in 3D showed that the BaTiO3 particles have a rod shape with an average particle size of 116 nm which in agreement with 3D TEM result.

Core-shell carbon nanosphere-TiO2 composite and hollow TiO2 nanospheres prepared by atomic layer deposition

NASA Astrophysics Data System (ADS)

Bakos, L. P.; Justh, N.; Hernádi, K.; Kiss, G.; Réti, B.; Erdélyi, Z.; Parditka, B.; Szilágyi, I. M.

2016-10-01

Core-shell carbon-TiO2 composite and hollow TiO2 nanospheres were prepared using carbon nanospheres as hard-templates, coating them with TiO2 using atomic layer deposition, and subsequent burning out of the carbon cores. The bare carbon, the composite carbon-TiO2 and the hollow TiO2 nanospheres were characterized with TG/DTA-MS, FTIR, XRD and SEM-EDX.

Characterization and evaluation of antibacterial activity of plant mediated calcium oxide (CaO) nanoparticles by employing Mentha pipertia extract

NASA Astrophysics Data System (ADS)

Ijaz, Umber; Bhatti, Ijaz Ahmed; Mirza, Saima; Ashar, Ambreen

2017-10-01

The antibacterial activity of green synthesized calcium oxide nanoparticles was investigated using leaf extract of Mentha piperita in this study. The synthesized nanomaterial was subjected to characterization using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), and energy dispersive x-ray spectroscopy (EDX). The SEM images showed agglomeration of disc shaped nanoparticles, and FTIR and EDX spectroscopy indicated intensive peaks for calcium ions and oxygen. Subsequently, the potential of nanoscale CaO was also evaluated for antimicrobial index against E. coli using the well diffusion method. A maximum zone of inhibition up to 42 mm was observed when 100 µg ml-1 material was loaded with inoculum size 50 µl of E. coli in sunlight exposure of 5 h. The experimental conditions were optimized using a central composite design using a response surface methodology. The maximum antimicrobial index of the CaO nanoparticle was 6 mm as a result of the optimized response. Furthermore, the minimum inhibitory concentration of the CaO nanoparticle showed 25 µg ml-1, an effective initial concentration for E.coli removal. The results revealed that the CaO nanocomposite synthesized via a green route was a promising candidate for the removal of E. coli present in drinking water, which is an important fecal indicator.

Magnesium prevents phosphate-induced vascular calcification via TRPM7 and Pit-1 in an aortic tissue culture model.

PubMed

Sonou, Tomohiro; Ohya, Masaki; Yashiro, Mitsuru; Masumoto, Asuka; Nakashima, Yuri; Ito, Teppei; Mima, Toru; Negi, Shigeo; Kimura-Suda, Hiromi; Shigematsu, Takashi

2017-06-01

Previous clinical and experimental studies have indicated that magnesium may prevent vascular calcification (VC), but mechanistic characterization has not been reported. This study investigated the influence of increasing magnesium concentrations on VC in a rat aortic tissue culture model. Aortic segments from male Sprague-Dawley rats were incubated in serum-supplemented high-phosphate medium for 10 days. The magnesium concentration in this medium was increased to demonstrate its role in preventing VC, which was assessed by imaging and spectroscopy. The mineral composition of the calcification was analyzed using Fourier transform infrared (FTIR) spectroscopic imaging, scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) mapping. Magnesium supplementation of high-phosphate medium dose-dependently suppressed VC (quantified as aortic calcium content), and almost ablated it at 2.4 mm magnesium. The FTIR images and SEM-EDX maps indicated that the distribution of phosphate (as hydroxyapatite), phosphorus and Mg corresponded with calcium content in the aortic ring and VC. The inhibitory effect of magnesium supplementation on VC was partially reduced by 2-aminoethoxy-diphenylborate, an inhibitor of TRPM7. Furthermore, phosphate transporter-1 (Pit-1) protein expression was increased in tissues cultured in HP medium and was gradually-and dose dependently-decreased by magnesium. We conclude that a mechanism involving TRPM7 and Pit-1 underpins the magnesium-mediated reversal of high-phosphate-associated VC.

Computer-aided screening system for cervical precancerous cells based on field emission scanning electron microscopy and energy dispersive x-ray images and spectra

NASA Astrophysics Data System (ADS)

Jusman, Yessi; Ng, Siew-Cheok; Hasikin, Khairunnisa; Kurnia, Rahmadi; Osman, Noor Azuan Bin Abu; Teoh, Kean Hooi

2016-10-01

The capability of field emission scanning electron microscopy and energy dispersive x-ray spectroscopy (FE-SEM/EDX) to scan material structures at the microlevel and characterize the material with its elemental properties has inspired this research, which has developed an FE-SEM/EDX-based cervical cancer screening system. The developed computer-aided screening system consisted of two parts, which were the automatic features of extraction and classification. For the automatic features extraction algorithm, the image and spectra of cervical cells features extraction algorithm for extracting the discriminant features of FE-SEM/EDX data was introduced. The system automatically extracted two types of features based on FE-SEM/EDX images and FE-SEM/EDX spectra. Textural features were extracted from the FE-SEM/EDX image using a gray level co-occurrence matrix technique, while the FE-SEM/EDX spectra features were calculated based on peak heights and corrected area under the peaks using an algorithm. A discriminant analysis technique was employed to predict the cervical precancerous stage into three classes: normal, low-grade intraepithelial squamous lesion (LSIL), and high-grade intraepithelial squamous lesion (HSIL). The capability of the developed screening system was tested using 700 FE-SEM/EDX spectra (300 normal, 200 LSIL, and 200 HSIL cases). The accuracy, sensitivity, and specificity performances were 98.2%, 99.0%, and 98.0%, respectively.

Chemical and structural analysis of gallstones from the Indian subcontinent.

PubMed

Ramana Ramya, J; Thanigai Arul, K; Epple, M; Giebel, U; Guendel-Graber, J; Jayanthi, V; Sharma, M; Rela, M; Narayana Kalkura, S

2017-09-01

Representative gallstones from north and southern parts of India were analyzed by a combination of physicochemical methods: X-ray diffraction (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), CHNS analysis, thermal analysis and Nuclear Magnetic Resonance (NMR) spectroscopy ( 1 H and 13 C). The stones from north Indian were predominantly consisting of cholesterol monohydrate and anhydrous cholesterol which was confirmed by XRD analysis. FTIR spectroscopy confirmed the presence of cholesterol and calcium bilirubinate in the south Indian gallstones. EDX spectroscopy revealed the presence of carbon, nitrogen, oxygen, calcium, sulfur, sodium and magnesium and chloride in both south Indian and north Indian gallstones. FTIR and NMR spectroscopy confirmed the occurrence of cholesterol in north Indian gallstones. The respective colour of the north Indian and south Indian gallstones was yellowish and black. The morphology of the constituent crystals of the north Indian and south Indian gallstones were platy and globular respectively. The appreciable variation in colour, morphology and composition of south and north Indian gallstones may be due to different food habit and habitat. Copyright © 2017 Elsevier B.V. All rights reserved.

Assessment of the Effects Exerted by Acid and Alkaline Solutions on Bone: Is Chemistry the Answer?

PubMed

Amadasi, Alberto; Camici, Arianna; Porta, Davide; Cucca, Lucia; Merli, Daniele; Milanese, Chiara; Profumo, Antonella; Rassifi, Nabila; Cattaneo, Cristina

2017-09-01

The treatment of corpses with extremely acid or basic liquids is sometimes performed in criminal contexts. A thorough characterization by chemical analysis may provide further help to macroscopic and microscopic analysis; 63 porcine bone samples were treated with solutions at different pH (1-14) for immersion periods up to 70 days, as well as in extremely acidic sulfuric acid solutions (9 M/18 M) and extremely basic sodium hydroxide. Inductively coupled optical emission spectrometry (ICP-OES)/plasma mass spectrometry (ICP-MS), Fourier transform infrared spectroscopy (FT-IR), energy dispersive X-ray analysis (EDX), X-ray powder diffraction (XRPD), and scanning electron microscopy (SEM) showed that only the sulfuric acid solution 18 M was able to completely dissolve the sample. In addition, chemical analysis allowed to recognize the contact between bone and substances. Hydrated calcium sulfate arose from extreme pH. The possibility of detecting the presence of human material within the residual solution was demonstrated, especially with FT-IR, ICP-OES, and EDX. © 2017 American Academy of Forensic Sciences.

Green pigments of the Pompeian artists' palette

NASA Astrophysics Data System (ADS)

Aliatis, Irene; Bersani, Danilo; Campani, Elisa; Casoli, Antonella; Lottici, Pier Paolo; Mantovan, Silvia; Marino, Iari-Gabriel; Ospitali, Francesca

2009-08-01

Green colored samples on wall paintings and green powder from a pigment pot found in Pompeii area are investigated by micro-Raman, FT-IR and, for one sample, SEM-EDX. To obtain the green color, green earths and malachite were used, together with mixture of Egyptian blue and yellow ochre. The mineralogical identification of the green earths has been attempted through the comparison of the vibrational features, discriminating between celadonite and glauconite spectra. Traces of a modern synthetic pigment containing copper phthalocyanine were found in a fresco fragment.

Green pigments of the Pompeian artists' palette.

PubMed

Aliatis, Irene; Bersani, Danilo; Campani, Elisa; Casoli, Antonella; Lottici, Pier Paolo; Mantovan, Silvia; Marino, Iari-Gabriel; Ospitali, Francesca

2009-08-01

Green colored samples on wall paintings and green powder from a pigment pot found in Pompeii area are investigated by micro-Raman, FT-IR and, for one sample, SEM-EDX. To obtain the green color, green earths and malachite were used, together with mixture of Egyptian blue and yellow ochre. The mineralogical identification of the green earths has been attempted through the comparison of the vibrational features, discriminating between celadonite and glauconite spectra. Traces of a modern synthetic pigment containing copper phthalocyanine were found in a fresco fragment.

Antimicrobial cellulosic hydrogel from olive oil industrial residue.

PubMed

Dacrory, Sawsan; Abou-Yousef, Hussein; Abouzeid, Ragab E; Kamel, Samir; Abdel-Aziz, Mohamed S; El-Badry, Mohamed

2018-05-25

The cellulose-based antimicrobial hydrogel was prepared from seed and husk cellulosic fibers of olive industry residues by load silver nanoparticles (AgNPs) onto grafted acrylamide monomer (Am) cellulosic fibers. The grafting approach was the free radical mechanism by utilizing ceric ammonium nitrate (CAN) as initiator in aqueous medium and N,N methylene bisacrylamide (MBAm) as a cross linker. The effect of different grafting conditions on the properties of produced hydrogels has been studied by determining the grafting parameters, i.e. concentration of Am, MBAm, grafting time and temperature to optimize grafting yield (G %), grafting efficiency (GE %), and swelling %. Characterizations of the obtained hydrogels were performed through monitoring swelling behavior, FTIR spectroscopy, SEM, and EDX. AgNPs were grown into the prepared hydrogel. Hydrogel/AgNPs were characterized by FT-IR spectroscopy, X-ray diffraction (XRD) and scanning electron microscopy (SEM). The hydrogel loaded AgNPs exhibit high efficient antimicrobial activity against Staphylococcus aureus, Pseudomonas aeruginosa, and Candida albicans. Copyright © 2018. Published by Elsevier B.V.

Eco-friendly and green synthesis of BiVO4 nanoparticle using microwave irradiation as photocatalayst for the degradation of Alizarin Red S

NASA Astrophysics Data System (ADS)

Abraham, S. Daniel; David, S. Theodore; Bennie, R. Biju; Joel, C.; Kumar, D. Sanjay

2016-06-01

Bismuth vanadate (BiVO4) nanocrystals have been successfully synthesised using microwave-assisted combustion synthesis (MCS), and characterised using Fourier transform infrared (FT-IR) and Raman spectra, surface area analysis (BET), X-ray diffraction (XRD), scanning electron microscopy (SEM), Energy Dispersive X-ray analysis (EDX), diffused reflectance spectroscopy (DRS) and Photoluminescence (PL) spectroscopy. The XRD results confirmed the formation of monoclinic bismuth vanadate. The formations of BiO & VO43-vibrations were ascertained from FT-IR data. The morphology of hallow internal structural micro entities were confirmed by SEM. The optical properties were determined by DRS and PL spectra. Hence, the influence of the preparation methods on the structure, morphology and optical activities of bismuth vanadate was investigated systematically. Photocatalytic degradation (PCD) of Alizarin Red S (ARS), an effective disrupting chemical in aqueous medium was investigated using BiVO4 nanoparticles. The kinetics of PCD was found to follow pseudo first-order.

Phytoremediation of arsenic by Trapa natans in a hydroponic system.

PubMed

Baruah, Sangita; Borgohain, Jayasree; Sarma, K P

2014-05-01

Phytoremediation of arsenic (As) by water chestnut (Trapa natans) in a hydroponic system was studied. Plants were grown at two concentrations of arsenic, 1.28 mg/L and 10.80 mg/L, in a single metal solution. Scanning Electron Microscope-Energy Dispersive X-ray (SEM-EDX) confirmed highest arsenic concentration in the roots, followed by shoots and leaves. SEM-EDX also confirmed internalization of arsenic in T. natans and the damage caused due to arsenic exposure. Fourier Transform Infra Red Spectroscopy (FT-IRS) indicated that the binding characteristics of the arsenic ions involved the hydroxyl, amide, amino, and thiol groups in the biomass. Chlorophyll concentration decreased with increasing metal concentration and duration of exposure, but proline content increases with increasing concentration in the plant. Morphological changes were studied on the 3rd, 5th and 7th day. Unhealthy growth and chlorosis were found to be related with arsenic toxicity. From the above studies it is clear that T. natans can be used successfully for the removal of arsenic ions by a phytoremediation process.

Novel Gemini cationic surfactants as anti-corrosion for X-65 steel dissolution in oilfield produced water under sweet conditions: Combined experimental and computational investigations

NASA Astrophysics Data System (ADS)

Migahed, M. A.; elgendy, Amr.; EL-Rabiei, M. M.; Nady, H.; Zaki, E. G.

2018-05-01

Two new sequences of Gemini di-quaternary ammonium salts were synthesized characterized by FTIR and 1HNMR spectroscopic techniques and evaluated as corrosion inhibitor for X-65 steel dissolution in deep oil wells formation water saturated with CO2. The anti-corrosion performance of these compounds was studied by different electrochemical techniques i.e. (potentiodynamic polarization and AC impedance methods), Surface morphology (SEM and EDX) analysis and quantum chemical calculations. Results showed that the synthesized compounds were of mixed-type inhibitors and the inhibition capability was influenced by the inhibitor dose and the spacer substitution in their structure as indicated by Tafel plots. Surface active parameters were determined from the surface tension profile. The synthesized compounds adsorbed via Langmuir adsorption model with physiochemical adsorption as inferred from the standard free energy (ΔG°ads) values. Surface morphology (SEM and EDX) data for inhibitor (II) shows the development of adsorbed film on steel specimen. Finally, the experimental results were supported by the quantum chemical calculations using DFT theory.

Nanostructural Characters of β-SiC Nanoparticles Prepared from Indonesian Natural Resource using Sonochemical Method

NASA Astrophysics Data System (ADS)

Fuad, A.; Kultsum, U.; Taufiq, A.; Hartatiek; Latifah, E.

2018-04-01

Silicon carbide (SiC) nanoparticles become one of the interesting non-oxide ceramics due to their physical and chemical properties. For an extended period, SiC nanoparticles have been prepared by several methods that usually performed at high temperatures ranging from 1200 - 2000 °C from inexpensive commercial precursors. In this work, we prepared SiC nanoparticles from the low priced precursor of Indonesia natural resource using the sonochemical method at a temperature that is lower than 1000 °C. To produce samples with particular characters, we varied the sintering holding time (1, 10, and 20 hours) and the sintering temperatures (850, 950, and 1050 °C) during the synthesis. The samples were then characterized using XRD, SEM-EDX, TEM, and FTIR. The XRD data analysis showed that the samples have a dominant phase of SiC in the form of β-SiC with a 3C-SiC structure and SiO2 phase in a low composition within a good agreement with the EDX characterization. Interestingly, the sample prepared at the sintering temperature of 850 °C for 1 hour showed a non-crystallite phase. Using a Scherer’s equation, the particles of the samples sized from 13 to 18 nm, which were validated by SEM and TEM images. Furthermore, the FT-IR spectra presented several peaks, i.e., at wavenumbers of 482.2 and 1150 cm-1 representing Si-O-Si bonding and also at 798.5 cm-1 regarding with Si-C bonding.

Hydroxyapatite for Keratoprosthesis Biointegration

PubMed Central

Wang, Liqiang; Jeong, Kyung Jae; Chiang, Homer H.; Zurakowski, David; Behlau, Irmgard; Chodosh, James; Dohlman, Claes H.; Langer, Robert

2011-01-01

Purpose. Integration of keratoprosthesis with the surrounding cornea is very important in preventing bacterial invasion, which may cause ocular injury. Here the authors investigated whether hydroxyapatite (HAp) coating can improve keratoprosthesis (KPro) biointegration, using polymethyl methacrylate (PMMA)—the principal component of the Boston KPro—as a model polymer. Methods. HAp coatings were induced on PMMA discs after treatment with concentrated NaOH and coating with poly-dopamine (PDA) or polydopamine and then with 11-mercaptoundecanoic acid (11-MUA). Coatings were characterized chemically (Fourier transform infrared spectroscopy [FTIR], energy dispersive X-ray spectroscopy [EDX]) and morphologically (SEM) and were used as substrates for keratocyte growth in vitro. Cylinders of coated PMMA were implanted in porcine corneas ex vivo for 2 weeks, and the force required to pull them out was measured. The inflammatory reaction to coated discs was assessed in the rabbit cornea in vivo. Results. FTIR of the coatings showed absorption bands characteristic of phosphate groups, and EDX showed that the Ca/P ratios were close to those of HAp. By SEM, each method resulted in morphologically distinct HAp films; the 11-MUA group had the most uniform coating. The hydroxyapatite coatings caused comparable enhancement of keratocyte proliferation compared with unmodified PMMA surfaces. HAp coating significantly increased the force and work required to pull PMMA cylinders out of porcine corneas ex vivo. HAp coating of implants reduced the inflammatory response around the PMMA implants in vivo. Conclusions. These results are encouraging for the potential of HAp-coated surfaces for use in keratoprostheses. PMID:21849419

Synthesis and characterization of palm oil fuel ash (POFA) and metakaolin based geopolymer for possible application in nanocoating

NASA Astrophysics Data System (ADS)

Khan, Ihsan Ullah; Bhat, A. H.; Masset, Patrick J.; Khan, Farman Ullah; Rehman, Wajid Ur

2016-11-01

The main aim of this study was to synthesize and characterize highly amorphous geopolymer from palm oil fuel ash (POFA) and metakaolin, to be used as nanocoating. Geopolymers are man-made aluminosilicate materials that are amorphous analogues of zeolites. The geopolymers were made by condensing a mixture of raw materials metakaolin and palm oil fuel ash (POFA) with alkaline activator at a fixed ratio at room temperature. The kaolin type clay was calcined at 700 °C for 4hrs to transform it into amorphous metakaolin which is more reactive precursor for geopolymer formation. The characteristics of metakaolin and geopolymers (metakaolin and palm oil fuel ash based geopolymers) were analyzed by using x-ray fluorescence (XRF), Fourier transform infra-red spectrometry (FTIR), Thermogravimetric analysis (TG/DTA) and scanning electron microscopy with energy dispersive x-ray analysis (SEM-EDX). FTIR revealed the presence of Al-O and Si-O stretching vibrations of amorphous alumino-silicate structure for metakaolin, palm oil fuel ash and geopolymers. SEM-EDX images showed the presence of reaction product complementary to NASH (N = Na2O, A = Al2O3, S = SiO2, H = H2O) solid. The resulting geopolymers that were synthesized with NaOH/Na2SiO3 solution cured at 60 °C for 3 days. The results demonstrated the suitability of metakaolin and palm oil fuel ash (POFA) for synthesis of geopolymer at room temperatures.

Boletus edulis loaded with γ-Fe2O3 nanoparticles as a magnetic sorbent for preconcentration of Co(II) and Sn(II) prior to their determination by ICP-OES.

PubMed

Ozdemir, Sadin; Serkan Yalcin, M; Kilinc, Ersin; Soylak, Mustafa

2017-12-20

The authors show that the fungus Boletus edulis loaded with γ-Fe 2 O 3 nanoparticles is a viable sorbent for magnetic solid phase extraction of trace levels of Co(II) and Sn(II). The surface structure of immobilized magnetized B. edulis was characterized by FT-IR, SEM and EDX. Experimental parameters were optimized. Following elution with 1 M HCl, the ions were quantified by ICP-OES. The limits of detection are 21 pg·mL -1 for Co(II), and 19 pg·mL -1 for Sn(II). The preconcentration factors are 100 for both ions. The sorption capacities of the sorbent are 35.8 mg·g -1 for Co(II) and 29.6 mg·g -1 for Sn(II). The method was applied to the analysis of certificated reference materials and gave ≥95% recoveries with low RSDs. It was also successfully applied to the quantification of Co(II) and Sn(II) in spiked environmental and food samples. Graphical abstract The fungus Boletus edulis loaded with γ-Fe 2 O 3 nanoparticles is a viable biosorbent for magnetic solid phase extraction (MSPE) of trace levels of Co(II) and Sn(II). The surface structure of immobilized magnetized B. edulis was characterized by FT-IR, SEM and EDX. Experimental parameters were optimized.

Synthesize of zinc nanoparticles using Indonesian velvet bean (Mucuna pruriens) extract and evaluate its potency in lowering catalepsy in mice

NASA Astrophysics Data System (ADS)

Eko Sardjono, Ratnaningsih; Khoerunnisa, Fitri; Musthopa, Iqbal; Khairunisa, Dinar; Astuti Suganda, Putri; Rachmawati, Rahmi

2018-01-01

This study aims to synthesize zinc nanoparticles using Indonesian velvet bean (Mucuna pruriens) seed extract and evaluate its potency in lowering catalepsy in mice. The research conducted consist of extraction of M. pruriens seed powder, synthesis of zinc-M. pruriens seed extract nanoparticles (Zn-MPn), characterization of Zn-MPn, and catalepsy test of Zn-MPn. M. pruriens seed powder was extracted by maceration using ethanol-water (1:1) at pH 3 adjusted with citric acid. The Zn-MPn was synthesized by reacting zinc acetate dihydrate (Zn(CH3COO2)2.2H2O) solution with M. pruriens seed extract for 40 min, dispersibility of the reaction was controlled by using sonication and ultrasonic homogenizer. The Zn-MPn obtained was characterized by scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDX), transmission electron microscopy (TEM), and Fourier-transform infrared (FTIR). Catalepsy test of Zn-MPn was conducted at doses of 5, 10, 15, 20 and 25 mg/kg body weight. The results of SEM-EDX and TEM analysis showed that the Zn-MPn formed nanoparticles with a particle diameter of 55 nm. Based on FTIR analysis, the absorption band at 464.8 cm-1 was a typical absorption indicated the Zn-O interaction on Zn-MPn. Catalepsy test showed that Zn-MPn on the all five doses were able to lower the catalepsy in mice with the best dose was 10 mg/kg body weight.

Biosorption of Microelements by Spirulina: Towards Technology of Mineral Feed Supplements

PubMed Central

Chojnacka, Katarzyna

2014-01-01

Surface characterization and metal ion adsorption properties of Spirulina sp. and Spirulina maxima were verified by various instrumental techniques. FTIR spectroscopy and potentiometric titration were used for qualitative and quantitative determination of metal ion-binding groups. Comparative FTIR spectra of natural and Cu(II)-treated biomass proved involvement of both phosphoryl and sulfone groups in metal ions sorption. The potentiometric titration data analysis provided the best fit with the model assuming the presence of three types of surface functional groups and the carboxyl group as the major binding site. The mechanism of metal ions biosorption was investigated by comparing the results from multielemental analyses by ICP-OES and SEM-EDX. Biosorption of Cu(II), Mn(II), Zn(II), and Co(II) ions by lyophilized Spirulina sp. was performed to determine the metal affinity relationships for single- and multicomponent systems. Obtained results showed the replacement of naturally bound ions: Na(I), K(I), or Ca(II) with sorbed metal ions in a descending order of Mn(II) > Cu(II) > Zn(II) > Co(II) for single- and Cu(II) > Mn(II) > Co(II) > Zn(II) for multicomponent systems, respectively. Surface elemental composition of natural and metal-loaded material was determined both by ICP-OES and SEM-EDX analysis, showing relatively high value of correlation coefficient between the concentration of Na(I) ions in algal biomass. PMID:25386594

Formation of cerussite and hydrocerussite during adsorption of lead from aqueous solution on oxidized carbons by cold oxygen plasma

NASA Astrophysics Data System (ADS)

De Velasco Maldonado, Paola S.; Hernández-Montoya, Virginia; Concheso, A.; Montes-Morán, Miguel A.

2016-11-01

A new procedure of elimination of Pb2+ from aqueous solution using carbon adsorbents, in which high amounts of cerussite and hydrocerussite are deposited on the carbon surfaces, is reported. The procedure includes the preparation of carbons from selected lignocellulosic wastes (pecan nut shells and peach stones) by single carbonization and further oxidation with cold oxygen plasma. The materials prior and after the oxidation treatment were characterized using elemental analysis, FT-IR spectroscopy, SEM/EDX analysis, adsorption of N2 at -196 °C and X-ray photoelectron spectroscopy. The adsorption of Pb2+ was carried out in batch systems under constant agitation. The formation of cerussite and hydrocerussite on the spent carbon surfaces was confirmed by XRD, SEM/EDX and FT-IR. A Pb2+ removal mechanism is proposed in which a co-precipitation of lead nitrate and calcium carbonate would render the formation of the lead carbonates. In such mechanism, the occurrence of CaCO3 on the surface of the adsorbents plays a crucial role. The presence of calcium carbonate on the precursors is understood on the basis of the thermal evolution of calcium oxalate originally present in the biomass. The oxygen plasma treatment helps to expose the calcium carbonate nanocrystals thus improving dramatically the removal capacity of Pb2+. Accordingly, retention capacities as high as 63 mg of Pb2+ per gram of adsorbent have been attained.

The Effects of a Macromolecular Charring Agent with Gas Phase and Condense Phase Synergistic Flame Retardant Capability on the Properties of PP/IFR Composites

PubMed Central

Chen, Hongda; Wang, Jihui; Ding, Anxin; Han, Xia; Sun, Ziheng

2018-01-01

In order to improve the efficiency of intumescent flame retardants (IFRs), a novel macromolecular charring agent named poly(ethanediamine-1,3,5-triazine-p-4-amino-2,2,6,6-tetramethylpiperidine) (PETAT) with gas phase and condense phase synergistic flame-retardant capability was synthesized and subsequently dispersed into polypropylene (PP) in combination with ammonium polyphosphate (APP) via a melt blending method. The chemical structure of PETAT was investigated by Fourier transform infrared spectroscopy (FTIR), and 1H nuclear magnetic resonance (NMR) spectroscopy. Thermal properties of the PETAT and IFR systems were tested by thermogravimetric-derivative thermogravimetric analysis (TGA-DTG) and thermogravimetry–Fourier transform infrared spectroscopy (TG-FTIR). The mechanical properties, thermal stability, flame-retardant properties, water resistance, and structures of char residue in flame-retardant composites were characterized using tensile and flexural strength property tests, TGA, limiting oxygen index (LOI) values before and after soaking, underwritten laboratory-94 (UL-94) vertical burning test, cone calorimetric test (CCT), scanning electron microscopy with energy dispersive X-ray spectrometry (SEM-EDXS), and FTIR. The results indicated that PETAT was successfully synthesized, and when the ratio of APP to PETAT was 2:1 with 25 wt % loading, the novel IFR system could reduce the deterioration of tensile strength and enhance the flexural strength of composites. Meanwhile, the flame-retardant composite was able to pass the UL-94 V-0 rating with an LOI value of 30.3%, and the peak of heat release rate (PHRR), total heat release (THR), and material fire hazard values were considerably decreased compared with others. In addition, composites also exhibited excellent water resistance properties compared with traditional IFR composites. SEM-EDXS and FTIR analyses of the char residues, as well as TG-FTIR analyses of IFR were used to investigate the flame-retardant mechanism of the APP/PETAT IFR system. The results indicated that the efficient flame retardancy of PP/IFR composites could be attributed to the synergism of the free radical-quenching and char layer-protecting mechanisms in the gas phase and condense phase, respectively. PMID:29324716

The Effects of a Macromolecular Charring Agent with Gas Phase and Condense Phase Synergistic Flame Retardant Capability on the Properties of PP/IFR Composites.

PubMed

Chen, Hongda; Wang, Jihui; Ni, Aiqing; Ding, Anxin; Han, Xia; Sun, Ziheng

2018-01-11

In order to improve the efficiency of intumescent flame retardants (IFRs), a novel macromolecular charring agent named poly(ethanediamine-1,3,5-triazine-p-4-amino-2,2,6,6-tetramethylpiperidine) (PETAT) with gas phase and condense phase synergistic flame-retardant capability was synthesized and subsequently dispersed into polypropylene (PP) in combination with ammonium polyphosphate (APP) via a melt blending method. The chemical structure of PETAT was investigated by Fourier transform infrared spectroscopy (FTIR), and ¹H nuclear magnetic resonance (NMR) spectroscopy. Thermal properties of the PETAT and IFR systems were tested by thermogravimetric-derivative thermogravimetric analysis (TGA-DTG) and thermogravimetry-Fourier transform infrared spectroscopy (TG-FTIR). The mechanical properties, thermal stability, flame-retardant properties, water resistance, and structures of char residue in flame-retardant composites were characterized using tensile and flexural strength property tests, TGA, limiting oxygen index (LOI) values before and after soaking, underwritten laboratory-94 (UL-94) vertical burning test, cone calorimetric test (CCT), scanning electron microscopy with energy dispersive X-ray spectrometry (SEM-EDXS), and FTIR. The results indicated that PETAT was successfully synthesized, and when the ratio of APP to PETAT was 2:1 with 25 wt % loading, the novel IFR system could reduce the deterioration of tensile strength and enhance the flexural strength of composites. Meanwhile, the flame-retardant composite was able to pass the UL-94 V-0 rating with an LOI value of 30.3%, and the peak of heat release rate (PHRR), total heat release (THR), and material fire hazard values were considerably decreased compared with others. In addition, composites also exhibited excellent water resistance properties compared with traditional IFR composites. SEM-EDXS and FTIR analyses of the char residues, as well as TG-FTIR analyses of IFR were used to investigate the flame-retardant mechanism of the APP/PETAT IFR system. The results indicated that the efficient flame retardancy of PP/IFR composites could be attributed to the synergism of the free radical-quenching and char layer-protecting mechanisms in the gas phase and condense phase, respectively.

Group 12 dithiocarbamate complexes: Synthesis, spectral studies and their use as precursors for metal sulfides nanoparticles and nanocomposites

NASA Astrophysics Data System (ADS)

Ajibade, Peter A.; Ejelonu, Benjamin C.

2013-09-01

Zn(II), Cd(II) and Hg(II) dithiocarbamate complexes have been synthesized and characterized by elemental analysis, thermogravimetric analysis, UV-Vis, FTIR, 1H- and 13C NMR spectroscopy. The complexes were thermolysed at 180 °C and used as single molecule precursors for the synthesis of HDA capped ZnS, CdS and HgS nanoparticles and polymethylmethacrylate (PMMA) nanocomposites. The optical and structural properties of the nanoparticles and nanocomposites were studied by UV-Vis, PL, XRD and SEM. The crystallites sizes of the nanoparticles varied between 3.03 and 23.45 nm. SEM and EDX analyses of the nanocomposites confirmed the presence of the nanoparticles in the polymer matrix.

Photocatalytic hollow TiO2 and ZnO nanospheres prepared by atomic layer deposition.

PubMed

Justh, Nóra; Bakos, László Péter; Hernádi, Klára; Kiss, Gabriella; Réti, Balázs; Erdélyi, Zoltán; Parditka, Bence; Szilágyi, Imre Miklós

2017-06-28

Carbon nanospheres (CNSs) were prepared by hydrothermal synthesis, and coated with TiO 2 and ZnO nanofilms by atomic layer deposition. Subsequently, through burning out the carbon core templates hollow metal oxide nanospheres were obtained. The substrates, the carbon-metal oxide composites and the hollow nanospheres were characterized with TG/DTA-MS, FTIR, Raman, XRD, SEM-EDX, TEM-SAED and their photocatalytic activity was also investigated. The results indicate that CNSs are not beneficial for photocatalysis, but the crystalline hollow metal oxide nanospheres have considerable photocatalytic activity.

Monodispersed fabrication and dielectric studies on ethylenediamine passivated α-manganese dioxide nanorods

DOE Office of Scientific and Technical Information (OSTI.GOV)

Joseph, A. Martin; Kumar, R. Thilak, E-mail: manojthilak@yahoo.com

2016-09-15

Highlights: • Monodispersed ethylenediamine (EDA) passivated α-MnO{sub 2} nanorods were fabricated by inexpensive wet chemical method. • FTIR analysis indicated that surface passivation is strongly influenced by the introduction of the organic ligand. • XRD and HR-SEM revealed the structure and morphology of the fabricated α-MnO{sub 2} nanorods with an average size of about 40 × 200 nm. • Dielectric studies pointed out that the fabricated α-MnO{sub 2} is semiconducting in nature with resistivity, ρ = 1.46 to 5.76 × 10{sup 3} Ωcm. • The optical energy gap for the fabricated α-MnO{sub 2} nanorods is found to be around 1.37more » eV. - Abstract: In this present work, pure α-MnO{sub 2} nanorods were fabricated by the reduction of 0.2 m/L of KMnO{sub 4} with 0.2 m/L of Na{sub 2}S{sub 2}O{sub 3}·5H{sub 2}O and by passivating with the organic ligand Ethylenediamine (EDA). The structural, functional, morphological and chemical composition of the nanorods were investigated by X-Ray Diffractometer (XRD), Fourier Transform Infrared Spectrometer (FTIR), High Resolution Scanning Electron Microscope (HR-SEM) and Energy Dispersive X-Ray Spectrometry (EDX). The XRD analysis indicated high crystalline nature of the product and FTIR confirmed the contribution of the organic ligand in surface passivation. HR-SEM image revealed the morphology of the α-MnO{sub 2} nanorods with an average size of about 40 × 200 nm. EDX confirmed the presence of Mn and O in the material. UV–visible spectrophotometery was used to determine the absorption behavior of the nanorods and an indirect band gap of 1.37 eV was acquired by Taucplot. Dielectric studies were carried out using Broadband Dielectric Spectrometer(BDS) and the resistivity was found to be around the semiconductor range (ρ = 1.46 to 5.76 × 10{sup 3} Ωcm).« less

Effect of chitosan addition to characteristic and antimicrobial activity of zinc doped hydroxyapatite

NASA Astrophysics Data System (ADS)

Rasyida, A.; Wicaksono, S. T.; Pradita, N. N.; Ardhyananta, H.; Purnomo, A.

2017-07-01

Hydroxyapatite (HAp) doping with zinc was prepared using sol gel method; different chitosan content were further added to prepare the composite, namely 10, 15 and 20% wt. The samples were characterized using FTIR, XRD, SEM-EDX, and AAS. In vitro antimicrobial activities of the composite were evaluated against gram positive and negative bacteria. FTIR results revealed that there were no important changes in the structure of composite, while 10% wt of chitosan in composite shows the highest inhibition zone against Escherichia coli after 24 h incubation. In addition, after 7 days of immersion in simulated body fluid, there were apatite formations in the surface of the composite. These might indicate that this composite could be used as a material candidate for bone substitute applications.

Micro-Raman and FT-IR spectroscopic studies of ceramic shards excavated from ancient Stratonikeia city at Eskihisar village in West-South Turkey

NASA Astrophysics Data System (ADS)

Bahçeli, Semiha; Güleç, Gamze; Erdoğan, Hasan; Söğüt, Bilal

2016-02-01

In this study, micro-Raman and Fourier transformed infrared (FT-IR) spectroscopies, X-ray diffraction (XRD) and scanning electron microscope with energy dispersive X-ray (SEM-EDX) were used to characterize the mineralogical structures of pigments of four ceramic fragments in which one of them belongs to Hellenistic period (1st - IVth century BC) and other three ceramic shards belong to Early Rome (IVth century BC- 1st century AD) excavated from Stratonikeia ancient city. In the results of investigations on these four ceramic fragments, the various phases were identified: quartz, kaolinite, albit (or Na-feldspar), calcite, anastase, hematite and magnetite. Furthermore, the obtained findings indicate that firing temperature is about 800-850 °C for all the shards.

Green biosynthesis of silver nanoparticles using leaves extract of Artemisia vulgaris and their potential biomedical applications.

PubMed

Rasheed, Tahir; Bilal, Muhammad; Iqbal, Hafiz M N; Li, Chuanlong

2017-10-01

Biosynthesis of nanoparticles from plant extracts is receiving enormous interest due to their abundant availability and a broad spectrum of bioactive reducing metabolites. In this study, the reducing potential of Artemisia vulgaris leaves extract (AVLE) was investigated for synthesizing silver nanoparticles without the addition of any external reducing or capping agent. The appearance of blackish brown color evidenced the complete synthesis of nanoparticles. The synthesized silver nanoparticles were characterized by UV-vis spectroscopy, scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDX), transmission electron microscope (TEM), atomic force microscopy (AFM) and Fourier transforms infrared spectroscopy (FT-IR) analysis. UV-vis absorption profile of the bio-reduced sample elucidated the main peak around 420nm, which correspond to the surface plasmon resonance of silver nanoparticles. SEM and AFM analyses confirmed the morphology of the synthesized nanoparticles. Similarly, particles with a distinctive peak of silver were examined with EDX. The average diameter of silver nanoparticles was about 25nm from Transmission Electron Microscopy (TEM). FTIR spectroscopy scrutinized the involvement of various functional groups during nanoparticle synthesis. The green synthesized nanoparticles presented effective antibacterial activity against pathogenic bacteria than AVLE alone. In-vitro antioxidant assays revealed that silver nanoparticles (AV-AgNPs) exhibited promising antioxidant properties. The nanoparticles also displayed a potent cytotoxic effect against HeLa and MCF-7 cell lines. In conclusion, the results supported the advantages of employing a bio-green approach for developing silver nanoparticles with antimicrobial, antioxidant, and antiproliferative activities in a simple and cost- competitive manner. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparation and characterization of a novel adsorbent from Moringa oleifera leaf

NASA Astrophysics Data System (ADS)

Bello, Olugbenga Solomon; Adegoke, Kayode Adesina; Akinyunni, Opeyemi Omowumi

2017-06-01

A new and novel adsorbent was obtained by impregnation of Moringa oleifera leaf in H2SO4 and NaOH, respectively. Prepared adsorbents were characterized using elemental analysis, FT-IR, SEM, TGA and EDX analyses, respectively. The effects of operational parameters, such as pH, moisture content, ash content, porosity and iodine number on these adsorbents were investigated and compared with those of commercial activated carbon (CAC). EDX results of acid activated M. oleifera leaf have the highest percentage of carbon by weight (69.40 %) and (76.11 %) by atom, respectively. Proximate analysis showed that the fixed carbon content of acid activated M. oleifera leaf (69.14 ± 0.01) was the highest of all adsorbents studied. Conclusively, the present investigation shows that acid activated M. oleifera leaf is a good alternative adsorbent that could be used in lieu of CAC for recovery of dyes and heavy metal from aqueous solutions and other separation techniques.

Facile Synthesis and Characterization of ZrO₂ Nanoparticles via Modified Co-Precipitation Method.

PubMed

Ramachandran, M; Subadevi, R; Liu, Wei-Ren; Sivakumar, M

2018-01-01

The crystalline Zirconium oxide (ZrO2) nano particles were synthesized using optimized content of Zirconium nitrate (Zr(NO3)2·3H2O) with varying KOH concentration (0.5, 1 and 1.5 M) by co-precipitation method. The thermal history of the precursor was carefully analyzed through Thermogravimetric (TG/DTA) measurement. The as prepared samples were characterized to ensure structural, functional, morphological, compositional, chemical composition and band gap by X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR), Laser Raman, scanning electron microscopy (SEM), High resolution Transverse Electron Microscopy (HR-TEM), X-ray photo electron spectroscopy (XPS), EDX, Photo luminescence spectroscopy (PL). The monoclinic structure with space group P21/c has been confirmed from XRD (JCPDS 89-9066). The Zr-O stretching vibration and Zr-O2-Zr bending vibrations were confirmed through FTIR analysis. The well dispersed particles with spherical morphology were confirmed through SEM and TEM analysis. The oxidation states of Zr, O and C were confirmed through XPS analysis. The oxygen vacancies and band gap of the particles were investigated through PL analysis.

Thermal, structural, functional, optical and magnetic studies of pure and Ba doped CdO nanoparticles.

PubMed

Sivakumar, S; Venkatesan, A; Soundhirarajan, P; Khatiwada, Chandra Prasad

2015-12-05

In this research, a chemical precipitation method was used to synthesize undoped and doped cadmium oxide nanoparticles and studied by TG-DTA, XRD, FT-IR, SEM, with EDX and antibacterial activities, respectively. The melting points, thermal stability and the kinetic parameters like entropy (ΔS), enthalpy (ΔH), Gibb's energy (ΔG), activation energy (E), frequency factor (A) were evaluated from TG-DTA measurements. X-ray diffraction analysis (XRD) brought out the information about the synthesized products exist in spherical in shape with cubic structure. The functional groups and band area of the samples were established by Fourier transform infrared (FT-IR) spectroscopy. The direct and indirect band gap energy of pure and doped samples were determined by UV-Vis-DRS. The surface morphological, elemental compositions and particles sizes were evaluated by scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). Finally, antibacterial activities indicated the Gram-positive and Gram-negative bacteria are more active in transporter, dehydrogenize and periplasmic enzymatic activities of pure and doped samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Evaluation of antibacterial and Antibiofilm activity of Synthesized Zinc-Hydroxyapatite Biocomposites from Labeo rohita fish scale waste

NASA Astrophysics Data System (ADS)

Sathiskumar, Swamiappan; Vanaraj, Sekar; Sabarinathan, Devaraj; Preethi, Kathirvel

2018-02-01

Materials based on hydroxyapatite (HAp) Synthesized from bio-wastes have been regarded as useful, novel, eco-friendly medical applications that are targeted primarily for their antibacterial nature. In the present study, HAp was Synthesized from the fish scales of Labeo rohita using alkaline heat treatment and subsequently mixed with 1, 2 and 3 wt% of zinc (Zn) at 800 °C using calcination method to yield Zn-HAp composites. A detailed characterization of the generated composites was analysed by XRD, FT-IR, SEM, EDX and DLS methods. Further, antibacterial and biofilm inhibitory activity of the generated composites was determined using strains of Staphylococcus aureus and Escherichia coli. The confirmation of the presence of zinc, confirmed by EDAX spectra, XRD, FT-IR, SEM and DLS observations, established that HAp and Zn-HAp composites were without impurities, irregular in shape and were 848 nm sized particles. Although 1-3 wt% Zn-HAp composites showed antibacterial activity, the 3 wt% Zn-HAp composite was found suitable to kill the surrounding bacterial growth and showed potent inhibitory activity against biofilm formation.

Waterborne Superhydrophobic and Superoleophobic Coatings for the Protection of Marble and Sandstone

PubMed Central

Aslanidou, Dimitra; Lampakis, Dimitrios

2018-01-01

Silica nanoparticles were dispersed in an aqueous emulsion of alkoxy silanes and organic fluoropolymer. The dispersion was sprayed onto white marble and sandstone. The deposited composite coatings exhibited (i) superhydrophobicity and superoleophobicity, as evidenced by the high (>150°) static contact angles of water and oil drops as well as (ii) water and oil repellency according to the low (<7°) corresponding tilt contact angles. Apart from marble and sandstone, the coatings with extreme wetting properties were deposited onto concrete, silk, and paper, thus demonstrating the versatility of the method. The siloxane/fluoropolymer product was characterized using Fourier Transform Infrared Spectroscopy (FT-IR), Raman spectroscopy and Scanning Electron Microscopy equipped with an Energy Dispersive X-ray Spectrometer (SEM-EDX). Moreover, SEM and FT-IR were used to reveal the surface structures of the composite coatings and their transition from superhydrophobicity to superhydrophilicity which occurred after severe thermal treatment. The composite coatings slightly reduced the breathability of marble and sandstone and had practically no optical effect on the colour of the two stones. Moreover, the coatings offered good protection against water penetration by capillarity. PMID:29642652

Plasma nanocoating of thiophene onto MoS2 nanotubes

NASA Astrophysics Data System (ADS)

Türkaslan, Banu Esencan; Dikmen, Sibel; Öksüz, Lütfi; Öksüz, Aysegul Uygun

2015-12-01

MoS2 nanotubes were coated with conductive polymer thiophene by atmospheric pressure radio-frequency (RF) glow discharge. MoS2 nanotubes were prepared by thermal decomposition of hexadecylamine (HDA) intercalated laminar MoS2 precursor on anodized aluminum oxide template and the thiophene was polymerized directly on surface of these nanotubes as in situ by plasma method. The effect of plasma power on PTh/MoS2 nanocomposite properties has been investigated by means of Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM and EDX), and X-ray diffraction spectroscopy (XRD). The presence of PTh bands in the FTIR spectra of PTh/MoS2 nanotube nanocomposites corresponding XRD results indicates that the polythiophene coating onto MoS2 nanotube. The chemical structure of PTh is not changed when the plasma power of discharge differ from 117 to 360 W. SEM images of nanocomposites show that when the discharge power is increased between 117 and 360 W the average diameter of PTh/MoS2 nanotube nanocomposites are changed and the structure become more uniformly.

[Biosorption of Radionuclide Uranium by Deinococcus radiodurans].

PubMed

Yang, Jie; Dong, Fa-qin; Dai, Qun-wei; Liu, Ming-xue; Nie, Xiao-qin; Zhang, Dong; Ma, Jia-lin; Zhou, Xian

2015-04-01

As a biological adsorbent, Living Deinococcus radiodurans was used for removing radionuclide uranium in the aqueous solution. The effect factors on biosorption of radionuclide uranium were researched in the present paper, including solution pH values and initial uranium concentration. Meanwhile, the biosorption mechanism was researched by the method of FTIR and SEM/EDS. The results show that the optimum conditions for biosorption are as follows: pH = 5, co = 100 mg · L(-1) and the maximum biosorption capacity is up to 240 mgU · g(-1). According to the SEM results and EDXS analysis, it is indicated that the cell surface is attached by lots of sheet uranium crystals, and the main biosorpiton way of uranium is the ion exchange or surface complexation. Comparing FTIR spectra and FTIR fitting spectra before and after biosorption, we can find that the whole spectra has a certain change, particularly active groups (such as amide groups of the protein, hydroxy, carboxyl and phosphate group) are involved in the biosorption process. Then, there is a new peak at 906 cm(-1) and it is a stretching vibration peak of UO2(2+). Obviously, it is possible that as an anti radiation microorganism, Deinococcus radiodurans could be used for removing radionuclide uranium in radiation environment.

Group 12 dithiocarbamate complexes: synthesis, spectral studies and their use as precursors for metal sulfides nanoparticles and nanocomposites.

PubMed

Ajibade, Peter A; Ejelonu, Benjamin C

2013-09-01

Zn(II), Cd(II) and Hg(II) dithiocarbamate complexes have been synthesized and characterized by elemental analysis, thermogravimetric analysis, UV-Vis, FTIR, (1)H- and (13)C NMR spectroscopy. The complexes were thermolysed at 180 °C and used as single molecule precursors for the synthesis of HDA capped ZnS, CdS and HgS nanoparticles and polymethylmethacrylate (PMMA) nanocomposites. The optical and structural properties of the nanoparticles and nanocomposites were studied by UV-Vis, PL, XRD and SEM. The crystallites sizes of the nanoparticles varied between 3.03 and 23.45 nm. SEM and EDX analyses of the nanocomposites confirmed the presence of the nanoparticles in the polymer matrix. Copyright © 2013 Elsevier B.V. All rights reserved.

Characterisation of calcium phosphate crystals on calcified human aortic vascular smooth muscle cells and potential role of magnesium.

PubMed

Louvet, Loïc; Bazin, Dominique; Büchel, Janine; Steppan, Sonja; Passlick-Deetjen, Jutta; Massy, Ziad A

2015-01-01

Cardiovascular disease including vascular calcification (VC) remains the leading cause of death in patients suffering from chronic kidney disease (CKD). The process of VC seems likely to be a tightly regulated process where vascular smooth muscle cells are playing a key role rather than just a mere passive precipitation of calcium phosphate. Characterisation of the chemical and crystalline structure of VC was mainly led in patients or animal models with CKD. Likewise, Mg2+ was found to be protective in living cells although a potential role for Mg2+ could not be excluded on crystal formation and precipitation. In this study, the crystal formation and the role of Mg2+ were investigated in an in vitro model of primary human aortic vascular smooth muscle cells (HAVSMC) with physical techniques. In HAVSMC incubated with increased Ca x Pi medium, only calcium phosphate apatite crystals (CPA) were detected by Micro-Fourier Transform InfraRed spectroscopy (µFTIR) and Field Effect Scanning Electron Microscope (FE-SEM) and Energy Dispersive X-ray spectrometry (EDX) at the cell layer level. Supplementation with Mg2+ did not alter the crystal composition or structure. The crystal deposition was preferentially positioned near or directly on cells as pictured by FE-SEM observations and EDX measurements. Large µFTIR maps revealed spots of CPA crystals that were associated to the cellular layout. This qualitative analysis suggests a potential beneficial effect of Mg2+ at 5 mM in noticeably reducing the number and intensities of CPA µFTIR spots. For the first time in a model of HAVSMC, induced calcification led to the formation of the sole CPA crystals. Our data seems to exclude a physicochemical role of Mg2+ in altering the CPA crystal growth, composition or structure. Furthermore, Mg2+ beneficial role in attenuating VC should be linked to an active cellular role.

Characterisation of Calcium Phosphate Crystals on Calcified Human Aortic Vascular Smooth Muscle Cells and Potential Role of Magnesium

PubMed Central

Louvet, Loïc; Bazin, Dominique; Büchel, Janine; Steppan, Sonja; Passlick-Deetjen, Jutta; Massy, Ziad A.

2015-01-01

Background Cardiovascular disease including vascular calcification (VC) remains the leading cause of death in patients suffering from chronic kidney disease (CKD). The process of VC seems likely to be a tightly regulated process where vascular smooth muscle cells are playing a key role rather than just a mere passive precipitation of calcium phosphate. Characterisation of the chemical and crystalline structure of VC was mainly led in patients or animal models with CKD. Likewise, Mg2+ was found to be protective in living cells although a potential role for Mg2+ could not be excluded on crystal formation and precipitation. In this study, the crystal formation and the role of Mg2+ were investigated in an in vitro model of primary human aortic vascular smooth muscle cells (HAVSMC) with physical techniques. Methodology/Principal Findings In HAVSMC incubated with increased Ca x Pi medium, only calcium phosphate apatite crystals (CPA) were detected by Micro-Fourier Transform InfraRed spectroscopy (µFTIR) and Field Effect Scanning Electron Microscope (FE — SEM) and Energy Dispersive X-ray spectrometry (EDX) at the cell layer level. Supplementation with Mg2+ did not alter the crystal composition or structure. The crystal deposition was preferentially positioned near or directly on cells as pictured by FE — SEM observations and EDX measurements. Large µFTIR maps revealed spots of CPA crystals that were associated to the cellular layout. This qualitative analysis suggests a potential beneficial effect of Mg2+ at 5 mM in noticeably reducing the number and intensities of CPA µFTIR spots. Conclusions/Significance For the first time in a model of HAVSMC, induced calcification led to the formation of the sole CPA crystals. Our data seems to exclude a physicochemical role of Mg2+ in altering the CPA crystal growth, composition or structure. Furthermore, Mg2+ beneficial role in attenuating VC should be linked to an active cellular role. PMID:25607936

Synthesis of sodium lauryl sulphate (SLS)-modified activated carbon from risk husk for waste lead (Pb) removal

NASA Astrophysics Data System (ADS)

Al-Latief, D. N.; Arnelli, Astuti, Y.

2015-12-01

Surfactant-modified active carbon (SMAC) has been successfully synthesized from waste rice husk using a series of treatments i.e. carbonization, activation with H3PO4 and surface modification using sodium lauryl sulfate (SLS). The synthesized SMAC was characterized using SEM-EDX and FTIR. The adsorption results show that the SMAC synthesized using H3PO4 treatment for 8 hours followed with SLS treatment for 5 hours had efficiency and capacity of the waste lead removal of 99.965% and 0.499825 mg.g-1, respectively.

Application of micro-Fourier transform infrared spectroscopy to the examination of paint samples

NASA Astrophysics Data System (ADS)

Zięba-Palus, J.

1999-11-01

The examination and identification of automobile paints is an important problem in road accidents investigations. Since the real sample available is very small, only sensitive microtechniques can be applied. The methods of optical microscopy and micro-Fourier transform infrared spectroscopy (MK-FTIR) supported by scanning electron microscopy together with X-ray microanalysis (SEM-EDX) allow one to carry out the examination of each paint layer without any separation procedure. In this paper an attempt is made to discriminate between different automobile paints of the same colour by the use of these methods for criminalistic investigations.

Novel Organically Modified Core-Shell Clay for Epoxy Composites-"SOBM Filler 1".

PubMed

Iheaturu, Nnamdi Chibuike; Madufor, Innocent Chimezie

2014-01-01

Preparation of a novel organically modified clay from spent oil base drilling mud (SOBM) that could serve as core-shell clay filler for polymers is herein reported. Due to the hydrophilic nature of clay, its compatibility with polymer matrix was made possible through modification of the surface of the core clay sample with 3-aminopropyltriethoxysilane (3-APTES) compound prior to its use. Fourier transform infrared (FT-IR) spectroscopy was used to characterize clay surface modification. Electron dispersive X-ray diffraction (EDX) and scanning electron microscopy (SEM) were used to expose filler chemical composition and morphology, while electrophoresis measurement was used to examine level of filler dispersion. Results show an agglomerated core clay powder after high temperature treatment, while EDX analysis shows that the organically modified clay is composed of chemical inhomogeneities, wherein elemental compositions in weight percent vary from one point to the other in a probe of two points. Micrographs of the 3-APTES coupled SOBM core-shell clay filler clearly show cloudy appearance, while FT-IR indicates 25% and 5% increases in fundamental vibrations band at 1014 cm(-1) and 1435 cm(-1), respectively. Furthermore, 3-APTES coupled core-shell clay was used to prepare epoxy composites and tested for mechanical properties.

Novel Organically Modified Core-Shell Clay for Epoxy Composites—“SOBM Filler 1”

PubMed Central

Iheaturu, Nnamdi Chibuike; Madufor, Innocent Chimezie

2014-01-01

Preparation of a novel organically modified clay from spent oil base drilling mud (SOBM) that could serve as core-shell clay filler for polymers is herein reported. Due to the hydrophilic nature of clay, its compatibility with polymer matrix was made possible through modification of the surface of the core clay sample with 3-aminopropyltriethoxysilane (3-APTES) compound prior to its use. Fourier transform infrared (FT-IR) spectroscopy was used to characterize clay surface modification. Electron dispersive X-ray diffraction (EDX) and scanning electron microscopy (SEM) were used to expose filler chemical composition and morphology, while electrophoresis measurement was used to examine level of filler dispersion. Results show an agglomerated core clay powder after high temperature treatment, while EDX analysis shows that the organically modified clay is composed of chemical inhomogeneities, wherein elemental compositions in weight percent vary from one point to the other in a probe of two points. Micrographs of the 3-APTES coupled SOBM core-shell clay filler clearly show cloudy appearance, while FT-IR indicates 25% and 5% increases in fundamental vibrations band at 1014 cm−1 and 1435 cm−1, respectively. Furthermore, 3-APTES coupled core-shell clay was used to prepare epoxy composites and tested for mechanical properties. PMID:27355022

Bioaccumulation characterization of uranium by a novel Streptomyces sporoverrucosus dwc-3.

PubMed

Li, Xiaolong; Ding, Congcong; Liao, Jiali; Du, Liang; Sun, Qun; Yang, Jijun; Yang, Yuanyou; Zhang, Dong; Tang, Jun; Liu, Ning

2016-03-01

The biosorption mechanisms of uranium on an aerobic bacterial strain Streptomyces sporoverrucosus dwc-3, isolated from a potential disposal site for (ultra-)low uraniferous radioactive waste in Southwest China, were evaluated by using transmission electron microscopy (TEM), energy dispersive X-ray (EDX) analysis, Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), proton induced X-ray emission (PIXE) and enhanced proton backscattering spectrometry (EPBS). Approximately 60% of total uranium at an initial concentration of 10mg/L uranium nitrate solution could be absorbed on 100mg S. sporoverrucosus dwc-3 with an adsorption capacity of more than 3.0mg/g (wet weight) after 12hr at room temperature at pH3.0. The dynamic biosorption process of S. sporoverrucosus dwc-3 for uranyl ions was well described by a pseudo second-order model. S. sporoverrucosus dwc-3 could accumulate uranium on cell walls and within the cell, as revealed by SEM and TEM analysis as well as EDX spectra. XPS and FT-IR analysis further suggested that the absorbed uranium was bound to amino, phosphate and carboxyl groups of the cells. Additionally, PIXE and EPBS results confirmed that ion exchange also contributed to the adsorption process of uranium. Copyright © 2015. Published by Elsevier B.V.

Solid Lubricated Rolling Element Bearings

DTIC Science & Technology

1980-02-15

ball paths (as received), at various SEM magnifications and EDX scrutiny 17 i. ■.- ■■ ••.■■ ■? • r 8. TMI TiC/MoS^ sputtered...MoS? removed with Oakite 126 HD), at various SEM magmtications and EDX scrutiny 19 10. TMI TiC/MoS^ sputtered 52100 gyro bearing inner race...ball path (MoS^ removed with Oakite 126 HD), at various SEM magnifications and EDX scrutiny 20 11. TMI TiC/MoS^ sputtered 52100 gyro bearing

Surface modification of SiO2 coated ZnO nanoparticles for multifunctional cotton fabrics.

PubMed

El-Naggar, Mehrez E; Hassabo, Ahmed G; Mohamed, Amina L; Shaheen, Tharwat I

2017-07-15

A simple chemical synthetic route was designed to prepare zinc oxide nanoparticles (ZnO-NPs) by using sodium alginate as anti-agglomeration agent in the presence of sodium hydroxide as alkali. Next, surface modification of ZnO-NPs with SiO 2 nanoparticles was achieved as per to sol-gel process. Further enhancing of the multifunctional properties of SiO 2 @ZnO-NPs was conducted successfully thanks to (aminopropyl)triethoxysilan (APTES) and vinyltriethoxysilan (VTES) which, in turns, increase the affinity of the SiO 2 @ZnO-NPs nanocomposite towards glycosidic chains of cotton fabrics. Thorough characterizations of synthesized ZnO-NPs, SiO 2 @ZnO-NPs, SiO 2 @ZnO-NPs/APTES and SiO 2 @ZnO-NPs/VTES were conducted by the making use of well advanced techniques such as FT-IR, XRD, TEM, DLS and SEM-EDX. The data obtained clarified the formation of an interfacial chemical bond between ZnO and SiO 2 as affirmed by FT-IR and XRD analysis. In addition, the results revealed by TEM, zeta sizer and SEM-EDX techniques, declared that the amorphous layers of SiO 2 , APTES or VTES evenly coated the surface of ZnO-NPs. For these nanocomposites, the work was extended to render cotton fabrics multifunctional properties such as antibacterial and UV protection with high durability even after 20 washing cycles using pad dry cure method. Taking the advantages of the silane compounds terminated by active groups such as OH, NH 2 , etc., open the door for further functionalization of the cotton fabrics' surfaces by durable multifunctional agents applied in various applications. Copyright © 2017 Elsevier Inc. All rights reserved.

Determination of the post mortem interval in skeletal remains by the comparative use of different physico-chemical methods: Are they reliable as an alternative to 14C?

PubMed

Amadasi, Alberto; Cappella, Annalisa; Cattaneo, Cristina; Cofrancesco, Pacifico; Cucca, Lucia; Merli, Daniele; Milanese, Chiara; Pinto, Andrea; Profumo, Antonella; Scarpulla, Valentina; Sguazza, Emanuela

2017-05-01

The determination of the post-mortem interval (PMI) of skeletal remains is a challenging aspect in the forensic field. Previous studies focused their attention on different macroscopic and morphological aspects but a thorough and complete evaluation of the potential of chemical and physical analyses in this field of research has not been performed. In addition to luminol test and Oxford histology index (OHI) reported in a recent paper, widely spread and accessible methods based on physical aspect and chemical characteristics of skeletal remains have been investigated as potential alternatives to dating by determination of 14 C. The investigation was performed on a total of 24 archeological and forensic bone samples with known PMI, with inductively coupled plasma optical emission spectrometer (ICP-OES), inductively coupled plasma quadruple mass spectrometry (ICP-MS), Fourier transform infrared (FT-IR) spectroscopy, energy dispersive X-ray analysis (EDX), powder X-ray diffraction analysis (XRPD) and scanning electron microscopy (SEM). Finally, the feasibility of such alternative methods was discussed. Some results such as carbonates/phosphates ratio from FT-IR, the amounts of organic and inorganic matter by EDX, crystallite sizes with XRPD, and surface morphology obtained by SEM, showed significant trends along with PMI. Though, from a chemical point of view cut-off values and gold-standard methods still present challenges, and rather different techniques together can provide useful information toward the assessment of the PMI of skeletal remains. It is however clear that in a hypothetical flowchart those methods may be placed practically at the same level and a choice should always consider the evaluation of results by each technique, execution times and a costs/benefits relationship. Copyright © 2017 Elsevier GmbH. All rights reserved.

Kinetic study on removal of heavy metal ions from aqueous solution by using soil.

PubMed

Lim, Soh-Fong; Lee, Agnes Yung Weng

2015-07-01

In the present study, the feasibility of soil used as a low-cost adsorbent for the removal of Cu(2+), Zn(2+), and Pb(2+) ions from aqueous solution was investigated. The kinetics for adsorption of the heavy metal ions from aqueous solution by soil was examined under batch mode. The influence of the contact time and initial concentration for the adsorption process at pH of 4.5, under a constant room temperature of 25 ± 1 °C were studied. The adsorption capacity of the three heavy metal ions from aqueous solution was decreased in order of Pb(2+) > Cu(2+) > Zn(2+). The soil was characterized by Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopic-energy dispersive X-ray (SEM-EDX), and Brunauer, Emmett, and Teller (BET) surface area analyzer. From the FTIR analysis, the experimental data was corresponded to the peak changes of the spectra obtained before and after adsorption process. Studies on SEM-EDX showed distinct adsorption of the heavy metal ions and the mineral composition in the study areas were determined to be silica (SiO2), alumina (Al2O3), and iron(III) oxide (FeO3). A distinct decrease of the specific surface area and total pore volumes of the soil after adsorption was found from the BET analysis. The experimental results obtained were analyzed using four adsorption kinetic models, namely pseudo-first-order, pseudo-second-order, Elovich, and intraparticle diffusion. Evaluating the linear correlation coefficients, the kinetic studies showed that pseudo-second-order equation described the data appropriable than others. It was concluded that soil can be used as an effective adsorbent for removing Cu(2+), Zn(2+), and Pb(2+) ions from aqueous solution.

Synthesis of ZSM-5 zeolite from coal fly ash and rice husk: characterization and application for partial oxidation of methane to methanol

NASA Astrophysics Data System (ADS)

Krisnandi, Y. K.; Yanti, F. M.; Murti, S. D. S.

2017-04-01

Indonesian fly ash (SiO2/Al2O3 mole ratio = 3.59) was used together with rice husk (SiO2 92%) as raw material for mesoporous ZSM-5 zeolite synthesis. Prior being used, coal fly ash and rice husk were subjected to pre-treatment in order to extract silicate (SiO4 4-) and aluminate (AlO4 5-) and to remove the impurities. Then the ZSM-5 zeolite were synthesized through hydrothermal treatment using two types of templates (TPAOH and PDDA). The as-synthesized ZSM-5 was characterized using FTIR, XRD, SEM-EDX, and BET. The result of FTIR showed peaks at 1250-950 cm-1 (v asymetric T-O), 820-650 cm-1 (v symetric T-O), and at 650-500 cm-1 confirming the presence of the five number ring of the pentasil structure. The result of XRD showed the appearance of certain peaks in the position 2 theta between 7-9° and 22-25° indicative of ZSM-5 structure, but also showed the pattern of low intensity magnetite and hematite. The SEM image showed the rough surface of hexagonal crystals from ZSM-5 structure, indicative of mesoporosity in the structure. EDX result showed Si/Al ratio of 20, while surface area analysis gave SA of 43.16. The ZSM-5 zeolites then was modified with cobalt oxide through impregnation method. The catalytic activity as heterogeneous catalysts in partial oxidation of methane was tested. The result showed that hence the catalytic activity of ZSM-5 and Co/ZSM-5 from fly ash and rice husk were still inferior compared to the pro-analysis sourced-counterpart, they were potential to be used as catalyst in the partial oxidation of methane to methanol.

Poly(methyl methacrylate) with TiO2 nanoparticles inclusion for stereolitographic complete denture manufacturing - the fututre in dental care for elderly edentulous patients?

PubMed

Totu, Eugenia Eftimie; Nechifor, Aurelia Cristina; Nechifor, Gheorghe; Aboul-Enein, Hassan Y; Cristache, Corina Marilena

2017-04-01

The aim of this study was to obtain a Poly(methylmethacrylate) (PMMA)-TiO 2 nanocomposite material with improved antibacterial characteristics, suitable for manufacturing 3D printed dental prosthesis. 0.2, 0.4, 0.6, 1, 2.5 by weight% of TiO 2 nanoparticles have been added to the commercially available stereolithographic PMMA material and the obtained nanocomposites have been analyzed using FTIR, SEM and also tested for antimicrobial efficacy against bacterial cultures from Candida species (C. scotti). SEM images and EDX results highlighted the presence of TiO 2 in PMMA nanocomposites. The elemental composition (EDX) also showed the presence of other fillers included in stereolithographic PMMA solution. FTIR analysis clearly revealed changes in polymeric matrix structure when adding TiO 2 nanoparticles. Sample containing 0.4, 1 and 2.5wt% TiO 2 nanoparticles inhibited the growth of Candida scotti strain in standard conditions according to the toxicity control method (DHA). Increasing quantity of nano-titania has resulted in particles fooling, forming new aggregates instead of the homogenous dispersion of nanoparticles with modified viscosity characteristics and expected lower mechanical parameters. Significant improvements in polymer characteristics and nice dispersion of the TiO 2 nanoparticles have been noticed for 0.4wt%, therefore it was used for stereolitographic complete denture prototyping. Incorporation of TiO 2 nanoparticles in PMMA polymer matrix was proved to have antibacterial effects, specifically on Candida species. The newly obtained 0.4% nanocomposite was successfully used with stereolitographic technique for complete denture manufacturing. However, mechanical and biocompatibility tests need to be performed in order to extend the clinical usage. Copyright © 2017 Elsevier Ltd. All rights reserved.

Nail Damage (Severe Onychodystrophy) Induced by Acrylate Glue: Scanning Electron Microscopy and Energy Dispersive X-Ray Investigations

PubMed Central

Pinteala, Tudor; Chiriac, Anca Eduard; Rosca, Irina; Larese Filon, Francesca; Pinteala, Mariana; Chiriac, Anca; Podoleanu, Cristian; Stolnicu, Simona; Coros, Marius Florin; Coroaba, Adina

2017-01-01

Background Scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) techniques have been used in various fields of medical research, including different pathologies of the nails; however, no studies have focused on obtaining high-resolution microscopic images and elemental analysis of disorders caused by synthetic nails and acrylic adhesives. Methods Damaged/injured fingernails caused by the use of acrylate glue and synthetic nails were investigated using SEM and EDX methods. Results SEM and EDX proved that synthetic nails, acrylic glue, and nails damaged by contact with acrylate glue have a different morphology and different composition compared to healthy human nails. Conclusions SEM and EDX analysis can give useful information about the aspects of topography (surface sample), morphology (shape and size), hardness or reflectivity, and the elemental composition of nails. PMID:28232921

Spinel NixZn1-xFe2O4 (0.0 ≤ x ≤ 1.0) nano-photocatalysts: Synthesis, characterization and photocatalytic degradation of methylene blue dye

NASA Astrophysics Data System (ADS)

Padmapriya, G.; Manikandan, A.; Krishnasamy, V.; Jaganathan, Saravana Kumar; Antony, S. Arul

2016-09-01

Spinel NixZn1-xFe2O4 (x = 0.0 to 1.0) nanoparticles were successfully synthesized by a simple microwave combustion method (MCM) using metal nitrates as raw materials and glycine as the fuel. The structural, morphological and opto-magnetic properties of the spinel NixZn1-xFe2O4 ferrites were determined by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray (EDX) spectroscopy, high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED) pattern, UV-Visible diffuse reflectance spectroscopy (DRS), photoluminescence (PL) spectroscopy and vibrating sample magnetometer (VSM). Powder XRD, and EDX analysis was confirmed the formation of pure phase of spinel ferrites. HR-SEM and HR-TEM analysis was confirmed the formation of sphere like-particle morphology of the samples with smaller agglomeration. VSM analysis clearly showed the superparamagnetic and ferromagnetic nature of the samples. The Ms value is 3.851 emu/g for undoped ZnFe2O4 sample and it increased with increase in Ni content. Photo-catalytic degradation (PCD) of methylene blue (MB) dye using the samples were carried out and observed good PCD results.

Application of SEM and EDX in studying biomineralization in plant tissues.

PubMed

He, Honghua; Kirilak, Yaowanuj

2014-01-01

This chapter describes protocols using formalin-acetic acid-alcohol (FAA) to fix plant tissues for studying biomineralization by means of scanning electron microscopy (SEM) and qualitative energy-dispersive X-ray microanalysis (EDX). Specimen preparation protocols for SEM and EDX mainly include fixation, dehydration, critical point drying (CPD), mounting, and coating. Gold-coated specimens are used for SEM imaging, while gold- and carbon-coated specimens are prepared for qualitative X-ray microanalyses separately to obtain complementary information on the elemental compositions of biominerals. During the specimen preparation procedure for SEM, some biominerals may be dislodged or scattered, making it difficult to determine their accurate locations, and light microscopy is used to complement SEM studies. Specimen preparation protocols for light microscopy generally include fixation, dehydration, infiltration and embedding with resin, microtome sectioning, and staining. In addition, microwave processing methods are adopted here to speed up the specimen preparation process for both SEM and light microscopy.

In-vitro bioactivity of zirconia doped borosilicate glasses

DOE Office of Scientific and Technical Information (OSTI.GOV)

Samudrala, Rajkumar; Azeem, P. Abdul, E-mail: rk.satyaswaroop@gmail.com, E-mail: drazeem2002@yahoo.com

2015-06-24

Glass composition 31B{sub 2}O{sub 3}-20SiO{sub 2}-24.5Na{sub 2}O-(24.5-x) CaO-xZrO{sub 2} x=1,2,3,4,5 were prepared by melt-quenching Technique. The formation of hydroxyapatite layer on the surface of glasses after immersion in simulated body fluid (SBF) was explored through XRD, Fourier transform infrared (FTIR) and Scanning electron microscopy (SEM-EDX) analyses. In this report, we observed that hydroxyapatite formation for 5days of immersion time. Also observed that with increasing the immersion time up to 15days, higher amount of hydroxyapatite layer formation on the surface of glasses. The varying composition of zirconia in glass samples influences shown by XRD, FTIR studies. The present results indicate that,more » in-vitro bioactivity of glasses decreased with increasing zirconia incorporation.« less

Synthesis of nanocrystalline CdS thin film by SILAR and their characterization

NASA Astrophysics Data System (ADS)

Mukherjee, A.; Satpati, B.; Bhattacharyya, S. R.; Ghosh, R.; Mitra, P.

2015-01-01

Cadmium sulphide (CdS) thin film was prepared by successive ion layer adsorption and reaction (SILAR) technique using ammonium sulphide as anionic precursor. Characterization techniques of XRD, SEM, TEM, FTIR and EDX were utilized to study the microstructure of the films. Structural characterization by x-ray diffraction reveals the polycrystalline nature of the films. Cubic structure is revealed from X-ray diffraction and selected area diffraction (SAD) patterns. The particle size estimated using X-ray line broadening method is approximately 7 nm. Instrumental broadening was taken into account while particle size estimation. TEM shows CdS nanoparticles in the range 5-15 nm. Elemental mapping using EFTEM reveals good stoichiometric composition of CdS. Characteristic stretching vibration mode of CdS was observed in the absorption band of FTIR spectrum. Optical absorption study exhibits a distinct blue shift in band gap energy value of about 2.56 eV which confirms the size quantization.

Preparation of MWCNT-Fe3O4 Nanocomposites from Iron Sand Using Sonochemical Route

NASA Astrophysics Data System (ADS)

Rahmawati, R.; Melati, A.; Taufiq, A.; Sunaryono; Diantoro, M.; Yuliarto, B.; Suyatman, S.; Nugraha, N.; Kurniadi, D.

2017-05-01

The composites of multi-walled carbon nanotube (MWCNT) and magnetite (Fe3O4) nanoparticles from iron sand were successfully prepared via the sonochemical route. In this experiment, the MWCNT-Fe3O4 nanocomposites were prepared with different compositions of MWCNT (0.01%, 0.02%, and 0.04%) with the constant composition of Fe3O4 particles. The characterizations were performed by means of X-Ray Diffractometry (XRD), Fourier Transform Infra-Red (FTIR) Spectrometer and Scanning Electron Microscopy (SEM) integrated with Energy Dispersive X-Ray (EDX). The XRD data analysis showed that the Fe3O4 crystallize in spinel structure in nanometric size. Furthermore, the crystallinity of the samples tended to reduce by increasing the MWCNT compositions. The SEM images showed that Fe3O4 tend to agglomerate in nanometric size. The FTIR spectra detected the functional groups of Fe-O bonding that showed the existence of Fe2+ and Fe3+. In the composites, the Fe3O4 nanoparticles were physically mixed with the MWCNTs constructing a unique structure. The as prepared MWCNT-Fe3O4 nanocomposites have the potential for bio-applications.

Ultrasonic-assisted synthesis of ZrO2 nanoparticles and their application to improve the chemical stability of Nafion membrane in proton exchange membrane (PEM) fuel cells.

PubMed

Taghizadeh, Mohammad Taghi; Vatanparast, Morteza

2016-12-01

Zirconium dioxide (ZrO2) nanoparticles were fabricated successfully via ultrasonic-assisted method using ZrO(NO3)2·H2O, ethylenediamine and hydrazine as precursors in aqueous solution. Morphology, structure and composition of the obtained products were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), dynamic light scattering (DLS), Fourier transform infrared spectroscopy (FT-IR) and diffuse reflectance spectroscopy (DRS). Then, the synthesized nanoparticles were used to prepare Nafion/ZrO2 nanocomposite membranes. The properties of the membranes were studied by ion exchange capacity (IEC) proton conductivity (σ), thermal stability and water uptake measurements. The ex-situ Fenton's test was used to investigate the chemical stability of the membranes. From our results, compared with Nafion membrane, the nanocomposite membrane exhibited lower fluoride release and weight loss. Therefore, it can concluded that Nafion/ZrO2 nanocomposite exhibit more chemical stability than the pure Nafion membrane. ATR-FTIR spectra and SEM surface images of membranes also confirm these results. Copyright © 2016 Elsevier Inc. All rights reserved.

Green synthesis of silver nanoparticles using tannins

NASA Astrophysics Data System (ADS)

Raja, Pandian Bothi; Rahim, Afidah Abdul; Qureshi, Ahmad Kaleem; Awang, Khalijah

2014-09-01

Colloidal silver nanoparticles were prepared by rapid green synthesis using different tannin sources as reducing agent viz. chestnut (CN), mangrove (MG) and quebracho (QB). The aqueous silver ions when exposed to CN, MG and QB tannins were reduced which resulted in formation of silver nanoparticles. The resultant silver nanoparticles were characterized using UV-Visible, X-ray diffraction (XRD), scanning electron microscopy (SEM/EDX), and transmission electron microscopy (TEM) techniques. Furthermore, the possible mechanism of nanoparticles synthesis was also derived using FT-IR analysis. Spectroscopy analysis revealed that the synthesized nanoparticles were within 30 to 75 nm in size, while XRD results showed that nanoparticles formed were crystalline with face centered cubic geometry.

Low cost heterogenous catalyst from (Achatina Fulica) snail shell and its application for biodiesel conversion via microwave irradiation

NASA Astrophysics Data System (ADS)

Fatimah, Is; Kurniastuti, E. A.; Basthiani, I. A.; Fakhri, A.

2017-11-01

Research on preparation of heterogenous catalyst from Achatina Fulica snail shell and its application biodiesel conversion has been investigation. Research aimed to obtain low cost and reusable catalyst for biodiesel production. The catalyst was prepared by grinding and calcining the snail shell at 900°C for 2 hours. The obtained solid was analysed by using XRD, SEM-EDX. FTIR, and also basicity measurement. Catalyst was used in the cenvertion of rice bran oil transesterification at varied volume of oil methanol ratio of 20-80 under microwave and reflux methode. The transesterification result were analyzed by using GCMS.

Erosion of mylar and protection by thin metal films

NASA Technical Reports Server (NTRS)

Fraundorf, P.; Lindstrom, D.; Sandford, S.; Swan, P.; Walker, R.; Zinner, E.; Pailer, N.

1983-01-01

Mylar strips, 2.5 microns thick, uncoated and coated with 50A, 100A and 200A of Al, Pd, and Au/Pd were exposed on STS-5 in order to measure the erosion of mylar and to test means of protecting thin plastic foils commonly used for space experiments in low earth orbit. Analysis by optical microscopy, SEM and STEM investigation, EDX measurements, FTIR spectroscopy and weight loss measurements showed that while up to 75 percent of the uncoated mylar was eroded during exposure, thin coatings of the above metals can protect mylar for integrated oxygen-fluxes of at least 10 to the 21st atoms/sq cm.

Synthesis of hybrid interfacial silica-based nanospheres composite as a support for ultra-small palladium nanoparticle and application of PdNPs/HSN in Mizoroki-Heck reaction

NASA Astrophysics Data System (ADS)

Rostamnia, Sadegh; Kholdi, Saba

2017-12-01

The silica based hollow nanosphere (silica-HNS) containing polymer of polyaniline was synthesized and chosen as a promising support for PdNPs. Then it was applied as a green catalyst in the reaction of Heck coupling with high yield. TEM and SEM-EDX/mapping images were used to study the structure and morphology. FT-IR spectroscopy, Thermal gravimetry analysis (TGA), and BET were used to characterize and investigate the catalyst. Also, the amounts of Pd loading were characterized by ICP-AES technique. Catalyst recyclability showed 5 successful runs for the reaction.

Silica functionalized Cu(II) acetylacetonate Schiff base complex: An efficient catalyst for the oxidative condensation reaction of benzyl alcohol with amines

NASA Astrophysics Data System (ADS)

Anbarasu, G.; Malathy, M.; Karthikeyan, P.; Rajavel, R.

2017-09-01

Silica functionalized Cu(II) acetylacetonate Schiff base complex via the one pot reaction of silica functionalized 3-aminopropyltriethoxysilane with acetyl acetone and copper acetate has been reported. The synthesized material was well characterized by analytical techniques such as FT-IR, UV-DRS, XRD, SEM-EDX, HR-TEM, EPR, ICP-AES and BET analysis. The characterization results confirmed the grafting of Cu(II) Schiff base complex on the silica surface. The catalytic activity of synthesized silica functionalized Cu(II) acetylacetonate Schiff base complex was evaluated through the oxidative condensation reaction of benzyl alcohol to imine.

Synthesis and characterization of nanocrystalline graphite from coconut shell with heating process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wachid, Frischa M., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Perkasa, Adhi Y., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id; Prasetya, Fandi A., E-mail: frischamw@yahoo.com, E-mail: adhiyudhaperkasa@yahoo.com, E-mail: afandisar@yahoo.com, E-mail: nurulrosyidah92@gmail.com, E-mail: darminto@physics.its.ac.id

Graphite were synthesized and characterized by heating process of coconut shell with varying temperature (400, 800 and 1000°C) and holding time (3 and 5 hours). After heating process, the samples were characterized by X-ray diffraction (XRD) and analyzed by X'pert HighScore Plus Software, Scanning Electron Microcope-Energy Dispersive X-Ray (SEM-EDX) and Transmission Electron Microscope-Energy Dispersive X-Ray (TEM-EDX). Graphite and londsdaelite phase were analyzed by XRD. According to EDX analysis, the sample was heated in 1000°C got the highest content of carbon. The amorphous carbon and nanocrystalline graphite were observed by SEM-EDX and TEM-EDX.

Characterization, Antibacterial and Antioxidant Properties of Silver Nanoparticles Synthesized from Aqueous Extracts of Allium sativum, Zingiber officinale, and Capsicum frutescens

PubMed Central

Otunola, Gloria Aderonke; Afolayan, Anthony Jide; Ajayi, Emmanuel Olusegun; Odeyemi, Samuel Wale

2017-01-01

Background: Herbal drug delivery is limited by poor solubility and bioavailability which can be overcome with suitable nanomaterials that will enhance their pharmacokinetics and performance. Objective: This study aimed to analyze the synthesis, characterization, and biological activities of silver nanoparticles (AgNPs) from three spices. Materials and Methods: AgNPs were prepared using 0.1 M silver nitrate and aqueous extracts of Allium sativum L. (garlic), Zingiber officinale Rosc. (ginger), and Capsicum frutescens L. (cayenne pepper). The AgNPs were characterized using ultraviolet-visible (UV-Vis) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray, X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. Results: The AgNPs were formed within an hour of the reaction and showed maximum UV-Vis absorption in the 375–480 nm range. SEM and TEM revealed well-dispersed spherical particles with little agglomeration, average sizes of 3–6 nm, 3–22 nm, and 3–18 nm for garlic, ginger, and cayenne pepper, respectively. FTIR showed that amine, protein, phenolic, aromatic, and alkynes groups contributed to AgNP synthesis and XRD confirmed their crystalline and face-centered cubic nature. Antibacterial action of the AgNPs was in the following order: ginger (minimum inhibitory concentration [MIC] <25 μg/mL) > garlic> cayenne pepper (MIC 125 μg/mL). Antioxidant action showed cayenne pepper > ginger > garlic (inhibitory concentration 50% [IC50]: 40, 240, and 250 μg/mL, respectively) against 2,2-Azino-bis (3-ethylbenzthiazoline-6-sulfonic acid) and garlic > cayenne pepper > ginger (IC50: <31.25, 40, and 120 μg/mL, respectively) against 1,1-diphenyl-2-picrylhydrazyl. Conclusion: Optimization of this green synthesis would support the production of AgNPs with great therapeutic potentials. SUMMARY The synthesis, characterization, and biological activities of silver nanoparticles (AgNPs) from garlic, ginger and cayenne pepper were evaluatedThe AgNPs formed were characterized using UV-Vis spectroscopy, SEM and TEM microscopy, as well as EDX, XRD and FTIR spectroscopy AgNPs were well dispersed with spherical shapes and average sizes of 3-6nm, 3-22nm and 3-18 nm for garlic, ginger and cayenne pepper respectivelyAmine, protein, phenolic and alkyne groups were revealed as the capping agents for the nanoparticlesThe silver nanoparticles were confirmed to be crystalline with characteristic face centred cubic natureThe antibacterial and antioxidant activities of the AgNPs confirmed the therapeutic potential of the AgNPs. Abbreviations used: AgNPs: Silver nanoparticles; UV-Vis: ultraviolet-visible; SEM: Scanning electron microscopy; TEM: Transmission electron microscopy; EDX: Energy dispersive X-ray; XRD: X-ray diffraction; FTIR: Fourier transform infrared; GaNPs: Garlic nanoparticles; GiNPs: Ginger nanoparticles; C.PeNPs: Cayenne pepper nanoparticles; FCC: Face centred cubic; SPR: Surface Plasmon resonance; ABTS-2: 2-Azino-bis (3-ethylbenzthiazoline-6-sulfonic acid); DPPH-1: 1-diphenyl-2-picrylhydrazyl. PMID:28808381

Characterization, Antibacterial and Antioxidant Properties of Silver Nanoparticles Synthesized from Aqueous Extracts of Allium sativum, Zingiber officinale, and Capsicum frutescens.

PubMed

Otunola, Gloria Aderonke; Afolayan, Anthony Jide; Ajayi, Emmanuel Olusegun; Odeyemi, Samuel Wale

2017-07-01

Herbal drug delivery is limited by poor solubility and bioavailability which can be overcome with suitable nanomaterials that will enhance their pharmacokinetics and performance. This study aimed to analyze the synthesis, characterization, and biological activities of silver nanoparticles (AgNPs) from three spices. AgNPs were prepared using 0.1 M silver nitrate and aqueous extracts of Allium sativum L. (garlic), Zingiber officinale Rosc. (ginger), and Capsicum frutescens L. (cayenne pepper). The AgNPs were characterized using ultraviolet-visible (UV-Vis) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray, X-ray diffraction (XRD), and Fourier transform infrared (FTIR) spectroscopy. The AgNPs were formed within an hour of the reaction and showed maximum UV-Vis absorption in the 375-480 nm range. SEM and TEM revealed well-dispersed spherical particles with little agglomeration, average sizes of 3-6 nm, 3-22 nm, and 3-18 nm for garlic, ginger, and cayenne pepper, respectively. FTIR showed that amine, protein, phenolic, aromatic, and alkynes groups contributed to AgNP synthesis and XRD confirmed their crystalline and face-centered cubic nature. Antibacterial action of the AgNPs was in the following order: ginger (minimum inhibitory concentration [MIC] <25 μg/mL) > garlic> cayenne pepper (MIC 125 μg/mL). Antioxidant action showed cayenne pepper > ginger > garlic (inhibitory concentration 50% [IC50]: 40, 240, and 250 μg/mL, respectively) against 2,2-Azino-bis (3-ethylbenzthiazoline-6-sulfonic acid) and garlic > cayenne pepper > ginger (IC50: <31.25, 40, and 120 μg/mL, respectively) against 1,1-diphenyl-2-picrylhydrazyl. Optimization of this green synthesis would support the production of AgNPs with great therapeutic potentials. The synthesis, characterization, and biological activities of silver nanoparticles (AgNPs) from garlic, ginger and cayenne pepper were evaluatedThe AgNPs formed were characterized using UV-Vis spectroscopy, SEM and TEM microscopy, as well as EDX, XRD and FTIR spectroscopy AgNPs were well dispersed with spherical shapes and average sizes of 3-6nm, 3-22nm and 3-18 nm for garlic, ginger and cayenne pepper respectivelyAmine, protein, phenolic and alkyne groups were revealed as the capping agents for the nanoparticlesThe silver nanoparticles were confirmed to be crystalline with characteristic face centred cubic natureThe antibacterial and antioxidant activities of the AgNPs confirmed the therapeutic potential of the AgNPs. Abbreviations used: AgNPs: Silver nanoparticles; UV-Vis: ultraviolet-visible; SEM: Scanning electron microscopy; TEM: Transmission electron microscopy; EDX: Energy dispersive X-ray; XRD: X-ray diffraction; FTIR: Fourier transform infrared; GaNPs: Garlic nanoparticles; GiNPs: Ginger nanoparticles; C.PeNPs: Cayenne pepper nanoparticles; FCC: Face centred cubic; SPR: Surface Plasmon resonance; ABTS-2: 2-Azino-bis (3-ethylbenzthiazoline-6-sulfonic acid); DPPH-1: 1-diphenyl-2-picrylhydrazyl.

Determination of anisotropy and multimorphology in fly ash based geopolymers

DOE Office of Scientific and Technical Information (OSTI.GOV)

Khan, M. Irfan, E-mail: mirfanwazir@gmail.com; Azizli, Khairun, E-mail: khairun-azizli@petronas.com.my; Sufian, Suriati, E-mail: suriati@petronas.com.my

2015-07-22

In this study, Malaysian coal fly ash-based geopolymers were investigated for its morphology and chemical composition using scanning electron microscopy coupled with energy dispersive X-rays (SEM-EDX). Geopolymer was synthesized using sodium hydroxide as activator. SEM studies revealed multiphasous structure of the material, composed of geopolymeric gel, partially reacted fly ashparticles and selectively leached particles. EDX analysis confirmed the chemical composition of different regions. Infra red spectroscopic studies supported the SEM-EDX analysis by confirming presence of unreacted quartzite and mullite in geopolymers. It is concluded that geopolymers possese a non uniform chemistry through out the structure.

Determination of anisotropy and multimorphology in fly ash based geopolymers

NASA Astrophysics Data System (ADS)

Khan, M. Irfan; Azizli, Khairun; Sufian, Suriati; Man, Zakaria; Siyal, Ahmer Ali; Ullah, Hafeez

2015-07-01

In this study, Malaysian coal fly ash-based geopolymers were investigated for its morphology and chemical composition using scanning electron microscopy coupled with energy dispersive X-rays (SEM-EDX). Geopolymer was synthesized using sodium hydroxide as activator. SEM studies revealed multiphasous structure of the material, composed of geopolymeric gel, partially reacted fly ashparticles and selectively leached particles. EDX analysis confirmed the chemical composition of different regions. Infra red spectroscopic studies supported the SEM-EDX analysis by confirming presence of unreacted quartzite and mullite in geopolymers. It is concluded that geopolymers possese a non uniform chemistry through out the structure.

GUIDELINES FOR THE APPLICATION OF SEM/EDX ANALYTICAL TECHNIQUES FOR FINE AND COARSE PM SAMPLES

EPA Science Inventory

Scanning Electron Microscopy (SEM) coupled with Energy-Dispersive X-ray analysis (EDX) is a powerful tool in the characterization and source apportionment of environmental particulate matter (PM), providing size, chemistry, and morphology of particles as small as a few tenths ...

EVALUATION OF COMPUTER-CONTROLLED SCANNING ELECTRON MICROSCOPY APPLIED TO AN AMBIENT URBAN AEROSOL SAMPLE

EPA Science Inventory

Recent interest in monitoring and speciation of particulate matter has led to increased application of scanning electron microscopy (SEM) coupled with energy-dispersive x-ray analysis (EDX) to individual particle analysis. SEM/EDX provides information on the size, shape, co...

GO-Cu7S4 catalyzed ortho-aminomethylation of phenol derivatives with N,N-dimethylbenzylamines: site-selective oxidative CDC.

PubMed

Gupta, Sonu; Chandna, Nisha; Dubey, Pooja; Singh, Ajai K; Jain, Nidhi

2018-06-21

Copper chalcogenide nanoparticles (Cu7S4) supported on graphene oxide (GO) have been synthesized for the first time from Cu2S, and used as highly efficient heterogeneous catalysts for oxidative ortho-selective C-H aminomethylation of phenols with N,N-dimethylbenzylamines. The NPs (30-80 nm) have been characterized by HRTEM, SEM-EDX, PXRD, FTIR, Raman, ICP-AES and XPS analyses. The NP catalyzed sp2-sp3 cross dehydrogenative coupling (CDC) features a broad substrate scope, excellent functional group tolerance, high yields, use of an inexpensive and reusable copper catalyst, mild conditions, and no need for pre-functionalization of substrates.

Fabrication and characterization of spiral interdigitated electrodes based biosensor for salivary glucose detection

NASA Astrophysics Data System (ADS)

Adelyn, P. Y. P.; Hashim, U.; Arshad, M. K. Md; Voon, C. H.; Liu, Wei-Wen; Kahar, S. M.; Huda, A. R. N.; Lee, H. Cheun

2017-03-01

This work introduces the non-invasive glucose monitoring technique by using the Complementary Metal Oxide Semiconductor (CMOS) technologically fabricated spiral Interdigitated Electrodes (IDE) based biosensor. Scanning Electron Microscopy (SEM) image explores the morphology of spiral IDE while Energy Dispersive X-Ray (EDX) determines the elements induced in spiral IDE. Oral saliva of two patients are collected and tested on the spiral IDE sensor with electrical characterization as glucose detection results. However, both patients exhibit their glucose level characteristics inconsistently. Therefore, this work could be extended and enhanced by adding Glutaraldehyde in between 3-Aminoproply)triethoxysilane (APTES) modified and glucose oxidase (GOD) enzyme immobilized layer with FTIR validation for bonding attachment.

Expulsion of selenium/protein nanoparticles through vesicle-like structures by Saccharomyces cerevisiae under microaerophilic environment.

PubMed

Zhang, Liang; Li, Daping; Gao, Ping

2012-12-01

Nano-selenium/protein is a kind of lower toxic supplement to human. Many microorganisms can reduce selenite/selenate to intracellular or extracellular selenium nanoparticles. This study examined the influence of dissolved oxygen on the expulsion of extracellular selenium/protein produced in Saccharomyces cerevisiae. More of the added selenite was reduced to extracellular selenium nanoparticles by yeast cells only under oxygen-limited condition than under aerobic or anaerobic condition. For the first time, we evidenced that selenium/protein nanoparticles synthesized in vivo were transported out of the cells by vesicle-like structures under microaerophilic environment. The characterizations of the extracellular spherical selenium/protein nanoparticles were also examined by SEM, TEM, EDX and FTIR.

Synthesis and Characterization of Sulfonated Graphene Oxide Nanofiller for Polymer Electrolyte Membrane

NASA Astrophysics Data System (ADS)

Ch'ng, Y. Y.; Loh, K. S.; Daud, W. R. W.; Mohamad, A. B.

2016-11-01

In this study, sulfonated graphene oxide (SGO) nanocomposite were produced as potential nanofiller to improve the properties of polymer electrolyte membrane (PEM) for fuel cell applications. The GO is produced by modified Hummers's method and the as-synthesized GO was used to prepare SGO with three distinctive precursors, namely 3- mercaptomethoxysilane (MPTMS), sulfanilic acid (SA) and butane sultone (BS). The SGO samples were characterized with several physical characterization techniques (XRD, FTIR, SEM-EDX and XPS) to provide the insights into the morphology; the state of homogenization; the crystallography and the functional groups. The experimental result indicated that the sulfonic acid group has been successfully incorporated with GO and can be used as filler in PEM.

A novel copper complex supported on magnetic reduced graphene oxide: an efficient and green nanocatalyst for the synthesis of 1-amidoalkyl-2-naphthol derivatives

NASA Astrophysics Data System (ADS)

Kooti, M.; Karimi, M.; Nasiri, E.

2018-02-01

A new Cu(II) complex supported on magnetic reduced graphene oxide was prepared and characterized by various techniques, such as FT-IR, XRD, SEM, EDX, TEM, TGA, BET, ICP, and VSM. The synthesized nanocomposite, which has size distribution of 25-30 nm, was employed as catalyst in one-pot synthesis of 1-amidoalkyl-2-naphthols via three-component condensation reaction of amides, aromatic aldehydes, and 2-naphthol, under solvent-free conditions. The introduced catalysis procedure for the synthesis of 1-amidoalkyl-2-naphthol derivatives offers several advantages namely, short reaction times, high yields, facile recyclability, and cost effectiveness. [Figure not available: see fulltext.

Porous carbon materials synthesized using IRMOF-3 and furfuryl alcohol as precursor

NASA Astrophysics Data System (ADS)

Deka, Pemta Tia; Ediati, Ratna

2016-03-01

IRMOF-3 crystals have been synthesized using solvothermal method by adding zinc nitrate hexahydrate with 2-amino-1,4-benzenedicarboxylic acid in N'N-dimethylformamide (DMF) at 100°C for 24 (note as IR-24) and 72 h (note as IR-72). The obtained crystals were characterized using X-ray Diffraction (XRD), SEM (Scanning Electron Microscopy) and Scanning Electron Microscopy-Energy Dispersive X-ray (SEM-EDX), FTIR and Isothermal adsorption-desorption N2. The diffractogram solids synthesized show characteristic peak at 2θ 6.8, 9.6 and 13.7°. SEM micrograph show cubic shape of IRMOF-3 crystal. Based on FTIR characterization, IRMOF-3 appear at wavelength (1691,46; 1425,3; 1238,21; 1319,22 dan 3504,42)cm-1. The Isotherm of crystal IRMOF-3 at heating time 24 h and 72 h are type IV. The surface area of IR-24 and IR-72 are respectively 24,758 m2/g and 29,139 m2/g with its dominant mesopores. Carbonaceous materials has been successfully synthesized using IR-24, IR-72 and furfuryl alcohol (FA) as second carbon precursor with variation of carbonation temperature 550, 700 and 850°C. The XRD result from both carbonaceous materials show formation of amorphous carbon and caharacteristic peak of ZnO oxide. Micrograph SEM show that carbonaceous materials have cubic shape as IRMOF-3 and SEM-EDX result indicate Zn and nitrogen content of these materials has decrease until temperature 850°C. Porous carbon using IR-24 and FA (notes as C-24) has increased surface area with higher carbonation temperature. The highest surface area is 1495,023 m2/g. Total pore volume and pore size of C-24 from low to high temperature respectively as (0,338; 0,539 and 1,598) cc/g; (0,107; 0,152 and 0,610) cc/g. Porous carbon using IR-72 and FA (notes as C-72) has smaller surface area than C-24 but its also increased during higher carbonation heating. The highest surface area is 1029,668 m2/g.The total pore volume and pore size of these carbon materials from low to high temperature respectively as (0,390; 0,727 and 1,345) cc/g and (0,065; 0,157 and 0,381) cc/g. Carbonaceous materials with high porosity and nitrogen content will be expected increase mechanical properties and hydrogen storage from these materials.

Intercalated chitosan/hydroxyapatite nanocomposites: Promising materials for bone tissue engineering applications.

PubMed

Nazeer, Muhammad Anwaar; Yilgör, Emel; Yilgör, Iskender

2017-11-01

Preparation and characterization of chitosan/hydroxyapatite (CS/HA) nanocomposites displaying an intercalated structure is reported. Hydroxyapatite was synthesized through sol-gel process. Formic acid was introduced as a new solvent to obtain stable dispersions of nano-sized HA particles in polymer solution. CS/HA dispersions with HA contents of 5, 10 and 20% by weight were prepared. Self-assembling of HA nanoparticles during the drying of the solvent cast films led to the formation of homogeneous CS/HA nanocomposites. Composite films were analyzed by scanning electron microscopy (SEM), atomic force microscopy (AFM), energy dispersive X-rays (EDX) analysis, Fourier transform infrared (FTIR) spectroscopy, X-rays diffraction (XRD) analysis and thermogravimetric analysis (TGA). SEM and AFM confirmed the presence of uniformly distributed HA nanoparticles on the chitosan matrix surface. XRD patterns and cross-sectional SEM images showed the formation of layered nanocomposites. Complete degradation of chitosan matrix in TGA experiments, led to the formation of nanoporous 3D scaffolds containing hydroxyapatite, β-tricalcium phosphate and calcium pyrophosphate. CS/HA composites can be considered as promising materials for bone tissue engineering applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

Fabrication of novel metal ion imprinted xanthan gum-layered double hydroxide nanocomposite for adsorption of rare earth elements.

PubMed

Iftekhar, Sidra; Srivastava, Varsha; Hammouda, Samia Ben; Sillanpää, Mika

2018-08-15

The work focus to enhance the properties of xanthan gum (XG) by anchoring metal ions (Fe, Zr) and encapsulating inorganic matrix (M@XG-ZA). The fabricated nanocomposite was characterized by Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Energy-dispersive X-ray spectroscopy (EDX), Fourier Transform Infrared Spectroscopy (FTIR), surface area (BET) and zeta potential analysis. The adsorption of Sc, Nd, Tm and Yb was investigated after screening of synthesized materials in detail to understand the influence of pH, contact time, temperature and initial REE (rare earth element) concentration both in single and multicomponent system via batch adsorption. The adsorption mechanism was verified by FTIR, SEM and elemental mapping. The SEM images of Zr@XG-ZA demonstrate scutes structure, which disappeared after adsorption of REEs. The maximum adsorption capacities were 132.30, 14.01, 18.15 and 25.73 mg/g for Sc, Nd, Tm and Yb, respectively. The adsorption efficiency over Zr@XG-ZA in multicomponent system was higher than single system and the REEs followed the order: Sc > Yb > Tm > Nd. The Zr@XG-ZA demonstrate good adsorption behavior for REEs up to five cycles and then it can be used as photocatalyst for the degradation of tetracycline. Thus, the work adds a new insight to design and preparation of efficient bifunctional adsorbents from sustainable materials for water purification. Copyright © 2018 Elsevier Ltd. All rights reserved.

Foulant Analysis of Three RO Membranes Used in Treating Simulated Brackish Water of the Iraqi Marshes

PubMed Central

Sachit, Dawood Eisa; Veenstra, John N.

2017-01-01

In this work, three different types of Reverse Osmosis (RO) (Thin-Film Composite (SE), Cellulose Acetate (CE), and Polyamide (AD)) were used to perform foulant analysis (autopsy) study on the deposited materials from three different simulated brackish surface feed waters. The brackish surface water qualities represented the water quality in Iraqi marshes. The main foulants from the simulated feed waters were characterized by using Scanning Electron Microscope (SEM) images and Energy-Dispersive X-ray Spectroscopy (EDXS) spectra. The effect of feed water temperatures (37 °C and 11 °C) on the formation of the fouled material deposited on the membrane surface was examined in this study. Also, pretreatment by a 0.1 micron microfiltration (MF) membrane of the simulated feed water in advance of the RO membrane on the precipitated material on the membrane surface was investigated. Finally, Fourier Transform Infrared Spectroscopy (FTIR) analysis was used to identify the functional groups of the organic matter deposited on the RO membrane surfaces. The SEM images and EDSX spectra suggested that the fouled material was mainly organic matter, and the major crystal deposited on the RO membrane was calcium carbonate (CaCO3). The FTIR spectra of the fouled RO membranes suggested that the constituents of the fouled material included aliphatic and aromatic compounds. PMID:28406468

Synthesis, characterization and cytotoxicity of rare earth metal ion complexes of N,N‧-bis-(2-thiophenecarboxaldimine)-3,3‧-diaminobenzidene, Schiff base ligand

NASA Astrophysics Data System (ADS)

Shakir, Mohammad; Abbasi, Ambreen; Faraz, Mohammad; Sherwani, Asif

2015-12-01

Lanthanide complexes of La3+, Pr3+, Nd3+, Gd3+, Er3+ of general formula [Ln2 L(H2O)4(NO3)4](NO3)2·2H2O have been synthesized from Schiff base, N,N‧-bis-(2-thiophenecarboxaldimine)-3,3‧-diaminobenzidene. The complexes were characterized by elemental analysis, molar conductance, UV-Vis, fluorescence, FT-IR,1H NMR, mass spectroscopy, EDX, SEM and thermal analysis. FT-IR spectral data suggested that ligand coordinate with metal ions through azomethine nitrogen and uncondensed amino group. Molar conductance data revealed 1:2 electrolytic nature of complexes. From the analytical data, the stoichiometry of the complexes was found to be 1:2 (ligand:metal). Thephysico-chemical data suggested eight coordination number for Ln(III)Schiffbase complexes. SEM analysis shows morphological changes in the surfaces of complexes as compared to free ligand. Thermal decomposition profiles were consistent with proposed formulations. The anticancer activity of the complexes and theSchiffbase ligand has been studied towards human cervical cancer celllines (HeLa) and human breast cancer cell lines (MCF-7) and it was found that complexes exhibited greater activity than theSchiffbase.

The Green synthesis of gold nanoparticles using an aqueous root extract of Morinda citrifolia L

NASA Astrophysics Data System (ADS)

Suman, T. Y.; Radhika Rajasree, S. R.; Ramkumar, R.; Rajthilak, C.; Perumal, P.

2014-01-01

In the present work, we describe the synthesis of gold nanoparticles using an aqueous root extract of Morinda citrifolia. UV-vis spectroscopy, XRD, FTIR, FE-SEM, EDX and TEM were performed to characterize the formation of gold nanoparticles. The synthesized gold nanoparticles were characterized by a peak at 540 nm in the UV-vis spectrum. The XRD peaks at 38°, 44°, 64° and 77° can be indexed to the (1 1 1), (2 0 0), (2 2 0) and (3 1 1) Bragg's reflections of cubic structure of metallic gold, respectively. The FTIR result showed that extract containing protein might be responsible for the formation of the nanoparticles and may play an important role in the stabilization of the formed nanoparticles. FESEM images revealed that the particles were triangle and mostly spherical in shape. TEM images clearly revealed the size of the nanoparticles were 12.17-38.26 nm in size.

The Green synthesis of gold nanoparticles using an aqueous root extract of Morinda citrifolia L.

PubMed

Suman, T Y; Rajasree, S R Radhika; Ramkumar, R; Rajthilak, C; Perumal, P

2014-01-24

In the present work, we describe the synthesis of gold nanoparticles using an aqueous root extract of Morinda citrifolia. UV-vis spectroscopy, XRD, FTIR, FE-SEM, EDX and TEM were performed to characterize the formation of gold nanoparticles. The synthesized gold nanoparticles were characterized by a peak at 540 nm in the UV-vis spectrum. The XRD peaks at 38°, 44°, 64° and 77° can be indexed to the (111), (200), (220) and (311) Bragg's reflections of cubic structure of metallic gold, respectively. The FTIR result showed that extract containing protein might be responsible for the formation of the nanoparticles and may play an important role in the stabilization of the formed nanoparticles. FESEM images revealed that the particles were triangle and mostly spherical in shape. TEM images clearly revealed the size of the nanoparticles were 12.17-38.26 nm in size. Copyright © 2013 Elsevier B.V. All rights reserved.

Iron oxide impregnated Morus alba L. fruit peel for biosorption of Co(II): biosorption properties and mechanism.

PubMed

Koduru, Janardhan Reddy; Chang, Yoon-Young; Yang, Jae-Kyu; Kim, Im-Soon

2013-01-01

Biosorption is an ecofriendly wastewater treatment technique with high efficiency and low operating cost involving simple process for the removal of heavy metal ions from aqueous solution. In the present investigation, Morus alba L. fruit peel powder (MAFP) and iron oxide impregnated Morus alba L. fruit peel powder (IO-MAFP) were prepared and used for treating Co(II) contaminated aqueous solutions. Further the materials were characterized by using FTIR and SEM-EDX analysis. From FT-IR analysis it was found that hydroxyl, methoxy, and carbonyl groups are responsible for Co(II) biosorption. The kinetic data obtained for both biosorbents was well fitted with pseudo-second-order kinetic model. The equilibrium data was in tune with the Langmuir and Freundlich isotherm models. The thermodynamic studies were also carried and it was observed that sorption process was endothermic at 298-328 K. These studies demonstrated that both biosorbents were promising, efficient, economic, and biodegradable sorbents.

Radioactive Cobalt(II) Removal from Aqueous Solutions Using a Reusable Nanocomposite: Kinetic, Isotherms, and Mechanistic Study

PubMed Central

Wang, Ximing; Chen, Zhangjing

2017-01-01

A lignocellulose/montmorillonite (LMT) nanocomposite was prepared as a reusable adsorbent for cobalt(II) ions, and characterized by nitrogen (N2) adsorption/desorption isotherm, X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), Transmission Electron Microscopy (TEM), and Fourier Transform Infrared Spectroscopy (FTIR). LMT exhibited efficient adsorption of cobalt ions (Co(II)), and the adsorbed Co(II) was readily desorbed by nitric acid (HNO3). All parameters affecting the adsorption and/or desorption of Co(II), including initial Co(II) concentration, pH value, temperature, HNO3 concentration, and time, were optimized. The kinetic data analysis showed that the adsorption followed the pseudo-second-order kinetic model and fit well into the Langmuir isotherm equation. Notably, the nanocomposite can be used four times without significantly losing adsorbent capability. The Energy-Dispersive X-ray (EDX) and FTIR spectra analysis also revealed that the adsorption mechanism may be mainly a chemical adsorption dominated process. PMID:29186794

Novel nanofiberous membrane fabricated via electrospinning of wastage fuzzes of mechanized carpet used for dye removal of the carpet dyeing wastewater.

PubMed

Akbari, Ahmad; Sheshdeh, Farhad Jokari; Jabbari, Vahid

2012-01-01

Novel nanofibrous membrane was fabricated by using electrospinning of wastage fuzzes of mechanized carpet which was used to remove the dye of the textile wastewater. SEM images showed that nanofibers with average diameters of 200 nm were successfully fabricated by electrospinning technique. The physicochemical properties of electrospun nanofiberous membranes were studied by differential scanning calorimetry (DSC), energy-dispersive X-ray (EDX), and Fourier transform infrared (FTIR) spectroscopy. FTIR confirmed the presence of C≡N, C=N, and C‒N groups in the electrospun nanofibers which are the main functional groups of polyacrilonitrile (PAN). The resulting membrane showed dye retention of 96% of carpet dyeing wastewater, demonstrating the high separation potential of such membrane for wastewater treatment. We believe that simple approaches such as the present one would open up enormous possibilities in effective uses of wastage fuzzes of textile industry, considering the fact that electrospinning is a cost-effective method for the mass scale production of nanofibers.

Iron Oxide Impregnated Morus alba L. Fruit Peel for Biosorption of Co(II): Biosorption Properties and Mechanism

PubMed Central

Koduru, Janardhan Reddy; Chang, Yoon-Young; Yang, Jae-Kyu; Kim, Im-Soon

2013-01-01

Biosorption is an ecofriendly wastewater treatment technique with high efficiency and low operating cost involving simple process for the removal of heavy metal ions from aqueous solution. In the present investigation, Morus alba L. fruit peel powder (MAFP) and iron oxide impregnated Morus alba L. fruit peel powder (IO-MAFP) were prepared and used for treating Co(II) contaminated aqueous solutions. Further the materials were characterized by using FTIR and SEM-EDX analysis. From FT-IR analysis it was found that hydroxyl, methoxy, and carbonyl groups are responsible for Co(II) biosorption. The kinetic data obtained for both biosorbents was well fitted with pseudo-second-order kinetic model. The equilibrium data was in tune with the Langmuir and Freundlich isotherm models. The thermodynamic studies were also carried and it was observed that sorption process was endothermic at 298–328 K. These studies demonstrated that both biosorbents were promising, efficient, economic, and biodegradable sorbents. PMID:24324384

Morphology and phase identification of micron to nanosized manganese oxide (MnO) with variations in sintering time

NASA Astrophysics Data System (ADS)

Sasongko, Muhammad Ilman Nur; Puspitasari, Poppy; Yazirin, Cepi; Tsamroh, Dewi Izzatus; Risdanareni, Puput

2017-09-01

Manganese oxide (MnO) occurs in many rock types and may take the form of minerals. MnO has its drawbacks, namely highly reactive oxidizing species classified as dangerous and explosive at temperatures above 55 °C. Despite this,MnO has excellent magnetic, electrochemical, and conductivity properties, which should be reduced to nano-size to maximize their use and improve the properties of MnO. Phase and morphology characterization of powder this research aims to reduce the grain size of the MnO from micro to nano using the sol-gel method with various sintering times. Sol-gel is a simple synthesis method that has been proven capable of synthesizing a wide variety of micro-sized oxide materials into nano. Sintering time is a technique performed in the synthesis process to dry the material to a temperature above the normal temperature. The temperature used for sintering starting from 600 °C to 1000 °C. Characterizations were done using XRD, SEM, EDX, and FTIR machines. The sintering processes in this study used a temperature of 600 °C with different sintering periods of 30, 60 and 90 minutes. The XRD characterization with a 30-minute sintering time resulted in the smallest MnO in the form crystalline powder of 47.3 nm. The highest intensity (degree of crystallinity) found in MnO sintered for 90 minutes. The results of the morphological characterization of SEM showed a morphological change in MnO from micro-sized triangular to nano-sized spherical shape. The EDX characterization results indicated that the 30-minute sintering caused the lowest change in Mn and the highest change in O. The results of FTIR characterization showed a shift in C-H and Mn-O followed by an increase in the group of N-H, C=O and Mn-O.

Synthesize, characterization, and anti-Parkinson activity of silver-Indonesian velvet beans (Mucuna pruriens) seed extract nanoparticles (AgMPn)

NASA Astrophysics Data System (ADS)

Sardjono, R. E.; Khoerunnisa, F.; Musthopa, I.; Akasum, N. S. M. M.; Rachmawati, R.

2018-05-01

Parkinson is one of the progressive neurodegenerative diseases. Various efforts are made in handling this disease, one of them is the utilization of plant extracts that have anti-Parkinson activity, for example, velvet bean (Mucuna pruriens L.). Changing the particle size of the extract into nanoscale particle is expected to increase its anti-parkinson activity. The research was conducted to synthesize silver-velvet bean (Mucuna pruriens L.) seed extract nanoparticles (AgMPn) and to evaluate its antiparkinson activity through the catalepsy test in mice. The research consisted of several stages i.e. extraction of velvet bean seed powder, synthesis and characterization of AgMPn, and catalepsy test of AgMPn. Velvet bean seed powder was extracted by maceration method using ethanol-water (1:1) at pH 3 adjusted with citric acid. AgMPn was synthesized by reacting the silver nitrate (AgNO3) solution with the extract of velvet bean seed for 40 min, dispersibility of solution during the reaction was controlled by using sonication and ultrasonic processor homogenizer. Characterization of AgMPn was done by using Fourier transform infrared (FT-IR), scanning electron microscopy-energy dispersive X-ray (SEM-EDX), and transmission electron microscopy (TEM). Catalepsy test was conducted on AgMpn at the doses of 5, 10, 15, 20 and 25 mg/kg body weight. The results of SEM-EDX and TEM showed that AgMPn formed aggregates with several shapes such as rectangle, oval, and spherical, with the average particle diameter was 36.5 nm. FT-IR spectra showed a band at 464.8 cm-1 absorbance area which is typical band indicated the interaction of Ag-O of AgMPn. Catalepsy test demonstrated that AgMPn at the doses of 5, 15, and 20 mg/kg body weight lowered the catalepsy symptoms in mice significantly, with the best dose was 5 mg/kg body weight.

Potentiating the antibacterial effect of silver nanospheres by surface-capping with chlorhexidine gluconate

NASA Astrophysics Data System (ADS)

Priyadarshini, Balasankar Meera; Fawzy, Amr S.

2017-04-01

In this work, the commercial polyvinylpyrrolidone (PVP)-capped silver nanospheres (Ag-NSP) were surface decorated with chlorhexidine gluconate (CHXg) for potentiating the antibacterial properties of Ag-NSP. Different formulations of CHXg-loaded Ag-NSP (Ag-NSP/CHXg) were prepared by varying the incubation times (0.5, 1.5, and 3 h). A thorough characterization of Ag-NSP/CHXg nanospheres has been carried out by dynamic light scattering (DLS), transmission electron microscopy (TEM), energy-dispersive surface elemental composition spectral analysis (SEM/EDX), Fourier transform infrared spectroscopy (FTIR), percentage (%) CHXg loading efficiency (LE), in vitro CHXg and Ag+ ion release, antibacterial/biofilm inhibition assay, and human mesenchymal stem cells (hMSCs) cytotoxicity evaluation. DLS measured nanospheres to be <160 nm and indicated that CHXg treatment drastically shifted the surface charge from negative to high positive values, with homogenous distribution. TEM revealed spherical Ag-NSP/CHXg nanospheres with a clearly visible surface coating of CHXg. FTIR confirmed association of CHXg with Ag-NSP nanospheres, whereas SEM/EDX data verified presence of spectral peaks specific to silver (Ag), CHXg, and PVP. The %LE gradually increased with increasing incubation times. In vitro CHXg release exhibited a bi-phasic fashion showing maximum release of 74.83 ± 20.67% from Ag-NSP/CHXg-3h at 14 days. A slow release of Ag+ ions was detected; however, the surface decoration of Ag-NSP substantially hampered/restricted the liberation of ions. Agar well diffusion, MTS (3-(4,5-dimethylthiazol-2-yl)-5-(3-carboxymethoxyphenyl)-2-(4-sulfophenyl)-2H-tetrazolium), and crystal violet assay suggested good antibacterial/antibiofilm activity of Ag-NSP/CHXg that correlated with the increasing %LE of nanospheres. hMSCs cytotoxicity study showed low toxicity properties of all nanosphere formulations, except for Ag-NSP/CHXg-3h, affecting the cell viability at all proposed concentrations and exposure time points. CHXg accentuated the antibacterial properties of Ag-NSP.

Biosynthesis of zinc oxide nanoparticles using leaf extract of Calotropis gigantea: characterization and its evaluation on tree seedling growth in nursery stage

NASA Astrophysics Data System (ADS)

Chaudhuri, Sadhan Kumar; Malodia, Lalit

2017-11-01

Green synthesis of zinc oxide nanoparticles was carried out using Calotropis leaf extract with zinc acetate salt in the presence of 2 M NaOH. The combination of 200 mM zinc acetate salt and 15 ml of leaf extract was ideal for the synthesis of less than 20 nm size of highly monodisperse crystalline nanoparticles. Synthesized nanoparticles were characterized through UV-Vis spectroscopy, dynamic light scattering (DLS), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), EDX (energy dispersive X-ray), and AFM (atomic force microscopy). Effects of biogenic zinc oxide (ZnO) nanoparticles on growth and development of tree seedlings in nursery stage were studied in open-air trenches. The UV-Vis absorption maxima showed peak near 350 nm, which is characteristic of ZnO nanoparticles. DLS data showed that single peak is at 11 nm (100%) and Polydispersity Index is 0.245. XRD analysis showed that these are highly crystalline ZnO nanoparticles having an average size of 10 nm. FTIR spectra were recorded to identify the biomolecules involved in the synthesis process, which showed absorption bands at 4307, 3390, 2825, 871, 439, and 420 cm-1. SEM images showed that the particles were spherical in nature. The presence of zinc and oxygen was confirmed by EDX and the atomic % of zinc and oxygen were 33.31 and 68.69, respectively. 2D and 3D images of ZnO nanoparticles were obtained by AFM studies, which indicated that these are monodisperse having size ranges between 1.5 and 8.5 nm. Significant enhancement of growth was observed in Neem ( Azadirachta indica), Karanj ( Pongamia pinnata), and Milkwood-pine ( Alstonia scholaris) seedlings in foliar spraying ZnO nanoparticles to nursery stage of tree seedlings. Out of the three treated saplings, Alstonia scholaris showed maximum height development.

Scanning Electron Microscope-Cathodoluminescence Analysis of Rare-Earth Elements in Magnets.

PubMed

Imashuku, Susumu; Wagatsuma, Kazuaki; Kawai, Jun

2016-02-01

Scanning electron microscope-cathodoluminescence (SEM-CL) analysis was performed for neodymium-iron-boron (NdFeB) and samarium-cobalt (Sm-Co) magnets to analyze the rare-earth elements present in the magnets. We examined the advantages of SEM-CL analysis over conventional analytical methods such as SEM-energy-dispersive X-ray (EDX) spectroscopy and SEM-wavelength-dispersive X-ray (WDX) spectroscopy for elemental analysis of rare-earth elements in NdFeB magnets. Luminescence spectra of chloride compounds of elements in the magnets were measured by the SEM-CL method. Chloride compounds were obtained by the dropwise addition of hydrochloric acid on the magnets followed by drying in vacuum. Neodymium, praseodymium, terbium, and dysprosium were separately detected in the NdFeB magnets, and samarium was detected in the Sm-Co magnet by the SEM-CL method. In contrast, it was difficult to distinguish terbium and dysprosium in the NdFeB magnet with a dysprosium concentration of 1.05 wt% by conventional SEM-EDX analysis. Terbium with a concentration of 0.02 wt% in an NdFeB magnet was detected by SEM-CL analysis, but not by conventional SEM-WDX analysis. SEM-CL analysis is advantageous over conventional SEM-EDX and SEM-WDX analyses for detecting trace rare-earth elements in NdFeB magnets, particularly dysprosium and terbium.

Characterization of electron-beam-modified surface coated clay fillers and their influence on physical properties of rubbers

NASA Astrophysics Data System (ADS)

Ray, Sudip; Bhowmick, Anil K.; Sarma, K. S. S.; Majali, A. B.; Tikku, V. K.

2002-12-01

A novel process of surface modification of clay filler has been developed by coating this with an acrylate monomer, trimethylol propane triacrylate (TMPTA) or a silane coupling agent, triethoxy vinyl silane (TEVS) followed by electron beam irradiation. Characterization of these surface modified fillers has been carried out by Fourier-transform infrared analysis (FTIR), electron spectroscopy for chemical analysis (ESCA), wettability by dynamic wicking method measuring the rise of a liquid through a filler-packed capillary tube and water flotation test, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), thermogravimetric analysis (TGA), and X-ray diffraction (XRD). Presence of the acrylate and the silane coupling agent on the modified fillers has been confirmed from FTIR, ESCA, and EDX studies, which has also been supported by TGA studies. The contact angle measurement by dynamic wicking method suggests improvement in hydrophobicity of the treated fillers, which is supported by water flotation test especially in the case of silanized clay. However, XRD studies demonstrate that the entire modification process does not affect the bulk properties of the fillers. Finally, both unmodified and modified clay fillers have been incorporated in styrene butadiene rubber (SBR) and nitrile rubber (NBR). Rheometric and mechanical properties reveal that there is a definite improvement using these modified fillers specially in the case of silanized clay compared to the control sample, probably due to successful enhancement in interaction between the treated clay and the base polymer.

Structural studies on Demospongiae sponges from Gökçeada Island in the Northern Aegean Sea

NASA Astrophysics Data System (ADS)

Bayari, Sevgi Haman; Şen, Elif Hilal; Ide, Semra; Topaloglu, Bülent

2018-03-01

The Demospongiae is the largest Class in the phylum Porifera (sponges). Most sponge species in the Class Demospongiae have a skeleton of siliceous spicules and/or protein spongin or both. The first aim of this study was to perform the morphological and structural characterization of the siliceous spicules of four species belonging to Class Demospongiae (Suberites domuncula, Axinella polypoides, Axinella damicornis and Agelas oroides) collected around Gökçeada Island-Turkey (Northern Aegean Sea). The characterizations were carried out using a combination of Scanning Electron Microscopy with Energy Dispersive X-ray Spectroscopy (SEM/EDX), Attenuated Total Reflection-Fourier Transform Infrared Spectroscopy (ATR-FTIR) and Small Angle X-ray Scattering (SAXS) techniques. The sponge Chondrosia reniformis (Porifera, Demospongiae) lacks a structural skeleton of spicules or the spongin. It consists mainly of a collagenous tissue. The collagen with sponge origin is an important source in biomedical and pharmaceutical applications. The second aim of this study was to provide more information on the molecular structure of collagen of outer (ectosome) and inner (choanosome) regions of the Chondrosia reniformis using ATR-FTIR spectroscopy. Hierarchical clustering analysis (HCA) was also used for the discrimination of ATR-FTIR spectra of species.

In Situ Characterization of Boehmite Particles in Water Using Liquid SEM

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yao, Juan; Arey, Bruce W.; Yang, Li

In situ imaging and elemental analysis of boehmite (AlOOH) particles in water is realized using the System for Analysis at the Liquid Vacuum Interface (SALVI) and Scanning Electron Microscopy (SEM). This paper describes the method and key steps in integrating the vacuum compatible SAVLI to SEM and obtaining secondary electron (SE) images of particles in liquid in high vacuum. Energy dispersive x-ray spectroscopy (EDX) is used to obtain elemental analysis of particles in liquid. A synthesized AlOOH particle is used as a model in the liquid SEM illustration. Our results demonstrate that particles can be imaged in the SE modemore » with good resolution. The AlOOH EDX spectrum shows significant signal from the Al compared with deionized water and the empty channel control. In situ liquid SEM is a powerful technique to study particles in liquid with many exciting applications. This procedure aims to provide technical details in how to conduct liquid SEM imaging and EDX analysis using SALVI and reduce potential pitfalls using this approach for other researchers.« less

Enhanced EDX images by fusion of multimodal SEM images using pansharpening techniques.

PubMed

Franchi, G; Angulo, J; Moreaud, M; Sorbier, L

2018-01-01

The goal of this paper is to explore the potential interest of image fusion in the context of multimodal scanning electron microscope (SEM) imaging. In particular, we aim at merging the backscattered electron images that usually have a high spatial resolution but do not provide enough discriminative information to physically classify the nature of the sample, with energy-dispersive X-ray spectroscopy (EDX) images that have discriminative information but a lower spatial resolution. The produced images are named enhanced EDX. To achieve this goal, we have compared the results obtained with classical pansharpening techniques for image fusion with an original approach tailored for multimodal SEM fusion of information. Quantitative assessment is obtained by means of two SEM images and a simulated dataset produced by a software based on PENELOPE. © 2017 The Authors Journal of Microscopy © 2017 Royal Microscopical Society.

Synthesis of hydroxyapatite nanoparticles from egg shells by sol-gel method

NASA Astrophysics Data System (ADS)

Azis, Y.; Adrian, M.; Alfarisi, C. D.; Khairat; Sri, R. M.

2018-04-01

Hydroxyapatite, [Ca10(PO4)6(OH)2, (HAp)] is widely used in medical fields especially as a bone and teeth substitute. Hydroxyapatite nanoparticles have been succesfully synthesized from egg shells as a source of calcium by using sol-gel method. The egg shells were calcined, hydrated (slaking) and undergone carbonation to form Precipitated Calcium Carbonate (PCC).Then the PCC was added (NH4)2HPO4 to form HAp with variation the mole ratio Ca and P (1.57; 1.67 and 1.77), aging time (24, 48, and 72 hr) and under basic condition pH (9, 10 and 11). The formation of hydroxyapatite biomaterial was characterized using XRD, FTIR, SEM-EDX. The XRD patterns showed that the products were hydroxyapatite crystals. The best result was obtained at 24 hr aging time, pH 9 with hexagonal structure of hydroxyapatite. Particle size of HAp was 35-54 nm and the morphology of hydroxyapatite observed using SEM, it showed that the uniformity crystal of hydroxyapatite.

Investigation on the effect of collagen and vitamins on biomimetic hydroxyapatite coating formation on titanium surfaces.

PubMed

Ciobanu, Gabriela; Ciobanu, Octavian

2013-04-01

This study uses an in vitro experimental approach to investigate the roles of collagen and vitamins in regulating the deposition of hydroxyapatite layer on the pure titanium surface. Titanium implants were coated with a hydroxyapatite layer under biomimetic conditions by using a supersaturated calcification solution (SCS), modified by adding vitamins A and D3, and collagen. The hydroxyapatite deposits on titanium were investigated by means of scanning electron microscopy (SEM) coupled with X-ray analysis (EDX), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) spectroscopy. The results obtained have shown that hydroxyapatite coatings were produced in vitro under vitamins and collagen influence. Copyright © 2012 Elsevier B.V. All rights reserved.

Highly stretchable nanoalginate based polyurethane elastomers.

PubMed

Daemi, Hamed; Barikani, Mehdi; Barmar, Mohammad

2013-06-20

Highly stretchable elastomeric samples based on cationic polyurethane dispersions-sodium alginate nanoparticles (CPUD/SA) were prepared by the solution blending of sodium alginate and aqueous polyurethane dispersions. CPUDs were synthesized by step growth polymerization technique using N-methyldiethanolamine (MDEA) as a source of cationic emulsifier. The chemical structure and thermal-mechanical properties of these systems were characterized using FTIR and DMTA, respectively. The presence of nanoalginate particles including nanobead and nanorod particles were proved by SEM and EDX. It was observed that thermal properties of composites increased with increasing SA content. All prepared samples were known as thermoplastic-elastomers with high percentages of elongation. Excellent compatibility of prepared nanocomposites was proved by the DMTA data. Copyright © 2013 Elsevier Ltd. All rights reserved.

Synthesis and characterization of ionic liquid immobilized on magnetic nanoparticles: A recyclable heterogeneous organocatalyst for the acetylation of alcohols

NASA Astrophysics Data System (ADS)

Ghorbani-Choghamarani, Arash; Norouzi, Masoomeh

2016-03-01

Herein, we describe a simple and efficient procedure for the preparation of 3-((3-(trisilyloxy)propyl)propionamide)-1-methylimidazolium chloride ionic liquid supported on magnetic nanoparticle (TPPA-IL-Fe3O4). The structure of this magnetic ionic liquid is fully characterized by FT-IR, TGA, XRD, VSM, SEM, EDX and DLS techniques. TPPA-IL-Fe3O4 is employed as a catalyst for the acetylation of alcohols with acetic anhydride under mild and heterogeneous conditions at room temperature with good to excellent yields. The magnetic catalyst could be readily separate from the reaction media by simple magnetic decantation, and reused several times without significant loss of its catalytic activity.

How biological crusts are stabilizing the soil surface? The devolpment of organo-mineral interactions in the initial phase

NASA Astrophysics Data System (ADS)

Fischer, T.; Veste, M.; Wiehe, W.; Lange, P.

2009-04-01

First colonizers of new land surfaces are cryptogames which often form biological soil crusts (BSC) covering the first millimetre of the top soil in many ecosystems from polar to desert ecosystems. These BSC are assemblages of cyanobacteria, green algae, mosses, liverworts, fungi and/or lichens. The development of soil surface crusts plays a major role for the further vegetation pattern through changes to the physico-chemical conditions and influencing various ecosystem processes. We studied the development of BSC on quaternary substrate of an initial artificial water catchment in Lusatia, Germany. Due to lack of organic matter in the geological substrate, photoautotrophic organisms like green algae and cyanobacteria dominated the initial phases of ecosystem development and, hence, of organo-mineral ineractions. We combined SEM/EDX and FTIR microscopy to study the contact zone of extracellular polymeric substances (EPS) of green algae and cyanobacteria with quartz, spars and mica on a >40 µm scale in undisturbed biological soil crusts, which had a maximum thickness of approx. 2 mm. SEM/EDX microscopy was used to determine the spatial distribution of S, Ca, Fe, Al, Si and K in the profiles, organic compounds were identified using FTIR microscopy. Exudates of crust organisms served as cementing material between sand particles. The crust could be subdivided into two horizontal layers. The upper layer, which had a thickness of approx. 200 µm, is characterized by accumulation of Al and K, but absence of Fe in microbial derived organic matter, indicating capture of weathering products of feldspars and mica by microbial exudates. The pore space between mineral particles was entirely filled with organic matter here. The underlying layer can be characterized by empty pores and organo-mineral bridges between the sand particles. Contrarily to the upper layer of the crust, Fe, Al and Si were associated with organic matter here but K was absent. Highest similarity of the FTIR spectra of EPS was observed with carbohydrates, using cellulose, dextran and humic acid Na salt as controls. Obviously, humification does not play a key role during this initial phase of soil formation. It was hypothesized that biological soil crusts facilitate the weathering of mineral substrate by (I) circumventing loss of fine particles with erosion, (II) by chemical treatment of minerals and (III) by catching small mineral-particles by glutinous EPS on the soil surface from the surrounding area.

Synthesis and controlled release properties of 2,4-dichlorophenoxy acetate–zinc layered hydroxide nanohybrid

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bashi, Abbas M., E-mail: abbasmatrood@yahoo.com; Hussein, Mohd Zobir; Zainal, Zulkarnain

2013-07-15

Direct reaction of ZnO with 2,4-dichlorophenoxyacetic acid (24D) solutions of different concentrations allows obtaining new organic–inorganic nanohybrid materials formed by intercalation of 24D into interlayers of zinc layered hydroxide (ZLH). XRD patterns show a progressive evolution of the structure as 24D concentration increases. The nanohybrid obtained at higher 24D concentration (24D–ZLH(0.4)) reveals a well ordered layered structure with two different basal spacings at 25.2 Å and 24 Å. The FTIR spectrum showing the vibrations bands of the functional groups of 24D and of the ZLH confirms the intercalation. SEM images are in agreement with the structural evolution observed by XRDmore » and reveal the ribbon morphology of the nanohybrids. The release studies of 24D showed a rapid release of 94% for the first 100 min governed by the pseudo-second order kinetic model. - Graphical abstract: The phenomenon indicates that the optical energy gap is enlarged with the increase of molar concentrations in 2,4-dichlorophenoxy acetate anion content into ZnO to create a ZLH–24D nanohybrid. - Highlights: • Nanohybrid was synthesized from 2,4-dichlorophenoxy acetate with-Zinc LHD, using wet chemistry. • Characterized using SEM, TEM, EDX, FTIR, XRD and TGA. • Ribbon-shaped 24D–Zn-layered hydroxide nanoparticles with (003) diffractions of 2.5 nm phase were synthesized.« less

In Situ Characterization of Boehmite Particles in Water Using Liquid SEM.

PubMed

Yao, Juan; Arey, Bruce W; Yang, Li; Zhang, Fei; Komorek, Rachel; Chun, Jaehun; Yu, Xiao-Ying

2017-09-27

In situ imaging and elemental analysis of boehmite (AlOOH) particles in water is realized using the System for Analysis at the Liquid Vacuum Interface (SALVI) and Scanning Electron Microscopy (SEM). This paper describes the method and key steps in integrating the vacuum compatible SAVLI to SEM and obtaining secondary electron (SE) images of particles in liquid in high vacuum. Energy dispersive x-ray spectroscopy (EDX) is used to obtain elemental analysis of particles in liquid and control samples including deionized (DI) water only and an empty channel as well. Synthesized boehmite (AlOOH) particles suspended in liquid are used as a model in the liquid SEM illustration. The results demonstrate that the particles can be imaged in the SE mode with good resolution (i.e., 400 nm). The AlOOH EDX spectrum shows significant signal from the aluminum (Al) when compared with the DI water and the empty channel control. In situ liquid SEM is a powerful technique to study particles in liquid with many exciting applications. This procedure aims to provide technical know-how in order to conduct liquid SEM imaging and EDX analysis using SALVI and to reduce potential pitfalls when using this approach.

Glass-ceramic coating material for the CO2 laser based sintering of thin films as caries and erosion protection.

PubMed

Bilandžić, Marin Dean; Wollgarten, Susanne; Stollenwerk, Jochen; Poprawe, Reinhart; Esteves-Oliveira, Marcella; Fischer, Horst

2017-09-01

The established method of fissure-sealing using polymeric coating materials exhibits limitations on the long-term. Here, we present a novel technique with the potential to protect susceptible teeth against caries and erosion. We hypothesized that a tailored glass-ceramic material could be sprayed onto enamel-like substrates to create superior adhesion properties after sintering by a CO 2 laser beam. A powdered dental glass-ceramic material from the system SiO 2 -Na 2 O-K 2 O-CaO-Al 2 O 3 -MgO was adjusted with individual properties suitable for a spray coating process. The material was characterized using X-ray fluorescence analysis (XRF), heating microscopy, dilatometry, scanning electron microscopy (SEM), grain size analysis, biaxial flexural strength measurements, fourier transform infrared spectroscopy (FTIR), and gas pycnometry. Three different groups of samples (each n=10) where prepared: Group A, powder pressed glass-ceramic coating material; Group B, sintered hydroxyapatite specimens; and Group C, enamel specimens (prepared from bovine teeth). Group B and C where spray coated with glass-ceramic powder. All specimens were heat treated using a CO 2 laser beam process. Cross-sections of the laser-sintered specimens were analyzed using laser scanning microscopy (LSM), energy dispersive X-ray analysis (EDX), and SEM. The developed glass-ceramic material (grain size d50=13.1mm, coefficient of thermal expansion (CTE)=13.310 -6 /K) could be spray coated on all tested substrates (mean thickness=160μm). FTIR analysis confirmed an absorption of the laser energy up to 95%. The powdered glass-ceramic material was successfully densely sintered in all sample groups. The coating interface investigation by SEM and EDX proved atomic diffusion and adhesion of the glass-ceramic material to hydroxyapatite and to dental enamel. A glass-ceramic material with suitable absorption properties was successfully sprayed and laser-sintered in thin films on hydroxyapatite as well as on bovine enamel. The presented novel technique of tooth coating with a dental glass-ceramic using a CO 2 -laser holds a great potential as a possible method to protect susceptible teeth against caries and erosion. Copyright © 2017 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Using ICP-OES and SEM-EDX in biosorption studies

PubMed Central

Chojnacka, Katarzyna; Marycz, Krzysztof

2010-01-01

We have compared the analytical results obtained by inductively coupled plasma optical emission spectroscopy (ICP-OES) and by scanning electron microscopy with an energy dispersive X-ray analytical system (SEM-EDX) in order to explore the mechanism of metal ions biosorption by biomass using two independent methods. The marine macroalga Enteromorpha sp. was enriched with Cu(II), Mn(II), Zn(II), and Co(II) ions via biosorption, and the biosorption capacity of alga determined from the solution and biomass composition before and after biosorption process was compared. The first technique was used to analyze the composition of the natural and metal-loaded biomass, and additionally the composition of the solution before and after biosorption. The second technique was used to obtain a picture of the surface of natural and metal ion-loaded macroalgae, to map the elements on the cell wall of dry biomass, and to determine their concentration before and after biosorption. ICP-OES showed a better precision and lower detection limit than EDX, but SEM-EDX gave more information regarding the sample composition of Enteromorpha sp. Both techniques confirmed that biosorption is a surface phenomenon, in which alkali and alkaline earth metal ions were exchanged by metal ions from aqueous solution. Figure The advantages and disadvantages of ICP-OES and SEM-EDX techniques Electronic supplementary material The online version of this article (doi:10.1007/s00604-010-0468-0) contains supplementary material, which is available to authorized users. PMID:21423317

Using ICP-OES and SEM-EDX in biosorption studies.

PubMed

Michalak, Izabela; Chojnacka, Katarzyna; Marycz, Krzysztof

2011-02-01

We have compared the analytical results obtained by inductively coupled plasma optical emission spectroscopy (ICP-OES) and by scanning electron microscopy with an energy dispersive X-ray analytical system (SEM-EDX) in order to explore the mechanism of metal ions biosorption by biomass using two independent methods. The marine macroalga Enteromorpha sp. was enriched with Cu(II), Mn(II), Zn(II), and Co(II) ions via biosorption, and the biosorption capacity of alga determined from the solution and biomass composition before and after biosorption process was compared. The first technique was used to analyze the composition of the natural and metal-loaded biomass, and additionally the composition of the solution before and after biosorption. The second technique was used to obtain a picture of the surface of natural and metal ion-loaded macroalgae, to map the elements on the cell wall of dry biomass, and to determine their concentration before and after biosorption. ICP-OES showed a better precision and lower detection limit than EDX, but SEM-EDX gave more information regarding the sample composition of Enteromorpha sp. Both techniques confirmed that biosorption is a surface phenomenon, in which alkali and alkaline earth metal ions were exchanged by metal ions from aqueous solution.FigureThe advantages and disadvantages of ICP-OES and SEM-EDX techniques ELECTRONIC SUPPLEMENTARY MATERIAL: The online version of this article (doi:10.1007/s00604-010-0468-0) contains supplementary material, which is available to authorized users.

Gunshot residue testing in suicides: Part I: Analysis by scanning electron microscopy with energy-dispersive X-ray.

PubMed

Molina, D Kimberley; Martinez, Michael; Garcia, James; DiMaio, Vincent J M

2007-09-01

Several different methods can be employed to test for gunshot residue (GSR) on a deceased person's hands, including scanning electron microscopy with energy-dispersive x-ray spectroscopy (SEM-EDX) and inductively coupled plasma-atomic emission spectrometry (ICP-AES). Each of these techniques has been extensively studied, especially on living individuals. The current studies (Part I and Part II) were designed to compare the use and utility of the different GSR testing techniques in a medical examiner setting. In Part I, the hands of deceased persons who died from undisputed suicidal handgun wounds were tested for GSR by SEM-EDX over a 4-year period. A total of 116 cases were studied and analyzed for caliber of weapon, proximity of wound, and results of GSR testing, including spatial deposition upon the hands. It was found that in only 50% of cases with a known self-inflicted gunshot wound was SEM-EDX positive for at least 1 specific particle for GSR. In 18% of the cases there was a discernible pattern (spatial distribution) of the particles on the hand such that the manner in which the weapon was held could be determined. Since only 50% of cases where the person is known to have fired a weapon immediately prior to death were positive for GSR by SEM-EDX, this test should not be relied upon to determine whether a deceased individual has discharged a firearm. Furthermore, in only 18% of cases was a discernible pattern present indicating how the firearm was held. The low sensitivity, along with the low percentage of cases with a discernible pattern, limits the usefulness of GSR test results by SEM-EDX in differentiating self-inflicted from non-self-inflicted wounds.

SEM-EDX analysis of an unknown "known" white powder found in a shipping container from Peru

NASA Astrophysics Data System (ADS)

Albright, Douglas C.

2009-05-01

In 2008, an unknown white powder was discovered spilled inside of a shipping container of whole kernel corn during an inspection by federal inspectors in the port of Baltimore, Maryland. The container was detained and quarantined while a sample of the powder was collected and sent to a federal laboratory where it was screened using chromatography for the presence of specific poisons and pesticides with negative results. Samples of the corn kernels and the white powder were forwarded to the Food and Drug Administration, Forensic Chemistry Center for further analysis. Stereoscopic Light Microscopy (SLM), Scanning Electron Microscopy/Energy Dispersive X-ray Spectrometry (SEM/EDX), and Polarized Light Microscopy/Infrared Spectroscopy (PLM-IR) were used in the analysis of the kernels and the unknown powder. Based on the unique particle analysis by SLM and SEM as well as the detection of the presence of aluminum and phosphorous by EDX, the unknown was determined to be consistent with reacted aluminum phosphide (AlP). While commonly known in the agricultural industry, aluminum phosphide is relatively unknown in the forensic community. A history of the use and acute toxicity of this compound along with some very unique SEM/EDX analysis characteristics of aluminum phosphide will be discussed.

Sea urchin skeleton: Structure, composition, and application as a template for biomimetic materials

NASA Astrophysics Data System (ADS)

Shapkin, Nikolay P.; Khalchenko, Irina G.; Panasenko, Alexander E.; Drozdov, Anatoly L.

2017-07-01

SEM and optical microscopy, chemical and EDX analysis, XRD, and FT-IR spectroscopy of three sea urchins skeletons (tests) show that the test is a spongy stereom, consisting of calcite with high content of magnesium. The tests are composed of mineral-organic composite of calcite-magnesite crystals, coated with organic film, containing silicon in form of polyphenylsiloxane. In the test of sea urchin pore spaces are linked into united system of regular structure with structure motive period about 20 um. This developed three-dimensional structure was used as a template for polymer material based on polyferrofenilsiloxane [OSiC6H5OH]x[OSiC6H5O]y[OFeO]z, which is chemically similar to the native film, coating sea urchins skeleton.

Zinc oxide nanorod clusters deposited seaweed cellulose sheet for antimicrobial activity.

PubMed

Bhutiya, Priyank L; Mahajan, Mayur S; Abdul Rasheed, M; Pandey, Manoj; Zaheer Hasan, S; Misra, Nirendra

2018-06-01

Seaweed cellulose was isolated from green seaweed Ulva fasciata using a common bleaching agent. Sheet containing porous mesh was prepared from the extracted seaweed crystalline cellulose along with zinc oxide (ZnO) nanorod clusters grown over the sheet by single step hydrothermal method. Seaweed cellulose and zinc oxide nanorod clusters deposited seaweed cellulose sheet was characterized by FT-IR, XRD, TGA, and SEM-EDX. Morphology showed that the diameter of zinc oxide nanorods were around 70nm. Zinc oxide nanorod clusters deposited on seaweed cellulose sheet gave remarkable antibacterial activity towards gram-positive (Staphylococcus aureus, Bacillus ceresus, Streptococcus thermophilis) and gram-negative (Escherichia coli, Pseudomonas aeruginous) microbes. Such deposited sheet has potential applications in pharmaceutical, biomedical, food packaging, water treatment and biotechnological industries. Copyright © 2018 Elsevier B.V. All rights reserved.

Biosynthesis and characterization of Acalypha indica mediated copper oxide nanoparticles and evaluation of its antimicrobial and anticancer activity.

PubMed

Sivaraj, Rajeshwari; Rahman, Pattanathu K S M; Rajiv, P; Narendhran, S; Venckatesh, R

2014-08-14

Copper oxide nanoparticles were synthesized by biological method using aqueous extract of Acalypha indica leaf and characterized by UV-visible spectroscopy, XRD, FT-IR, SEM TEM and EDX analysis. The synthesised particles were highly stable, spherical and particle size was in the range of 26-30 nm. The antimicrobial activity of A.indica mediated copper oxide nanoparticles was tested against selected pathogens. Copper oxide nanoparticles showed efficient antibacterial and antifungal effect against Escherichia coli, Pseudomonas fluorescens and Candida albicans. The cytotoxicity activity of A.indica mediated copper nanoparticles was evaluated by MTT assay against MCF-7 breast cancer cell lines and confirmed that copper oxide nanoparticles have cytotoxicity activity. Copyright © 2014 Elsevier B.V. All rights reserved.

Single-step biological fabrication of colloidal silver nanoparticles using Hugonia mystax: larvicidal potential against Zika virus, dengue, and malaria vector mosquitoes.

PubMed

Govindarajan, Marimuthu; Kadaikunnan, Shine; Alharbi, Naiyf S; Benelli, Giovanni

2017-11-01

Mosquito control is facing key challenges, including outbreaks of new arbovirus threats. We proposed an eco-friendly synthesis of silver nanoparticles (AgNPs) employing a low-cost extract of Hugonia mystax. AgNPs were specified by UV, XRD, FTIR and EDX spectroscopy, SEM and TEM. AgNPs were more toxic to Anopheles stephensi, Aedes aegypti, and Culex quinquefasciatus larvae (LC 50 : 14.45, 15.86, and 17.46 μg/mL) if compared to aquatic biocontrol organisms Gambusia affinis, Diplonychus indicus, and Anisops bouvieri (LC 50 : 2567.15, 1075.16, and 829.63 μg/ml). Overall, we shed light on the mosquito larvicidal efficacy of H. mystax, a possible biological resource for low-cost fabrication of AgNPs.

Adsorption and inhibitive properties of sildenafil (Viagra) for zinc in hydrochloric acid solution

NASA Astrophysics Data System (ADS)

Fouda, A. S.; Ibrahim, H.; Atef, M.

Sildenafil (Viagra) was investigated as corrosion inhibitor for Zn in 1 M HCl solution using chemical and electrochemical methods at 25 °C. Electrochemical results showed that this drug is efficient inhibitor for Zn in HCl and the inhibition efficiency (IE) reached to 91% at 300 ppm. The IE increases with the drug concentration and decreases with increasing temperature. The adsorption of this drug on Zn surface follows Langmuir adsorption isotherm. The polarization plots revealed that Sildenafil acts as a mixed-type inhibitor. The thermodynamic parameters of activation and adsorption were calculated and discussed. The surface morphology of the Zn specimens was evaluated using scanning electron microscope (SEM), energy dispersive X-ray (EDX), atomic force microscopy (AFM) and Fourier transform infrared spectroscopy (FTIR) techniques.

Fly ash-TiO2 nanocomposite material for multi-pollutants wastewater treatment.

PubMed

Visa, Maria; Andronic, Luminita; Duta, Anca

2015-03-01

This paper reports on the synthesis, characterization and adsorption properties of a novel nano-composite obtained using the hydrothermal method applied to a fly ash-TiO2 slurry and hexadecyltrimethyl-ammonium bromide, as surface controlling agent. The new adsorbent was investigated in terms of crystallinity (XRD), surface properties (AFM, SEM, and porosity and BET surface) and surface chemistry (EDX, FTIR). The nanocomposite's properties were sequentially tested in adsorption and photocatalysis processes applied to multi-pollutant synthetic wastewaters loaded with copper cations and two industrial dyes: the acid dye Bemacid Blau and the reactive dye Bemacid Rot; the nano-composite substrate allowed reaching high removal efficiencies, above 90%, both in adsorption and in photodegradation experiments, in optimised conditions. Copyright © 2014. Published by Elsevier Ltd.

A novel injectable temperature-sensitive zinc doped chitosan/β-glycerophosphate hydrogel for bone tissue engineering.

PubMed

Niranjan, Ramesh; Koushik, Chandru; Saravanan, Sekaran; Moorthi, Ambigapathi; Vairamani, Mariappanadar; Selvamurugan, Nagarajan

2013-03-01

Hydrogels are hydrophilic polymers that have a wide range of biomedical applications including bone tissue engineering. In this study we report preparation and characterization of a thermosensitive hydrogel (Zn-CS/β-GP) containing zinc (Zn), chitosan (CS) and beta-glycerophosphate (β-GP) for bone tissue engineering. The prepared hydrogel exhibited a liquid state at room temperature and turned into a gel at body temperature. The hydrogel was characterized by SEM, EDX, XRD, FT-IR and swelling studies. The hydrogel enhanced antibacterial activity and promoted osteoblast differentiation. Thus, we suggest that the Zn-CS/β-GP hydrogel could have potential impact as an injectable in situ forming scaffold for bone tissue engineering applications. Copyright © 2012 Elsevier B.V. All rights reserved.

An efficient and heterogeneous recyclable silicotungstic acid with modified acid sites as a catalyst for conversion of fructose and sucrose into 5-hydroxymethylfurfural in superheated water.

PubMed

Jadhav, Arvind H; Kim, Hern; Hwang, In Taek

2013-03-01

Acidity modified silver exchanged silicotungstic acid (AgSTA) catalyst was prepared and characterized by X-ray diffraction, FT-IR spectroscopy, Raman spectroscopy, FT-IR pyridine adsorption, SEM imaging, EDX mapping, and antimicrobial activity was also tested. The catalytic activity was evaluated for the dehydration of fructose and sucrose in superheated water. As a result, 98% conversion of fructose with 85.7% HMF yield and 87.4% HMF selectivity in 120 min reaction time at 120 °C reaction temperature using 10 wt.% of AgSTA catalyst was achieved. While, 92% sucrose conversion with 62.5% of HMF yield was obtained from sucrose at uniform condition in 160 min. The effect of reaction parameters, such as reaction temperature, time, catalyst dosage, and effect acidity on HMF yield was also investigated. The AgSTA catalyst was separated from the reaction mixture by filtration process at end of the reaction and reused eight times without loss of catalytic activity. Copyright © 2013 Elsevier Ltd. All rights reserved.

Synthesis and characterization of fluorapatite-titania (FAp-TiO 2) nanocomposite via mechanochemical process

NASA Astrophysics Data System (ADS)

Ebrahimi-Kahrizsangi, Reza; Nasiri-Tabrizi, Bahman; Chami, Akbar

2010-09-01

In this paper, synthesis of bionanocomposite of fluorapatite-titania (FAp-TiO 2) was studied by using one step mechanochemical process. Characterization of the products was accomplished by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, energy dispersive X-ray spectroscopy (EDX), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) techniques. Based on XRD patterns and FT-IR spectroscopy, correlation between the structural features of the nanostructured FAp-TiO 2 and the process conditions was discussed. Variations in crystallite size, lattice strain, and volume fraction of grain boundary were investigated during milling and the following heat treatment. Crystallization of the nanocomposite occurred after thermal treatment at 650 °C. Morphological features of powders were influenced by the milling time. The resulting FAp-20 wt.%TiO 2 nanocomposite powder exhibited an average particle size of 15 nm after 20 h of milling. The results show that the one step mechanosynthesis technique is an effective route to prepare FAp-based nanocomposites with excellent morphological and structural features.

Zn(1-x)Cu(x)O (0.02 ≤ x ≤ 0.1) Nanomaterials Prepared by Ball Milling, Citrate Sol Gel, and Molten Salt Flux Methods.

PubMed

Balamurugan, S; Melba, K

2015-06-01

The Cu doped ZnO, (Zn(1-x)Cu(x))O (x = 0.02, 0.04, 0.06, 0.08, and 0.1) nanomaterials were prepared by ball milling technique (BMT), citrate sol gel (CSG), and molten salt flux (MSF) methods. The various as-prepared (Zn(1-x)Cu(x))O materials were analyzed by powder X-ray diffraction (pXRD), FT-IR, and SEM-EDX measurements in order to check the phase formation, purity, surface morphology and elements present in the annealed materials. Due to the preparation methods as well as doping of 'x' slight variations in cell parameters are seen. The average crystalline size of CSG method shows smaller size (25-35 nm) than BMT and MSF approaches. The materials obtained by MSF technique reveal the average crystalline size in the range of 32-72 nm whereas the BMT materials exhibit 36-50 nm for the composition, 0.02 ≤ x ≤ 0.1. The presence of functional groups and the chemical bonding in (Zn(1-x)Cu(x))O system is confirmed through FT-IR measurements. It is evident from the FT-IR data that bands seen at 400-500 cm(-1) are characteristics of M-O (M = metal ion) bonding in the studied materials. The micro images observed by SEM exhibiting polycrystalline character as compared with the crystallite size obtained from XRD. Among the three approaches employed in the present investigations, in terms of average particle size the CSG method may be concluded as an efficient method for the preparation of Zn(1-x)Cu(x)O nanomaterials.

H3PW12O40 Encapsulation by Nanoporous Metal Organic Framework HKUST-1: Synthesis, Characterization, Activity and Stability.

PubMed

Rafiee, Ezzat; Nobakht, Narges

2016-01-01

Hybrid composite material was obtained through encapsulation of H3PW12O40 (PW) into HKUST-1 (Cu3(BTC)2, BTC = 1,3,5-benzenetricarboxylic acid), in molar composition of 5 Cu(NO3)2 · 3H2O/2.8 BTC/0.3 PW/0.6 CTAB by adding solutions of PW and copper salts to mixture of BTC and surfactant. The catalyst was characterized by various techniques including powder X-ray diffraction (XRD), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), laser particle size analyzer, Brunauer Emmett-Teller (BET). The acidity of the catalyst was measured by a potentiometric titration with n-butylamine and PW/HKUST-1 presented very strong acidic sites with Ei > 100 mV. This nano catalyst was successfully used for the synthesis of various β-keto enol ethers at 45 °C with 51-98% yield after 5-75 min. The catalyst was easily recycled and reused at least four times without significant loss of its activity (94% yield after forth run). The presence of the PW in PW/HKUST-1 and reused PW/HKUST-1 structure, eliminating any doubt about collapse of the HKUST-1 after catalytic reaction and can be followed by FT-IR, XRD and SEM techniques. Brönsted and Lewis acidity of the PW/HKUST-1 catalyst was distinguished by studying the FT-IR and determined by chemisorption of pyridine. The strength and dispersion of the protons on PW/HKUST-1 was considerably high and active surface protons became more available for reactant.

Enhanced bioactive properties of BiodentineTM modified with bioactive glass nanoparticles.

PubMed

Corral Nuñez, Camila; Covarrubias, Cristian; Fernandez, Eduardo; Oliveira, Osmir Batista de

2017-01-01

To prepare nanocomposite cements based on the incorporation of bioactive glass nanoparticles (nBGs) into BiodentineTM (BD, Septodent, Saint-Maur-des-Fosses Cedex, France) and to assess their bioactive properties. nBGs were synthesised by the sol-gel method. BD nanocomposites (nBG/BD) were prepared with 1 and 2% nBGs by weight; unmodified BD and GC Fuji IX (GIC, GC Corporation, Tokyo, Japan) were used as references. The in vitro ability of the materials to induce apatite formation was assessed in SBF by X-ray diffraction (XRD), attenuated total reflectance with Fourier transform infrared spectroscopy (ATR-FTIR), and scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis. BD and nBG/BD were also applied to dentine discs for seven days; the morphology and elemental composition of the dentine-cement interface were analysed using SEM-EDX. One and two percent nBG/BD composites accelerated apatite formation on the disc surface after short-term immersion in SBF. Apatite was detected on the nBG/BD nanocomposites after three days, compared with seven days for unmodified BD. No apatite formation was detected on the GIC surface. nBG/BD formed a wider interfacial area with dentine than BD, showing blockage of dentine tubules and Si incorporation, suggesting intratubular precipitation. The incorporation of nBGs into BD improves its in vitro bioactivity, accelerating the formation of a crystalline apatite layer on its surface after immersion in SBF. Compared with unmodified BD, nBG/BD showed a wider interfacial area with greater Si incorporation and intratubular precipitation of deposits when immersed in SBF.

Rapid degradation of phenol by ultrasound-dispersed nano-metallic particles (NMPs) in the presence of hydrogen peroxide: A possible mechanism for phenol degradation in water.

PubMed

Singh, Jiwan; Yang, Jae-Kyu; Chang, Yoon-Young

2016-06-15

The present study was carried out to investigate the degradation of phenol by ultrasonically dispersed nano-metallic particles (NMPs) in an aqueous solution of phenol. Leaching liquor from automobile shredder residue (ASR) was used to obtain the NMPs. The prepared NMPs were analyzed by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), and by X-ray diffraction (XRD). The SEM images show that the diameters of the NMPs were less than 50 nm. An SEM-EDX elemental analysis reveals that Fe was the most commonly found element (weight %) in the NMPs. The FTIR and XRD peaks indicate the presence of metals oxides on the surfaces of the NMPs. The results of the XPS analysis indicate that various elements (e.g., C, O, Zn, Cu, Mn, Fe) are present on the surfaces of the NMPs. The effects of the NMP dose, the initial solution pH, and of different concentrations of phenol and H2O2 on the phenol degradation characteristics were evaluated. The results of this study demonstrate that phenol degradation can be improved by increasing the amount of NMPs, whereas it is reduced with an increase in the phenol concentration. The degradation of phenol by ultrasonically dispersed NMPs followed the pseudo-first-order kinetics. The probable mechanism of phenol degradation by ultrasonically dispersed NMPs was the oxidation of phenol caused by the hydroxyl radicals produced during the reaction between H2O2 and the NMPs during the ultrasonication process. Copyright © 2016 Elsevier Ltd. All rights reserved.

Removal of industrial dyes and heavy metals by Beauveria bassiana: FTIR, SEM, TEM and AFM investigations with Pb(II).

PubMed

Gola, Deepak; Malik, Anushree; Namburath, Maneesh; Ahammad, Shaikh Ziauddin

2017-10-01

Presence of industrial dyes and heavy metal as a contaminant in environment poses a great risk to human health. In order to develop a potential technology for remediation of dyes (Reactive remazol red, Yellow 3RS, Indanthrene blue and Vat novatic grey) and heavy metal [Cu(II), Ni(II), Cd(II), Zn(II), Cr(VI) and Pb(II)] contamination, present study was performed with entomopathogenic fungi, Beauveria bassiana (MTCC no. 4580). High dye removal (88-97%) was observed during the growth of B. bassiana while removal percentage for heavy metals ranged from 58 to 75%. Further, detailed investigations were performed with Pb(II) in terms of growth kinetics, effect of process parameters and mechanism of removal. Growth rate decreased from 0.118 h -1 (control) to 0.031 h -1 , showing 28% reduction in biomass at 30 mg L -1 Pb(II) with 58.4% metal removal. Maximum Pb(II) removal was observed at 30 °C, neutral pH and 30 mg L -1 initial metal concentration. FTIR analysis indicated the changes induced by Pb(II) in functional groups on biomass surface. Further, microscopic analysis (SEM and atomic force microscopy (AFM)) was performed to understand the changes in cell surface morphology of the fungal cell. SEM micrograph showed a clear deformation of fungal hyphae, whereas AFM studies proved the increase in surface roughness (RSM) in comparison to control cell. Homogenous bioaccumulation of Pb(II) inside the fungal cell was clearly depicted by TEM-high-angle annular dark field coupled with EDX. Present study provides an insight into the mechanism of Pb(II) bioremediation and strengthens the significance of using entomopathogenic fungus such as B. bassiana for metal and dye removal.

Electrospun composites of PHBV, silk fibroin and nano-hydroxyapatite for bone tissue engineering.

PubMed

Paşcu, Elena I; Stokes, Joseph; McGuinness, Garrett B

2013-12-01

Electrospinning of fibrous scaffolds containing nano-hydroxyapatite (nHAp) embedded in a matrix of functional biomacromolecules offers an attractive route to mimicking the natural bone tissue architecture. Functional fibrous substrates will support cell attachment, proliferation and differentiation, while the role of HAp is to induce cells to secrete extracellular matrix (ECM) for mineralization to form bone. Electrospinning of biomaterials composed of polyhydroxybutyrate-co-(3-hydroxyvalerate) with 2% valerate fraction (PHBV), nano-hydroxyapatite (nHAp), and Bombyx mori silk fibroin essence (SF), Mw=90KDa, has been achieved for nHAp and SF solution concentrations of 2 (w/vol) % each and 5 (w/vol) % each. The structure and properties of the nanocomposite fibrous membranes were investigated by means of Scanning Electron Microscopy in combination with Energy Dispersive X-Ray Analysis (SEM/EDX), Fourier Transformed Infrared Spectroscopy (FT-IR), uniaxial tensile and compressive mechanical testing, degradation tests and in vitro bioactivity tests. SEM images showed smooth, uniform and continuous fibre deposition with no bead formation, and fibre diameters of between 10 and 15 μm. EDX and FT-IR confirmed the presence of nHAp and SF. After one month in deionised water, tests showed less than 2% weight loss with the samples retaining their fibrous morphology, confirming that this material biodegrades slowly. After 28 days of immersion in Simulated Body Fluid (SBF) an apatite layer was visible on the surface of the fibres, proving their bioactivity. Preliminary in vitro biological assessment showed that after 1 and 3 days in culture, cells were attached to the fibres, retaining their morphology while presenting a flattened appearance and elongated shape on the surface of fibres. Young's modulus was found to increase from 0.7 kPa (±0.33 kPa) for electrospun samples of PHBV only to 1.4 kPa (±0.54 kPa) for samples with 2 (w/vol) % each of nHAp and SF. Samples prepared with 5 (w/vol) % each of nHAp and SF did not show a similar improvement. © 2013 Elsevier B.V. All rights reserved.

Retrieving the Quantitative Chemical Information at Nanoscale from Scanning Electron Microscope Energy Dispersive X-ray Measurements by Machine Learning

NASA Astrophysics Data System (ADS)

Jany, B. R.; Janas, A.; Krok, F.

2017-11-01

The quantitative composition of metal alloy nanowires on InSb(001) semiconductor surface and gold nanostructures on germanium surface is determined by blind source separation (BSS) machine learning (ML) method using non negative matrix factorization (NMF) from energy dispersive X-ray spectroscopy (EDX) spectrum image maps measured in a scanning electron microscope (SEM). The BSS method blindly decomposes the collected EDX spectrum image into three source components, which correspond directly to the X-ray signals coming from the supported metal nanostructures, bulk semiconductor signal and carbon background. The recovered quantitative composition is validated by detailed Monte Carlo simulations and is confirmed by separate cross-sectional TEM EDX measurements of the nanostructures. This shows that SEM EDX measurements together with machine learning blind source separation processing could be successfully used for the nanostructures quantitative chemical composition determination.

1998 Technology Showcase. JOAP International Condition Monitoring Conference.

DTIC Science & Technology

1998-04-01

Systems using Automated SEM/ EDX and New Diagnostic Routines 276 N. W Farrant & T. Luckhurst ADVANCED DIAGNOSTIC SYSTEMS Model-Based Diagnostics of Gas...Microscopy with Energy Dispersive X-Ray (SEM/ EDX ) micro analysis packages and Energy Dispersive X-Ray Fluorescence (EDXRF) analytical equipment. Therqfore...wear particles separated by ferrogram method. a- I WEAR PARTICLE A SLAS 97 (HOME PAGE) Fig I Home Page NONFE;RROUS MATERIAL A wW~ a48 -1, rV fr , ý b

Synthesis, characterization, and antibacterial activities of ZnLaFe2O4/NiTiO3 nanocomposite

NASA Astrophysics Data System (ADS)

Sobhani-Nasab, Ali; Zahraei, Zohreh; Akbari, Maryam; Maddahfar, Mahnaz; Hosseinpour-Mashkani, S. Mostafa

2017-07-01

In this research, for the first time, ZnLaFe2O4/NiTiO3 nanocomposites have been synthesized through a polyol assistant sol-gel method. To investigate the effect of different surfactants on the morphology and particle size of ZnLaFe2O4 nanostructure, cetrimonium bromide, sodium dodecyl sulfate, polyvinylpyrrolidone, polyvinyl alcohol, and oleic acid were used as surfactant agents. Based on the SEM results, it was found that morphology and particle size of the products could be affected by these surfactants. Furthermore, study on antibacterial effect of ZnLaFe2O4/NiTiO3 nanocomposites by colony forming unit (CFU) reduction assay showed that ZnLaFe2O4/NiTiO3 nanocomposites have antibacterial activity against Gram-negative Escherchia coli (ATCC 10536) and Gram-positive Staphylococcus aureus (ATCC 29737). Antibacterial results demonstrate that nanocomposite significantly reduced the growth rate of E. coli bacteria and S. aureus after 120 min. The structure and morphology of the resulting particles were characterized by XRD, FT-IR, EDX, and SEM analysis.

Synthesis of calcium hydrogen phosphate and hydroxyapatite coating on SS316 substrate through pulsed electrodeposition.

PubMed

Chakraborty, Rajib; Sengupta, Srijan; Saha, Partha; Das, Karabi; Das, Siddhartha

2016-12-01

The orthopaedic implants for human body are generally made of different biomaterials like stainless steels or Ti based alloys. However, it has been found that from surface properties point of view, none of these materials is attractive for fast tissue or cell growth on the surface of implant. This is one of the most important criteria to assure quick bonding between implant and body tissues vis-à-vis minimum recovery time for the patient. Keeping in view of the above facts, this work involves the pulsed electro-deposition coating of biocompatible hydroxyapatite and its group compounds from a diluted bath of calcium and phosphate salt at various current densities over the biomaterial sheet of SS316. SEM study confirms different morphologies of the coatings at different current densities. Characterization techniques like X-ray diffraction, SEM with EDX and FTIR have been used to confirm the phase and percentage quantity of hydroxyapatite compound in the depositions. This coating can serve as a medium for faster tissue growth over the metallic implants. Copyright © 2016 Elsevier B.V. All rights reserved.

Synthesis of N-doped potassium tantalate perovskite material for environmental applications

NASA Astrophysics Data System (ADS)

Rao, Martha Purnachander; Nandhini, Vellangattupalayam Ponnusamy; Wu, Jerry J.; Syed, Asad; Ameen, Fuad; Anandan, Sambandam

2018-02-01

Nitrogen containing potassium tantalate perovskite material has been synthesized by the solvothermal method using urea (CH4N2O) as a nitrogen source. The as-prepared sample was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), diffuse reflectance spectroscopy (DRS), scanning electron microscope (SEM), and energy-dispersive X-ray spectroscopy (EDX) and X-ray photoelectron spectroscopy (XPS). The particle size of nitrogen containing KTaO3 observed from SEM images was found to be 100-150 nm. Doping KTaO3 with nitrogen causes reduction of band gap from 3.5 to 2.54 eV. The incorporation of Nitrogen into the crystal lattice of KTaO3 not only extended the absorption of light from UV (ultraviolet) region to visible region and also enhanced the photocatalytic activity. As prepared nitrogen containing KTaO3 samples exhibit cubic-like morphology and noticed efficient photocatalytic activity towards methylene blue dye degradation under visible light illumination. The intermediates formed during photodegradation were identified by mass spectrometry (GC-MS) and proposed suitable degradation pathway.

Nano-sized ZnO powders prepared by co-precipitation method with various pH

DOE Office of Scientific and Technical Information (OSTI.GOV)

Purwaningsih, S. Y., E-mail: sriyanisaputri@gmail.com; Pratapa, S.; Triwikantoro,

2016-04-19

In this work, nano-sized ZnO powders have been synthesized by the co-precipitation method with Zn(CH3COOH)2.2H2O, HCl, and NH3.H2O as raw materials in various pH ranging from 8 to 10. The purity, microstructure, chemical group analysis, morphology of the prepared ZnO powders were studied by X-ray diffraction (XRD), Fourier transform infrared spectrometer (FTIR), energy dispersive X-ray spectrometry (EDX), and scanning electron microscope (SEM), respectively. Rietveld refinement of XRD data showed that ZnO crystallizes in the wurtzite structure with high purity. The obtained powders were nano-sized particles with the average crystallite size about 17.9 ± 2.1 nm synthesized with pH of 9.5, atmore » 85°C, and stirring time of 6 h. The SEM results have visualied the morphology of ZnO nanoparticles with spherical-like shape. The effect of processing conditions on morphology of ZnO was also discussed.« less

Piper betle-mediated green synthesis of biocompatible gold nanoparticles

NASA Astrophysics Data System (ADS)

Punuri, Jayasekhar Babu; Sharma, Pragya; Sibyala, Saranya; Tamuli, Ranjan; Bora, Utpal

2012-08-01

Here, we report the novel use of the ethonolic leaf extract of Piper betle for gold nanoparticle (AuNP) synthesis. The successful formation of AuNPs was confirmed by UV-visible spectroscopy, and different parameters such as leaf extract concentration (2%), gold salt concentration (0.5 mM), and time (18 s) were optimized. The synthesized AuNPs were characterized with different biophysical techniques such as transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), and energy-dispersive X-ray spectroscopy (EDX). TEM experiments showed that nanoparticles were of various shapes and sizes ranging from 10 to 35 nm. FT-IR spectroscopy revealed that AuNPs were functionalized with biomolecules that have primary amine group -NH2, carbonyl group, -OH groups, and other stabilizing functional groups. EDX showed the presence of the elements on the surface of the AuNPs. FT-IR and EDX together confirmed the presence of biomolecules bounded on the AuNPs. Cytotoxicity of the AuNPs was tested on HeLa and MCF-7 cancer cell lines, and they were found to be nontoxic, indicating their biocompatibility. Thus, synthesized AuNPs have potential for use in various biomedical applications.

Green synthesis of silver nanoparticles using Cordia dichotoma fruit extract and its enhanced antibacterial, anti-biofilm and photo catalytic activity

NASA Astrophysics Data System (ADS)

Bharathi, Devaraj; Vasantharaj, Seerangaraj; Bhuvaneshwari, V.

2018-05-01

The present study describes the antibacterial, anti-biofilm and photo catalytic activity of silver nanoparticles synthesized using Cordia dichotoma fruits (Cd-AgNPs) for the first time. The phyto-synthesized Cd-AgNPs were characterized by UV-Visible spectroscopy, Field emission-scanning electron microscopy (FE-SEM), Transmission electron microscopy (TEM), Energy dispersive x-ray spectrometer (EDX), Fourier transform infrared spectroscopy (FT-IR), and x-ray diffraction (XRD). FE-SEM and TEM observation showed that the average size of 2–60 nm with spherical shape of Cd-AgNPs and the presence of phyto-compounds which are responsible for capping and reduction were studied by FT-IR. XRD studies revealed the face-centered cubic structure of Cd-AgNPs. The synthesized Cd-AgNPs showed significant antibacterial activity against Gram-positive Staphylococcus aureus and Gram-negative Escherichia coli, assayed using agar well diffusion method. Phyto-synthesized Cd-AgNPs exhibited more than 90% inhibition of biofilm activity formed by S. aureus and E. coli. Furthermore, photocatalytic degradation of crystal violet (CV) under UV light irradiation using Cd-AgNPs was performed. Synthesized Cd-AgNPs exhibited ∼85% degradation activity for CV. Collectively, our findings suggest that C.dichotoma is a green source for the eco-friendly synthesis of Cd-AgNPs, which further can be used as a novel biocidal agent against bacterial pathogens and a potent photo catalytic agent.

Extracellular synthesis of silver nanoparticles using Bacillus megaterium against malarial and dengue vector (Diptera: Culicidae).

PubMed

Banu, A Najitha; Balasubramanian, C

2015-11-01

Biosynthesis of silver nanoparticles has provoked nowadays and alternative to physical and chemical approaches. In the present study, silver nanoparticles (AgNPs) were synthesized extracellular method using Bacillus megaterium. The AgNPs formations were confirmed initially through color change, and the aliquots were characterized through UV-visible spectrophotometer, followed by scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) spectroscopy, and Fourier transform infrared (FTIR) spectra. The surface plasmon resonance band was shown at 430 nm in UV-vis spectrophotometer. The bioreduction was categorized through identifying the compounds responsible for the AgNP synthesis, and the functional group present in B. megaterium cell-free culture was scrutinized using FTIR. The topography and morphology of the particles were determined using SEM. In addition, this biosynthesized AgNPs were found to show higher insecticidal efficacy against vector mosquitoes. The LC50 and LC90 were found to be 0.567, 2.260; 0.90, 4.44; 1.349, 8.269; and 1.640, 9.152 and 0.240, 0.955; 0.331, 1.593; 0.494, 2.811; and 0.700, 4.435 with respect to the first, second, third, and fourth instar larvae of Culex quinquefasciatus and Aedes aegypti. All the calculated χ (2) values are highly significant compared with the tabulated value. Therefore, B. megaterium-synthesized silver nanoparticles would be used as a potent larvicidal agent against Cx. quinquefasciatus and Ae. aegypti.

Novel nanohybrids of cobalt(III) Schiff base complexes and clay: synthesis and structural determinations.

PubMed

Kianfar, Ali Hossein; Mahmood, Wan Ahmad Kamil; Dinari, Mohammad; Azarian, Mohammad Hossein; Khafri, Fatemeh Zare

2014-06-05

The [Co(Me(2)Salen)(PBu(3))(OH(2))]BF4 and [Co(Me(2)Salen)(PPh(3))(Solv)]BF(4), complexes were synthesized and characterized by FT-IR, UV-Vis, (1)H NMR spectroscopy and elemental analysis techniques. The coordination geometry of [Co(Me(2)Salen)(PPh(3))(H(2)O)]BF(4) was determined by X-ray crystallography. It has been found that the complex is containing [Co(Me(2)Salen)(PPh(3))(H(2)O)]BF(4) and [Co(Me(2)Salen)(PPh(3))(EtOH)]BF(4) hexacoordinate species in the solid state. Cobalt atom exhibits a distorted octahedral geometry and the Me(2)Salen ligand has the N2O2 coordinated environment in the equatorial plane. The [Co(Me(2)Salen)(PPh(3))(H(2)O)]BF(4) complex shows a dimeric structure via hydrogen bonding between the phenolate oxygen and hydrogens of coordinated H2O molecule. These complexes were incorporated into Montmorillonite-K10 nanoclay. The modified clays were identified by FT-IR, XRD, EDX, TGA/DTA, SEM and TEM techniques. According to the XRD results of the new nanohybrid materials, the Schiff base complexes are intercalated in the interlayer spaces of the clay. SEM and TEM micrographs show that the resulting hybrid nanomaterials have layer structures. Also, TGA/DTG results show that the intercalation reaction was taken place successfully. Copyright © 2014. Published by Elsevier B.V.

Magnetic cellulose/Ag as a novel eco-friendly nanobiocomposite to catalyze synthesis of chromene-linked nicotinonitriles.

PubMed

Maleki, Ali; Movahed, Hamed; Ravaghi, Parisa

2017-01-20

In this work, design, preparation and performance of magnetic cellulose/Ag nanobiocomposite as a recyclable and highly efficient heterogeneous nanocatalyst is described. Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD) pattern, vibrating sample magnetometer (VSM) curve, field-emission scanning electron microscopy (FE-SEM) image, energy dispersive X-ray (EDX) analysis and thermogravimetric analysis/differential thermal analysis (TGA/DTA) were used for the characterization. Then, its activity was investigated in the synthesis of 2-amino-6-(2-oxo-2H-chromen-3-yl)-4-phenylnicotinonitrile derivatives. The main advantages of the reaction are high yields and short reaction times. The remarkable magnetic property of the nanobiocomposite catalyst provides easy separation from the reaction mixture by an external magnet without considerable loss of its catalytic activity. Copyright © 2016 Elsevier Ltd. All rights reserved.

Yellow colored blooms of Argemone mexicana and Turnera ulmifolia mediated synthesis of silver nanoparticles and study of their antibacterial and antioxidant activity

NASA Astrophysics Data System (ADS)

Chandrasekhar, N.; Vinay, S. P.

2017-11-01

In the present work, AgNPs were prepared using a simple bio-reduction method. This is ecologically welcoming and cost-effective method. Yellow colored blooms concentrate of Argemone mexicana and Turnera ulmifolia are used as bio reducing agents in the study. The formation of silver nanoparticles was confirmed by UV-Vis spectrophotometer and characterization of the nanoparticles was done by FTIR, SEM, XRD and EDX. The Antibacterial action of silver nanoparticles was tested against Staphylococus aureus, Pseudomonas aeruginosa, Escherichia coli and Klebsiella aerogenes. The phytochemical analysis of the blooms concentrate has shown the existence of saponins, alkaloids, amino acids, phenols, tannins, terpenoids, flavonoids and cardiac glycosides. In vitro anti-oxidant action of both A. mexicana and T. ulmifolia AgNPs were studied by DPPH assay and reducing power assay.

Green synthesis and spectral characterization of silver nanoparticles from Lakshmi tulasi (Ocimum sanctum) leaf extract

NASA Astrophysics Data System (ADS)

Subba Rao, Y.; Kotakadi, Venkata S.; Prasad, T. N. V. K. V.; Reddy, A. V.; Sai Gopal, D. V. R.

2013-02-01

A simple method for the green synthesis of silver nanoparticles (AgNPs) using aqueous extract of Lakshmi tulasi (Ocimum sanctum) leaf as a reducing and stabilizing agent. AgNPs were rapidly synthesized using aqueous extract of tulasi leaf with AgNO3 solution within 15 min. The green synthesized AgNPs were characterized using physic-chemical techniques viz., UV-Vis, X-ray diffraction (XRD), scanning electron microscope (SEM) coupled with X-ray energy dispersive spectroscopy (EDX) and Fourier transform-infrared spectroscopy (FT-IR). Characterization data reveals that the particles were crystalline in nature and triangle shaped with an average size of 42 nm. The zeta potential of AgNPs were found to be -55.0 mV. This large negative zeta potential value indicates repulsion among AgNPs and their dispersion stability.

Evaluation of barium hydroxide treatment efficacy on a dolomitic marble.

PubMed

Toniolo, L; Colombo, C; Realini, M; Peraio, A; Positano, M

2001-01-01

The Arch of Peace, by Luigi Cagnola, is one of the most famous neoclassical monuments in Milan. It has been subjected to conservative intervention in 1998. In the present paper the efficacy of the consolidation by means of barium hydroxide has been evaluated. The stone material showed severe degradation phenomena as: erosion, pulverisation, exfoliation. The analytical data acquired through X-ray diffraction (XRD), infrared spectrophotometry (FTIR) and scanning electron microscopy (SEM-EDX), allowed to compare the conditions of stone before and after the treatment with barium hydroxide. The presence of barium has been put in evidence mainly on the surface as barium sulphate, whereas barium is only sporadically present within the thickness of the decayed material. The treatment was judged not satisfying and its inefficacy is, most probably, due to a not suitable cleaning procedure carried out before the consolidation.

Adsorption Isotherm of Chromium (Vi) into Zncl2 Impregnated Activated Carbon Derived by Jatropha Curcas Seed Hull

NASA Astrophysics Data System (ADS)

Mohammad, M.; Yakub, I.; Yaakob, Z.; Asim, N.; Sopian, K.

2017-12-01

Hexavalent chromium is carcinogenic and should be removed from industrial wastewater before discharged into water resources. Adsorption by using activated carbon from biomass is an economic and conventional way on removing the heavy metal ions from wastewater. In this research, activated carbon is synthesized from Jatropha curcas L. seed hull through chemical activation with ZnCl2 and carbonized at 800 °C (JAC/ZnCl2). The activated carbon has been characterized using FTIR, SEM-EDX, BET and CHNS-O analyzer. Adsorption isotherms have been analysed using Langmuir and Freundlich models to determine its removal mechanism. The maximum adsorption capacity of Cr (VI) metal ions onto JAC/ZnCl2 activated carbon is 25.189 mg/g and following Langmuir isotherm model which is monolayer adsorption.

Sonochemical fabrication of fluorinated mesoporous titanium dioxide microspheres

NASA Astrophysics Data System (ADS)

Yu, Changlin; Yu, Jimmy C.; Chan, Mui

2009-05-01

A sonochemical-hydrothermal method for preparing fluorinated mesoporous TiO 2 microspheres was developed. Formation of mesoporous TiO 2 and doping of fluorine was achieved by sonication and then hydrothermal treatment of a solution containing titanium isopropoxide, template, and sodium fluoride. The as-synthesized TiO 2 microspheres were characterized by X-ray diffraction (XRD), Fourier translation infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray (EDX) spectroscopy, photoluminescence spectroscopy (PL), and BET surface areas. The P123 template was removed completely during the hydrothermal and washing steps, which was different from the conventional calcination treatment. The as- synthesized TiO 2 microspheres had good crystallinity and high stability. Results from the photocatalytic degradation of methylene blue (MB) showed that fluorination could remarkably improve the photocatalytic activity of titanium dioxide.

Ferrocene-functionalized graphene electrode for biosensing applications.

PubMed

Rabti, Amal; Mayorga-Martinez, Carmen C; Baptista-Pires, Luis; Raouafi, Noureddine; Merkoçi, Arben

2016-07-05

A novel ferrocene-functionalized reduced graphene oxide (rGO)-based electrode is proposed. It was fabricated by the drop casting of ferrocene-functionalized graphene onto polyester substrate as the working electrode integrated within screen-printed reference and counter electrodes. The ferrocene-functionalized rGO has been fully characterized using FTIR, XPS, contact angle measurements, SEM and TEM microscopy, and cyclic voltammetry. The XPS and EDX analysis showed the presence of Fe element related to the introduced ferrocene groups, which is confirmed by a clear CV signal at ca. 0.25 V vs. Ag/AgCl (0.1 KCl). Mediated redox catalysis of H2O2 and bio-functionalization with glucose oxidase for glucose detection were achieved by the bioelectrode providing a proof for potential biosensing applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Enhanced electrical properties in sub-10-nm WO3 nanoflakes prepared via a two-step sol-gel-exfoliation method

PubMed Central

2014-01-01

The morphology and electrical properties of orthorhombic β-WO3 nanoflakes with thickness of ~7 to 9 nm were investigated at the nanoscale with a combination of scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), current sensing force spectroscopy atomic force microscopy (CSFS-AFM, or PeakForce TUNA™), Fourier transform infra-red absorption spectroscopy (FTIR), linear sweep voltammetry (LSV) and Raman spectroscopy techniques. CSFS-AFM analysis established good correlation between the topography of the developed nanostructures and various features of WO3 nanoflakes synthesized via a two-step sol-gel-exfoliation method. It was determined that β-WO3 nanoflakes annealed at 550°C possess distinguished and exceptional thickness-dependent properties in comparison with the bulk, micro and nanostructured WO3 synthesized at alternative temperatures. PMID:25221453

Characterization, antibacterial, antioxidant, antidiabetic, anti-inflammatory and antityrosinase activity of green synthesized silver nanoparticles using Calophyllum tomentosum leaves extract

NASA Astrophysics Data System (ADS)

Govindappa, M.; Hemashekhar, B.; Arthikala, Manoj-Kumar; Ravishankar Rai, V.; Ramachandra, Y. L.

2018-06-01

The current research study is to develop an easy and eco-friendly method for the synthesis of AgNPs using aqueous leaf extract of Calophyllum tomentosum (CtAgNPs) and evaluated the extract to know the effects of anti-bacterial, antioxidant, anti-diabetic, anti-inflammatory and anti-tyrosinase activity. Using UV-vis spectrophotometer, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX) characterized the Calophyllum tomentosum mediated silver nanoparticles. The leaf extract of C. tomentosum yielded flavonoids, saponins, tannins, alkaloids, glycosides, phenols, terpenoids and coumarins. AgNPs formation was confirmed by UV-vis spectra at 438 nm. Crystalline structure with a face centered cubic (fcc) of AgNPs was observed in XRD. FTIR had shown that the phytochemicals were responsible for the reduction and capping material of silver nanoparticles. The size and shape of the AgNPs were determined using SEM. From EDX study analysed the strong absorption property of AgNPs. The CtAgNPs have showed significant antibacterial activity on multi drug resistance bacteria. The CtAgNPs had shown strong antioxidant (DPPH, H2O2 scavenging, nitric oxide scavenging power, reducing power) activities. The CtAgNPs had strongly inhibited the α-glucosidase and DPPIV compared to α-amylase. The CtAgNPs exhibited strong anti-inflammatory activity (albumin denaturation, membrane stabilization, heat haemolytic, protein inhibitory, lipoxygenase, xanthine oxidase) and tyrosinase inhibitory activity. To our best knowledge, this is the first attempt on the synthesis of silver nanoparticles using Calophyllum tomentosum leaves extract. Hence, to validate our results the in vivo studies at molecular level are needed to develop an antioxidant, anti-diabetic and anti-inflammatory agent.

Synthesis and structural characterization of magnetic cadmium sulfide-cobalt ferrite nanocomposite, and study of its activity for dyes degradation under ultrasound

NASA Astrophysics Data System (ADS)

Farhadi, Saeed; Siadatnasab, Firouzeh

2016-11-01

Cadmium sulfide-cobalt ferrite (CdS/CFO) nanocomposite was easily synthesized by one-step hydrothermal decomposition of cadmium diethyldithiocarbamate complex on the CoFe2O4 nanoparticles at 200 °C. Spectroscopic techniques of powder X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), UV-visible spectroscopy, field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), Brunauer-Emmett-Teller (BET), and magnetic measurements were applied for characterizing the structure and morphology of the product. The results of FT-IR, XRD and EDX indicated that the CdS/CFO was highly pure. SEM and TEM results revealed that the CdS/CFO nanocomposite was formed from nearly uniform and sphere-like nanoparticles with the size of approximately 20 nm. The UV-vis absorption spectrum of the CdS/CFO nanocomposite showed the band gap of 2.21 eV, which made it suitable for sono-/photo catalytic purposes. By using the obtained CdS/CFO nanocomposite, an ultrasound-assisted advanced oxidation process (AOP) has been developed for catalytic degradation of methylene blue (MB), Rhodamine B (RhB), and methyl orange (MO)) in the presence of H2O2 as a green oxidant. CdS/CFO nanocomposite exhibited excellent sonocatalytic activity, so that, dyes were completely degraded in less than 10 min. The influences of crucial factors such as the H2O2 amount and catalyst dosage on the degradation efficiency were evaluated. The as-prepared CdS/CFO nanocomposite exhibited higher catalytic activity than pure CdS nanoparticles. Moreover, the magnetic property of CoFe2O4 made the nanocomposite recyclable.

Investigation of ultrashort-pulsed laser on dental hard tissue

NASA Astrophysics Data System (ADS)

Uchizono, Takeyuki; Awazu, Kunio; Igarashi, Akihiro; Kato, Junji; Hirai, Yoshito

2007-02-01

Ultrashort-pulsed laser (USPL) can ablate various materials with precious less thermal effect. In laser dentistry, to solve the problem that were the generation of crack and carbonized layer by irradiating with conventional laser such as Er:YAG and CO II laser, USPL has been studied to ablate dental hard tissues by several researchers. We investigated the effectiveness of ablation on dental hard tissues by USPL. In this study, Ti:sapphire laser as USPL was used. The laser parameter had the pulse duration of 130 fsec, 800nm wavelength, 1KHz of repetition rate and the average power density of 90~360W/cm2. Bovine root dentin plates and crown enamel plates were irradiated with USPL at 1mm/sec using moving stage. The irradiated samples were analyzed by SEM, EDX, FTIR and roughness meter. In all irradiated samples, the cavity margin and wall were sharp and steep, extremely. In irradiated dentin samples, the surface showed the opened dentin tubules and no smear layer. The Ca/P ratio by EDX measurement and the optical spectrum by FTIR measurement had no change on comparison irradiated samples and non-irradiated samples. These results confirmed that USPL could ablate dental hard tissue, precisely and non-thermally. In addition, the ablation depths of samples were 10μm, 20μm, and 60μm at 90 W/cm2, 180 W/cm2, and 360 W/cm2, approximately. Therefore, ablation depth by USPL depends on the average power density. USPL has the possibility that can control the precision and non-thermal ablation with depth direction by adjusting the irradiated average power density.

Photocatalytic activity of undoped and Ag-doped TiO{sub 2}-supported zeolite for humic acid degradation and mineralization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lazau, C.; Ratiu, C.; National Institute for Research and Development in Microtechnologies, Erou Iancu Nicolae Street, 077190 Bucharest

2011-11-15

Highlights: {yields} Hybrid materials based on natural zeolite and TiO{sub 2} obtained by solid-state reaction. {yields} XRD proved the presence of anatase form of undoped and Ag-doped TiO{sub 2} onto zeolite. {yields} FT-IR spectra evidenced the presence on TiO{sub 2} bounded at the zeolite network. {yields} Ag-doped TiO{sub 2} onto zeolitic matrix exhibited an enhanced photocatalytic activity. -- Abstract: The hybrid materials based on natural zeolite and undoped and Ag-doped TiO{sub 2}, i.e., Z-Na-TiO{sub 2} and Z-Na-TiO{sub 2}-Ag, were successfully synthesized by solid-state reaction in microwave-assisted hydrothermal conditions. Undoped TiO{sub 2} and Ag-doped TiO{sub 2} nanocrystals were previously synthesized bymore » sol-gel method. The surface characterization of undoped TiO{sub 2}/Ag-doped TiO{sub 2} and natural zeolite hybrid materials has been investigated by X-ray diffraction, DRUV-VIS spectroscopy, FT-IR spectroscopy, BET analysis, SEM microscopy and EDX analysis. The results indicated that anatase TiO{sub 2} is the dominant crystalline type as spherical form onto zeolitic matrix. The presence of Ag into Z-Na-TiO{sub 2}-Ag was confirmed by EDX analysis. The DRUV-VIS spectra showed that Z-Na-TiO{sub 2}-Ag exhibited absorption within the range of 400-500 nm in comparison with Z-Na-TiO{sub 2} catalyst. The enhanced photocatalytic activity of Z-Na-TiO{sub 2}-Ag catalyst is proved through the degradation and mineralization of humic acid under ultraviolet and visible irradiation.« less

Fabrication of mesoporous iron (Fe) doped copper sulfide (CuS) nanocomposite in the presence of a cationic surfactant via mild hydrothermal method for supercapacitors

NASA Astrophysics Data System (ADS)

Brown, J. William; Ramesh, P. S.; Geetha, D.

2018-02-01

We report fabrication of mesoporous Fe doped CuS nanocomposites with uniform mesoporous spherical structures via a mild hydrothermal method employing copper nitrate trihydrate (Cu (NO3).3H2O), Thiourea (Tu,Sc(NH2)2 and Iron tri nitrate (Fe(No3)3) as initial materials with cationic surfactant cetyltrimethylamoniame bromide (CTAB) as stabilizer/size controller and Ethylene glycol as solvent at 130 °C temperature. The products were characterized by XRD, SEM/EDX, TEM, FTIR and UV analysis. X-ray diffraction (XRD) spectra confirmed the Fe doped CuS nanocomposites which are crystalline in nature. EDX and XRD pattern confirmed that the product is hexagonal CuS phase. Fe doped spherical structure of CuS with grain size of 21 nm was confirmed by XRD pattern. Fe doping was identified by energy dispersive spectrometry (EDS). The Fourier-transform infrared (FTIR) spectroscopy results revealed the occurrence of active functional groups required for the reduction of copper ions. Studies showed that after a definite time relining on the chosen copper source, the obtained Fe-CuS nanocomposite shows a tendency towards self-assembly and creating mesoporous like nano and submicro structures by TEM/SAED. The achievable mechanism of producing this nanocomposite was primarily discussed. The electrochemical study confirms the pseudocapacitive nature of the CuS and Fe-CuS electrodes. The CuS and Fe-CuS electrode shows a specific capacitance of about 328.26 and 516.39 Fg-1 at a scan rate of 5 mVs-1. As the electrode in a supercapacitor, the mesoporous nanostructured Fe-CuS shows excellent capacitance characteristics.

A Data Matrix Method for Improving the Quantification of Element Percentages of SEM/EDX Analysis

NASA Technical Reports Server (NTRS)

Lane, John

2009-01-01

A simple 2D M N matrix involving sample preparation enables the microanalyst to peer below the noise floor of element percentages reported by the SEM/EDX (scanning electron microscopy/ energy dispersive x-ray) analysis, thus yielding more meaningful data. Using the example of a 2 3 sample set, there are M = 2 concentration levels of the original mix under test: 10 percent ilmenite (90 percent silica) and 20 percent ilmenite (80 percent silica). For each of these M samples, N = 3 separate SEM/EDX samples were drawn. In this test, ilmenite is the element of interest. By plotting the linear trend of the M sample s known concentration versus the average of the N samples, a much higher resolution of elemental analysis can be performed. The resulting trend also shows how the noise is affecting the data, and at what point (of smaller concentrations) is it impractical to try to extract any further useful data.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yang, Li; Zhu, Zihua; Yu, Xiao-Ying

In this study, we report new results of in situ study of 5 nm goat anti-mouse IgG gold nanoparticles in a novel portable vacuum compatible microfluidic device using scanning electron microscope (SEM) and time-of-flight secondary ion mass spectrometry (ToF-SIMS). The unique feature of the liquid flow cell is that the detection window is open to the vacuum allowing direct probing of the liquid surface. The flow cell is composed of a silicon nitride (SiN) membrane and polydimethylsiloxane (PDMS), and it is fully compatible with vacuum operations for surface analysis. The aperture can be drilled through the 100 nm SiN membranemore » using a focused ion beam. Characteristic signals of the conjugated gold nanoparticles were successfully observed through the aperture by both energy-dispersive X-ray spectroscopy (EDX) in SEM and ToF-SIMS. Comparison was also made among wet samples, dry samples, and liquid sample in the flow cell using SEM/EDX. Stronger gold signal can be observed in our novel portable device by SEM/EDX compared with the wet or dry samples, respectively. Our results indicate that analyses of the nanoparticle components are better made in their native liquid environment. This is made possible using our unique microfluidic flow cell.« less

Surface analysis characterisation of gum binders used in modern watercolour paints

NASA Astrophysics Data System (ADS)

Sano, Naoko; Cumpson, Peter J.

2016-02-01

Conducting this study has demonstrated that not only SEM-EDX but also XPS can be an efficient tool for characterising watercolour paint surfaces. We find that surface effects are mediated by water. Once the powdered components in the watercolour come into contact with water they dramatically transform their chemical structures at the surface and show the presence of pigment components with a random dispersion within the gum layer. Hence the topmost surface of the paint is confirmed as being composed of the gum binder components. This result is difficult to confirm using just one analytical technique (either XPS or SEM-EDX). In addition, peak fitting of C1s XPS spectra suggests that the gum binder in the commercial watercolour paints is probably gum arabic (by comparison with the reference materials). This identification is not conclusive, but the combination techniques of XPS and SEM shows the surface structure with material distribution of the gum binder and the other ingredients of the watercolour paints. Therefore as a unique technique, XPS combined with SEM-EDX may prove a useful method in the study of surface structure for not only watercolour objects but also other art objects; which may in future help in the conservation for art.

Scanning electron microscopy study of new bone formation following small and large defects preserved with xenografts supplemented with pamidronate-A pilot study in Fox-Hound dogs at 4 and 8 weeks.

PubMed

Lozano-Carrascal, Naroa; Satorres-Nieto, Marta; Delgado-Ruiz, Rafael; Maté-Sánchez de Val, José Eduardo; Gehrke, Sergio Alexandre; Gargallo-Albiol, Jorge; Calvo-Guirado, José Luis

2017-01-01

The aim of the present study was to evaluate the feasibility of SEM and EDX microanalysis on evaluating the effect of porcine xenografts (MP3 ® ) supplemented with pamidronate during socket healing. Mandibular second premolars (P2) and first molars (M1) were extracted from six Beagle dogs. P2 were categorized as small defects (SD) and M1 as large defects (LD). Four random groups were created: SC (small control defects with MP3 ® ), ST (small test defects MP3 ® +pamidronate), LC (large control defects with MP3 ® ), and LT (large test defects MP3 ® +pamidronate). At four and eight weeks of healing the samples were evaluated fisically through scanning electron microscopy (SEM), and chemical element mapping was carried out by Energy dispersive X-ray spectroscopy (EDX). After four weeks of healing, SEM and EDX analysis revealed more mineralized bone in ST and LT groups compared with control groups (p<0.05). After eight weeks, Ca/P ratios were slightly higher for small defects (groups SC and ST); in SEM description, in both control and test groups, trabecular bone density was similar to the adjacent mineralized cortical bone. Within the limitations of this experimental study, SEM description and EDX elemental microanalysis have demonstrated to be useful techniques to assess bone remodelling of small and large defects. Both techniques show increased bone formation in test groups (MP3 ® modified with pamidronate) after four and eight weeks of healing. Copyright © 2016 Elsevier GmbH. All rights reserved.

Synthesis of hydrophobic cross-linked polyzwitterionic acid for simultaneous sorption of Eriochrome black T and chromium ions from binary hazardous waters.

PubMed

Saleh, Tawfik A; Muhammad, Auwal M; Ali, Shaikh A

2016-04-15

Hydrophobic cross-linked polyzwitterionic acid (HCPZA) containing long chain (C18) hydrophobes and residues of a glutamic acid having unquenched nitrogen valency was synthesized. Exploiting the chelating ability of the amino acid residues to scavenge toxic metals and the hydrophobic surface to scoop up the organic contaminants, the resin HCPZA was evaluated for simultaneous removal of chromium and Eriochrome black T (EBT) from wastewaters. The structure and morphology of the polymer before and after sorption were characterized by using FTIR, TGA, EDX and SEM. The effect of various parameters such as contact time, pH and initial concentrations were investigated to arrive at optimum conditions. The adsorption of Eriochrome black T and Cr (III) on HCPZA reached equilibrium in 30 min. The mechanism of adsorption was investigated using kinetic, diffusion and isotherm models. The adsorption kinetic data were described well by the pseudo-second order model and by the Freundlich isotherm model. EDX analysis confirmed the adsorption of Cr (III) and EBT on the polymer. The hydrophobic resin exhibited a remarkable simultaneous adsorption capacity for EBT and Cr (III) and thus demonstrated its potential to be a promising adsorbent for removal of dyes and heavy metal ions from wastewaters. Copyright © 2016 Elsevier Inc. All rights reserved.

Study of the Wall Paintings of the Cenador Del Leon in the Real Alcazar of Seville

NASA Astrophysics Data System (ADS)

Robador, Maria Dolores; Mancera, Inmaculada; Perez-Maqueda, Rafael; Albardonedo, Antonio

2017-10-01

The paintings on the walls of the Cenador del Leon located in the gardens of the Real Alcazar in Seville next to the Pabellon de Carlos V in the Jardin Ingles area have been studied. The components of the wall paintings cross-sections, which were prepared using small samples taken from the walls of Cenador del Leon, were characterized using infrared spectroscopy (FTIR), X-ray diffraction (XRD) and scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis. The cross-sections of the collected samples indicated that the paint layer is well adhered to the preparation layer without any discontinuity, and only one carbonation layer exists at the top of the sequence of layers. These data suggest that the paint was applied on a fresco surface, and therefore, the adopted technique was fresco. Based on the different elements detected by EDX analysis of the cross-sections, the detected pigments included iron oxides accompanied by clay minerals (or earths) in the red pink, golden yellow and yellow colours, blue smelt for the blue colour and basic copper chloride (atacamite) for the green colour. In one sample, the particles were composed of Ba and S from barium sulphate and Ti and O from rutile titanium oxide due to a modern pigment.

Novelty of Dynamic Process in the Synthesis of Biocompatible Silica Nanotubes by Biomimetic Glycyldodecylamide as a Soft Template.

PubMed

Choi, Hyejung; Kim, Joong-Jo; Mo, Yong-Hwan; Reddy, Benjaram M; Park, Sang-Eon

2017-10-10

A dynamic process in the synthesis of silica nanotubes (SNTs) by utilizing glycyldodecylamide (GDA) as a soft template was thoroughly investigated. The morphological evolution from GDA to SNTs was deeply explored to elucidate the formation mechanism for optimizing the synthesis procedure. Various analytical tools, namely, XRD, FTIR, SEM, TEM, Z-potential, and N 2 adsorption/desorption isotherms, were employed during the synthesis procedure. The interactive structure of GDA was also investigated using TEM-EDX as a function of aging time. These studies revealed the stepwise morphology of nanograin, nanofiber, curved plate, and nanotube in the ethanol/water solution when aged at room temperature. The supramolecular GDA molded the vesicle type nanostructure which was surrounded by silica and facilitated the formation of uniform SNTs. The stimulus for GDA to be curved into a vesicle was the intermolecular hydrogen bonding between adjacent amide groups of the template molecules. This was illustrated by FTIR spectra of GDA-silica intermediate by detecting the transition of amide I peak from 1678 to 1635 cm -1 . The effect of hydrogen bonding became stronger when the sample was aged.

Enhanced bioactive properties of BiodentineTM modified with bioactive glass nanoparticles

PubMed Central

CORRAL NUÑEZ, Camila; COVARRUBIAS, Cristian; FERNANDEZ, Eduardo; de OLIVEIRA, Osmir Batista

2017-01-01

Abstract Objective To prepare nanocomposite cements based on the incorporation of bioactive glass nanoparticles (nBGs) into BiodentineTM (BD, Septodent, Saint-Maur-des-Fosses Cedex, France) and to assess their bioactive properties. Material and Methods nBGs were synthesised by the sol-gel method. BD nanocomposites (nBG/BD) were prepared with 1 and 2% nBGs by weight; unmodified BD and GC Fuji IX (GIC, GC Corporation, Tokyo, Japan) were used as references. The in vitro ability of the materials to induce apatite formation was assessed in SBF by X-ray diffraction (XRD), attenuated total reflectance with Fourier transform infrared spectroscopy (ATR-FTIR), and scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis. BD and nBG/BD were also applied to dentine discs for seven days; the morphology and elemental composition of the dentine-cement interface were analysed using SEM-EDX. Results One and two percent nBG/BD composites accelerated apatite formation on the disc surface after short-term immersion in SBF. Apatite was detected on the nBG/BD nanocomposites after three days, compared with seven days for unmodified BD. No apatite formation was detected on the GIC surface. nBG/BD formed a wider interfacial area with dentine than BD, showing blockage of dentine tubules and Si incorporation, suggesting intratubular precipitation. Conclusions The incorporation of nBGs into BD improves its in vitro bioactivity, accelerating the formation of a crystalline apatite layer on its surface after immersion in SBF. Compared with unmodified BD, nBG/BD showed a wider interfacial area with greater Si incorporation and intratubular precipitation of deposits when immersed in SBF. PMID:28403358

Study on fabrication of the superhydrophobic sol-gel films based on copper wafer and its anti-corrosive properties

NASA Astrophysics Data System (ADS)

Fan, Youhua; Li, Changzhu; Chen, Zejun; Chen, Hong

2012-06-01

In the present study, superhydrophobic copper wafer was prepared by a sol-gel deposition method. Different molar ratios of vinyltrimethoxysilane (VTES), ethanol (EtOH), water (H2O) and ammonia water (NH3·OH) were involved in this research. The morphologies, chemical compositions and hydrophobicity of the films were analyzed by scanning electron microscopy (SEM), energy dispersive X-ray detector (EDX), Fourier transfer infrared spectrometer (FTIR) and water contact angle measurement (CA). It was shown by the surface morphological study that different structures, such as pyramid-shaped protrusions, nipple-shaped protrusions or ball-shaped silica particles, were distributed on the copper substrate. The films had a high water contact angle larger than 155.4°. The durability properties revealed that the films had a good superhydrophobicity deposited in 3.5 wt.% sodium chloride solution for up to 14 days.

Novel preparation of highly photocatalytically active copper chromite nanostructured material via a simple hydrothermal route

PubMed Central

Beshkar, Farshad; Zinatloo-Ajabshir, Sahar; Bagheri, Samira; Salavati-Niasari, Masoud

2017-01-01

Highly photocatalytically active copper chromite nanostructured material were prepared via a novel simple hydrothermal reaction between [Cu(en)2(H2O)2]Cl2 and [Cr(en)3]Cl3.3H2O at low temperature, without adding any pH regulator or external capping agent. The as-synthesized nanostructured copper chromite was analyzed by transmission electron microscopy (TEM), UV–vis diffuse reflectance spectroscopy, energy dispersive X-ray microanalysis (EDX), scanning electron microscopy (SEM), X-ray diffraction (XRD) and Fourier transform infrared (FT-IR) spectroscopy. Results of the morphological investigation of the as-synthesized products illustrate that the shape and size of the copper chromite depended on the surfactant sort, reaction duration and temperature. Moreover, the photocatalytic behavior of as-obtained copper chromite was evaluated by photodegradation of acid blue 92 (anionic dye) as water pollutant. PMID:28582420

Rapid and solvent-free solid-state synthesis and characterization of Zn3V2O8 nanostructures and their phenol red aqueous solution photodegradation

NASA Astrophysics Data System (ADS)

Mazloom, Fatemeh; Masjedi-Arani, Maryam; Salavati-Niasari, Masoud

2017-08-01

Zinc vanadate (Zn3V2O8) nanostructures have been successfully synthesized via simple, rapid and solvent-free solid-state method by using different complex precursors of Zn and NH4VO3 as novel starting materials. Effects of various zinc (II) Schiff base complex precursors and calcination temperatures were investigated to reach optimum condition. It was found that particle size and optical property of the as-prepared products could be greatly influenced via these parameters. The products were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectra, energy dispersive X-ray microanalysis (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Photoluminescence and ultraviolet-visible (UV-Vis) spectroscopy. The photocatalytic activity of zinc vanadate nano and bulk structures were compared by degradation of phenol red aqueous solution.

Multi-functional magnetic water purifier for disinfection and removal of dyes and metal ions with superior reusability.

PubMed

Wu, Yao; Chen, Lei; Long, Xuwei; Zhang, Xiaolin; Pan, Bingcai; Qian, Jieshu

2018-04-05

It is of great practical importance but rarely reported to design a multifunctional scavenger for water purification. In this study, we describe a sophisticated preparation of an inorganic/organic composite sample for the simultaneous removal of anionic dyes and metal ions, as well as disinfection. The sample has a stable structure formed by the covalent connection between a magnetic silica (MS) core and a polyethylenimine derived quaternary ammonium compound (QAC) corona. We characterized the sample in details by SEM, TEM, EDX, FT-IR, XRD, TGA, VSM, and zeta potential. Our QAC-MS sample exhibited superior performance and reusability in the disinfection and adsorption experiments towards acid fuchsin and Cu 2+ . With the virtue of easy separation from solution, our sample should be an ideal candidate for water purification application. Copyright © 2017 Elsevier B.V. All rights reserved.

TiO2@TDI@DMAPA: an amine-modified nanoparticle, tailored to act as an economic basic heterogeneous nanocatalyst

NASA Astrophysics Data System (ADS)

Esfahanian, Farzane; Amoozadeh, Ali; Bitaraf, Mehrnoosh

2018-06-01

This study has represented an easy and inexpensive method for the synthesis of a new basic nanocatalyst. In this regard, 3-dimethylaminopropylamine (DMAPA), an economic, industrial, and readily obtainable basic compound, has been grafted onto nano-titania particles by the use of 2,4-toluene diisocyanate (TDI) as a bi-functional, inexpensive, and highly reactive linker. The prepared catalyst has been characterized using the spectroscopic FT-IR method, XRD, FE-SEM, EDX, and back titration. Furthermore, it was identified as an effective catalyst in the preparation of DHPM derivatives and pyranopyrazoles which results in high purity and high yields of products. Response surface methodology (RSM) based on a central composite design (CCD) was employed to reach the optimal conditions. The catalyst can be readily separated and recycled up to six times. [Figure not available: see fulltext.

Creating ligand-free silicon germanium alloy nanocrystal inks.

PubMed

Erogbogbo, Folarin; Liu, Tianhang; Ramadurai, Nithin; Tuccarione, Phillip; Lai, Larry; Swihart, Mark T; Prasad, Paras N

2011-10-25

Particle size is widely used to tune the electronic, optical, and catalytic properties of semiconductor nanocrystals. This contrasts with bulk semiconductors, where properties are tuned based on composition, either through doping or through band gap engineering of alloys. Ideally, one would like to control both size and composition of semiconductor nanocrystals. Here, we demonstrate production of silicon-germanium alloy nanoparticles by laser pyrolysis of silane and germane. We have used FTIR, TEM, XRD, EDX, SEM, and TOF-SIMS to conclusively determine their structure and composition. Moreover, we show that upon extended sonication in selected solvents, these bare nanocrystals can be stably dispersed without ligands, thereby providing the possibility of using them as an ink to make patterned films, free of organic surfactants, for device fabrication. The engineering of these SiGe alloy inks is an important step toward the low-cost fabrication of group IV nanocrystal optoelectronic, thermoelectric, and photovoltaic devices.

Antioxidant and anti-inflammatory activities of zinc oxide nanoparticles synthesized using Polygala tenuifolia root extract.

PubMed

Nagajyothi, P C; Cha, Sang Ju; Yang, In Jun; Sreekanth, T V M; Kim, Kwang Joong; Shin, Heung Mook

2015-05-01

The exploitation of various plant materials for the green synthesis of nanoparticles is considered an eco-friendly technology because it does not involve toxic chemicals. In this study, zinc oxide nanoparticles (ZnO NPs) were synthesized using the root extract of Polygala tenuifolia. Synthesized ZnO NPs were characterized by UV-Vis spectroscopy, FTIR, TGA, TEM, SEM and EDX. Anti-inflammatory activity was investigated in LPS-stimulated RAW 264.7 macrophages, whereas antioxidant activity was examined using a DPPH free radical assay. ZnO NPs demonstrated moderate antioxidant activity by scavenging 45.47% DPPH at 1mg/mL and revealed excellent anti-inflammatory activity by dose-dependently suppressing both mRNA and protein expressions of iNOS, COX-2, IL-1β, IL-6 and TNF-α. Copyright © 2015 Elsevier B.V. All rights reserved.

One - step nanosecond laser microstructuring, sulfur hyperdoping, and annealing of silicon surfaces in liquid carbondisulfide

NASA Astrophysics Data System (ADS)

Van Luong, Nguyen; Danilov, P. A.; Ionin, A. A.; Khmel'nitskii, P. A.; Kudryashov, S. I.; Mel'nik, N. N.; Saraeva, I. N.; Смirnov, H. A.; Rudenko, A. A.; Zayarny, D. A.

2017-09-01

We perform a single-shot IR nanosecond laser processing of commercial silicon wafers in ambient air and under a 2 mm thick carbon disulfide liquid layer. We characterize the surface spots modified in the liquid ambient and the spots ablated under the same conditions in air in terms of its surface topography, chemical composition, band-structure modification, and crystalline structure by means of SEM and EDX microscopy, as well as of FT-IR and Raman spectroscopy. These studies indicate that single-step microstructuring and deep (up to 2-3% on the surface) hyperdoping of the crystalline silicon in its submicron surface layer, preserving via pulsed laser annealing its crystallinity and providing high (103 - 104 cm-1) spectrally at near- and mid-IR absorption coefficients, can be obtained in this novel approach, which is very promising for thin - film silicon photovoltaic devices

Preparation of zeolite nanorods by corona discharge plasma for degradation of phenazopyridine by heterogeneous sono-Fenton-like process.

PubMed

Khataee, Alireza; Rad, Tannaz Sadeghi; Vahid, Behrouz; Khorram, Sirous

2016-11-01

The plasma-modified clinoptilolite (PMC) nanorods were prepared from natural clinoptilolite (NC) utilizing environmentally-friendly corona discharge plasma. The PMC and NC were characterized by XRD, FT-IR, SEM, EDX, XPS and BET, which confirmed the nanocatalyst formation. The catalytic performance of the PMC in the heterogeneous sono-Fenton-like process was greater than the NC for treatment of phenazopyridine (PhP). The desired amounts were obtained for experimental parameters including initial pH (5), PMC dosage (2g/L), K2S2O8 concentration (2mmol/L), ultrasonic power (300W) and PhP concentration (10mg/L). Reactive oxygen species scavengers decreased the removal efficiency of the PhP. The treatment process followed pseudo-first order kinetic and seven degradation intermediates were identified by the GC-MS technique. Copyright © 2016 Elsevier B.V. All rights reserved.

Nanoporous Polymer Films of Cyanate Ester Resins Designed by Using Ionic Liquids as Porogens.

PubMed

Fainleib, Alexander; Vashchuk, Alina; Starostenko, Olga; Grigoryeva, Olga; Rogalsky, Sergiy; Nguyen, Thi-Thanh-Tam; Grande, Daniel

2017-12-01

Novel nanoporous film materials of thermostable cyanate ester resins (CERs) were generated by polycyclotrimerization of dicyanate ester of bisphenol E in the presence of varying amounts (from 20 to 40 wt%) of an ionic liquid (IL), i.e., 1-heptylpyridinium tetrafluoroborate, followed by its quantitative extraction after complete CER network formation. The completion of CER formation and IL extraction was assessed using gel fraction content determination, FTIR, 1 H NMR, and energy-dispersive X-ray spectroscopy (EDX). SEM and DSC-based thermoporometry analyses demonstrated the formation of nanoporous structures after IL removal from CER networks, thus showing the effective role of IL as a porogen. Pore sizes varied from ~20 to ~180 nm with an average pore diameter of around 45-60 nm depending on the initial IL content. The thermal stability of nanoporous CER-based films was investigated by thermogravimetric analysis.

Adsorptive removal of patulin from aqueous solution using thiourea modified chitosan resin.

PubMed

Liu, Bingjie; Peng, Xiaoning; Chen, Wei; Li, Yang; Meng, Xianghong; Wang, Dongfeng; Yu, Guangli

2015-09-01

In the present paper, thiourea modified chitosan resin (TMCR) was firstly prepared through converting hydroxyl groups of chitosan resin into thiol groups, using glutaraldehyde as cross-linking agent and thiourea as modification agent. TMCR was characterized by FTIR, EDXS, SEM, XRD and AFM technologies. Batch adsorption experiments were performed to study the adsorption capacity of TMCR for patulin at different pH, temperature, contact time and patulin concentration. The result showed that TMCR was effective in removal of patulin from aqueous solution. The adsorption capacity of TMCR for patulin was 1.0 mg/g at pH 4.0, 25 °C for 24 h. Adsorption process could be well described by pseudo-first order model, Freundlich isotherm model and intraparticle diffusion model. It indicated that TMCR is expected to be a new material for patulin adsorption from aqueous solutions. Copyright © 2015 Elsevier B.V. All rights reserved.

A one-step method to fabricate PLLA scaffolds with deposition of bioactive hydroxyapatite and collagen using ice-based microporogens

PubMed Central

Li, Jiashen; Chen, Yun; Mak, Arthur F.T.; Tuan, Rocky S.; Li, Lin; Li, Yi

2010-01-01

Porous poly(L-lactic acid) (PLLA) scaffolds with bioactive coatings were prepared by a novel one-step method. In this process, ice-based microporogens containing bioactive molecules, such as hydroxyapatite (HA) and collagen, served as both porogens to form the porous structure and vehicles to transfer the bioactive molecules to the inside of PLLA scaffolds in a single step. Based on scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) analysis, the bioactive components were found to be transferred successfully from the porogens to PLLA scaffolds evenly. Osteoblast cells were used to evaluate the cellular behaviors of the composite scaffolds. After 8 days culturing, MTT assay and alkaline phosphatase (ALP) activity results suggested that HA/collagen could improve the interactions between osteoblast cells and the polymeric scaffold. PMID:20004261

Development of CMC hydrogels loaded with silver nano-particles for medical applications.

PubMed

Hebeish, Ali; Hashem, M; El-Hady, M M Abd; Sharaf, S

2013-01-30

Innovative CMC-based hydrogels with great potentials for usage in medical area were principally synthesized as per two strategies .The first involved reaction of epichlorohydrin in alkaline medium containing silver nitrate to yield silver nano-particles (AgNPs)-loaded CMC hydrogel. While CMC acted as stabilizing for AgNPs, trisodium citrate was added to the reaction medium to assist CMC in establishing reduction of Ag(+) to AgNPs. The second strategy entailed preparation of CMC hydrogel which assists the in situ preparation of AgNPs under the same conditions. In both strategies, factors affecting the characterization of AgNPs-loaded CMC hydrogels were studied. Analysis and characterization of the so obtained hydrogels were performed through monitoring swelling behavior, FTIR spectroscopy, SEM, EDX, UV-vis spectrophotometer and TEM. Antimicrobial activity of the hydrogels was examined and mechanisms involved in their synthesis were reported. Copyright © 2012 Elsevier Ltd. All rights reserved.

Characterization of Sorolla's gouache pigments by means of spectroscopic techniques

NASA Astrophysics Data System (ADS)

Roldán, Clodoaldo; Juanes, David; Ferrazza, Livio; Carballo, Jorgelina

2016-02-01

This paper presents the characterization of the Joaquín Sorolla's gouache sketches for the oil on canvas series "Vision of Spain" commissioned by A. M. Huntington to decorate the library of the Hispanic Society of America in New York. The analyses were focused on the identification of the elemental composition of the gouache pigments by means of portable EDXRF spectrometry in a non-destructive mode. Additionally, SEM-EDX and FTIR analyses of a selected set of micro-samples were carried out to identify completely the pigments, the paint technique and the binding media. The obtained results have confirmed the identification of lead and zinc white, vermillion, earth pigments, ochre, zinc yellow, chrome yellow, ultramarine, Prussian blue, chromium based and copper-arsenic based green pigments, bone black and carbon based black pigments, and the use of gum arabic as binding media in the gouache pigments.

Identification and characterization of the intermediate phase in hybrid organic-inorganic MAPbI3 perovskite.

PubMed

Guo, Xin; McCleese, Christopher; Kolodziej, Charles; Samia, Anna C S; Zhao, Yixin; Burda, Clemens

2016-03-07

Perovskite films were prepared using single step solution deposition at different annealing temperatures and annealing times. The crystal structure, phases and grain size were investigated with XRD, XPS and SEM/EDX. The prepared films show a typical orientation of tetragonal perovskite phase and a gradual transition at room temperature from the yellow intermediate phase to the black perovskite phase. Films with high purity were obtained by sintering at 100 °C. In addition, the chemical composition and crystal structure of intermediate phase were investigated in detail. FTIR, UV-vis and NMR spectra revealed the occurance of DMF complexes. Interestingly, the intermediate phase could be transformed to the black perovskite phase upon X-ray irradiation. In addition, the recovery of the aged perovskite films from a yellow intermediate phase back to the black perovskite was shown to be viable via heating and X-ray irradiation.

Synthesis and Characterization of Multiwalled Carbon Nanotubes/Poly(HEMA-co-MMA) by Utilizing Click Chemistry.

PubMed

Bach, Long Giang; Cao, Xuan Thang; Islam, Md Rafiqul; Jeong, Yeon Tae; Kim, Jong Su; Lim, Kwon Taek

2016-03-01

The hybrid material consisting of multi walled carbon nanotubes (MWNTs) and poly(2-hydroxyethylmethacrylate-co-methylmethacrylate) [poly(HEMA-co-MMA)] was synthesized by a combination of RAFT and Click chemistry. In the primary stage, the copolymer poly(HEMA-co-MMA) was prepared by applying RAFT technique. Alkynyl side groups were incorporated onto the poly(HEMA-co-MMA) backbone by esterification reaction. Then, MWNTs-N3 was prepared by treating MWNTs with 4-azidobutylamine. The click coupling reaction between azide-functionalized MWNTs (MWNTs-N3) and the alkyne-functionalized random copolymer ((HEMA-co-MMA)-Alkyne) with the Cu(I)-catalyzed [3+2] Huisgen cycloaddition afforded the hybrid compound. The structure and properties of poly(MMA-co-HEMA)-g-MWNTs were investigated by FT-IR, EDX and TGA measurements. The copolymer brushes were observed to be immobilized onto the functionalized MWNTs by SEM and TEM analysis.

Biosynthesis, characterization and antimicrobial action of silver nanoparticles from root bark extract of Berberislycium Royle.

PubMed

Mehmood, Ansar; Murtaza, Ghulam; Bhatti, Tariq Mahmood; Kausar, Rehana; Ahmed, Muhammad Jamil

2016-01-01

Various biological methods are being recognized for the fabrication of silver nanoparticles, which are used in several fields. The phytosynthesis of nanoparticles came out as a cost effective and enviro-friendly approach. When root bark extract of Berberis lycium was treated with silver ions, they reduced to silver nanoparticles, which were spherical, crystalline, size ranged from 10-100nm and capped by biomolecules. Synthesized silver nanoparticles were characterized by UV-visible spectroscopy, Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDX), Transmission Electron Microscopy (TEM), X-Ray Diffraction (XRD) and Fourier Transform Infra Red Spectroscopy (FTIR). The plant mediated synthesized silver nanoparticles showed pronounced antimicrobial activities against both Gram negative bacteria (Escherichia coli, Klebseilla pneumoniae, Pseudomonas aeruginosa) and Gram positive bacteria (Staphylococcus aureus and Bacillus subtilis). The plant mediated process proved to be non-toxic and low cost contender as reducing agent for synthesizing stable silver nanoparticles.

From waste to high-value product: Jackfruit peel derived pectin/apatite bionanocomposites for bone healing applications.

PubMed

Govindaraj, Dharman; Rajan, Mariappan; Hatamleh, Ashraf A; Munusamy, Murugan A

2018-01-01

Public requirements encouraged by the current asset framework drive industry to expand its general effectiveness by enhancing existing procedures or finding new uses for waste. Thus, the aim of this study was the isolation, fabrication, and characterization of pectin derived from jackfruit (Artocarpus heterophyllus) peels and the generation of hybrid of pectin (P)/apatite (HA) (P/HA) bionanocomposites. In this process, the natural pectin polymer derived from the peel of jackfruits was used in different concentrations for the fabrication of HA bionanocomposites. Characterization of the isolated pectin and bionanocomposites samples was performed with 1 H NMR and 13 C NMR, FTIR, XRD, SEM-EDX, and HR-TEM. Cytocompatibility, ALP, fibroblast stem cells, anti-inflammatory and cell adhesion testing of the fabricated bionanocomposites was showed good biocompatibility. Our results signify that the fabricated bionanocomposites might be applicable as bone graft materials. Copyright © 2017 Elsevier B.V. All rights reserved.

Explanation of the photocurrent generation of Cu2O quantum dots (QDs) sensitized p-CuSCN stable photoelectrochemical cells

NASA Astrophysics Data System (ADS)

Karunarathna, P. G. D. C. K.; Samarakoon, S. P. A. U. K.; Fernando, C. A. N.

2018-01-01

Fabrication of Cu2O quantum dots (QDs) sensitized p-CuSCN photoelectrode provides a significant photocurrent enhancement in photoelectrochemical medium for the first time. The variation of photocurrent quantum efficiency (Ф%) with Cu2O amount formed on p-CuSCN was presented. Here, two maxima of photocurrent could be observed in Cu/p-CuSCN/Cu2O photoelectrodes. The first photocurrent peak was due to the Cu2O QDs sensitization on p-CuSCN layer, and the second photocurrent peak was due to the formation of p-n junction. Time development of the photocurrent for Cu/p-CuSCN/n-Cu2O photoelectrodes and material characterization from Fourier transform infrared (FTIR) spectra, scanning electron microscope (SEM) images, energy dispersive x-ray spectroscopy (EDX) and x-ray diffraction (XRD) were done in this study in detailed.

Nanoporous Polymer Films of Cyanate Ester Resins Designed by Using Ionic Liquids as Porogens

NASA Astrophysics Data System (ADS)

Fainleib, Alexander; Vashchuk, Alina; Starostenko, Olga; Grigoryeva, Olga; Rogalsky, Sergiy; Nguyen, Thi-Thanh-Tam; Grande, Daniel

2017-02-01

Novel nanoporous film materials of thermostable cyanate ester resins (CERs) were generated by polycyclotrimerization of dicyanate ester of bisphenol E in the presence of varying amounts (from 20 to 40 wt%) of an ionic liquid (IL), i.e., 1-heptylpyridinium tetrafluoroborate, followed by its quantitative extraction after complete CER network formation. The completion of CER formation and IL extraction was assessed using gel fraction content determination, FTIR, 1H NMR, and energy-dispersive X-ray spectroscopy (EDX). SEM and DSC-based thermoporometry analyses demonstrated the formation of nanoporous structures after IL removal from CER networks, thus showing the effective role of IL as a porogen. Pore sizes varied from 20 to 180 nm with an average pore diameter of around 45-60 nm depending on the initial IL content. The thermal stability of nanoporous CER-based films was investigated by thermogravimetric analysis.

Electrospinning of curcumin loaded chitosan/poly (lactic acid) nanofilm and evaluation of its medicinal characteristics

NASA Astrophysics Data System (ADS)

Dhurai, Bhaarathi; Saraswathy, Nachimuthu; Maheswaran, Ramasamy; Sethupathi, Ponnusamy; Vanitha, Palanisamy; Vigneshwaran, Sukumar; Rameshbabu, Venugopal

2013-12-01

The curcumin loaded chitosan/poly (lactic acid) (PLA) nanofibers were produced using electrospinning. Box—Behnken experimental design was used for the optimization of variables (-1, 0, + 1 coded level) like chitosan/PLA strength (% w/v), curcumin strength (% w/v) and applied voltage (kV) to obtain uniform fiber diameter. The morphology of nanofibers was shown by SEM. Molecular interactions and the presence of each chemical compound of curcumin loaded chitosan/PLA fibers were characterized by FTIR and EDX analysis. Antioxidant, drug release and in vitro cytotoxicity tests were performed to evaluate the suitability of nanofibers that would be used for wound healing. In vivo wound healing studies on excision and incision wounds created on rat model showed significant reduction of wound area when compared to untreated. The better healing efficiency can be attributed to the presence of curcumin and chitosan.

Single Particulate SEM-EDX Analysis of Iron-Containing Coarse Particulate Matter in an Urban Environment: Sources and Distribution of Iron within Cleveland, Ohio

EPA Science Inventory

The physicochemical properties of coarse-mode, iron-containing particles, and their temporal and spatial distributions are poorly understood. Single particle analysis combining x-ray elemental mapping and computer-controlled scanning electron microscopy (CCSEM-EDX) of passively ...

Determination of the sequence of intersecting lines using Focused Ion Beam/Scanning Electron Microscope.

PubMed

Kim, Jiye; Kim, MinJung; An, JinWook; Kim, Yunje

2016-05-01

The aim of this study was to verify that the combination of focused ion beam (FIB) and scanning electron microscope/energy-dispersive X-ray (SEM/EDX) could be applied to determine the sequence of line crossings. The samples were transferred into FIB/SEM for FIB milling and an imaging operation. EDX was able to explore the chemical components and the corresponding elemental distribution in the intersection. The technique was successful in determining the sequence of heterogeneous line intersections produced using gel pens and red sealing ink with highest success rate (100% correctness). These observations show that the FIB/SEM was the appropriate instrument for an overall examination of document. © 2016 American Academy of Forensic Sciences.

Sonochemical synthesis and DFT studies of nano novel Schiff base cadmium complexes: Green, efficient, recyclable catalysts and precursors of Cd NPs

NASA Astrophysics Data System (ADS)

Parsaee, Zohreh

2017-10-01

Novel asymmetric (N4) Schiff bases (Ln, n = 1-3) and their nanosized cadmium complexes derived of 4,4'-(pentylazanediyl) dibenzaldehyde and aminobenzaldehyde are synthesized by sonochemical method and characterized based on physicochemical analysis including 1H NMR, 13C NMR, SEM, TGA, Mass, FT-IR, UV-Vis spectroscopy, elemental analysis, magnetic moment and molar conductance measurements. According to the analytic results of the NMR, UV-Vis and magnetic moment studies, it is found that the geometrical structures of these complexes [CdII2LnCl4], (L = C45H40N5X, X = CH3, Cl, OH) are square planer. The synthesized complexes were so effective as nanocatalyst on the oxidation of primary and secondary alcohols. The oxidation reactions were carried out in ethyl-methyl-imidazolium ionic liquid in presence of NaOCl. In addition Cd NPs were synthesized through the thermal decomposition of mentioned complexes and characterized by using FT-IR, SEM, TEM, EDX and XRD methods, which indicated close accordance to the standard pattern of CdO nanoparticles and an acceptable size at the nanorange (22-27 nm). Furthermore geometrical optimization of the Cd2LnCl4 calculated using DFT/B3LYP with LanL2DZ/6-311+G (d,p) level. The electronic parameter including HOMO-LUMO orbitals, bond gap, chemical hardness-softness, electronegativity, electrophilicity, NMR chemical shifts and IR frequencies were calculated. The calculated NMR shifts and vibrational frequencies showed excellent agreement with experimental data.

Scanning Electron Microscopy-Energy-Dispersive X-Ray (SEM/EDX): A Rapid Diagnostic Tool to Aid the Identification of Burnt Bone and Contested Cremains.

PubMed

Ellingham, Sarah T D; Thompson, Tim J U; Islam, Meez

2018-03-01

This study investigates the use of Scanning electron microscopy-energy-dispersive X-ray (SEM-EDX) as a diagnostic tool for the determination of the osseous origin of samples subjected to different temperatures. Sheep (Ovis aries) ribs of two experimental groups (fleshed and defleshed) were burned at temperatures of between 100°C and 1100°C in 100°C increments and subsequently analyzed with the SEM-EDX to determine the atomic percentage of present elements. Three-factor ANOVA analysis showed that neither the exposure temperature, nor whether the burning occurred with or without soft tissue present had any significant influence on the bone's overall elemental makeup (p > 0.05). The Ca/P ratio remained in the osseous typical range of between 1.6 and 2.58 in all analyzed samples. This demonstrates that even faced with high temperatures, the overall gross elemental content and atomic percentage of elements in bone remain stable, creating a unique "fingerprint" for osseous material, even after exposure to extreme conditions. © 2017 American Academy of Forensic Sciences.

Mn-Cr isotopic systematics of Chainpur chondrules and bulk ordinary chondrites

NASA Technical Reports Server (NTRS)

Nyquist, L.; Lindstrom, D.; Wiesmann, H.; Bansal, B.; Shih, C.-Y.; Mittlefehldt, D.; Martinez, R.; Wentworth, S.

1994-01-01

We report on ongoing study of the Mn-Cr systematics of individual Chainpur (LL3.4) chondrules and compare the results to those for bulk ordinary chondrites. Twenty-eight chondrules were surveyed for abundances of Mn, Cr, Na, Fe, Sc, Hf, Ir, and Zn by INAA. Twelve were chosen for SEM/EDX and high-precision Cr-isotopic studies on the basis of LL-chondrite-normalized Mn(LL), Sc(LL), (Mn/Fe)(LL), and (Sc/Fe)(LL) as well as their Mn/Cr ratios. Classification into textural types follows from SEM/EDX examination of interior surfaces.

Remineralization of enamel subsurface lesions with casein phosphopeptide-amorphous calcium phosphate: A quantitative energy dispersive X-ray analysis using scanning electron microscopy: An in vitro study

PubMed Central

Hegde, Mithra N; Moany, Anu

2012-01-01

Aim: The objective of this study was to quantitatively evaluate the remineralization potential of casein phosphopeptide-amor-phous calcium phosphate paste on enamel subsurface lesions using scanning electron microscopy with energy dispersive X-ray analysis (SEM-EDX). Materials and Methods: Ninety enamel specimens were prepared from extracted human molars. All specimens were evaluated for mineral content (% weight) using SEM-EDX. The specimens were placed in demineralizing solution for four days to produce artificial carious lesions. The mineral content (calcium/phosphorus ratios, Ca/P ratios) was remeasured using SEM-EDX. The specimens were then randomly assigned to five study groups and one control group of 15 specimens per group. Except for the control group, all group specimens were incubated in remineralizing paste (CPP-ACP paste) for 7, 14, 21, 28, and 35 days twice daily for three minutes. The control group received no treatment with remineralizing paste. All the 90 specimens were stored in artificial saliva at 37°C. After remineralization, the mineral content (% weight) of the samples was measured using SEM-EDX. Results: All the study groups showed very highly significant differences between Ca/P ratios of the demineralized and remineralized samples. There was no significant difference seen in the control group. Conclusion: CPP-ACP paste could significantly remineralize the artificial enamel subsurface lesions in vitro: the remineralizing rates increasing with the time for which the samples were kept in the remineralizing paste. Energy dispersive X-ray analysis is an efficient way to quantitatively assess the changes in mineral content during demineralization and in vitro remineralization processes. PMID:22368338

Effect of stoichiometry on magnetic and transport properties in polycrystalline Y2Ir2O7

NASA Astrophysics Data System (ADS)

Dwivedi, Vinod Kumar; Mukhopadhyay, Soumik

2018-05-01

In this paper we discuss synthesis of polycrystalline Y2Ir2O7 by solid state reaction route. XRD analysis shows deviation from stoichiometry which is also confirmed by SEM-EDX analysis. SEM analysis indicates average particle size ranging from 100 nm to 800 µm. EDX analysis gives clear evidence for deviation of stoichiometry of the product. Magnetic analysis is indicating effect of stoichiometry and showing ferromagnetic interaction unlike antiferromagnetic feature. Electrical resistivity is showing similar behavior as reported earlier and reveals no effect of different size of grains or grain boundaries from room temperature to 125 K.

Scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDX) and aerosol time-of-flight mass spectrometry (ATOFMS) single particle analysis of metallurgy plant emissions.

PubMed

Arndt, J; Deboudt, K; Anderson, A; Blondel, A; Eliet, S; Flament, P; Fourmentin, M; Healy, R M; Savary, V; Setyan, A; Wenger, J C

2016-03-01

The chemical composition of single particles deposited on industrial filters located in three different chimneys of an iron-manganese (Fe-Mn) alloy manufacturing plant have been compared using aerosol time-of-flight mass spectrometry (ATOFMS) and scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDX). Very similar types of particles were observed using both analytical techniques. Calcium-containing particles dominated in the firing area of the sintering unit, Mn and/or Al-bearing particles were observed at the cooling area of the sintering unit, while Mn-containing particles were dominant at the smelting unit. SEM-EDX analysis of particles collected downstream of the industrial filters showed that the composition of the particles emitted from the chimneys is very similar to those collected on the filters. ATOFMS analysis of ore samples was also performed to identify particulate emissions that could be generated by wind erosion and manual activities. Specific particle types have been identified for each emission source (chimneys and ore piles) and can be used as tracers for source apportionment of ambient PM measured in the vicinity of the industrial site. Copyright © 2015 Elsevier Ltd. All rights reserved.

Synthesis, spectroscopic and electrochemical performance of pasted β-nickel hydroxide electrode in alkaline electrolyte

NASA Astrophysics Data System (ADS)

Shruthi, B.; Bheema Raju, V.; Madhu, B. J.

2015-01-01

β-Nickel hydroxide (β-Ni(OH)2) was successfully synthesized using precipitation method. The structure and property of the β-Ni(OH)2 were characterized by X-ray diffraction (XRD), Fourier Transform infra-red (FT-IR), Raman spectra and thermal gravimetric-differential thermal analysis (TG-DTA). The results of the FTIR spectroscopy and TG-DTA studies indicate that the β-Ni(OH)2 contains water molecules and anions. The microstructural and composition studies have been performed using Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray (EDX) analysis. A pasted-type electrode is prepared using β-Ni(OH)2 powder as the active material on a nickel sheet as a current collector. Cyclic voltammetry (CV) and Electrochemical impedance spectroscopy (EIS) studies were performed to evaluate the electrochemical performance of the β-Ni(OH)2 electrode in 6 M KOH electrolyte. CV curves showed a pair of strong redox peaks as a result of the Faradaic redox reactions of β-Ni(OH)2. The proton diffusion coefficient (D) for the present β-Ni(OH)2 electrode material is found to be 1.44 × 10-12 cm2 s-1. Further, electrochemical impedance studies confirmed that the β-Ni(OH)2 electrode reaction processes are diffusion controlled.

Synthesis, spectroscopic and electrochemical performance of pasted β-nickel hydroxide electrode in alkaline electrolyte.

PubMed

Shruthi, B; Bheema Raju, V; Madhu, B J

2015-01-25

β-Nickel hydroxide (β-Ni(OH)2) was successfully synthesized using precipitation method. The structure and property of the β-Ni(OH)2 were characterized by X-ray diffraction (XRD), Fourier Transform infra-red (FT-IR), Raman spectra and thermal gravimetric-differential thermal analysis (TG-DTA). The results of the FTIR spectroscopy and TG-DTA studies indicate that the β-Ni(OH)2 contains water molecules and anions. The microstructural and composition studies have been performed using Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray (EDX) analysis. A pasted-type electrode is prepared using β-Ni(OH)2 powder as the active material on a nickel sheet as a current collector. Cyclic voltammetry (CV) and Electrochemical impedance spectroscopy (EIS) studies were performed to evaluate the electrochemical performance of the β-Ni(OH)2 electrode in 6M KOH electrolyte. CV curves showed a pair of strong redox peaks as a result of the Faradaic redox reactions of β-Ni(OH)2. The proton diffusion coefficient (D) for the present β-Ni(OH)2 electrode material is found to be 1.44×10(-12) cm(2) s(-1). Further, electrochemical impedance studies confirmed that the β-Ni(OH)2 electrode reaction processes are diffusion controlled. Copyright © 2014 Elsevier B.V. All rights reserved.

RF magnetron sputtering of a hydroxyapatite target: A comparison study on polytetrafluorethylene and titanium substrates

NASA Astrophysics Data System (ADS)

Surmenev, Roman A.; Surmeneva, Maria A.; Grubova, Irina Yu.; Chernozem, Roman V.; Krause, Bärbel; Baumbach, Tilo; Loza, Kateryna; Epple, Matthias

2017-08-01

A pure hydroxyapatite (HA) target was used to prepare the biocompatible coating of HA on the surface of a polytetrafluorethylene (PTFE) substrate, which was placed on the same substrate holder with technically pure titanium (Ti) in the single deposition runs by radio-frequency (RF) magnetron sputtering. The XPS, XRD and FTIR analyses of the obtained surfaces showed that for all substrates, instead of the HA coating deposition, the coating of a mixture of calcium carbonate and calcium fluoride was grown. According to SEM investigations, the surface of PTFE was etched, and the surface topography of uncoated Ti was preserved after the depositions. The FTIR results reveal no phosphate bonds; only calcium tracks were observed in the EDX-spectra on the surface of the coated PTFE substrates. Phosphate oxide (V), which originated from the target, could be removed using a vacuum pump system, or no phosphate-containing bonds could be formed on the substrate surface because of the severe substrate bombardment process, which prevented the HA coating deposition. The observed results may be connected with the surface re-sputtering effect of the growing film by high-energy negatively charged ions (most probably oxygen or fluorine), which are accelerated in the cathode dark sheath.

Chamomile flower extract-directed CuO nanoparticle formation for its antioxidant and DNA cleavage properties.

PubMed

Duman, Fatih; Ocsoy, Ismail; Kup, Fatma Ozturk

2016-03-01

In this study, we report the synthesis of copper oxide nanoparticles (CuO NPs) using a medicinal plant (Matricaria chamomilla) flower extract as both reducing and capping agent and investigate their antioxidant activity and interaction with plasmid DNA (pBR322).The CuO NPs were characterized using Uv-Vis spectroscopy, FT-IR (Fourier transform infrared spectroscopy), DLS (dynamic light scattering), XRD (X-ray diffraction), EDX (energy-dispersive X-ray) spectroscopy and SEM (scanning electron microscopy). The CuO NPs exhibited nearly mono-distributed and spherical shapes with diameters of 140 nm size. UV-Vis absorption spectrum of CuO NPs gave a broad peak around 285 and 320 nm. The existence of functional groups on the surface of CuO NPs was characterized with FT-IR analysis. XRD pattern showed that the NPs are in the form of a face-centered cubic crystal. Zeta potential value was measured as -20 mV due to the presence of negatively charged functional groups in plant extract. Additionally, we demonstrated concentration-dependent antioxidant activity of CuO NPs and their interaction with plasmid DNA. We assumed that the CuO NPs both cleave and break DNA double helix structure. Copyright © 2015 Elsevier B.V. All rights reserved.

Three-dimensional mapping of soil chemical characteristics at micrometric scale: Statistical prediction by combining 2D SEM-EDX data and 3D X-ray computed micro-tomographic images

NASA Astrophysics Data System (ADS)

Hapca, Simona

2015-04-01

Many soil properties and functions emerge from interactions of physical, chemical and biological processes at microscopic scales, which can be understood only by integrating techniques that traditionally are developed within separate disciplines. While recent advances in imaging techniques, such as X-ray computed tomography (X-ray CT), offer the possibility to reconstruct the 3D physical structure at fine resolutions, for the distribution of chemicals in soil, existing methods, based on scanning electron microscope (SEM) and energy dispersive X-ray detection (EDX), allow for characterization of the chemical composition only on 2D surfaces. At present, direct 3D measurement techniques are still lacking, sequential sectioning of soils, followed by 2D mapping of chemical elements and interpolation to 3D, being an alternative which is explored in this study. Specifically, we develop an integrated experimental and theoretical framework which combines 3D X-ray CT imaging technique with 2D SEM-EDX and use spatial statistics methods to map the chemical composition of soil in 3D. The procedure involves three stages 1) scanning a resin impregnated soil cube by X-ray CT, followed by precision cutting to produce parallel thin slices, the surfaces of which are scanned by SEM-EDX, 2) alignment of the 2D chemical maps within the internal 3D structure of the soil cube, and 3) development, of spatial statistics methods to predict the chemical composition of 3D soil based on the observed 2D chemical and 3D physical data. Specifically, three statistical models consisting of a regression tree, a regression tree kriging and cokriging model were used to predict the 3D spatial distribution of carbon, silicon, iron and oxygen in soil, these chemical elements showing a good spatial agreement between the X-ray grayscale intensities and the corresponding 2D SEM-EDX data. Due to the spatial correlation between the physical and chemical data, the regression-tree model showed a great potential in predicting chemical composition in particular for iron, which is generally sparsely distributed in soil. For carbon, silicon and oxygen, which are more densely distributed, the additional kriging of the regression tree residuals improved significantly the prediction, whereas prediction based on co-kriging was less consistent across replicates, underperforming regression-tree kriging. The present study shows a great potential in integrating geo-statistical methods with imaging techniques to unveil the 3D chemical structure of soil at very fine scales, the framework being suitable to be further applied to other types of imaging data such as images of biological thin sections for characterization of microbial distribution. Key words: X-ray CT, SEM-EDX, segmentation techniques, spatial correlation, 3D soil images, 2D chemical maps.

Cytotoxic evaluation of hydroxyapatite-filled and silica/hydroxyapatite-filled acrylate-based restorative composite resins: An in vitro study.

PubMed

Chadda, Harshita; Naveen, Sangeetha Vasudevaraj; Mohan, Saktiswaren; Satapathy, Bhabani K; Ray, Alok R; Kamarul, Tunku

2016-07-01

Although the physical and mechanical properties of hydroxyapatite-filled dental restorative composite resins have been examined, the biocompatibility of these materials has not been studied in detail. The purpose of this in vitro study was to analyze the toxicity of acrylate-based restorative composite resins filled with hydroxyapatite and a silica/hydroxyapatite combination. Five different restorative materials based on bisphenol A-glycidyl methacrylate (bis-GMA) and tri-ethylene glycol dimethacrylate (TEGDMA) were developed: unfilled (H0), hydroxyapatite-filled (H30, H50), and silica/hydroxyapatite-filled (SH30, SH50) composite resins. These were tested for in vitro cytotoxicity by using human bone marrow mesenchymal stromal cells. Surface morphology, elemental composition, and functional groups were determined by scanning electron microscopy (SEM), energy-dispersive x-ray spectroscopy (EDX), and Fourier-transformed infrared spectroscopy (FTIR). The spectra normalization, baseline corrections, and peak integration were carried out by OPUS v4.0 software. Both in vitro cytotoxicity results and SEM analysis indicated that the composite resins developed were nontoxic and supported cell adherence. Elemental analysis with EDX revealed the presence of carbon, oxygen, calcium, silicon, and gold, while the presence of methacrylate, hydroxyl, and methylene functional groups was confirmed through FTIR analysis. The characterization and compatibility studies showed that these hydroxyapatite-filled and silica/hydroxyapatite-filled bis-GMA/TEGDMA-based restorative composite resins are nontoxic to human bone marrow mesenchymal stromal cells and show a favorable biologic response, making them potential biomaterials. Copyright © 2016 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

Biosynthesis, Antimicrobial and Cytotoxic Effect of Silver Nanoparticles Using a Novel Nocardiopsis sp. MBRC-1

PubMed Central

Manivasagan, Panchanathan; Senthilkumar, Kalimuthu; Sivakumar, Kannan; Kim, Se-Kwon

2013-01-01

The biosynthesis of nanoparticles has been proposed as a cost effective environmental friendly alternative to chemical and physical methods. Microbial synthesis of nanoparticles is under exploration due to wide biomedical applications, research interest in nanotechnology and microbial biotechnology. In the present study, an ecofriendly process for the synthesis of nanoparticles using a novel Nocardiopsis sp. MBRC-1 has been attempted. We used culture supernatant of Nocardiopsis sp. MBRC-1 for the simple and cost effective green synthesis of silver nanoparticles. The reduction of silver ions occurred when silver nitrate solution was treated with the Nocardiopsis sp. MBRC-1 culture supernatant at room temperature. The nanoparticles were characterized by UV-visible, TEM, FE-SEM, EDX, FTIR, and XRD spectroscopy. The nanoparticles exhibited an absorption peak around 420 nm, a characteristic surface plasmon resonance band of silver nanoparticles. They were spherical in shape with an average particle size of 45 ± 0.15 nm. The EDX analysis showed the presence of elemental silver signal in the synthesized nanoparticles. The FTIR analysis revealed that the protein component in the form of enzyme nitrate reductase produced by the isolate in the culture supernatant may be responsible for reduction and as capping agents. The XRD spectrum showed the characteristic Bragg peaks of 1 2 3, 2 0 4, 0 4 3, 1 4 4, and 3 1 1 facets of the face centered cubic silver nanoparticles and confirms that these nanoparticles are crystalline in nature. The prepared silver nanoparticles exhibited strong antimicrobial activity against bacteria and fungi. Cytotoxicity of biosynthesized AgNPs against in vitro human cervical cancer cell line (HeLa) showed a dose-response activity. IC50 value was found to be 200 μg/mL of AgNPs against HeLa cancer cells. Further studies are needed to elucidate the toxicity and the mechanism involved with antimicrobial and anticancer activity of the synthesized AgNPs as nanomedicine. PMID:23936787

Biosynthesis, antimicrobial and cytotoxic effect of silver nanoparticles using a novel Nocardiopsis sp. MBRC-1.

PubMed

Manivasagan, Panchanathan; Venkatesan, Jayachandran; Senthilkumar, Kalimuthu; Sivakumar, Kannan; Kim, Se-Kwon

2013-01-01

The biosynthesis of nanoparticles has been proposed as a cost effective environmental friendly alternative to chemical and physical methods. Microbial synthesis of nanoparticles is under exploration due to wide biomedical applications, research interest in nanotechnology and microbial biotechnology. In the present study, an ecofriendly process for the synthesis of nanoparticles using a novel Nocardiopsis sp. MBRC-1 has been attempted. We used culture supernatant of Nocardiopsis sp. MBRC-1 for the simple and cost effective green synthesis of silver nanoparticles. The reduction of silver ions occurred when silver nitrate solution was treated with the Nocardiopsis sp. MBRC-1 culture supernatant at room temperature. The nanoparticles were characterized by UV-visible, TEM, FE-SEM, EDX, FTIR, and XRD spectroscopy. The nanoparticles exhibited an absorption peak around 420 nm, a characteristic surface plasmon resonance band of silver nanoparticles. They were spherical in shape with an average particle size of 45 ± 0.15 nm. The EDX analysis showed the presence of elemental silver signal in the synthesized nanoparticles. The FTIR analysis revealed that the protein component in the form of enzyme nitrate reductase produced by the isolate in the culture supernatant may be responsible for reduction and as capping agents. The XRD spectrum showed the characteristic Bragg peaks of 1 2 3, 2 0 4, 0 4 3, 1 4 4, and 3 1 1 facets of the face centered cubic silver nanoparticles and confirms that these nanoparticles are crystalline in nature. The prepared silver nanoparticles exhibited strong antimicrobial activity against bacteria and fungi. Cytotoxicity of biosynthesized AgNPs against in vitro human cervical cancer cell line (HeLa) showed a dose-response activity. IC50 value was found to be 200 μg/mL of AgNPs against HeLa cancer cells. Further studies are needed to elucidate the toxicity and the mechanism involved with antimicrobial and anticancer activity of the synthesized AgNPs as nanomedicine.

Structural, morphological and gas sensing study of zinc doped tin oxide nanoparticles synthesized via hydrothermal technique

NASA Astrophysics Data System (ADS)

Singh, Davender; Kundu, Virender Singh; Maan, A. S.

2016-07-01

The pure and Zn-doped SnO2 nanoparticles were prepared successfully by hydrothermal route on large scale having different doping concentration of zinc from 0 to 0.20%. The calcined nanoparticles were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM) for structural and morphological studies. XRD analyses reveal that the nanoparticles of these doping concentrations are polycrystalline in nature and existed as tetragonal rutile structure, SEM study of images confirms the existence of very small, homogeneously distributed, and spherical nanoparticles. The particles size of the nanoparticles was calculated by Scherrer formula and was found in the range of 9-21 nm. The presence of dopant (i.e. zinc) and formation of Sn-O phase and hydrous nature of Zn-doped SnO2 nanoparticles are confirmed by EDX and FTIR study. The gas sensing properties of pure and Zn-doped SnO2 nanoparticles were investigated for various concentrations of methanol, ethanol and acetone at different operating temperatures and it has been found that with doping concentration of zinc (x = 0.20%) shows the maximum response 78% to methanol, 65% to ethanol and 62% to acetone respectively at different operating temperature within the measurement limit for a concentration of 100 ppm of each gases.

Biological influence of Ca/P ratio on calcium phosphate coatings by sol-gel processing.

PubMed

Catauro, M; Papale, F; Sapio, L; Naviglio, S

2016-08-01

The objective of this work has been to develop low temperature sol-gel glass coatings to modify the substrate surface and to evaluate their bioactivity and biocompatibility. Glasses, based on SiO2·CaO·P2O5, were synthesized by the sol-gel technique using tetraethyl orthosilicate, calcium nitrate tetrahydrate and triethyl phosphate as precursors of SiO2, CaO and P2O5, respectively. Those materials, still in the sol phase, have been used to coat substrates by means of the dip-coating technique. Attenuated total reflectance Fourier transform infrared (ATR-FTIR) has been used for characterize coatings and a microstructural analysis has been obtained using scanning electron microscopy (SEM). The potential applications of the coatings in the biomedical field were evaluated by bioactivity and biocompatibility tests. The coated substrate was immersed in simulated body fluid (SBF) for 21days and the hydroxyapatite deposition on its surface was subsequently evaluated via SEM-EDXS analysis, as an index of bone-bonding capability. In order to study the cell behavior and response to our silica based materials, prepared via the sol-gel method, with various Ca/P ratio and coating substrate, we have used the human osteoblast-like U2OS cell line. Copyright © 2016 Elsevier B.V. All rights reserved.

Development of a novel biomaterial with an important osteoinductive capacity for hard tissue engineering.

PubMed

Simu, Meda-Romana; Pall, Emoke; Radu, Teodora; Miclaus, Maria; Culic, Bogdan; Mesaros, Anca-Stefania; Muntean, Alexandrina; Filip, Gabriela Adriana

2018-06-01

In this study we designed a composite biomaterial based on a high viscosity soft propolis extract (70% propolis) and shell clam, with antiseptic and osteoinductive qualities, that can be used in dentistry, orthopedics and other areas where hard tissue regeneration is needed. We assessed it in interaction with stabilized human cells isolated from dental papilla of wisdom teeth (D1MSCs). We performed detailed characterization of the obtained material by Scanning Electronic Microscopy (SEM), X-Ray Diffraction (XRD), Energy Dispersive X-Ray Spectroscopy (EDX), Fourier Transform Infrared Spectroscopy (FTIR) techniques. SEM investigation revealed the roughness and porosity of the shell, which acted like a scaffold, as it allowed cells to penetrate the pores, proliferate on the surface, spread and grow in the depressions provided by the substrate. in vitro cell viability, proliferation and differentiation assays showed that the newly obtain biomaterial presented low toxicity on D1MSCs and determined the development of numerous osteogenic nodules that were in a higher number even than in the specific induction medium. Our results demonstrated that the shell-propolis based biomaterial promoted and sustained human stem cells attachment, proliferation and differentiation, presenting an important osteoinductive effect essential for mineralized tissue reparation process. Copyright © 2018 Elsevier Ltd. All rights reserved.

Focused ion beam (FIB)/scanning electron microscopy (SEM) in tissue structural research.

PubMed

Leser, Vladka; Milani, Marziale; Tatti, Francesco; Tkalec, Ziva Pipan; Strus, Jasna; Drobne, Damjana

2010-10-01

The focused ion beam (FIB) and scanning electron microscope (SEM) are commonly used in material sciences for imaging and analysis of materials. Over the last decade, the combined FIB/SEM system has proven to be also applicable in the life sciences. We have examined the potential of the focused ion beam/scanning electron microscope system for the investigation of biological tissues of the model organism Porcellio scaber (Crustacea: Isopoda). Tissue from digestive glands was prepared as for conventional SEM or as for transmission electron microscopy (TEM). The samples were transferred into FIB/SEM for FIB milling and an imaging operation. FIB-milled regions were secondary electron imaged, back-scattered electron imaged, or energy dispersive X-ray (EDX) analyzed. Our results demonstrated that FIB/SEM enables simultaneous investigation of sample gross morphology, cell surface characteristics, and subsurface structures. The same FIB-exposed regions were analyzed by EDX to provide basic compositional data. When samples were prepared as for TEM, the information obtained with FIB/SEM is comparable, though at limited magnification, to that obtained from TEM. A combination of imaging, micro-manipulation, and compositional analysis appears of particular interest in the investigation of epithelial tissues, which are subjected to various endogenous and exogenous conditions affecting their structure and function. The FIB/SEM is a promising tool for an overall examination of epithelial tissue under normal, stressed, or pathological conditions.

Green synthesis and characterization of zinc oxide nanoparticle using insulin plant (Costus pictus D. Don) and investigation of its antimicrobial as well as anticancer activities

NASA Astrophysics Data System (ADS)

Suresh, Joghee; Pradheesh, Ganeshan; Alexramani, Vincent; Sundrarajan, Mahalingam; Hong, Sun Ig

2018-03-01

In this work we aim to synthesize biocompatible ZnO nanoparticles from the zinc nitrate via green process using leaf extracts of the Costus pictus D. Don medicinal plant. FTIR studies confirm the presence of biomolecules and metal oxides. X-ray diffraction (XRD) structural analysis reveals the formation of pure hexagonal phase structures of ZnO nanoparticles. The surface morphologies of ZnO nanoparticles observed under a scanning electron microscope (SEM) suggest that most ZnO crystallites are hexagonal. EDX analysis confirms the presence of primarily zinc and oxygen. TEM images show that biosynthesized zinc oxide nanoparticles are hexagonal and spherical. The plausible formation mechanisms of zinc oxide nanoparticles are also predicted. The biosynthesized zinc oxide nanoparticles exhibit strong antimicrobial behavior against bacterial and fungal species when employing the agar diffusion method. Synthesized ZnO nanoparticles exhibit anticancer activity against Daltons lymphoma ascites (DLA) cells as well as antimicrobial activity against some bacterial and fungal strains.

Functional lignocellulosic materials prepared by ATRP from a wood scaffold.

PubMed

Cabane, Etienne; Keplinger, Tobias; Künniger, Tina; Merk, Vivian; Burgert, Ingo

2016-08-10

Wood, a natural and abundant source of organic polymers, has been used as a scaffold to develop novel wood-polymer hybrid materials. Through a two-step surface-initiated Atom Transfer Radical Polymerization (ATRP), the porous wood structure can be effectively modified with polymer chains of various nature. In the present study, polystyrene and poly(N-isopropylacrylamide) were used. As shown with various characterization techniques including confocal Raman microscopy, FTIR, and SEM/EDX, the native wood ultrastructure and features are retained and the polymer chains can be introduced deep within the wood, i.e. inside the wood cell walls. The physical properties of the new materials have been studied, and results indicate that the insertion of polymer chains inside the wood cell wall alters the intrinsic properties of wood to yield a hybrid composite material with new functionalities. This approach to the functionalization of wood could lead to the fabrication of a new class of interesting functional materials and promote innovative utilizations of the renewable resource wood.

Synthesis of silver nanoparticles using Solanum trilobatum fruits extract and its antibacterial, cytotoxic activity against human breast cancer cell line MCF 7

NASA Astrophysics Data System (ADS)

Ramar, Manikandan; Manikandan, Beulaja; Marimuthu, Prabhu Narayanan; Raman, Thiagarajan; Mahalingam, Anjugam; Subramanian, Palanisamy; Karthick, Saravanan; Munusamy, Arumugam

2015-04-01

In the present study, we have synthesized silver nanoparticles by a simple and eco-friendly method using unripe fruits of Solanum trilobatum. The aqueous silver ions when exposed to unripe fruits extract were reduced and stabilized over long time resulting in biosynthesis of surface functionalized silver nanoparticles. The bio-reduced silver nanoparticles were characterized by UV-visible spectroscopy, Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive spectroscopy (EDX) and X-ray diffraction (XRD). These biologically synthesized silver nanoparticles were tested for its antibacterial activity against few human pathogenic bacteria including Gram-positive (Streptococcus mutans, Enterococcus faecalis) and Gram-negative (Escherichia coli, Klebsiella pneumoniae) bacteria. In addition, we also demonstrated anticancer activity of these nanoparticles in vitro against human breast cancer cell line (MCF 7) using MTT, nuclear morphology assay, Western blot and RT-PCR expression. These results taken together show the potential applications of biosynthesized silver nanoparticles using S. trilobatum fruits.

Biogenic copper oxide nanoparticles synthesis using Tabernaemontana divaricate leaf extract and its antibacterial activity against urinary tract pathogen

NASA Astrophysics Data System (ADS)

Sivaraj, Rajeshwari; Rahman, Pattanathu K. S. M.; Rajiv, P.; Salam, Hasna Abdul; Venckatesh, R.

2014-12-01

This investigation explains the biosynthesis and characterization of copper oxide nanoparticles from an Indian medicinal plant by an eco-friendly method. The main objective of this study is to synthesize copper oxide nanoparticles from Tabernaemontana divaricate leaves through a green chemistry approach. Highly stable, spherical copper oxide nanoparticles were synthesized by using 50% concentration of Tabernaemontana leaf extract. Formation of copper oxide nanoparticles have been characterized by UV-Vis absorption spectroscopy, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) with energy dispersive X-ray analysis (EDX) and transmission electron microscopy (TEM) analysis. All the analyses revealed that copper oxide nanoparticles were 48 ± 4 nm in size. Functional groups and chemical composition of copper oxide were also confirmed. Antimicrobial activity of biogenic copper oxide nanoparticles were investigated and maximum zone of inhibition was found in 50 μg/ml copper oxide nanoparticles against urinary tract pathogen (Escherichia coli).

Investigation of electrical studies of spinel FeCo2O4 synthesized by sol-gel method

NASA Astrophysics Data System (ADS)

Lobo, Laurel Simon; Kalainathan, S.; Kumar, A. Ruban

2015-12-01

In this work, spinel FeCo2O4 is synthesized by sol-gel method using succinic acid as a chelating agent at 900 °C. The structural, spectroscopic and morphological characterization was carried out by using X-ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FT-IR) and Scanning Electron Microscopy equipped with Energy Dispersive X-ray spectrometer (SEM-EDX). The M-H loop at room temperature confirms the ferromagnetic property of the sample. The frequency and temperature dependence of dielectric constant (εʹ) and dielectric loss (tan δ) shows the presence of Maxwell-Wagner relaxation in the sample due to the presence of oxygen vacancy. Nyquist plot for frequency and temperature domain signifies the presence of grain effect, grain boundary effect and electrode interface in the conduction process. Electric modulus under suppression of electrode polarization shows the grain and grain boundary effects. The electrode polarization is observed in the lower frequency range of the conductivity graph.

Green synthesis of copper oxide (CuO) nanoparticles using banana peel extract and their photocatalytic activities

NASA Astrophysics Data System (ADS)

Aminuzzaman, Mohammod; Kei, Leong Mei; Liang, Wong Hong

2017-04-01

Copper oxide nanoparticles (CuO NPs) are interesting class of materials having multifunctional properties with promising applications in the areas of catalysts, gas sensors, batteries, magnetic storage media, solar energy, superconductors etc. Thus synthesis of CuO NPs has attracted tremendous interest to scientists and researchers Herein, we reported a green and simple method for biosynthesizing CuO NPs using banana peel extract as reducing and stabilizing agent. XRD, EDX, FE-SEM, FTIR have been used for characterization of biosynthesized CuO NPs. The results indicating that the CuO NPs synthesized by banana peel extract have high purity and the average particles size is 60 nm. The photocatalytic activity of the CuO NPs has been investigated by degradation of Congo red (CR) dye under solar irradiation. The extent of CR dye degradation by CuO NPs is monitored by using a UV-visible spectrophotometer. Due to the smaller size and high purity, the biosynthesized CuO NPs showed an excellent photocatlytic activity.

Characterization of leaf waste based biochar for cost effective hydrogen sulphide removal from biogas.

PubMed

Sahota, Shivali; Vijay, Virendra Kumar; Subbarao, P M V; Chandra, Ram; Ghosh, Pooja; Shah, Goldy; Kapoor, Rimika; Vijay, Vandit; Koutu, Vaibhav; Thakur, Indu Shekhar

2018-02-01

Installation of decentralized units for biogas production along with indigenous upgradation systems can be an effective approach to meet growing energy demands of the rural population. Therefore, readily available leaf waste was used to prepare biochar at different temperatures and employed for H 2 S removal from biogas produced via anaerobic digestion plant. It is found that biochar prepared via carbonization of leaf waste at 400 °C effectively removes 84.2% H 2 S (from 1254 ppm to 201 ppm) from raw biogas for 25 min in a continuous adsorption tower. Subsequently, leaf waste biochar compositional, textural and morphological properties before and after H 2 S adsorption have been analyzed using proximate analysis, CHNS, BET surface area, FTIR, XRD, and SEM-EDX. It is found that BET surface area, pore size, and textural properties of leaf waste biochar plays a crucial role in H 2 S removal from the biogas. Copyright © 2017 Elsevier Ltd. All rights reserved.

Antimicrobial, antioxidant, and waterproof RTV silicone-ethyl cellulose composites containing clove essential oil.

PubMed

Heredia-Guerrero, José A; Ceseracciu, Luca; Guzman-Puyol, Susana; Paul, Uttam C; Alfaro-Pulido, Alejandro; Grande, Chiara; Vezzulli, Luigi; Bandiera, Tiziano; Bertorelli, Rosalia; Russo, Debora; Athanassiou, Athanassia; Bayer, Ilker S

2018-07-15

Ethyl cellulose (EC)/polydimethylsiloxane (PDMS) composite films were prepared at various concentrations of PDMS in the films (0, 5, 10, 15, and 20 wt.%). Morphological and chemical analysis by EDX-SEM and ATR-FTIR showed that EC-rich matrices and PDMS-rich particles were formed, with the two polymers interacting through Hbonds. The number and diameter of particles in the composite depended on the PDMS content and allowed a fine tuning of several properties such as opacity, hydrophobicity, water uptake, and water permeability. Relative low amounts of clove essential oil were also added to the most waterproof composite material (80 wt.% ethyl cellulose and 20 wt.% PDMS). The essential oil increased the flexibility and the antioxidant capacity of the composite. Finally, the antimicrobial properties were tested against common pathogens such as Escherichia coli, Staphylococcus aureus and Pseudomonas aeruginosa. The presence of clove essential oil reduced the biofilm formation on the composites. Copyright © 2018 Elsevier Ltd. All rights reserved.

Photocatalytic application of Pd-ZnO-exfoliated graphite nanocomposite for the enhanced removal of acid orange 7 dye in water

NASA Astrophysics Data System (ADS)

Umukoro, Eseoghene H.; Madyibi, Siposetu S.; Peleyeju, Moses G.; Tshwenya, Luthando; Viljoen, Elvera H.; Ngila, Jane C.; Arotiba, Omotayo A.

2017-12-01

In this work, a nanocomposite photocatalyst which consists of palladium (Pd), zinc oxide (ZnO) as well as exfoliated graphite (EG) was synthesised, characterised and applied to the removal of acid orange 7 dye as a model organic pollutant. The Pd-ZnO-EG nanocomposite was synthesised by a one-pot hydrothermal technique in a Teflon-lined stainless steel autoclave at 160 °C for a period of 12 h, cooled, washed and dried. The nanocomposite was characterised by X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), scanning electronic microscopy (SEM) as well as energy dispersive X-ray spectrometry (EDX). The as-prepared materials were further applied for the degradation of acid orange 7 dye photocatalytically. Results obtained showed that Pd-ZnO-EG composite displayed a better photocatalytic performance, giving better removal efficiency of 87% in comparison with ZnO and Pd-ZnO which gave 3 and 25% percentage removal respectively.

Organic-inorganic hybrid polyionic liquid based polyoxometalate as nano porous material for selective oxidation of sulfides

NASA Astrophysics Data System (ADS)

Rafiee, Ezzat; Shahebrahimi, Shabnam

2017-07-01

Organic-inorganic hybrid nano porous materials based on poly(ionic liquid)-polyoxometalate (PIL-POM) were reported. These hybrid materials were synthesized by the reaction of 4-vinyl pyridine with 1,3-propanesultone, followed by the polymerization and also sulfonate-functionalized cross-linked poly(4-vinylpyridine) and combining these polymers with H5PMo10V2O40 (PMo10V2). Activity of prepared PIL-PMo10V2 hybrids were investigated as catalysts for oxidation of sulfides with H2O2 as oxidant. For understanding catalytic activities of the PIL-PMo10V2 hybrids in oxidation of sulfides, effect of catalyst composition, substrate, and reaction conditions were studied. The results show that the PIL-PMo10V2 hybrids are active as selective heterogeneous catalysts for oxidation of sulfides and can be recovered and reused. The catalyst was characterized by FT-IR, TGA-DSC, XRD, SEM/EDX, BET, CV and zeta potential measurement. Also, average molecular weight of prepared catalysts were measured.

Amine-functionalized mesoporous ZSM-5 zeolite adsorbents for carbon dioxide capture

NASA Astrophysics Data System (ADS)

Wang, Yisong; Du, Tao; Song, Yanli; Che, Shuai; Fang, Xin; Zhou, Lifeng

2017-11-01

ZSM-5 type zeolite with mesoporous structure was prepared and then amine-functionalized with tetraethylenepentamine (TEPA) by wet impregnation method to form a series of CO2 adsorbents (ZTx). The structural properties of ZSM-5 and ZTx were characterized by XRD, FTIR, TGA/DTG, nitrogen adsorption/desorption, SEM and EDX techniques. The adsorption capacity of the adsorbents with different amine loading was measured at a temperature from 40 to 100 °C and the adsorption capacity of ZT7 was 1.80 mmol/g at 100 °C. The adsorption process and mechanism were studied by fitting the experimental data used the three adsorption kinetic models, and a complex physical and chemical mixing process was produced as the amine entered the surface and pore size of the zeolite. The high adsorption selectivity at 10% CO2 concentration and the stability of the five adsorption desorption cycles indicated that ZT7 is a suitable and promising CO2 adsorbent for the purification of industrial flue gas.

Effects of a novel poly (AA-co-AAm)/AlZnFe₂O₄/potassium humate superabsorbent hydrogel nanocomposite on water retention of sandy loam soil and wheat seedling growth.

PubMed

Shahid, Shaukat Ali; Qidwai, Ansar Ahmad; Anwar, Farooq; Ullah, Inam; Rashid, Umer

2012-10-25

A novel poly(acrylic acid-co-acrylamide)AlZnFe₂O₄/potassium humate( )superabsorbent hydrogel nanocomposite (PHNC) was synthesized and its physical properties characterized using SEM, Energy Dispersive X-ray (EDX) and FTIR spectroscopic techniques. Air dried sandy loam soil was amended with 0.1 to 0.4 w/w% of PHNC to evaluate its soil moisture retention attributes. Effect of PHNC amendment on pH, electrical conductivity (EC), porosity, bulk density and hydraulic conductivity of sandy loam soil was also studied. The soil amendment with 0.1 to 0.4 w/w% of PHNC remarkably enhanced the moisture retention at field capacity as compared to the un-amended soils. Seed germination and seedling growth of wheat (Triticum aestivum L.) was considerably increased and a delay by 6-9 days in wilting of seedlings was observed in the soil amended with PHNC, resulting in improved wheat plant establishment and growth.

Functional lignocellulosic materials prepared by ATRP from a wood scaffold

PubMed Central

Cabane, Etienne; Keplinger, Tobias; Künniger, Tina; Merk, Vivian; Burgert, Ingo

2016-01-01

Wood, a natural and abundant source of organic polymers, has been used as a scaffold to develop novel wood-polymer hybrid materials. Through a two-step surface-initiated Atom Transfer Radical Polymerization (ATRP), the porous wood structure can be effectively modified with polymer chains of various nature. In the present study, polystyrene and poly(N-isopropylacrylamide) were used. As shown with various characterization techniques including confocal Raman microscopy, FTIR, and SEM/EDX, the native wood ultrastructure and features are retained and the polymer chains can be introduced deep within the wood, i.e. inside the wood cell walls. The physical properties of the new materials have been studied, and results indicate that the insertion of polymer chains inside the wood cell wall alters the intrinsic properties of wood to yield a hybrid composite material with new functionalities. This approach to the functionalization of wood could lead to the fabrication of a new class of interesting functional materials and promote innovative utilizations of the renewable resource wood. PMID:27506369

A Study of influence on sulfonated TiO2-Poly (Vinylidene fluoride-co-hexafluoropropylene) nano composite membranes for PEM Fuel cell application

NASA Astrophysics Data System (ADS)

kumar, K. Selva; Rajendran, S.; Prabhu, M. Ramesh

2017-10-01

The present work describes the sulfonated Titania directly blended with Poly (Vinylidene fluoride-co-hexafluoropropylene) as a host polymer by solvent casting technique for PEM fuel cell application. Characterization studies such as FT-IR, SEM, EDX, AFM, Proton conductivity, contact angle measurement, IEC, TG, water uptake, tensile strength were performed by for synthesized proton conducting polymer electrolytes. The maximum proton conductivity value was found to be 3.6 × 10-3S/cm for 25 wt% sulfonated Titania based system at 80 °C. The temperature dependent proton conductivity of the polymer electrolyte follows an Arrhenius relationship. Surface morphology of the composite membranes was investigated by tapping mode. Thermal stability of the system was studied by TG analysis. The fabricated composite membranes with high proton conductivity, good water uptake and IEC parameters exhibited a maximum fuel cell power density of 85 Mw/cm2for PEM fuel cell application.

Self-assembled structures of hydroxyapatite in the biomimetic coating on a bioinert ceramic substrate.

PubMed

Chakraborty, Jui; Sarkar, Soumi Dey; Chatterjee, Saradiya; Sinha, Mithlesh Kumar; Basu, Debabrata

2008-10-15

The tribological properties of alumina ceramic are excellent due in part to a high wettability because of the hydrophilic surface and fluid film lubrication that minimizes the adhesive wear. Such surfaces are further modified with bioactive glass/ceramic coating to promote direct bone apposition in orthopedic applications. The present communication reports the biomimetic coating of calcium hydroxyapatite (HAp) on dense (2-3% porosity) alumina (alpha-Al(2)O(3)) substrate (1cm x 1cm x 0.5 cm), at 37 degrees C. After a total period of 6 days immersion in simulated body fluid (SBF), at 37 degrees C, linear self-assembled porous (pore size: approximately 0.2 microm) structures (length: approximately 375.39 microm and width: 5-6 microm) of HAp were obtained. The phenomenon has been demonstrated by self-assembly and diffusion-limited aggregation (DLA) principles. Structural and compositional characterization of the coating was carried out using SEM with EDX facility, XRD and FT-IR data.

Novel symmetrical coralloid Cu 3D superstructures: Solid-state synthesis from a Cu-carboxylate MOF and their in-situ thermal conversion

NASA Astrophysics Data System (ADS)

Chen, Lingyun; Shen, Yongming; Bai, Junfeng; Wang, Chunzhao

2009-08-01

We describe here a one-step solid-state process for the synthesis of metal three-dimensional (3D) superstructures from a metal-organic framework (MOF). Novel symmetrical coralloid Cu 3D superstructures with surface interspersed with clusters of Cu nanoparticles were successfully synthesized by thermolysis of the [Cu 3( btc) 2] ( btc=benzene-1,3,5-tricarboxylato) MOF in a one-end closed horizontal tube furnace (OCTF). The obtained products were characterized by TGA, FT-IR, XRD, EDX, SEM, TEM, HRTEM and SAED. Different reaction conditions were discussed. Furthermore, the synthesized Cu samples were converted into CuO microstructures by in-situ calcination in the air. In addition, the possible formation mechanism was also proposed. This method is a simple and facile route, which builds a direct linkage between metal-carboxylate MOF crystals and metal nano- or microstructures and also opens a new application field of MOFs.

Mg-Enriched Engineered Carbon from Lithium-Ion Battery Anode for Phosphate Removal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Yan; Guo, Xingming; Yao, Ying

2016-02-10

Three Mg-enriched engineered carbons (mesocarbon microbeads, MCMB) were produced from lithium-ion battery anode using concentrated nitric acid oxidization and magnesium nitrate pretreatment. The obtained 15%Mg-MCMB, 30%Mg-MCMB, and 40%Mg-MCMB have magnesium level of 10.19, 19.13, and 19.96%, respectively. FTIR spectrum shows the functional groups present on the oxidized MCMB including OH, C=O, C–H, and C–O. XRD, SEM-EDX, and XPS analyses show that nanoscale Mg(OH) 2 and MgO particles were presented on the surface of the Mg-MCMB samples, which could serve as the main adsorption mechanism as to precipitate phosphate from aqueous solutions. The sorption experiments indicate that Mg modification dramatically promotesmore » MCMB’s phosphate removal ability and phosphate removal rates reach as high as 95%. Thus, modification of the spent LIBs anode could provide a novel direction of preparing wastewater adsorbent and develop an innovative way to achieve sustainable development.« less

Synthesis and characterization of mangenese(III) porphyrin supported on imidazole modified chloromethylated MIL-101(Cr): A heterogeneous and reusable catalyst for oxidation of hydrocarbons with sodium periodate

NASA Astrophysics Data System (ADS)

Zadehahmadi, Farnaz; Tangestaninejad, Shahram; Moghadam, Majid; Mirkhani, Valiollah; Mohammadpoor-Baltork, Iraj; Khosropour, Ahmad R.; Kardanpour, Reihaneh

2014-10-01

In the present work, chloromethylated MIL-101(Cr) modified with imidazole, Im-MIL-101, was applied as a support for immobilizing of tetraphenylporphyrinatomangenese(III) chloride. The imidazole-bound MIL-101, Im-MIL-101, not only used as support for immobilization of manganese porphyrin but also applied as a heterogeneous axial base. The Mn(TPP)Cl@Im-MIL-101 catalyst was characterized by UV-vis, FT-IR, X-ray diffraction (XRD), N2 adsorption, field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray (EDX), elemental analysis and inductively coupled plasma (ICP) methods. The catalytic activity of this new catalytic system was investigated in the alkene epoxidation and alkane hydroxylation using NaIO4 as an oxidant in CH3CN/H2O at room temperature. This heterogeneous catalyst is highly efficient, stable and reusable in the oxidation of hydrocarbons.

Two fold modified chitosan for enhanced adsorption of hexavalent chromium from simulated wastewater and industrial effluents.

PubMed

Kahu, S S; Shekhawat, A; Saravanan, D; Jugade, R M

2016-08-01

Ionic solid (Ethylhexadecyldimethylammoniumbromide) impregnated phosphated chitosan (ISPC) was synthesized and applied for enhanced adsorption of hexavalent chromium from industrial effluent. The compound obtained was extensively characterized using instrumental techniques like FT-IR, TGA-DTA, XRD, SEM, BET and EDX. ISPC showed high adsorption capacity of 266.67mg/g in accordance with Langmuir isotherm model at pH 3.0 due to the presence of multiple sites which contribute for ion pair and electrostatic interactions with Cr(VI) species. The sorption kinetics and thermodynamic studies revealed that adsorption of Cr(VI) followed pseudo-second-order kinetics with exothermic and spontaneous behaviour. Applicability of ISPC for higher sample volumes was discerned through column studies. The real chrome plating industry effluent was effectively treated with total chromium recovery of 94%. The used ISPC was regenerated simply by dilute ammonium hydroxide treatment and tested for ten adsorption-desorption cycles with marginal decrease in adsorption efficiency. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis, characteristics and antimicrobial activity of ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Janaki, A. Chinnammal; Sailatha, E.; Gunasekaran, S.

2015-06-01

The utilization of various plant resources for the bio synthesis of metallic nano particles is called green technology and it does not utilize any harmful protocols. Present study focuses on the green synthesis of ZnO nano particles by Zinc Carbonate and utilizing the bio-components of powder extract of dry ginger rhizome (Zingiber officinale). The ZnO nano crystallites of average size range of 23-26 nm have been synthesized by rapid, simple and eco friendly method. Zinc oxide nano particles were characterized by using X-ray diffraction (XRD), Scanning Electron Microscope (SEM), Energy Dispersive X-ray spectroscopy (EDX). FTIR spectra confirmed the adsorption of surfactant molecules at the surface of ZnO nanoparticles and the presence of ZnO bonding. Antimicrobial activity of ZnO nano particles was done by well diffusion method against pathogenic organisms like Klebsiella pneumonia, Staphylococcus aureus and Candida albicans and Penicillium notatum. It is observed that the ZnO synthesized in the process has the efficient antimicrobial activity.

Developing bioactive composite scaffolds for bone tissue engineering

NASA Astrophysics Data System (ADS)

Chen, Yun

Poly(L-lactic acid) (PLLA) films were fabricated using the method of dissolving and evaporation. PLLA scaffold was prepared by solid-liquid phase separation of polymer solutions and subsequent sublimation of solvent. Bonelike apatite coating was formed on PLLA films, PLLA scaffolds and poly(glycolic acid) (PGA) scaffolds in 24 hours through an accelerated biomimetic process. The ion concentrations in the simulated body fluid (SBF) were nearly 5 times of those in human blood plasma. The apatite formed was characterized using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). The apatite formed in 5SBF was similar in morphology and composition to that formed in the classical biomimetic process employing SBF or 1.5SBF, and similar to that of natural bone. This indicated that the biomimetic apatite coating process could be accelerated by using concentrated simulated body fluid at 37°C. Besides saving time, the accelerated biomimetic process is particularly significant to biodegradable polymers. Some polymers which degrade too fast to be coated with apatite by a classical biomimetic process, for example PGA, could be coated with bone-like apatite in an accelerated biomimetic process. Collagen and apatite were co-precipitated as a composite coating on poly(L-lactic acid) (PLLA) in an accelerated biomimetic process. The incubation solution contained collagen (1g/L) and simulated body fluid (SBF) with 5 times inorganic ionic concentrations as human blood plasma. The coating formed on PLLA films and scaffolds after 24 hours incubation was characterized using EDX, XRD, FTIR, and SEM. It was shown that the coating contained carbonated bone-like apatite and collagen, the primary constituents of natural bone. SEM showed a complex composite coating of submicron bone-like apatite particulates combined with collagen fibrils. This work provided an efficient process to obtain bone-like apatite/collagen composite coating. Saos-2 osteoblast-like cells were used to evaluate the cellular behaviors on these biomimetic coatings. Cell morphologies on the surfaces of PLLA films and scaffolds, PLLA films and scaffolds with apatite coating, and PLLA films and scaffolds with apatite/collagen composite coating were studied by SEM. Cell viability was assessed by the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrasodium bromide (MTT) assay. In addition, differentiated cell function was assessed by measuring alkaline phosphatase activity. These results suggested that the apatite coating and apatite/collagen composite coating fabricated through the accelerated biomimetic processes could improve the interactions between osteoblasts and PLLA. The composite coating was more effective than apatite coating in improving such interactions. PLLA scaffolds coated with submicron collagen fibrils and submicron apatite paticulates are expected to be one of the promising 3D substrates for bone tissue engineering. To facilitate coating into scaffolds, the flowing condition was introduced into the accelerated biomimetic process. The apatite formed in the different sites in the scaffold was characterized using SEM. It was found that the accelerated biomimetic process performed in the flowing condition yielded more uniform spatial distribution of apatite particles than that in the regular shaking condition. This work provides a novel condition for obtaining uniform spatial distribution of bone-like apatite within the scaffolds in a timely manner, which is expected to facilitate uniform distribution of attached cells within the scaffoldsin vitro and in vivo.

Structural and spectral properties of undoped and tungsten doped Zn3(PO4)2ZnO nanopowders

NASA Astrophysics Data System (ADS)

Satyavathi, K.; Subba Rao, M.; Nagabhaskararao, Y.; Cole, Sandhya

2018-01-01

Pure and tungsten doped Zn3(PO4)2ZnO nanopowders (NPs) are prepared using sol-gel method. It has the longest track record of used in dentistry. It is used for cementation of inlays, crowns and orthodontic appliances. The systematic investigations like X-ray Diffraction (XRD), Scanning electron microscope (SEM) with energy dispersive X-ray (EDX) spectroscope, Transmission electron microscope (TEM), Fourier transform infrared (FT-IR) spectroscopy, Optical absorption, Photoluminescence (PL) and Electron Paramagnetic Resonance (EPR) spectroscopic techniques are carried out for the prepared NPs. XRD pattern reveals that the prepared samples are in crystalline nature in which Zn3(PO4)2 corresponding to monoclinic phase and ZnO corresponding to hexagonal wurtzite phase, the average crystallite size of prepared nanopowders is in the range of 20-30 nm. The lattice strain, lattice cell parameters, unit cell volume and dislocation density of the prepared NPs are also calculated. The morphology of the prepared NPs is analyzed with SEM and TEM images. The distribution of Zn, P, O and W species in the prepared samples are identified by the chemical composition mapping through EDX. IR spectra of prepared samples exhibit the characteristic sharp absorption band peaks. The sharp absorption bands observed in the region 1200-900 cm-1 are due to complex stretching of characteristic PO43- groups. The absorption spectra exhibit a broad band around 696 nm is recognized due to 2B2g → 2B1g (dxy → dx2- y2) transition of tungsten ions. The PL spectra exhibit four emission peaks in the visible region indicating the quantum-confinement-induced photoluminescence. The CIE chromaticity diagram suggests that the prepared NPs have good color purity. The EPR spectra indicate that the W5+ ions occupy octahedral site symmetry in the host lattice.

In-vitro subsurface remineralisation of artificial enamel white spot lesions pre-treated with chitosan.

PubMed

Zhang, Jing; Boyes, Victoria; Festy, Frederic; Lynch, Richard J M; Watson, Timothy F; Banerjee, Avijit

2018-05-08

To test the null hypothesis that chitosan application has no impact on the remineralisation of artificial incipient enamel white spot lesions (WSLs). 66 artificial enamel WSLs were assigned to 6 experimental groups (n=11): (1) bioactive glass slurry, (2) bioactive glass containing polyacrylic acid (BG+PAA) slurry, (3) chitosan pre-treated WSLs with BG slurry (CS-BG), (4) chitosan pre-treated WSLs with BG+PAA slurry (CS-BG+PAA), (5) remineralisation solution (RS) and (6) de-ionised water (negative control, NC). Surface and cross-sectional Raman intensity mapping (960cm -1 ) were performed on 5 samples/group to assess mineral content. Raman spectroscopy and attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) were used to identify the type of newly formed minerals. Surface and cross-sectional Knoop microhardness were implemented to evaluate the mechanical properties after remineralisation. Surface morphologies and Ca/P ratio were observed using scanning electron microscopy (SEM) coupled with energy dispersive X-ray spectroscopy (EDX). Data were statistically analysed using one-way ANOVA with Tukey's test. BG+PAA, CS-BG, RS presented significantly higher mineral regain compared to NC on lesion surfaces, while CS-BG+PAA had higher subsurface mineral content. Newly mineralised crystals consist of type-B hydroxycarbonate apatite. CS-BG+PAA showed the greatest hardness recovery, followed by CS-BG, both significantly higher than other groups. SEM observations showed altered surface morphologies in all experimental groups except NC post-treatment. EDX suggested a higher content of carbon, oxygen and silicon in the precipitations in CS-BG+PAA group. There was no significant difference between each group in terms of Ca/P ratio. The null hypothesis was rejected. Chitosan pre-treatment enhanced WSL remineralisation with either BG only or with BG-PAA complexes. A further investigation using dynamic remineralisation/demineralisation system is required with regards to clinical application. Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.

[Revisiting the chemical diversity in prostatic calculi: a SEM and FT-IR investigation].

PubMed

Dessombz, A; Méria, P; Bazin, D; Foy, E; Rouzière, S; Weil, R; Daudon, M

2011-12-01

Revisiting the chemical diversity of the crystalline phases of prostatic calculi by means of SEM and FT-IR analysis. A set of 32 prostatic calculi has been studied by FT-IR and SEM. FT-IR analysis has determined the chemical composition of each prostatic calculus and the SEM observation has described the morphology of the calculi surfaces and layers. Infrared analysis revealed that 90.7% of the stones were mainly composed of calcium phosphates. However, several mineral phases previously not reported in prostatic calculi were observed, as brushite or octocalcium phosphate pentahydrate. Prostatic calculi exhibited a diversity of crystalline composition and morphology. As previously reported for urinary calculi, relationships between composition and morphology of prostatic stones and étiopathogenic conditions could be of interest in clinical practice. Copyright © 2011 Elsevier Masson SAS. All rights reserved.

A Potential Waste to be Selected as Media for Metal and Nutrient Removal

NASA Astrophysics Data System (ADS)

Zayadi, N.; Othman, N.; Hamdan, R.

2016-07-01

This study describes the potential of application of cassava peel, banana peel, coconut shell, and coconut coir to be selected as metal removal while limestone and steel slag for nutrient removal. The media were characterized by X-Ray Fluorescence (XRF), Fourier Transform Infrared (FTIR), Field Emission Scanning Electron Microscopy-Energy Dispersive X-Ray (FESEM-EDX), and X-Ray Powder Diffraction (XRD). The results of XRF analysis medias show the present of calcium oxide, CaO which confirm the high efficiency in adsorbing metal ions and nutrient which is in agreement with the result of XRD. The characteristics of medias by FTIR analysis also confirmed the involvement of alcohol, carboxylic, alkanes, amines and ethers which play important role to reduce ions while FESEM-EDX indicates the porous structures of study medias. The characterization analysis highlight that cassava peel and steel slag were selected as a potential media in this study.

The effect of concentration ratio and type of functional group on synthesis of CNT-ZnO hybrid nanomaterial by an in situ sol-gel process

NASA Astrophysics Data System (ADS)

Hosseini Largani, Sekineh; Akbarzadeh Pasha, Mohammad

2017-12-01

In this research, MWCNT-ZnO hybrid nanomaterials were synthesized by a simple sol-gel process using Zn(CH3COO)2·2H2O and functionalized MWCNT with carboxyl(COOH) and hydroxyl(OH) groups. Three different mass ratios of MWCNT:ZnO = 3:1, 1:1 and 1:3 were examined. The prepared nanomaterials were characterized by field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX) and Fourier transform infrared spectroscopy (FTIR). Successful growth of MWCNT-ZnO hybrids for both COOH and OH functional groups and all the three mass ratios were obtained. The ZnO nanoparticles attached on the surfaces of CNTs have rather spherical shapes and hexagonal crystal structure. By increasing the concentration of ZnO, the number and average size of ZnO nanoparticles decorated the body of CNTs in hybrid structures increase. By increasing the ZnO precursor, the distribution of ZnO nanoparticles that appeared on the surface of CNTs becomes more uniform. The SEM observation beside EDX analysis revealed that at the same concentration ratio the amount of ZnO loading on the surface of MWCNT-COOH is more than MWCNT-OH. Moreover, the average size of ZnO nanoparticles attached on the surface of COOH functionalized CNTs is relatively smaller than that of OH functionalized ones.

In vitro characterisation of a sol-gel derived in situ silica-coated silicate and carbonate co-doped hydroxyapatite nanopowder for bone grafting.

PubMed

Latifi, Seyed Mohsen; Fathi, Mohammadhossein; Sharifnabi, Ali; Varshosaz, Jaleh

2017-06-01

Design and synthesis of materials with better properties and performance are essential requirements in the field of biomaterials science that would directly improve patient quality of life. For this purpose, in situ silica-coated silicate and carbonate co-doped hydroxyapatite (Sc/S.C.HA) nanopowder was synthesized via the sol-gel method. Characterisation of the prepared nanopowder was carried out by XRD, FTIR, TEM, SEM, EDX, ICP, zeta potential, acid dissolution test, and cell culture test. The substitution of the silicate and carbonate ions into hydroxyapatite structure was confirmed by FTIR analysis. XRD analysis showed that silica is an amorphous phase, which played a role in covering the surface of the S.C.HA nanoparticles as confirmed by acid dissolution test. Low thickness and low integrity of the amorphous silica surface layer facilitated ions release from S.C.HA nanoparticles into physiological saline solution. Zeta potential of the prepared nanopowder suspended in physiological saline solution was -27.3±0.2mV at pH7.4. This negatively charged surface, due to the presence of amorphous silica layer upon the S.C.HA nanoparticles, not only had an accelerating effect on in vitro biomineralization of apatite, but also had a positive effect on cell attachment. Copyright © 2017 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Marliana, Ana, E-mail: na-cwith22@yahoo.co.id; Fitriani, Eka; Ramadhan, Fauzan

Waste fish bones is a problem stemming from activities in the field of fisheries and it has not been used optimally. Fish bones contain calcium as natural source that used to synthesize hydroxyapatite (HA). In this research, HA synthesized from waste fish bones as local wisdom in Semarang. The goal are to produce HA with cheaper production costs and to reduce the environmental problems caused by waste bones. The novelty of this study was using of local fish bone as a source of calcium and simple method of synthesis. Synthesis process of HA can be done through a maceration processmore » with firing temperatures of 1000°C or followed by a sol-gel method with firing at 550°C. The results are analyzed using FTIR (Fourier Transform Infrared), XRD (X-Ray Diffraction) and SEM-EDX (Scanning Electron Microscopy-Energy Dispersive X-Ray). FTIR spectra showed absorption of phosphate and OH group belonging to HA as evidenced by the results of XRD. The average grain size by maceration and synthesized results are not significant different, which is about 69 nm. The ratio of Ca/P of HA by maceration result is 0.89, then increase after continued in the sol-gel process to 1.41. Morphology of HA by maceration results are regular and uniform particle growth, while the morphology of HA after the sol-gel process are irregular and agglomerated.« less

Interaction of Pb(II) and biofilm associated extracellular polymeric substances of a marine bacterium Pseudomonas pseudoalcaligenes NP103

NASA Astrophysics Data System (ADS)

Kumari, Supriya; Mangwani, Neelam; Das, Surajit

2017-02-01

Three-dimensional excitation-emission matrix (3D EEM) fluorescence spectroscopy and attenuated total reflectance fourier-transformed infrared spectroscopy (ATR-FTIR) was used to evaluate the interaction of biofilm associated extracellular polymeric substances (EPS) of a marine bacterium Pseudomonas pseudoalcaligenes NP103 with lead [Pb(II)]. EEM fluorescence spectroscopic analysis revealed the presence of one protein-like fluorophore in the EPS of P. pseudoalcaligenes NP103. Stern-Volmer equation indicated the existence of only one binding site (n = 0.789) in the EPS of P. pseudoalcaligenes NP103. The interaction of Pb(II) with EPS was spontaneous at room temperature (Δ G = - 2.78 kJ/K/mol) having binding constant (Kb) of 2.59 M- 1. ATR-FTIR analysis asserted the involvement of various functional groups such as sulphydryl, phosphate and hydroxyl and amide groups of protein in Pb(II) binding. Scanning electron microscopy (SEM) and fluorescence microscopy analysis displayed reduced growth of biofilm with altered surface topology in Pb(II) supplemented medium. Energy dispersive X-ray spectroscopy (EDX) analysis revealed the entrapment of Pb in the EPS. Uronic acid, a characteristic functional group of biofilm, was observed in 1H NMR spectroscopy. The findings suggest that biofilm associated EPS are perfect organic ligands for Pb(II) complexation and may significantly augment the bioavailability of Pb(II) in the metal contaminated environment for subsequent sequestration.

Monodispersed spherical shaped selenium nanoparticles (SeNPs) synthesized by Bacillus subtilis and its toxicity evaluation in zebrafish embryos

NASA Astrophysics Data System (ADS)

Chandramohan, Subburaman; Sundar, Krishnan; Muthukumaran, Azhaguchamy

2018-02-01

Selenium is one of the essential elements involved in antioxidative and antiinflammatory effects in human body. By naturally, selenium ions are metabolised and converted into nano selenium. Now a days there is an increasing attention on applications of nanoparticles in therapeutic field. In the present study Bacillus subtilis was used to convert sodium selenite to SeNPs. The synthesized SeNPs were characterized by Fourier Transform Infrared Spectroscopy (FTIR), X Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM) coupled with Energy Dispersive X ray spectroscopy (EDX). The presence of SeNPs was confirmed by the formation of red colour. The bands were sharp with broad absorption peaks at 3562 cm-1 and 1678-1 cm in FTIR which showed that the bacterial proteins were responsible for the reduction of sodium selenite to SeNPs. The average size of the SeNPs was 334 nm and were spherical in shape with uniform distribution. The XRD data confirmed that SeNPs were of amorphous in nature. The zeta potential of SeNPs was negative in charge which indicated high stability. In the present study zebrafish embryos were used to study the toxicity of SeNPs and the results showed that the concentration beyond 10 μg ml-1 leads to toxic effects in embryos/hatchlings. The lesser concentration of SeNPs can be useful in various biomedical applications.

[Imprints of coronary plaque particles in the PTCA balloon surface during the dilatation processing].

PubMed

Werner, D; Behrend, D; Schmitz, K P; Urbaszek, W

1995-05-01

Seventy-six PTCA-balloons after coronary angioplasty were studied for superficial changes using scanning electron microscopy (SEM) after fixing in glutardialdehyde. Coronary plaque particles were identified on the balloon surface in 52 cases (68%). Twelve new and unused balloons were subjected to the same chemical treatment and SEM showed no imprints. The average length of the longest imprinted plaques was 128 +/- 201 microns and the average number of plaque particles per balloon was 4.9 +/- 2.7. The maximal dilatation pressure and the number of dilatations showed no influence on the impregnation of plaque particles. However, longer plaque imprints tended to occur under low dilatation pressure. Imprints of plaque particles were significantly higher in patients with low cholesterol (p = 0.0001) and low triglycerides (p = 0.0016). No correlation was seen between imprint length and lipid levels. Similarly, the different balloon materials (polyethylene, polyolefincopolymer) showed no significant differences with regard to plaque occurrence. The PTCA-balloons, plaque particles and six coronary plaques obtained after endatherectomy were subjected to energy dispersive x-ray analysis (EDX) under SEM as EDX reveals qualitative and quantitative information about the structural elements. Highly significant differences in calcium, sodium, phosphorus and silicon contents (p = 0.0000) between plaque particles and balloon surface were observed, owing to the absence of these in balloon material. Thus EDX offers additional advantages over SEM in that it clearly differentiates deformed balloon surface, plaque particle, and retained contrast medium. Plaque particles can be recovered from balloon surfaces after PTCA. Depending upon their size, they could lead to coronary spasm or microembolic phenomenon.

Identification of possible sources of particulate matter in the personal cloud using SEM/EDX

NASA Astrophysics Data System (ADS)

Conner, Teri L.; Williams, Ronald W.

2004-10-01

The United States Environmental Protection Agency (US EPA) conducted the Baltimore Particulate Matter (PM) Epidemiology-Exposure Study of the Elderly during the summer of 1998. The study design included PM2.5 samples obtained from elderly (65+ years of age) retirement facility residents using personal exposure sampling devices. These sampling devices were also used to obtain PM2.5 samples at fixed locations within the personal monitoring subjects' apartments. Selected personal and apartment samples were examined using scanning electron microscopy with individual-particle X-ray analysis (SEM/EDX), providing a qualitative assessment of the chemical and physical characteristics of geological and trace element particles collected within these micro-environments at the retirement facility. This information was used to identify possible indoor source particles. The manual surveys of the personal samples revealed that some particles larger than 2.5 μm reached the filter surface. Using SEM/EDX, several particle types with possible indoor origins were identified. The Al-Zr-Cl particle is likely to have originated from a personal antiperspirant product. Particles with a talc or alumino-silicate composition point to cosmetics as a possible source. Large cadmium-containing particles were also found, which may indicate the use of art pigments or ceramic glazes, or emissions from television screen phosphors. A greater variety of particles was observed in a personal sample compared with its corresponding fixed-location apartment sample.

Synthesis, characterization and catalytic activity of indium substituted nanocrystalline Mobil Five (MFI) zeolite

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shah, Kishor Kr.; Nandi, Mithun; Talukdar, Anup K., E-mail: anup_t@sify.com

2015-06-15

Highlights: • In situ modification of the MFI zeolite by incorporation of indium. • The samples were characterized by XRD, FTIR, TGA, UV–vis (DRS), SAA, EDX and SEM. • The incorporation of indium was confirmed by XRD, FT-IR, UV–vis (DRS), EDX and TGA. • Hydroxylation of phenol reaction was studied on the synthesized catalysts. - Abstract: A series of indium doped Mobil Five (MFI) zeolite were synthesized hydrothermally with silicon to aluminium and indium molar ratio of 100 and with aluminium to indium molar ratios of 1:1, 2:1 and 3:1. The MFI zeolite phase was identified by XRD and FT-IRmore » analysis. In XRD analysis the prominent peaks were observed at 2θ values of around 6.5° and 23° with a few additional shoulder peaks in case of all the indium incorporated samples suggesting formation of pure phase of the MFI zeolite. All the samples under the present investigation were found to exhibit high crystallinity (∼92%). The crystallite sizes of the samples were found to vary from about 49 to 55 nm. IR results confirmed the formation of MFI zeolite in all cases showing distinct absorbance bands near 1080, 790, 540, 450 and 990 cm{sup −1}. TG analysis of In-MFI zeolites showed mass losses in three different steps which are attributed to the loss due to adsorbed water molecules and the two types TPA{sup +} cations. Further, the UV–vis (DRS) studies reflected the position of the indium metal in the zeolite framework. Surface area analysis of the synthesized samples was carried out to characterize the synthesized samples The analysis showed that the specific surface area ranged from ∼357 to ∼361 m{sup 2} g{sup −1} and the pore volume of the synthesized samples ranged from 0.177 to 0.182 cm{sup 3} g{sup −1}. The scanning electron microscopy studies showed the structure of the samples to be rectangular and twinned rectangular shaped. The EDX analysis was carried out for confirmation of Si, Al and In in zeolite frame work. The catalytic activities of the synthesized samples were investigated with respect to hydroxylation of phenol, in which catechol and hydroquinone were found to be the major products. It is observed that under all reaction conditions catechol selectivity was higher than the hydroquinone selectivity. In-MFI zeolites were successfully synthesized and were used as an effective catalyst for the hydroxylation of phenol to synthesize catechol and hydroquinone as the major product.« less

Characterization of Chlorhexidine-Loaded Calcium-Hydroxide Microparticles as a Potential Dental Pulp-Capping Material.

PubMed

Priyadarshini, Balasankar M; Selvan, Subramanian T; Narayanan, Karthikeyan; Fawzy, Amr S

2017-06-22

This study explores the delivery of novel calcium hydroxide [Ca(OH)₂] microparticles loaded with chlorhexidine (CHX) for potential dental therapeutic and preventive applications. Herein, we introduce a new approach for drug-delivery to deep dentin-surfaces in the form of drug-loaded microparticles. Unloaded Ca(OH)₂ [Ca(OH)₂/Blank] and CHX-loaded/Ca(OH)₂ microparticles were fabricated by aqueous chemical-precipitation technique. The synthesized-microparticles were characterized in vitro for determination of surface-morphology, crystalline-features and thermal-properties examined by energy-dispersive X-ray scanning and transmission electron-microscopy (EDX-SEM/TEM), Fourier-transform infrared-spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA) and differential scanning-calorimetry (DSC). Time-related pH changes, initial antibacterial/biofilm-abilities and cytotoxicity of CHX-loaded/Ca(OH)₂ microparticles were evaluated. Microparticles were delivered to dentin-surfaces with subsequent SEM examination of treated dentin-substrates. The in vitro and ex vivo CHX-release profiles were characterized. Ca(OH)₂/Blank were hexagonal-shaped with highest z -average diameter whereas CHX-inclusion evidenced micro-metric spheres with distinguishable surface "rounded deposits" and a negative-shift in diameter. CHX:Ca(OH)₂/50 mg exhibited maximum encapsulation-efficiency with good antibacterial and cytocompatible properties. SEM examination revealed an intact layer of microparticles on exposed dentin-surfaces with retention of spherical shape and smooth texture. Microparticles loaded on dentin-surfaces showed prolonged release of CHX indicating substantial retention on dentin-substrates. This study validated the inherent-applicability of this novel drug-delivery approach to dentin-surfaces using micro-metric CHX-loaded/Ca(OH)₂ microparticles.

Evaluation of poly (vinyl alcohol) based cryogel-zinc oxide nanocomposites for possible applications as wound dressing materials.

PubMed

Chaturvedi, Archana; Bajpai, Anil K; Bajpai, Jaya; K Singh, Sunil

2016-08-01

In this investigation cryogels composed of poly (vinyl alcohol) (PVA) were prepared by repeated freeze thaw method followed by in situ precipitation of zinc oxide nanoparticles within the cryogel networks. Fourier transformed infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD), Energy dispersive X-ray spectroscopy (EDX) were used to characterize the nanocomposites. The morphologies of native PVA cryogels and PVA cryogel-ZnO nanocomposites were observed by scanning electron microscopy (SEM), transmission electron microscopy (TEM) techniques. The SEM analysis suggested that cryogels show a well-defined porous morphology whereas TEM micrographs revealed the presence of nearly spherical and well separated zinc oxide nanoparticles with diameter<100nm. XRD results showed all relevant Bragg's reflections for crystal structure of zinc oxide nanoparticles. Thermo gravimetric-differential thermal analysis (TG-DTA) was conducted to evaluate thermal stability of the nanocomposites. Mechanical properties of nanocomposites were determined in terms of tensile strength and percent elongation. Biocompatible nature was ascertained by anti-haemolytic activity, bovine serum albumin (blood protein) adsorption and in vitro cytotoxicity tests. The prepared nanocomposites were also investigated for swelling and deswelling behaviours. The results revealed that both the swelling and deswelling process depend on the chemical composition of the nanocomposites, number of freeze-thaw cycles, pH and temperature of the swelling medium. The developed biocompatible PVA cryogel-ZnO nanocomposites were also tested for antibacterial activities against both Gram-negative and Gram-positive bacteria. Copyright © 2016 Elsevier B.V. All rights reserved.

The Interior Analysis and 3-D Reconstruction of Internally-Mixed Light-Absorbing Atmospheric Particles

NASA Astrophysics Data System (ADS)

Conny, J. M.; Collins, S. M.; Anderson, I.; Herzing, A.

2010-12-01

Carbon-containing atmospheric particles may either absorb solar or outgoing long-wave radiation or scatter solar radiation, and thus, affect Earth’s radiative balance in multiple ways. Light-absorbing carbon that is common in urban air particles such as industrial coke dust, road dust, and diesel soot, often exists in the same particle with other phases that contain, for example, aluminum, calcium, iron, and sulfur. While the optical properties of atmospheric particles in general depend on overall particle size and shape, the inhomogeneity of chemical phases within internally-mixed particles may also greatly affect particle optical properties. In this study, a series of microscopic approaches were used to identify individual light-absorbing coarse-mode particles and to assess their interior structure and composition. Particle samples were collected in 2004 from one of the U.S. EPA’s Los Angeles Particulate Matter Supersites, and were likely affected substantially by road dust and construction dust. First, bright-field and dark-field light microscopy and computer-controlled scanning electron microscopy (SEM) with energy-dispersive x-ray spectroscopy (EDX) were used to distinguish predominantly light-absorbing carbonaceous particles from other particle types such as mineral dust, sea salt, and brake wear. Second, high-resolution SEM-EDX elemental mapping of individual carbonaceous particles was used to select particles with additional elemental phases that exhibited spatial inhomogeneity. Third, focused ion-beam SEM (FIB-SEM) with EDX was used to slice through selected particles to expose interior surfaces and to determine the spatial distribution of element phases throughout the particles. Fourth, study of the interior phases of a particle was augmented by the transmission electron microscopy (TEM) of a thin section of the particle prepared by FIB-SEM. Here, electron energy loss spectroscopy with TEM was used to study chemical bonding in the carbonaceous phase. Finally, automated serial slicing and imaging in the FIB-SEM generated a stack of secondary electron images of the particles’ interior surfaces that allowed for the 3-D reconstruction of the particles, a process known as FIB tomography. Interior surface of light-absorbing carbonaceous particle from FIB-SEM analysis.

New possibilities to analyse non-standard explosives and post blast residues in forensic practice

NASA Astrophysics Data System (ADS)

Kotrlý, Marek; Turková, Ivana

2005-05-01

Nonstandard and home-made explosives always pose a considerable threat for security forces in terms of their practically unlimited variability, both in composition and in construction of explosive devises. Electron microscopy - SEM with EDS/WDS is one of the key techniques for an analysis of non-standard explosives and post-blast residues. If the amount of materials allows it, a number of other analytical techniques are utilized, such as XRD that is capable of a direct phase identification of a crystalline substance, namely in mixtures. TLC has constantly proved itself useful for laboratory screening. Furthermore, combinations of FTIR, Raman spectrometry, LC MS, GC MS, XRF, micro XRF and other ones are applied. In the case of identification of post-blast residues, where an investigation is often conducted at the level of separate microscopic particles, the role of SEM is unsubstitutable, whereas the analysis of the organic phase from these often sporadic microparticles has been infeasible until recently. One of the very interesting options appears to be Raman spectrometry technique, which is nowadays obtainable as a supplement to SEM EDX. Newly available is the device that is fully confocal, SEM keeps full functionality and scan range, very high resolution (for green laser resolution 360nm FWHM; 430nm Rayleigh), it is fitted with high quality objective lens, enhances mapping through Raman spectrometry in a volume 250μm x 250μm x 250μm by piezo driven scanner (capacitive feedback linearized) and obtaining a high quality white light image (250μm x 250μm) immediately in the SEM chamber. This technique is currently undergoing intensive testing and it seems that the method could significantly help to address issues with the analysis of organic phases in electron microscopy not only in the case of post-blast residues and explosives.

SEM/EDX and vis spectrophotometry study of the stability of resin-bound mortars used for casting replicas and filling missing parts of historic stone fountains.

PubMed

Roig-Salom, José-Luis; Doménech-Carbó, María-Teresa; de la Cruz-Cañizares, Juana; Bolívar-Galiano, Fernando; Pelufo-Carbonell, María-José; Peraza-Zurita, Yaiza

2003-04-01

A study by SEM/EDX and spectrophotometry in the visible region attempting to assess the stability of new resin-bound mortars used for casting replicas of marble historic fountains is presented in this paper. Different accelerating tests such as thermal ageing, UV light ageing, ageing in an SO(2) pollutant chamber, freezing cycles ageing, salt crystallisation ageing, natural ageing and biological attack have been applied to a series of test specimens prepared with polyester-, epoxy- and gel-coat-bound mortars. Examination of morphology, measurement of chemical composition and chromatic coordinates before and after ageing treatments establish the higher stability and resistance properties of these resin-bound mortars by comparison to those from the natural marbles.

Effect of cement dosage and early curing towards Kuala Perlis dredged marine sediments: a ɛv - σv and SEM-EDX approach

NASA Astrophysics Data System (ADS)

Syakeera Nordin, Nurul; Chan, Chee-Ming

2017-11-01

Cement is the primary material used in solidifying the soft soils. This material was applied in solidifying Kuala Perlis dredged marine sediments (DMS). These unwanted sediments are classified as high plasticity silt, MH with 3.36 LL of wc/LL value. At dosage 10 and 20 % of cemented-DMS and 3 days curing time, compression curve results shows the settlement criteria were enhanced than the natural DMS. Unfortunately, the settlement criteria are not complies with the permissible settlement limit and applicable pressure. The formation of cementing compounds appears in the SEM micrograph for 10 and 20 % of cemented-DMS. EDX analysis shows the Ca:Si ratio were increased for cemented-DMS due to the formation of C-S-H gel.

Preparation and antibacterial effect of silver hydroxyapatite/titania nanocomposite thin film on titanium

NASA Astrophysics Data System (ADS)

Mo, Anchun; Liao, Juan; Xu, Wei; Xian, Suqin; Li, Yubao; Bai, Shi

2008-11-01

The composite which contains Ag + and nanosized hydroxyapatite with TiO 2 was deposited onto titanium by dipping method. The morphology, chemical components and structures of the thin film were characterized by XRD, scanning electronic microscope (SEM) and energy dispersive X-ray analysis (EDX). Staphylococcus aureus and Escherichia coli were utilized to test the antibacterial effect. XRD results demonstrated that the films have characteristic diffraction peaks of pure HA. EDX results showed that the deposited films consisted of Ca, P, Ti, O and Ag, all of which distribute uniformly. With regard to the antibacterial effect, 98% of S. aureus and more than 99% of E. coli were killed after 24 h incubation and pictures of SEM showed obviously fewer cells on the surface with coating.

Coatings of titanium substrates with xCaO · (1 - x)SiO2 sol-gel materials: characterization, bioactivity and biocompatibility evaluation.

PubMed

Catauro, M; Papale, F; Bollino, F

2016-01-01

The objective of this study has been to develop low temperature sol-gel coatings to modify the surface of commercially pure titanium grade 4 (a material generally used in dental application) and to evaluate their bioactivity and biocompatibility on the substrate. Glasses of composition expressed by the following general formula xCaO · (1 - x)SiO2 (0.0

Control of surface topography in biomimetic calcium phosphate coatings.

PubMed

Costa, Daniel O; Allo, Bedilu A; Klassen, Robert; Hutter, Jeffrey L; Dixon, S Jeffrey; Rizkalla, Amin S

2012-02-28

The behavior of cells responsible for bone formation, osseointegration, and bone bonding in vivo are governed by both the surface chemistry and topography of scaffold matrices. Bone-like apatite coatings represent a promising method to improve the osteoconductivity and bonding of synthetic scaffold materials to mineralized tissues for regenerative procedures in orthopedics and dentistry. Polycaprolactone (PCL) films were coated with calcium phosphates (CaP) by incubation in simulated body fluid (SBF). We investigated the effect of SBF ion concentration and soaking time on the surface properties of the resulting apatite coatings. CaP coatings were examined by scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectrometry (FTIR), and energy dispersive X-ray spectrometry (EDX). Young's modulus (E(s)) was determined by nanoindentation, and surface roughness was assessed by atomic force microscopy (AFM) and mechanical stylus profilometry. CaP such as carbonate-substituted apatite were deposited onto PCL films. SEM and AFM images of the apatite coatings revealed an increase in topographical complexity and surface roughness with increasing ion concentration of SBF solutions. Young's moduli (E(s)) of various CaP coatings were not significantly different, regardless of the CaP phase or surface roughness. Thus, SBF with high ion concentrations may be used to coat synthetic polymers with CaP layers of different surface topography and roughness to improve the osteoconductivity and bone-bonding ability of the scaffold. © 2012 American Chemical Society

An impedimetric immunosensor for highly sensitive detection of IL-8 in human serum and saliva samples: A new surface modification method by 6-phosphonohexanoic acid for biosensing applications.

PubMed

Aydın, Elif Burcu; Sezgintürk, Mustafa Kemal

2018-08-01

In this study, we fabricated a sensitive and label-free impedimetric immunosensor based on 6-phosphonohexanoic acid (PHA) modified ITO electrode for detection of interleukin-8 (IL-8) in human serum and saliva. PHA was first employed to cancer biomarker sensing platform. Anti-IL-8 antibody was used as a biorecognition element and the detection principle of this immunosensor was based on monitoring specific interaction between anti-IL-8 antibody and IL-8 antigen. The morphological characterization of each electrode modification step was analyzed by scanning electron microscopy (SEM), SEM-energy dispersive X-ray spectroscopy (EDX) and atomic force microscopy (AFM) while electrochemical characterization was performed by electrochemical impedance spectroscopy (EIS), cyclic voltammetry (CV) and single frequency impedance (SFI) techniques. Moreover, the antibody immobilization on the electrode surface was proved Fourier-transform infrared spectroscopy (FTIR) and Raman Spectroscopy. This proposed impedimetric immunosensor exhibited good performances with a wide linear in the range from 0.02 pg/mL to 3 pg/mL as well as a relative low detection limit of 6 fg/mL. The impedimetric immunosensor had a good specificity, stability and reproducibility. This study proved that PHA was a suitable interface material to fabricate an electrochemical biosensor. Copyright © 2018 Elsevier Inc. All rights reserved.

Mg2+ Doped into Electro-synthesized HKUST-1 and Their Initial Hydrogen Sorption Properties

NASA Astrophysics Data System (ADS)

Lestari, W. W.; Ni'maturrohmah, D.; Arrozi, U. S. F.; Suwarno, H.

2018-01-01

The hydrogen storage materials are essentially play important roles in supporting the utilization of hydrogen as a promising alternative energy. Several innovative materials have been proposed and intensively investigated in this regard, including Metal-Organic Framework (MOFs). MOFs type HKUST-1 [Cu3(BTC)2] (BTC = benzene-tri-carboxylate) is the most explored materials in hydrogen storage. In this research, HKUST-1 was electro-synthesized under 15 volt for 1.5 h. This material was ex-situ modified with magnesium(II) ion with variation: 3, 5 and 10 wt% to add attractive sites for hydrogen to form Mg2+@HKUST-1. The final materials were characterized by XRD, FTIR, SEM-EDX, and SAA. Hydrogen sorption measurement was conducted using Sievert system at 30 and 80 °C with pressure from 0.2 to 1.5 bar in 10 minutes for each condition. According to XRD analysis, the basic structure of Mg2+@HKUST-1 was remaining stable. In contrary, SEM analysis showed that HKUST-1 morphology was changed after modification with Mg2+. In addition, the surface area of materials significantly increased from 372.112 to 757.617m2/g, based on SAA analysis. The presence of Mg2+ in the HKUST-1 increased the hydrogen sorption capacity up to 0.475 wt% at 1.4 bar at 30 °C and 0.256 wt% at 80 °C (1.4 bar).

Preparation of porous 2,3-dialdehyde cellulose beads crosslinked with chitosan and their application in adsorption of Congo red dye.

PubMed

Ruan, Chang-Qing; Strømme, Maria; Lindh, Jonas

2018-02-01

Micrometer sized 2,3-dialdehyde cellulose (DAC) beads were produced via a recently developed method relying on periodate oxidation of Cladophora nanocellulose. The produced dialdehyde groups and pristine hydroxyl groups provided the DAC beads with a vast potential for further functionalization. The sensitivity of the DAC beads to alkaline conditions, however, limits their possible functionalization and applications. Hence, alkaline-stable and porous cellulose beads were prepared via a reductive amination crosslinking reaction between 2,3-dialdehyde cellulose beads and chitosan. The produced materials were thoroughly characterized with different methods. The reaction conditions, including the amount of chitosan used, conditions for reductive amination, reaction temperature and time, were investigated and the maintained morphology of the beads after exposure to 1M NaOH (aq.) was verified with SEM. Different washing and drying procedures were used and the results were studied by SEM and BET analysis. Furthermore, FTIR, TGA, EDX, XPS, DLS and elemental analysis were performed to characterize the properties of the prepared beads. Finally, the alkaline-stable porous chitosan cross-linked 2,3-dialdehyde cellulose beads were applied as adsorbent for the dye Congo red. The crosslinked beads displayed fast and high adsorption capacity at pH 2 and good desorption properties at pH 12, providing a promising sorption material. Copyright © 2017 Elsevier Ltd. All rights reserved.

The comparison of phosphate-titanate-silicate layers on the titanium and Ti6Al4V alloy base.

PubMed

Rokita, M

2011-08-15

The studied layers were composed of two parts: titanate-silicate underlayer for better adhesion and titanate-phosphate-silicate layers for potential bioparameters. The layers with different amounts of hydroxyapatite were deposited on titanium and Ti6Al4V alloy substrates using dipping sol-gel method and electrophoresis. The selection of sol/suspension composition, deposition time and heat treatment conditions have the decisive influence on the layers parameters. The obtained layers should be very thin and almost amorphous. The specific nature of ceramic layers on the metal substrates excludes the use of some measurements methods or makes it difficult to interpret the measurement results. All the obtained samples were compared using XRD analysis data (GID technique), SEM with EDX measurements and FTIR spectroscopy (transmission and reflection techniques) before and after soaking in simulated body fluid. FTIR spectroscopy with mathematical treatment of the spectra (BIO-RAD Win-IR program, Arithmetic-subtract function) was used to detect the increase or decrease of any phosphate phases during SBF soaking. Based on the FTIR results the processes of hydroxyapatite (HAp) growth or layer dissolution were estimated. The layers deposited on titanium substrate are more crystalline then the ones deposited on Ti6Al4V. During SBF soaking process the growth of small amount of microcrystalline carbonate hydroxyapatite was observed on titanium substrate. The layer on Ti6Al4V base contained amorphous carbonate apatite. During heating treatment above about 870-920 K this apatite transforms into carbonate hydroxyapatite. The Ti6Al4V substrate seems to be more advantageous in context of potentially bioactive materials obtaining. Copyright © 2010 Elsevier B.V. All rights reserved.

The comparison of phosphate-titanate-silicate layers on the titanium and Ti6Al4V alloy base

NASA Astrophysics Data System (ADS)

Rokita, M.

2011-08-01

The studied layers were composed of two parts: titanate-silicate underlayer for better adhesion and titanate-phosphate-silicate layers for potential bioparameters. The layers with different amounts of hydroxyapatite were deposited on titanium and Ti6Al4V alloy substrates using dipping sol-gel method and electrophoresis. The selection of sol/suspension composition, deposition time and heat treatment conditions have the decisive influence on the layers parameters. The obtained layers should be very thin and almost amorphous. The specific nature of ceramic layers on the metal substrates excludes the use of some measurements methods or makes it difficult to interpret the measurement results. All the obtained samples were compared using XRD analysis data (GID technique), SEM with EDX measurements and FTIR spectroscopy (transmission and reflection techniques) before and after soaking in simulated body fluid. FTIR spectroscopy with mathematical treatment of the spectra (BIO-RAD Win-IR program, Arithmetic-subtract function) was used to detect the increase or decrease of any phosphate phases during SBF soaking. Based on the FTIR results the processes of hydroxyapatite (HAp) growth or layer dissolution were estimated. The layers deposited on titanium substrate are more crystalline then the ones deposited on Ti6Al4V. During SBF soaking process the growth of small amount of microcrystalline carbonate hydroxyapatite was observed on titanium substrate. The layer on Ti6Al4V base contained amorphous carbonate apatite. During heating treatment above about 870-920 K this apatite transforms into carbonate hydroxyapatite. The Ti6Al4V substrate seems to be more advantageous in context of potentially bioactive materials obtaining.

Effects of erbium, chromium:YSGG laser irradiation on root surface: morphological and atomic analytical studies.

PubMed

Kimura, Y; Yu, D G; Kinoshita, J; Hossain, M; Yokoyama, K; Murakami, Y; Nomura, K; Takamura, R; Matsumoto, K

2001-04-01

The purpose of this study was to investigate the morphological and atomic changes on the root surface by stereoscopy, field emission-scanning electron microscopy (FE-SEM), and energy dispersive X-ray spectroscopy (SEM-EDX) after erbium, chromium:yttrium, scandium, gallium, garnet (Er,Cr:YSGG) laser irradiation in vitro. There have been few reports on morphological and atomic analytical study on root surface by Er,Cr:YSGG laser irradiation. Eighteen extracted human premolar and molar teeth were irradiated on root surfaces at a vertical position with water-air spray by an Er,Cr:YSGG laser at the parameter of 5.0 W and 20 Hz for 5 sec while moving. The samples were then morphologically observed by stereoscopy and FE-SEM and examined atomic-analytically by SEM-EDX. Craters having rough but clean surfaces and no melting or carbonization were observed in the samples. An atomic analytical examination showed that the calcium ratio to phosphorus showed no significant changes between the control and irradiated areas (p > 0.01). These results showed that the Er,Cr:YSGG laser has a good cutting effect on root surface and causes no burning or melting after laser irradiation.

A green chemistry approach for the synthesis and characterization of bioactive gold nanoparticles using Azolla microphylla methanol extract

NASA Astrophysics Data System (ADS)

Kunjiappan, Selvaraj; Chowdhury, Ranjana; Bhattacharjee, Chiranjib

2014-06-01

This article reports the environmentally benign synthesis of gold nanoparticles (GNPs) using methanol extract of Azolla microphylla as the stabilizing and reducing agent. The GNPs were characterized by UV-vis spectrophotometry and FTIR, and the morphological characteristics were analyzed by XRD, FESEM-EDX and HRTEM. The GNPs could be formed in very short time, even in less than 30 min. The nanoparticles measured by UV-spectrophotometer demonstrated a peak at 540 nm corresponding to surface plasmon resonance spectra, and the peaks showed by FTIR suggested the presence of organic biomolecules on the surface of the GNPs. XRD results confirmed the crystalline nature of the GNPs, and FESEM-EDX and HRTEM analyses had been performed in the size ranges of 17-40 nm and 1.25-17.5 nm respectively. The synthesized GNPs showed excellent antioxidant activity. This study shows the feasibility of using plant sources for the biosynthesis of GNPs.

Studies of Al-Ti Alloys by SEM

NASA Astrophysics Data System (ADS)

Yildiz, K.; Atici, Y.; Keşlİ Oǧlu, K.; Yaşar, E.

2007-04-01

Al-Ti (1, 2 wt. %) alloys were investigated by Scanning Electron Microscopy (SEM). SEM observations and energy-dispersive x-ray analyses (EDX) showed that the phase structure of Al-Ti (1 %) alloy at 165 μm/s is composed of Al matrix and C, Ni, Fe and Si particles and the Al-Ti (1 %) alloys at 16 and 8 μm/s have only the Al matrix and C particles. It was also found that the Al-Ti (2 %) form the Al matrix and intermetallic TiAl.

Enamel alteration following tooth bleaching and remineralization.

PubMed

Coceska, Emilija; Gjorgievska, Elizabeta; Coleman, Nichola J; Gabric, Dragana; Slipper, Ian J; Stevanovic, Marija; Nicholson, John W

2016-06-01

The purpose of this study was to compare the effects of professional tooth whitening agents containing highly concentrated hydrogen peroxide (with and without laser activation), on the enamel surface; and the potential of four different toothpastes to remineralize any alterations. The study was performed on 50 human molars, divided in two groups: treated with Opalescence(®) Boost and Mirawhite(®) Laser Bleaching. Furthermore, each group was divided into five subgroups, a control one and 4 subgroups remineralized with: Mirasensitive(®) hap+, Mirawhite(®) Gelleѐ, GC Tooth Mousse™ and Mirafluor(®) C. The samples were analysed by SEM/3D-SEM-micrographs, SEM/EDX-qualitative analysis and SEM/EDX-semiquantitative analysis. The microphotographs show that both types of bleaching cause alterations: emphasized perikymata, erosions, loss of interprizmatic substance; the laser treatment is more aggressive and loss of integrity of the enamel is determined by shearing off the enamel rods. In all samples undergoing remineralization deposits were observed, those of toothpastes based on calcium phosphate technologies seem to merge with each other and cover almost the entire surface of the enamel. Loss of integrity and minerals were detected only in the line-scans of the sample remineralized with GC Tooth Mousse™. The semiquantitative EDX analysis of individual elements in the surface layer of the enamel indicates that during tooth-bleaching with HP statistically significant loss of Na and Mg occurs, whereas the bleaching in combination with a laser leads to statistically significant loss of Ca and P. The results undoubtedly confirm that teeth whitening procedures lead to enamel alterations. In this context, it must be noted that laser bleaching is more aggressive for dental substances. However, these changes are reversible and can be repaired by application of remineralization toothpastes. © 2015 The Authors Journal of Microscopy © 2015 Royal Microscopical Society.

Mustard plant ash: a source of micronutrient and an adsorbent for removal of 2,4-dichlorophenoxyacetic acid.

PubMed

Trivedi, Nikhilesh S; Mandavgane, Sachin A; Kulkarni, Bhaskar D

2016-10-01

The work highlights the utilization of an agricultural waste mustard plant ash (MPA) as a soil additive and an adsorbent. MPA was characterized by X-ray fluorescence (XRF), energy-dispersive X-ray spectroscopy (EDX), proximate analysis, CHNS analysis, Brunauer-Emmett-Teller (BET) surface area analysis, zeta potential measurements, Fourier transform infrared (FTIR), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). XRF analysis confirmed the presence of CaO (31.35 %), K 2 O (18.55 %), and P 2 O 5 (6.99 %), all of which act as micronutrients to plants. EDX also confirms high amount of elemental O, Ca, K, and P. The adsorptive ability of MPA was investigated using a commonly used herbicide, 2,4-dichlorophenoxyacetic acid (2,4-D), as a representative chemical. Batch adsorption experiments were conducted to study the effect of different operational parameters such as adsorbent dose, initial 2,4-D concentration, contact time, and temperature on the adsorption process. Data from experiments were fitted to various kinetic and isothermal models. The pseudo-second-order kinetic model was found to show the best fit (R 2  > 0.99), with the highest k 2 value of the order 10 5 . Based on the study results, dosage of MPA/hectare for different crops has been recommended for effective removal of 2,4-D. To our knowledge, this is the first study in which MPA has been characterized in detail and investigated for dual applications (as an adsorbent and as a soil additive).

Mineralogical and physico-chemical characterization of Mbodiene palygorskite for pharmaceutical applications

NASA Astrophysics Data System (ADS)

Sylla Gueye, Rokhaya; Davy, Catherine A.; Cazaux, Frédéric; Ndiaye, Augustin; Diop, Mouhamadou Bassir; Skoczylas, Frédéric; Wele, Alassane

2017-11-01

This contribution provides a wide morphological, mineralogical, chemical and physical characterization of Mbodiene palygorskite (Senegal), to serve as a basis for the formulation of antidiarrheal and cosmetic products. Data are compared with other palygorskite deposits, either in Senegal or on other continents. Qualitative total rock XRD, semi-quantitative XRD of the clay fraction and quantitative X-Ray fluorescence (XRF) show the presence of 72%wt palygorskite (±2%wt), 13%wt montmorillonite (±2%wt), 8%wt dolomite (±2%wt), 5%wt quartz SiO2 (±2%wt) and 2%wt inter-stratified illite/smectite (±2%wt). Coupled SEM + EDX and TEM + EDX confirm the presence of fibrous palygorskite, with greater amounts of Mg than Al, and Fe substitution to Mg and Al, interspersed with dolomite cubes CaMg(CO3)2. The presence of carbonates in Mbodiene palygorskite may limit its use in the Pharmacopoeia, and make its purification necessary. A specific signature of Mbodiene palygorskite, relevant to the palygorskite family, is deduced from both FTIR and TGA analysis. In terms of physico-chemical characterization, Mbodiene palygorskite has usual values when compared to the literature (for its specific surface area, specific gravity, compressibility and Haussner indexes, CEC, loss on ignition, etc.). After grinding (down to a peak grain size of 500 nm), Mbodiene palygorskite is considered a normal clay, extremely highly plastic, with hard consistency owing to the values of its Atterberg plasticity and liquidity limits, with good flowability owing to its compressibility and Haussner indexes. Its physical characteristics are suitable for manufacturing pastes and colloidal suspensions.

TiO2/ZnO and ZnO/TiO2 core/shell nanofibers prepared by electrospinning and atomic layer deposition for photocatalysis and gas sensing

NASA Astrophysics Data System (ADS)

Boyadjiev, Stefan I.; Kéri, Orsolya; Bárdos, Péter; Firkala, Tamás; Gáber, Fanni; Nagy, Zsombor K.; Baji, Zsófia; Takács, Máté; Szilágyi, Imre M.

2017-12-01

In the present work, core TiO2 and ZnO oxide nanofibers were prepared by electrospinning, then shell oxide (ZnO, TiO2) layers were deposited on them by atomic layer deposition (ALD). The aim of preparing ZnO and TiO2 nanofibers, as well as ZnO/TiO2 and TiO2/ZnO nanocomposites is to study the interaction between the oxide materials when a pure oxide fiber is covered with thin film of the other oxide, and explore the influence of exchanging the core and shell materials on their photocatalytic and gas sensing properties. The composition, structure and morphology of the pure and composite nanofibers were studied by SEM-EDX, TEM, XRD, FTIR, UV-vis and Raman. The photocatalytic activity of the as-prepared materials was analyzed by UV-vis spectroscopy through decomposing aqueous methyl orange under UV irradiation. The gas sensing of the nanofibers was investigated by detecting 100 ppm NH3 at 150 and 220 °C using interdigital electrode based sensors.

Preparation and Characterization of Hydroxyapatite-Silica Composite Nanopowders

NASA Astrophysics Data System (ADS)

Latifi, S. M.; Fathi, M. H.; Golozar, M. A.

One of the most important objectives in the field of biomaterials science and engineering is development of new materials as bone substitutes. Silica (SiO2) has an important role in the biomineralization and biological responses. The aim of this research was to prepare and characterize hydroxyapatite-silica (HA-SiO2) composite nanopowder with different content of silica. Hydroxyapatite-silica composite nanopowders with 20 and 40 wt% silica were prepared using a sol-gel method at 600°C with phosphoric pentoxide and calcium nitrate tetrahydrate as a source of hydroxyapatite; also, tetraethylorthosilicate and methyltriethoxisilane as a source of silica. Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX) techniques were used for characterization and evaluation of the products. The results indicated the presence of nanocrystalline hydroxyapatite phase beside amorphous silica phase in prepared composite nanopowders. Moreover, by increasing the content of silica in composite nanopowders, the crystallinity will be decreased,and the ability of the product as a bone substitute material might be controlled by changing the content of the ingredients and subsequently its structure.

Nested seaweed cellulose fiber deposited with cuprous oxide nanorods for antimicrobial activity.

PubMed

Bhutiya, Priyank L; Misra, Nirendra; Abdul Rasheed, M; Zaheer Hasan, S

2018-05-30

Bird's nest type architectural network of cellulosic nanofibers was extracted, with nearly 34% yield, from green filamentous seaweed Chaetomorpha antennina using mild bleaching agent. Nanorods of cuprous oxide (Cu 2 O) were grown over the porous sheet, prepared from the seaweed cellulose, by one step hydrothermal method. The seaweed cellulose and Cu 2 O nanorods deposited seaweed cellulose sheets, were characterized by XRD, SEM-EDX, FT-IR, TGA and tensile test. XRD revealed that seaweed cellulose acted as reducing agent, reducing CuO to Cu 2 O. Morphology showed that the average diameter of seaweed cellulose and deposited Cu 2 O nanorods were 30 nm and 90 nm, respectively. Cuprous oxide nanorods deposited seaweed cellulose sheet gave very good antibacterial activity towards gram-positive (Staphylococcus aureus, Streptococcus thermophilis) and gram-negative (Pseudomonas aeruginous, Escherichia coli) microbes. The Cu 2 O nanorods deposited seaweed cellulose sheet can be viewed to have great potential in biomedical, packaging, biotechnological, textile, water treatment and pharmaceutical applications. Copyright © 2018 Elsevier B.V. All rights reserved.

Synthesis of magnetic biocomposite for efficient adsorption of azo dye from aqueous solution.

PubMed

Sivashankar, R; Sathya, A B; Krishnakumar, Uma; Sivasubramanian, V

2015-11-01

A novel magnetic biocomposite was synthesized using metal chlorides and aquatic macrophytes by co-precipitation method. The resulting product, magnetic biocomposite was characterized by Fourier transform infrared spectra (FTIR), X-ray diffraction (XRD), Energy-dispersive X-ray spectroscopy (EDX) and Scanning electron microscope (SEM). The adsorption performance of the magnetic biocomposite was tested with removal of Metanil Yellow dye from aqueous solution. The effect of influencing parameters such as initial dye concentration, solution pH and agitation were investigated. The equilibrium isotherm was well described by the Langmuir model with the with maximum adsorption capacity of 90.91mg/g. Adsorption kinetics experiments were carried out and the data were well fitted by a pseudo-second-order equation. The results revealed that the magnetic biocomposite could efficiently adsorb the azo dyes from aqueous solution, and the spent adsorbents could be recovered completely by magnetic separation process. Therefore, the prepared magnetic biocomposite could thus be used as promising adsorbent for the removal of azo dyes from polluted water. Copyright © 2015 Elsevier Inc. All rights reserved.

Enhanced reactive adsorption of hydrogen sulfide on the composites of graphene/graphite oxide with copper (hydr)oxychlorides.

PubMed

Mabayoje, Oluwaniyi; Seredych, Mykola; Bandosz, Teresa J

2012-06-27

Composites of copper (hydr)oxychlorides with graphite oxide or graphene were synthesized and used as adsorbents of hydrogen sulfide at dynamic conditions at ambient temperatures. The materials were extensively characterized before and after adsorption in order to link their performance to the surface features. X-ray diffraction, FTIR, thermal analysis, TEM, SEM/EDX, and adsorption of nitrogen were used. It was found that the composite with graphene has the most favorable surface features enhancing reactive adsorption of hydrogen sulfide. The presence of moisture in the H2S stream has a positive effect on the removal process owing to the dissociation process. H2S is retained on the surface via a direct replacement of OH groups and via acid-base reactions with the copper (hydr)oxide. Highly dispersed reduced copper species on the surface of the composite with graphene enhance activation of oxygen and cause formation of sulfites and sulfates. Higher conductivity of the graphene phase than that of graphite oxide helps in electron transfer in redox reactions.

Surface modification of a natural zeolite by treatment with cold oxygen plasma: Characterization and application in water treatment

NASA Astrophysics Data System (ADS)

De Velasco-Maldonado, Paola S.; Hernández-Montoya, Virginia; Montes-Morán, Miguel A.; Vázquez, Norma Aurea-Rangel; Pérez-Cruz, Ma. Ana

2018-03-01

In the present work the possible surface modification of natural zeolite using cold oxygen plasma was studied. The sample with and without treatment was characterized using nitrogen adsorption isotherms at -196 °C, FT-IR spectroscopy, SEM/EDX analysis and X-Ray Diffraction. Additionally, the two samples were used for the removal of lead and acid, basic, reactive and food dyes in batch systems. The natural zeolite was found to be a mesoporous material with a low specific surface area (23 m2/g). X-ray patterns confirmed that clinoptilolite was the main crystal structure present in the natural zeolite. The molecular properties of dyes and the zeolitic structure were studied using molecular simulation, with the purpose to understand the adsorption mechanism. The results pointed out that only the roughness of the clinoptilolite was affected by the plasma treatment, whereas the specific surface area, chemical functionality and crystal structure remained constant. Finally, adsorption results confirmed that the plasma treatment had no significant effects on the dyes and lead retention capacities of the natural zeolite.

Investigation of dielectric behavior of the PVC/BaTiO3 composite in low-frequencies

NASA Astrophysics Data System (ADS)

Berrag, A.; Belkhiat, S.; Madani, L.

2018-04-01

Polyvinyl chloride (PVC) is widely used as insulator in electrical engineering especially as cable insulation sheaths. In order to improve the dielectric properties, polymers are mixed with ceramics. In this paper, PVC composites with different weight percentages 2 wt.%, 5 wt.%, 8 wt.% and 10 wt.% were prepared and investigated. Loss index (𝜀″) and dielectric constant (𝜀‧) have been measured using an impedance analyzer RLC. Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM) equipped with energy dispersive X-ray (EDX) have been used as characterization techniques. The incorporation of BaTiO3 does not modify the crystallinity and the morphology of the PVC but reduces the space charges, therefore the dielectric losses. The frequency response analysis has been followed in the frequency ranges (20-140 Hz and 115-1 MHz). Relaxation frequencies have been evaluated in each frequency range. Experimental measurements have been validated using Cole-Cole’s model. Experimental results show well that BaTiO3 as a filler improves the dielectric properties of PVC.

Synthesis and characterization of TiO2 loaded cashew nut shell activated carbon and photocatalytic activity on BG and MB dyes under sunlight radiation

NASA Astrophysics Data System (ADS)

Ragupathy, S.; Raghu, K.; Prabu, P.

2015-03-01

Synthesis of titanium dioxide (TiO2) nanoparticles and TiO2 loaded cashew nut shell activated carbon (TiO2/CNSAC) had been undertaken using sol-gel method and their application in BG and MB dyes removal under sunlight radiation has been investigated. The synthesized photocatalysts were characterized by X-ray diffraction analysis (XRD), Fourier infra-red spectroscopy (FT-IR), UV-Vis-diffuse reflectance spectroscopy (DRS) and scanning electron microscopy (SEM) with energy dispersive X-ray analysis (EDX). The various experimental parameters like amount of catalyst, contact time for efficient dyes degradation of BG and MB were concerned in this study. Activity measurements performed under solar irradiation has shown good results for the photodegradation of BG and MB in aqueous solution. It was concluded that the higher photocatalytic activity in TiO2/CNSAC was due to parameters like band-gap, number of hydroxyl groups, surface area and porosity of the catalyst. The kinetic data were also described by the pseudo-first-order and pseudo-second-order kinetic models.

Simple hydrothermal synthesis of metal oxides coupled nanocomposites: Structural, optical, magnetic and photocatalytic studies

NASA Astrophysics Data System (ADS)

Ganeshraja, Ayyakannu Sundaram; Clara, Antoni Samy; Rajkumar, Kanniah; Wang, Yanjie; Wang, Yu; Wang, Junhu; Anbalagan, Krishnamoorthy

2015-10-01

The present article is focused on recent developments toward the preparation of room temperature ferromagnetic nanocomposites using better photocatalytic performance. These nanocomposites were successfully prepared by a simple hydrothermal method and their molecular formulas were confirmed as Ti0.90Sn0.10O2 (S1), 0.2CuO-Ti0.73Sn0.06Cu0.21O2-δ (S2), and Ti0.82Sn0.09Fe0.09O2-δ (S3). The ICP, XRD, DRS, FTIR, Raman, XAFS, XPS, EPR, SEM-EDX, HRSEM, HRTEM, photoluminescence and vibrating sample magnetometric measurements were employed to characterize the phase structures, morphologies, optical and magnetic properties of the photocatalysts. The local structures of Sn4+ and Fe3+ were confirmed by 119Sn and 57Fe Mössbauer analysis. The photocatalytic activities of the samples were evaluated by the degradation of methyl orange in water under visible light irradiation. Among the samples, tin doped TiO2 (S1) showed the best photocatalytic performance and stability.

Synthesis, characterization and catalytic activity of nanosized Ni complexed aminoclay

NASA Astrophysics Data System (ADS)

Ranchani, A. Amala Jeya; Parthasarathy, V.; Devi, A. Anitha; Meenarathi, B.; Anbarasan, R.

2017-11-01

A novel Ni complexed aminoclay (AC) catalyst was prepared by complexation method followed by reduction reaction. Various analytical techniques such as FTIR spectroscopy, UV-visible spectroscopy, DSC, TGA, SEM, HRTEM, EDX, XPS and WCA measurement are used to characterize the synthesized material. The AC-Ni catalyst system exhibited improved thermal stability and fiber-like morphology. The XPS results declared the formation of Ni nanoparticles. Thus, synthesized catalyst was tested towards the Schiff base formation reaction between various bio-medical polymers and aniline under air atmosphere at 85 °C for 24 h. The catalytic activity of the catalyst was studied by varying the % weight loading of the AC-Ni system towards the Schiff base formation. The Schiff base formation was quantitatively calculated by the 1H-NMR spectroscopy. While increasing the % weight loading of the AC-Ni catalyst, the % yield of Schiff base was also increased. The k app and Ti values were determined for the reduction of indole and α-terpineol in the presence of AC-Ni catalyst system. The experimental results were compared with the literature report.

Novel keratin modified bacterial cellulose nanocomposite production and characterization for skin tissue engineering.

PubMed

Keskin, Zalike; Sendemir Urkmez, Aylin; Hames, E Esin

2017-06-01

As it is known that bacterial cellulose (BC) is a biocompatible and natural biopolymer due to which it has a large set of biomedical applications. But still it lacks some desired properties, which limits its uses in many other applications. Therefore, the properties of BC need to be boosted up to an acceptable level. Here in this study for the first time, a new natural nanocomposite was produced by the incorporating keratin (isolated from human hair) to the BC (produced by Acetobacter xylinum) to enhance dermal fibroblast cells' attachment. Two different approaches were used in BC based nanocomposite production: in situ and post modifications. BC/keratin nanocomposites were characterized using SEM, FTIR, EDX, XRD, DSC and XPS analyses. Both production methods have yielded successful results for production of BC based nanocomposite-containing keratin. In vitro cell culture experiments performed with human skin keratinocytes and human skin fibroblast cells indicate the potential of the novel BC/keratin nanocomposites for use in skin tissue engineering. Copyright © 2017 Elsevier B.V. All rights reserved.

Generation of conductivity through transfer charge properties, for polyesters and polyamides with characteristic functional groups

NASA Astrophysics Data System (ADS)

Gonzalez, Carmen; Tagle, Luis Hernan; Terraza, Claudio A.; Barriga, Andres; Cabrera, A. L.; Volkmann, Ulrich G.

2011-03-01

Electro-optic properties of σ -conjugated polymers, as polysilylene; are associated with electron conjugation in the silicon atom, which allows a significant delocalization of electrons along of the chain. Thus, the conductivity is intimately connected to the mobility of charge carriers, which in turn depends on the structure and morphology of the system. We report the characterization of polyesters (PEFs) and polyamides (PAFs). Film thicknesses were obtained by ellipsometry. The vibration frequencies of the groups were determined by FT-IR and corroborated by Raman spectroscopy. Structural information was obtained from X-Ray diffraction (XRD). The structural and surface morphology were studied by scanning electron microscope (SEM). Electrical conductivity of the polymers was measured before and after exposure to iodine vapor, for films of different thicknesses. Morphological differentiation was studied by energy dispersive microscopy (EDX), showing a regular distribution of iodine within the polymer. Preliminary conductivity measurements showed adverse effects when oxidation of the polymer films is induced These effects are related to a certain grade of disorder within the system

Synthesis, structural properties and catalytic activity of MgO-SnO2 nanocatalysts

NASA Astrophysics Data System (ADS)

Perveen, Hina; Farrukh, Muhammad Akhyar; Khaleeq-ur-Rahman, Muhammad; Munir, Badar; Tahir, Muhammad Ashraf

2015-01-01

Surfactant controlled synthesis of magnesium oxide-tin oxide (MgO-SnO2) nanocatalysts was carried out via the hydrothermal method. Concentration of sodium dodecyl sulfate (SDS) was varied while all other reaction conditions were kept constant same for this purpose. Furthermore, MgO-SnO2 nanocatalysts were also prepared by changing the precursor's concentration. These precursors are magnesium nitrate Mg(NO3)2 · 6H2O and tin chloride (SnCl4 · 5H2O). The influence of these reaction parameters on the sizes and morphology of the nanocatalysts were studied by using Fourier transform infrared (FTIR) spectroscopy, Scanning electron microscopy-Energy dispersive X-ray (SEM-EDX), Powder X-ray diffraction (XRD), Transmission electron microscopy and Thermo gravimetric analysis (TGA). The catalytic efficiency of MgO-SnO2 was checked against 2,4-dinitrophenylhydrazine (DNPH), which is an explosive compound. The nanocatalysts were found as a good catalyst to degrade the DNPH. Catalytic activity of nanocatalysts was observed up to 19.13% for the degradation DNPH by using UV-spectrophotometer.

Efficient photo-catalytic degradation of malachite green using nickel tungstate material as photo-catalyst.

PubMed

Helaïli, N; Boudjamaa, A; Kebir, M; Bachari, K

2017-03-01

The present study focused on the evaluation of photo-catalytic and photo-electrochemical properties of the photo-catalyst based on nickel tungstate material prepared by a nitrate method through the degradation of malachite green (MG) dye's. The effect of catalyst loading and dye concentration was examined. Physico-chemical, optical, electrical, electrochemical, and photo-electrochemical properties of the prepared material were analyzed by X-ray diffraction (XRD), fourier transform-infrared spectroscopy (FTIR), BET analysis, optical reflectance diffuse (DR), scanning electron microscopy (SEM/EDX), electrical conductivity, cyclic voltammetry (CV), current intensity, mott-shottky, and nyquist. XRD revealed the formation of monoclinic structure with a small particle size. BET surface area of the sample was around 10 m 2 /g. The results show that the degradation of MG was more than 80%, achieved after 3 h of irradiation at pH 4.6 and with a catalyst loading of 75 mg. Also, it was found that the dye photo-degradation obeyed the pseudo-first order kinetic via Langmuir Hinshelwood model.

Environmental performance, mechanical and microstructure analysis of concrete containing oil-based drilling cuttings pyrolysis residues of shale gas.

PubMed

Wang, Chao-Qiang; Lin, Xiao-Yan; He, Ming; Wang, Dan; Zhang, Si-Lan

2017-09-15

The overall objective of this research project is to investigate the feasibility of incorporating oil-based drilling cuttings pyrolysis residues (ODPR) and fly ash serve as replacements for fine aggregates and cementitious materials in concrete. Mechanical and physical properties, detailed environmental performances, and microstructure analysis were carried out. Meanwhile, the early hydration process and hydrated products of ODPR concrete were analyzed with X-ray diffraction (XRD), Fourier transform infrared (FT-IR), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The results indicated that ODPR could not be categorize into hazardous wastes. ODPR had specific pozzolanic characteristic and the use of ODPR had certain influence on slump and compressive strength of concrete. The best workability and optimal compressive strength were achieved with the help of 35% ODPR. Environmental performance tests came to conclusion that ODPR as recycled aggregates and admixture for the preparation of concrete, from the technique perspective, were the substance of mere environmental contamination. Copyright © 2017 Elsevier B.V. All rights reserved.

XRF, μ-XRD and μ-spectroscopic techniques for revealing the composition and structure of paint layers on polychrome sculptures after multiple restorations.

PubMed

Franquelo, M L; Duran, A; Castaing, J; Arquillo, D; Perez-Rodriguez, J L

2012-01-30

This paper presents the novel application of recently developed analytical techniques to the study of paint layers on sculptures that have been restored/repainted several times across centuries. Analyses were performed using portable XRF, μ-XRD and μ-Raman instruments. Other techniques, such as optical microscopy, SEM-EDX and μ-FTIR, were also used. Pigments and other materials including vermilion, minium, red lac, ivory black, lead white, barium white, zinc white (zincite), titanium white (rutile and anatase), lithopone, gold and brass were detected. Pigments from both ancient and modern times were found due to the different restorations/repaintings carried out. μ-Raman was very useful to characterise some pigments that were difficult to determine by μ-XRD. In some cases, pigments identification was only possible by combining results from the different analytical techniques used in this work. This work is the first article devoted to the study of sculpture cross-section samples using laboratory-made μ-XRD systems. Copyright © 2011 Elsevier B.V. All rights reserved.

Cellular compatibility of nanocomposite scaffolds based on hydroxyapatite entrapped in cellulose network for bone repair.

PubMed

Beladi, Faranak; Saber-Samandari, Samaneh; Saber-Samandari, Saeed

2017-06-01

In the past few decades, artificial graft materials for bone tissue engineering have gained much importance. In this study, novel porous 3D nanocomposite scaffolds composed of polyacrylamide grafted cellulose and hydroxyapatite were proposed. They were characterized using scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), energy-dispersive X-ray spectroscopy (EDX), and X-ray diffraction analysis (XRD). The swelling behavior of the scaffolds was examined in both water and phosphate buffer saline (PBS) solution. The cytotoxicity of the scaffolds was determined by MTT assays on human fibroblast gum (HuGu) cells. Results showed that the nanocomposite scaffolds were highly porous with maximum porosity of 85.7% interconnected with a pore size of around 72-125μm. The results of cell culture experiments showed that the scaffolds extracts do not have cytotoxicity in any concentration. Obtained results suggested that the introduced scaffolds are comparable with the trabecular bone from the compositional, structural, and mechanical perspectives and have a great potential as a bone substitute. Copyright © 2017 Elsevier B.V. All rights reserved.

Synthesis of magnetic activated carbon/α-Fe2O3 nanocomposite and its application in the removal of acid yellow 17 dye from water.

PubMed

Ranjithkumar, V; Sangeetha, S; Vairam, S

2014-05-30

The adsorption of acid yellow 17 dye on activated carbon/α-Fe2O3 nanocomposite prepared by simple pyrolytic method using iron(II) gluconate was investigated by batch technique. The composite was characterized by Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), and vibrating sample magnetometry (VSM). The size of iron oxide nanoparticles formed from iron(II) gluconate precursor is in the range 5-17nm. The saturation magnetization (Ms), remanence (Mr) and coercivity (Hc) of the magnetic carbon nanocomposite is 5.6emu/g, 1.14emu/g and 448Oe, respectively. The adsorption data are found to fit well with Langmuir and, fairly well with Freundlich and Tempkin isotherms at higher concentration of dye (40-100mg/L). Kinetics data indicate that the adsorption of dye follows pseudo-second order kinetics model. Copyright © 2014 Elsevier B.V. All rights reserved.

Electrodeposition and Characterization of Hydroxyapatite on TiN/316LSS.

PubMed

Nam, Pham Thi; Lam, Tran Dai; Huong, Ho Thu; Phuong, Nguyen Thu; Trang, Nguyen Thi Thu; Hoang, Thai; Huong, Nguyen Thi Thanh; Thang, Le Ba; Drouet, Christophe; Grossin, David; Kergourlay, Emmanuelle; Bertrand, Ghislaine; Devilliers, Didier; Thanh, Dinh Thi Mai

2015-12-01

The deposition of TiN on stainless steel substrates may improve the stability and compatibility of this material with bone, which may be advantageously exploited for the elaboration of advanced pros- thetic devices. In this work, TiN-coated 316LSS (by way of DC magnetron sputtering) was used as a starting material for investigating the electrochemical post-deposition of hydroxyapatite (HAp) which has a composition close to that of bone. Electrodeposition was carried out starting from an aqueous medium containing solubilized Ca(NO3)2 and NH4H2PO4 in the presence of H2O2. We report the influence of experimental conditions on the morphology of the obtained HAp coating on TiN/316LSS. The effect of applied potential, temperature, H2O2 concentration, pH and duration of reaction were thoroughly discussed on the basis of X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier Transform Infrared (FTIR) spectroscopy and Energy Dispersive X-ray Spectroscopy (EDX) results. This method appears advantageous for producing HAp-coated implant materials.

Analysis and optimization of process parameters for production of polyhydroxyalkanoates along with wastewater treatment by Serratia sp. ISTVKR1.

PubMed

Gupta, Asmita; Kumar, Madan; Thakur, Indu Shekhar

2017-10-01

A previously reported biodegrading bacterial strain Serratia sp. ISTVKR1 was studied for polyhydroxyalkanoate (PHA) production along with wastewater contaminant removal. Nile red fluorescence, GC-MS, FT-IR, NMR and TEM confirmed the accumulation of homopolymer poly-3-hydroxyvalerate (PHV) within the bacterial cells. Analysis of culture after 72h of bacterial treatment showed maximum COD removal (8.4-fold), non-detection of organic contaminants such as 1H-Cyclopropa [a] naphthalene (R.T.=10.12) using GC-MS and increased proportion of elements like Cr, Mn, Fe, Ni, Cu, Cd and Pb in the bacterial cell pellets by SEM-EDX analysis. Optimization of process parameters for enhanced PHA production along with wastewater treatment done using Response Surface Methodology (RSM) showed 5% and 0.74% increase in the PHA production (0.3368±0.13gL -1 ) and % COD reduction (88.93±2.41) of wastewater, respectively. The study, thus established the production of PHA along with wastewater contaminant removal by Serratia sp. ISTVKR1. Copyright © 2017 Elsevier Ltd. All rights reserved.

Cloning and expression of gamma carbonic anhydrase from Serratia sp. ISTD04 for sequestration of carbon dioxide and formation of calcite.

PubMed

Srivastava, Shaili; Bharti, Randhir Kumar; Verma, Praveen Kumar; Thakur, Indu Shekhar

2015-01-01

Bacterial strains isolated from marble mines rock and enriched in the chemostat culture with different concentrations of sodium bicarbonate. The enriched consortium had six bacterial isolates. One of bacterium isolate showed carbonic anhydrase (CA) activity by catalyzing the reversible hydration reaction of carbon dioxide to bicarbonate. The bacterium was identified as Serratia sp. by 16S rRNA sequence analysis. The carbonic anhydrase gene from Serratia sp. was found to be homologous with gamma carbonic anhydrase. The carbonic anhydrase gene was cloned in PET21b(+) and expressed it in recombinant Escherichia coli BL21 (DE3) with His-tag at the C-terminus. The recombinant protein was purified efficiently by using one-step nickel affinity chromatography. Expected size of carbonic anhydrase was approximately 29 kDa in SDS-PAGE gel. Recombinant carbonic anhydrase enzyme was used for biomineralization-based conversion of atmospheric CO2 into valuable calcite minerals. The calcification was confirmed by using XRD, FTIR, EDX and SEM analysis. Copyright © 2015 Elsevier Ltd. All rights reserved.

Microbial-assisted synthesis and evaluation the cytotoxic effect of tellurium nanorods.

PubMed

Forootanfar, Hamid; Amirpour-Rostami, Sahar; Jafari, Mandana; Forootanfar, Amir; Yousefizadeh, Zahra; Shakibaie, Mojtaba

2015-04-01

The present study was designed to isolate bacterial strain capable of tellurium nanorods' (Te NRs) production followed by purification and evaluation of the cytotoxic effect of Te NRs. Among 25 environmental samples collected for screening of Te NR-producer bacterial strains one bacterial colony (isolated from hot spring and identified as Pseudomonas pseudoalcaligenes strain Te) was selected and applied for biosynthesis of Te NRs. Thereafter, an organic-aqueous partitioning system was applied for the purification of the biogenic Te NRs and the purified Te NRs were characterized using transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray (EDX), X-ray diffraction spectroscopy (XRD), UV-visible spectroscopy, and Fourier transform infrared spectroscopy (FTIR) techniques. The cytotoxic effect of biologically synthesized Te NRs and potassium tellurite on four cell lines of MCF-7, HT1080, HepG2 and A549 was then determined using the MTT assay method. The obtained results revealed lower toxicity for the rod-shaped biogenic tellurium nanostructures (~22nm diameter by 185nm length) compared to K2TeO3. Copyright © 2014. Published by Elsevier B.V.

Reutilization of the expired tetracycline for lithium ion battery anode.

PubMed

Hou, Hongying; Dai, Zhipeng; Liu, Xianxi; Yao, Yuan; Liao, Qishu; Yu, Chengyi; Li, Dongdong

2018-07-15

Waste antibiotics into the natural environment are the large challenges to the environmental protection and the human health, and the unreasonable disposal of the expired antibiotics is a major pollution source. Herein, to achieve the innocent treatment and the resource recovery, the expired tetracycline was tried to be reutilized as the electrode active material in lithium ion battery (LIB) for the first time. The micro-structure and element component of the expired tetracycline were characterized by scanning electron microscope (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR). Furthermore, the corresponding electrochemical performances were also investigated by galvanostatic charge/discharge and cyclic voltammetry (CV). To be satisfactory, the expired-tetracycline-based electrode delivered the initial specific discharge capacity of 371.6mAh/g and the reversible specific capacity of 304.1mAh/g after 200cycles. The decent results will not only offer an effective strategy to recycle the expired tetracycline, but also shed a new light on the cyclic economy and the sustainable development. Copyright © 2018 Elsevier B.V. All rights reserved.

A simple approach for morphology tailoring of alginate particles by manipulation ionic nature of polyurethanes.

PubMed

Daemi, Hamed; Barikani, Mehdi; Barmar, Mohammad

2014-05-01

A number of different ionic aqueous polyurethane dispersions (PUDs) were synthesized based on NCO-terminated prepolymers. Two different anionic and cationic polyurethane samples were synthesized using dimethylol propionic acid and N-methyldiethanolamine emulsifiers, respectively. Then, proper amounts of PUDs and sodium alginate were mixed to obtain a number of aqueous polyurethane dispersions-sodium alginate (PUD/SA) elastomers. The chemical structure, thermal, morphological, thermo-mechanical and mechanical properties, and hydrophilicity content of the prepared samples were studied by FTIR, EDX, DSC, TGA, SEM, DMTA, tensile testing and contact angle techniques. The cationic polyurethanes and their blends with sodium alginate showed excellent miscibility and highly stretchable properties, while the samples containing anionic polyurethanes and alginate illustrated a poor compatibility and no significant miscibility. The morphology of alginate particles shifted from nanoparticles to microparticles by changing the nature of PUDs from cationic to anionic types. The final cationic elastomers not only showed better mechanical properties but also were formulated easier than anionic samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Novel chemical synthesis and characterization of copper pyrovanadate nanoparticles and its influence on the flame retardancy of polymeric nanocomposites

NASA Astrophysics Data System (ADS)

Ghiyasiyan-Arani, Maryam; Masjedi-Arani, Maryam; Ghanbari, Davood; Bagheri, Samira; Salavati-Niasari, Masoud

2016-05-01

In this work, copper pyrovanadate (Cu3V2O7(OH)2(H2O)2) nanoparticles have been synthesized by a simple and rapid chemical precipitation method. Different copper-organic complexes were used to control the size and morphology of products. The morphology and structure of the as-synthesized products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectrum, electron dispersive X-ray spectroscopy (EDX), thermal gravimetric analysis (TGA), differential thermal analysis (DTA) and photoluminescence (PL) spectroscopy. The influence of copper pyrovanadate nanostructures on the flame retardancy of the polystyrene, poly vinyl alcohol and cellulose acetate was studied. Dispersed nanoparticles play the role of a magnetic barrier layer, which slows down product volatilization and prevents the flame and oxygen from the sample during decomposition of the polymer. Cu3V2O7(OH)2(H2O)2 is converted to Cu3V2O8 with an endothermic reaction which simultaneously releases water and decrease the temperature of the flame region.

Radiation induced deposition of copper nanoparticles inside the nanochannels of poly(acrylic acid)-grafted poly(ethylene terephthalate) track-etched membranes

NASA Astrophysics Data System (ADS)

Korolkov, Ilya V.; Güven, Olgun; Mashentseva, Anastassiya A.; Atıcı, Ayse Bakar; Gorin, Yevgeniy G.; Zdorovets, Maxim V.; Taltenov, Abzal A.

2017-01-01

Poly(ethylene terephthalate) PET, track-etched membranes (TeMs) with 400 nm average pore size were UV-grafted with poly(acrylic acid) (PAA) after oxidation of inner surfaces by H2O2/UV system. Carboxylate groups of grafted PAA chains were easily complexed with Cu2+ ions in aqueous solutions. These ions were converted into metallic copper nanoparticles (NPs) by radiation-induced reduction of copper ions in aqueous-alcohol solution by gamma rays in the dose range of 46-250 kGy. Copper ions chelating with -COOH groups of PAA chains grafted on PET TeMs form polymer-metal ion complex that prevent the formation of agglomerates during reduction of copper ions to metallic nanoparticles. The detailed analysis by X-Ray diffraction technique (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) confirmed the deposition of copper nanoparticles with the average size of 70 nm on the inner surface of nanochannels of PET TeMs. Samples were also investigated by FTIR, ESR spectroscopies to follow copper ion reduction.

Design of starch functionalized biodegradable P(MAA-co-MMA) as carrier matrix for l-asparaginase immobilization.

PubMed

Ulu, Ahmet; Koytepe, Suleyman; Ates, Burhan

2016-11-20

We prepared biodegradable P(MAA-co-MMA)-starch composite as carrier matrix for the immobilization of l-asparaginase (l-ASNase), an important chemotherapeutic agent in acute lymphoblastic leukemia. Chemical characteristics and thermal stability of the prepared composites were determined by FT-IR, TGA, DTA and, DSC, respectively. Also, biodegradability measurements of P(MAA-co-MMA)-starch composites were carried out to examine the effects of degradation of the starch. Then, l-ASNase was immobilized on the P(MAA-co-MMA)-starch composites. The surface morphology of the composite before and after immobilization was characterized by SEM, EDX, and AFM. The properties of the immobilized l-ASNase were investigated and compared with the free enzyme. The immobilized l-ASNase had better showed thermal and pH stability, and remained stable after 30days of storage at 25°C. Thus, based on the findings of the present work, the P(MAA-co-MMA)-starch composite can be exploited as the biocompatible matrix used for l-ASNase immobilization for medical applications due to biocompatibility and biodegradability. Copyright © 2016 Elsevier Ltd. All rights reserved.

One Step Synthesis of NiO Nanoparticles via Solid-State Thermal Decomposition at Low-Temperature of Novel Aqua(2,9-dimethyl-1,10-phenanthroline)NiCl2 Complex

PubMed Central

Barakat, Assem; Al-Noaimi, Mousa; Suleiman, Mohammed; Aldwayyan, Abdullah S.; Hammouti, Belkheir; Ben Hadda, Taibi; Haddad, Salim F.; Boshaala, Ahmed; Warad, Ismail

2013-01-01

[NiCl2(C14H12N2)(H2O)] complex has been synthesized from nickel chloride hexahydrate (NiCl2·6H2O) and 2,9-dimethyl-1,10-phenanthroline (dmphen) as N,N-bidentate ligand. The synthesized complex was characterized by elemental analysis, infrared (IR) spectroscopy, ultraviolet-visible (UV-vis) spectroscopy and differential thermal/thermogravimetric analysis (TG/DTA). The complex was further confirmed by single crystal X-ray diffraction (XRD) as triclinic with space group P-1. The desired complex, subjected to thermal decomposition at low temperature of 400 ºC in an open atmosphere, revealed a novel and facile synthesis of pure NiO nanoparticles with uniform spherical particle; the structure of the NiO nanoparticles product was elucidated on the basis of Fourier transform infrared (FT-IR), UV-vis spectroscopy, TG/DTA, XRD, scanning electron microscopy (SEM), energy-dispersive X-ray spectrometry (EDXS) and transmission electron microscopy (TEM). PMID:24351867

Rhodamine B removal on A-rGO/cobalt oxide nanoparticles composite by adsorption from contaminated water

NASA Astrophysics Data System (ADS)

Alwan, Salam H.; Alshamsi, Hassan A. Habeeb; Jasim, Layth S.

2018-06-01

Cobalt oxide nanoparticles@rGO composite is prepared by using graphene oxide (GO) as a supporting substance. GO is first treated with ascorbic acid to form rGO. Finally, cobalt oxide nanoparticles reaction with rGO sheets and using as the adsorbent to removal Rh.B dye from wastewater. The morphology and chemical structure of prepared samples were characterized by FTIR, X-ray spectroscopy, SEM-EDX, TEM, AFM and TGA. The adsorption of Rh.B dye on the A-rGO/Co3O4 composite was accomplished under different conditions that are equilibrium time, pH solution, ionic strength, and temperature. The adsorption isotherms of Rh.B dye on the A-rGO/Co3O4 composite could be illustrated well by the Langmuir, Freundlich and Tempkin model. The thermodynamic factors (ΔHo, ΔSo, and ΔGo) estimated from the temperature-dependent isotherms revealed that the adsorption reaction of Rh.B dye on the A-rGO/Co3O4 composite was an endothermic and spontaneous process.

Degradation of Al/SiCp composites produced with rice-hull ash and aluminum cans.

PubMed

Escalera-Lozano, R; Gutiérrez, C A; Pech-Canul, M A; Pech-Canul, M I

2008-01-01

The use of recycling aluminum from beverage containers and rice-hull ash (RHA) offers to be an attractive alternative for the economic production of Al/SiCp composites. However, corrosion phenomena in the composites represent technological barriers yet to be resolved before they can be exploited to their full potential. A simple methodology involving characterization by XRD, SEM, EDX, FTIR and ICP was designed in order to investigate the causes of the rapid degradation in a humid environment of Al/SiCp composites produced with RHA and aluminum cans. Results reveal that the use of RHA was beneficial to avoid degradation through the formation and subsequent hydration of the Al4C3 phase. However with condensed moisture acting as an electrolyte, localized corrosion took place with aggressive damage manifested by the disintegration of the composite into a powdery mixture. The relevant corrosion mechanism was mainly attributed to microgalvanic coupling between the Mg2Si intermetallic compound and the matrix (although other phases such as SiC, Si, MgAl2O4 could also work as microcathodes).

Thin chitosan films containing super-paramagnetic nanoparticles with contrasting capability in magnetic resonance imaging.

PubMed

Farjadian, Fatemeh; Moradi, Sahar; Hosseini, Majid

2017-03-01

Magnetic nanoparticles have found application as MRI contrasting agents. Herein, chitosan thin films containing super-paramagnetic iron oxide nanoparticles (SPIONs) are evaluated in magnetic resonance imaging (MRI). To determine their contrasting capability, super-paramagnetic nanoparticles coated with citrate (SPIONs-cit) were synthesized. Then, chitosan thin films with different concentrations of SPIONs-cit were prepared and their MRI data (i.e., r 2 and r 2 *) was evaluated in an aqueous medium. The synthesized SPIONs-cit and chitosan/SPIONs-cit films were characterized by FTIR, EDX, XRD as well as VSM with the morphology evaluated by SEM and AFM. The nanoparticle sizes and distribution confirmed well-defined nanoparticles and thin films formation along with high contrasting capability in MRI. Images revealed well-dispersed uniform nanoparticles, averaging 10 nm in size. SPIONs-cit's hydrodynamic size averaged 23 nm in diameter. The crystallinity obeyed a chitosan and SPIONs pattern. The in vitro cellular assay of thin films with a novel route was performed within Hek293 cell lines showing that thin films can be biocompatible.

Harvesting microalgal biomass using submerged microfiltration membranes.

PubMed

Bilad, M R; Vandamme, D; Foubert, I; Muylaert, K; Vankelecom, Ivo F J

2012-05-01

This study was performed to investigate the applicability of submerged microfiltration as a first step of up-concentration for harvesting both a freshwater green algae species Chlorella vulgaris and a marine diatom Phaeodactylum tricornutum using three lab-made membranes with different porosity. The filtration performance was assessed by conducting the improved flux step method (IFM) and batch up-concentration filtrations. The fouling autopsy of the membranes was performed by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and Fourier transform infrared spectroscopy (FTIR). The cost analysis was estimated based on the data of a related full-scale submerged membrane bioreactor (MBR). Overall results suggest that submerged microfiltration for algal harvesting is economically feasible. The IFM results indicate a low degree of fouling, comparable to the one obtained for a submerged MBR. By combining the submerged microfiltration with centrifugation to reach a final concentration of 22% w/v, the energy consumption to dewater C. vulgaris and P. tricornutum is 0.84 kW h/m(3) and 0.91 kW h/m(3), respectively. Copyright © 2012 Elsevier Ltd. All rights reserved.

Induction of calcite precipitation through heightened production of extracellular carbonic anhydrase by CO2 sequestering bacteria.

PubMed

Sundaram, Smita; Thakur, Indu Shekhar

2018-04-01

The thermo-alkalotolerant bacterium exhibiting heightened extracellular carbonic anhydrase (CA) activity, survived at 100 mM sodium bicarbonateand 5% gaseous CO 2 was identified as Bacillus sp. by 16S rRNA sequencing. Extracellular carbonic anhydrase was purified by ammonium sulfate precipitation, gel filtration chromatography and affinity chromatography with a yield of 46.61% and specific activity of 481.66 U/mg. The size of purified carbonic anhydrase was approximately 28 kDa in SDS-PAGE gel filtration and further their role in calcium carbonate production was correlated. The purified enzyme was stable with half-life of 25.36 min at 90 °C and pH 8. K M and Vmax values of the enzyme were 1.77 mg/mL and 385.69 U/mg respectively. The production of calcite was confirmed by Scanning Electron Microscopy (SEM) analysis, FTIR, and Energy-Dispersive X-ray (EDX) analysis. Carbonic anhydrase and calcite deposition coupled with CO 2 fixingbacteria is a significant approach for CO 2 sequestration. Copyright © 2018 Elsevier Ltd. All rights reserved.

Direct laser interference patterning of ophthalmic polydimethylsiloxane (PDMS) polymers

NASA Astrophysics Data System (ADS)

Sola, D.; Lavieja, C.; Orera, A.; Clemente, M. J.

2018-07-01

The inscription of diffractive elements in ophthalmic polymers and ocular tissues to induce refractive index changes is of great interest in the fields of Optics and Ophthalmology. In this work fabrication of linear periodic patterns in polydimethylsiloxane (PDMS) intraocular lenses by means of the direct laser interference patterning (DLIP) technique was studied. A Q-Switch Nd:YAG laser coupled to second and third harmonic modules emitting linearly polarized 4 ns pulses at 355 nm with 20 Hz repetition rate was used as the laser source. Laser processing parameters were modified to produce the linear patterns. Processed samples were characterized by means of optical confocal microscopy, Scanning Electron Microscopy SEM, Energy Dispersive X-ray Spectroscopy EDX, Attenuated Total Reflectance-Infrared Spectroscopy ATR-FTIR, and Raman Spectroscopy. Depending on the laser parameters both photo-thermal and photo-chemical damage were observed in the DLIP irradiated areas. Finally, diffractive techniques were used to characterize the diffraction gratings inscribed in the samples resulting in a refractive index change of 1.9 × 10-2 under illumination of a 632.8 nm He-Ne laser.

Synthesis of flexirubin-mediated silver nanoparticles using Chryseobacterium artocarpi CECT 8497 and investigation of its anticancer activity.

PubMed

Venil, Chidambaram Kulandaisamy; Sathishkumar, Palanivel; Malathi, Mahalingam; Usha, Rajamanickam; Jayakumar, Rajarajeswaran; Yusoff, Abdull Rahim Mohd; Ahmad, Wan Azlina

2016-02-01

In this work, the synthesis of silver nanoparticles from a pigment produced by a recently-discovered bacterium, Chryseobacterium artocarpi CECT 8497, was achieved, followed by an investigation of its anticancer properties. The bacterial pigment was identified as flexirubin following NMR ((1)H NMR and (13)C NMR), UV-Vis, and LC-MS analysis. An aqueous silver nitrate solution was treated with isolated flexirubin to produce silver nanoparticles. The synthesised silver nanoparticles were subsequently characterised by UV-Vis spectroscopy, Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDX), X-Ray Diffraction (XRD), and Fourier Transform Infrared (FTIR) Spectroscopy methodologies. Furthermore, the anticancer effects of synthesised silver nanoparticles in a human breast cancer cell line (MCF-7) were evaluated. The tests showed significant cytotoxicity activity of the silver nanoparticles in the cultured cells, with an IC50 value of 36μgmL(-1). This study demonstrates that silver nanoparticles, synthesised from flexirubin from C. artocarpi CECT 8497, may have potential as a novel chemotherapeutic agent. Copyright © 2015 Elsevier B.V. All rights reserved.

Synthesis of polyetherimide / halloysite nanotubes (PEI/HNTs) based nanocomposite membrane towards hydrogen storage

NASA Astrophysics Data System (ADS)

Muthu, R. Naresh; Rajashabala, S.; Kannan, R.

2018-04-01

Even though hydrogen is considered as green and clean energy sources of future, the blooming of hydrogen economy mainly relies on the development of safe and efficient hydrogen storage medium. The present work is aimed at the synthesis and characterization of polyetherimide/acid treated halloysite nanotubes (PEI/A-HNTs) nanocomposite membranes for solid state hydrogen storage medium, where phase inversion technique was adopted for the synthesis of nanocomposite membrane. The synthesized PEI/A-HNTs nanocomposite membranes were characterized by XRD, FTIR, SEM, EDX, CHNS elemental analysis and TGA. Hydrogenation studies were performed using a Sievert's-like hydrogenation setup. The important conclusions arrived from the present work are the PEI/A-HNTs nanocomposite membranes have better performance with a maximum hydrogen storage capacity of 3.6 wt% at 100 °C than pristine PEI. The adsorbed hydrogen possesses the average binding energy of 0.31 eV which lies in the recommended range of US- DOE 2020 targets. Hence it is expected that the PEI/A-HNTs nanocomposite membranes may have bright extent in the scenario of hydrogen fuel cell applications.

Chitosan supramolecularly cross linked with trimesic acid - Facile synthesis, characterization and evaluation of adsorption potential for chromium(VI).

PubMed

Bhatt, Ronak; Sreedhar, B; Padmaja, P

2017-11-01

A facile synthesis of Chitosan Supramolecularly cross-linked with Trimesic Acid (CTMA) is reported in this work. The adsorption potential of CTMA for removal of hexavalent chromium was evaluated and the influence of pH, temperature, contact time and adsorbent dose on the adsorption process was investigated. The experimental results showed that CTMA could efficiently adsorb Cr 6+ and partially reduce it to the less toxic Cr 3+ state. The maximum adsorption capacity of CTMA for Cr 6+ was found to be 129.53mg/g at pH 2.0. CTMA and chromium loaded CTMA were characterised by FT-IR, Raman, TGA-DSC, SEM-EDX, XRD, ESR and XPS spectroscopic techniques. Chitosan was observed to be cross- linked with TMA via ionic, hydrogen bonding and pi-pi supramolecular interactions while adsorption of chromium onto CTMA was by electrostatic forces and hydrogen bonding. From the observed results it was evident that CTMA was successfully applied for simultaneous removal of chromium, lead and iron from chrome plating effluent. Copyright © 2017 Elsevier B.V. All rights reserved.

Electrophoretic fabrication of chitosan-zirconium-oxide nanobiocomposite platform for nucleic acid detection.

PubMed

Das, Maumita; Dhand, Chetna; Sumana, Gajjala; Srivastava, A K; Nagarajan, R; Nain, Lata; Iwamoto, M; Manaka, Takaaki; Malhotra, B D

2011-03-14

The present work describes electrophoretic fabrication of nanostructured chitosan-zirconium-oxide composite (CHIT-NanoZrO(2)) film (180 nm) onto indium-tin-oxide (ITO)-coated glass plate. This nanobiocomposite film has been explored as immobilization platform for probe DNA specific to M. Tuberculosis as model biomolecule to investigate its sensing characteristics. It is revealed that pH-responsive behavior of CHIT and its cationic skeleton is responsible for the movement of CHIT-NanoZrO(2) colloids toward cathode during electrophoretic deposition. The FT-IR, SEM, TEM, and EDX techniques have been employed for the structural, morphological, and composition analysis of the fabricated electrodes. The morphological studies clearly reveal uniform inter-linking and dispersion of hexagonal nanograins of ZrO(2) (30-50 nm) into the chitosan matrix, resulting in homogeneous nanobiocomposite formation. Electrochemical response measurements of DNA/CHIT-NanoZrO(2)/ITO bioelectrode, carried out using cyclic voltammetry and differential pulse voltammetry, reveal that this bioelectrode can specifically detect complementary target DNA up to 0.00078 μM with sensitivity of 6.38 × 10(-6) AμM(-1).

Vitrification of radioactive contaminated soil by means of microwave energy

NASA Astrophysics Data System (ADS)

Yuan, Xun; Qing, Qi; Zhang, Shuai; Lu, Xirui

2017-03-01

Simulated radioactive contaminated soil was successfully vitrified by microwave sintering technology and the solidified body were systematically studied by Raman, XRD and SEM-EDX. The Raman results show that the solidified body transformed to amorphous structure better at higher temperature (1200 °C). The XRD results show that the metamictization has been significantly enhanced by the prolonged holding time at 1200 °C by microwave sintering, while by conventional sintering technology other crystal diffraction peaks, besides of silica at 2θ = 27.830°, still exist after being treated at 1200 °C for much longer time. The SEM-EDX discloses the micro-morphology of the sample and the uniform distribution of Nd element. All the results show that microwave technology performs vitrification better than the conventional sintering method in solidifying radioactive contaminated soil.

Toward Quantifying the Mass-Based Hygroscopicity of Individual Submicron Atmospheric Aerosol Particles with STXM/NEXAFS and SEM/EDX

NASA Astrophysics Data System (ADS)

Yancey Piens, D.; Kelly, S. T.; OBrien, R. E.; Wang, B.; Petters, M. D.; Laskin, A.; Gilles, M. K.

2014-12-01

The hygroscopic behavior of atmospheric aerosols influences their optical and cloud-nucleation properties, and therefore affects climate. Although changes in particle size as a function of relative humidity have often been used to quantify the hygroscopic behavior of submicron aerosol particles, it has been noted that calculations of hygroscopicity based on size contain error due to particle porosity, non-ideal volume additivity and changes in surface tension. We will present a method to quantify the hygroscopic behavior of submicron aerosol particles based on changes in mass, rather than size, as a function of relative humidity. This method results from a novel experimental approach combining scanning transmission x-ray microscopy with near-edge x-ray absorption fine spectroscopy (STXM/NEXAFS), as well as scanning electron microscopy with energy dispersive x-ray spectroscopy (SEM/EDX) on the same individual particles. First, using STXM/NEXAFS, our methods are applied to aerosol particles of known composition ‒ for instance ammonium sulfate, sodium bromide and levoglucosan ‒ and validated by theory. Then, using STXM/NEXAFS and SEM/EDX, these methods are extended to mixed atmospheric aerosol particles collected in the field at the DOE Atmospheric Radiation Measurement (ARM) Climate Research Facility at the Southern Great Planes sampling site in Oklahoma, USA. We have observed and quantified a range of hygroscopic behaviors which are correlated to the composition and morphology of individual aerosol particles. These methods will have implications for parameterizing aerosol mixing state and cloud-nucleation activity in atmospheric models.

Elemental composition study of heavy metal (Ni, Cu, Zn) in riverbank soil by electrokinetic-assisted phytoremediation using XRF and SEM/EDX

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jamari, Suhailly; Embong, Zaidi; Bakar, Ismail

Electrokinetic (EK)-assisted phytoremediation is one of the methods that have a big potential in enhancing the ability of plant uptake in soils remediation process. This research was conducted to investigate the difference in elemental composition concentration of riverbank soil and the change of pH between pre- and post-phytoremediation under the following condition: 1) control or as-receive sample; 2) Dieffenbachia spp plant with EK system (a pair of EK electrodes connected to a direct current (DC) power supply). After the electrodes were connected to a magnitude of 6V/cm{sup −1} electric field for 4 hours/day, the soil and plant samples were analyzedmore » using and X-ray Fluorescence Spectrometer (XRF) and Scanning Electron Microscope / Energy Dispersive X-ray Spectroscopy (SEM/EDX). The SEM/EDX analysis showed that concentration of elemental composition (Ni, Cu and Zn) in post-phytoremediation plant powder samples had increase while elemental concentrations in the post-phytoremediation soil samples were decreased. XRF analysis presented a variation in soil elemental composition concentration from anode to cathode where the concentration near anode region increased while decreased near the cathode region. A significant changes in soil pH were obtained where the soil pH increase in cathode region while decrease in anode region. The results reveal that the assistance of EK in phytoremediation process has increase the efficiency of plant uptake.« less

Aloe vera extract functionalized zinc oxide nanoparticles as nanoantibiotics against multi-drug resistant clinical bacterial isolates.

PubMed

Ali, Khursheed; Dwivedi, Sourabh; Azam, Ameer; Saquib, Quaiser; Al-Said, Mansour S; Alkhedhairy, Abdulaziz A; Musarrat, Javed

2016-06-15

ZnO nanoparticles (ZnONPs) were synthesised through a simple and efficient biogenic synthesis approach, exploiting the reducing and capping potential of Aloe barbadensis Miller (A. vera) leaf extract (ALE). ALE-capped ZnO nanoparticles (ALE-ZnONPs) were characterized using UV-Vis spectroscopy, X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM) analyses. XRD analysis provided the average size of ZnONPs as 15 nm. FTIR spectral analysis suggested the role of phenolic compounds, terpenoids and proteins present in ALE, in nucleation and stability of ZnONPs. Flow cytometry and atomic absorption spectrophotometry (AAS) data analyses revealed the surface binding and internalization of ZnONPs in Gram +ve (Staphylococcus aureus) and Gram -ve (Escherichia coli) cells, respectively. Significant antibacterial activity of ALE-ZnONPs was observed against extended spectrum beta lactamases (ESBL) positive E. coli, Pseudomonas aeruginosa, and methicillin resistant S. aureus (MRSA) clinical isolates exhibiting the MIC and MBC values of 2200, 2400 μg/ml and 2300, 2700 μg/ml, respectively. Substantial inhibitory effects of ALE-ZnONPs on bacterial growth kinetics, exopolysaccharides and biofilm formation, unequivocally suggested the antibiotic and anti-biofilm potential. Overall, the results elucidated a rapid, environmentally benign, cost-effective, and convenient method for ALE-ZnONPs synthesis, for possible applications as nanoantibiotics or drug carriers. Copyright © 2016 Elsevier Inc. All rights reserved.

Synthesis of High-Quality Biodiesel Using Feedstock and Catalyst Derived from Fish Wastes.

PubMed

Madhu, Devarapaga; Arora, Rajan; Sahani, Shalini; Singh, Veena; Sharma, Yogesh Chandra

2017-03-15

A low-cost and high-purity calcium oxide (CaO) was prepared from waste crab shells, which were extracted from the dead crabs, was used as an efficient solid base catalyst in the synthesis of biodiesel. Raw fish oil was extracted from waste parts of fish through mechanical expeller followed by solvent extraction. Physical as well as chemical properties of raw fish oil were studied, and its free fatty acid composition was analyzed with GC-MS. Stable and high-purity CaO was obtained when the material was calcined at 800 °C for 4 h. Prepared catalyst was characterized by XRD, FT-IR, and TGA/DTA. The surface structure of the catalyst was analyzed with SEM, and elemental composition was determined by EDX spectra. Esterification followed by transesterification reactions were conducted for the synthesis of biodiesel. The effect of cosolvent on biodiesel yield was studied in each experiment using different solvents such as toluene, diethyl ether, hexane, tetrahydrofuran, and acetone. High-quality and pure biodiesel was synthesized and characterized by 1 H NMR and FT-IR. Biodiesel yield was affected by parameters such as reaction temperature, reaction time, molar ratio (methanol:oil), and catalyst loading. Properties of synthesized biodiesel such as density, kinematic viscosity, and cloud point were determined according to ASTM standards. Reusability of prepared CaO catalyst was checked, and the catalyst was found to be stable up to five runs without significant loss of catalytic activity.

Characterization of banana peel by scanning electron microscopy and FT-IR spectroscopy and its use for cadmium removal.

PubMed

Memon, Jamil R; Memon, Saima Q; Bhanger, M I; Memon, G Zuhra; El-Turki, A; Allen, Geoffrey C

2008-10-15

This study describes the use of banana peel, a commonly produced fruit waste, for the removal of Cd(II) from environmental and industrial wastewater. The banana peel was characterized by FT-IR and scanning electron microscopy (SEM) coupled with energy dispersive X-ray (EDX) analysis. The parameters pH, contact time, initial metal ion concentration and temperature were investigated and found to be rapid ( approximately 97% within 10 min). The Langmuir adsorption isotherm was used to describe partitioning behavior for the system at room temperature. The value of Q(L) was found to be (35.52 mg g(-1)) higher than the previously reported materials. The binding of metal ions was found to be pH-dependent with the optimal sorption occurring at pH 8. The retained species were eluted with 5 mL of 5 x 10(-3)M HNO(3) with the detection limit of 1.7 x 10(-3)mg L(-1). Kinetics of sorption followed the pseudo-first-order rate equation with the rate constant k, equal to 0.13+/-0.01 min(-1). Thermodynamic parameters such as Gibbs free energy at 303K (-7.41+/-0.13 kJ mol(-1)) and enthalpy (40.56+/-2.34 kJ mol(-1)) indicated the spontaneous and endothermic nature of the sorption process. The developed method was utilized for the removal of Cd(II) ions from environmental and industrial wastewater samples using flame atomic absorption spectrophotometer (FAAS).

Extracellular synthesis of zinc oxide nanoparticle using seaweeds of gulf of Mannar, India

PubMed Central

2013-01-01

Background The biosynthesis of metal nanoparticles by marine resources is thought to be clean, nontoxic, and environmentally acceptable “green procedures”. Marine ecosystems are very important for the overall health of both marine and terrestrial environments. The use of natural sources like Marine biological resources essential for nanotechnology. Seaweeds constitute one of the commercially important marine living renewable resources. Seaweeds such as green Caulerpa peltata, red Hypnea Valencia and brown Sargassum myriocystum were used for synthesis of Zinc oxide nanoparticles. Result The preliminary screening of physico-chemical parameters such as concentration of metals, concentration of seaweed extract, temperature, pH and reaction time revealed that one seaweed S. myriocystum were able to synthesize zinc oxide nanoparticles. It was confirmed through the, initial colour change of the reaction mixture and UV visible spectrophotometer. The extracellular biosynthesized clear zinc oxide nanoparticles size 36 nm through characterization technique such as DLS, AFM, SEM –EDX, TEM, XRD and FTIR. The biosynthesized ZnO nanoparticles are effective antibacterial agents against Gram-positive than the Gram-negative bacteria. Conclusion Based on the FTIR results, fucoidan water soluble pigments present in S. myriocystum leaf extract is responsible for reduction and stabilization of zinc oxide nanoparticles. by this approach are quite stable and no visible changes were observed even after 6 months. These soluble elements could have acted as both reduction and stabilizing agents preventing the aggregation of nanoparticles in solution, extracellular biological synthesis of zinc oxide nanoparticles of size 36 nm. PMID:24298944

Extracellular synthesis of zinc oxide nanoparticle using seaweeds of gulf of Mannar, India.

PubMed

Nagarajan, Sangeetha; Arumugam Kuppusamy, Kumaraguru

2013-12-03

The biosynthesis of metal nanoparticles by marine resources is thought to be clean, nontoxic, and environmentally acceptable "green procedures". Marine ecosystems are very important for the overall health of both marine and terrestrial environments. The use of natural sources like Marine biological resources essential for nanotechnology. Seaweeds constitute one of the commercially important marine living renewable resources. Seaweeds such as green Caulerpa peltata, red Hypnea Valencia and brown Sargassum myriocystum were used for synthesis of Zinc oxide nanoparticles. The preliminary screening of physico-chemical parameters such as concentration of metals, concentration of seaweed extract, temperature, pH and reaction time revealed that one seaweed S. myriocystum were able to synthesize zinc oxide nanoparticles. It was confirmed through the, initial colour change of the reaction mixture and UV visible spectrophotometer. The extracellular biosynthesized clear zinc oxide nanoparticles size 36 nm through characterization technique such as DLS, AFM, SEM -EDX, TEM, XRD and FTIR. The biosynthesized ZnO nanoparticles are effective antibacterial agents against Gram-positive than the Gram-negative bacteria. Based on the FTIR results, fucoidan water soluble pigments present in S. myriocystum leaf extract is responsible for reduction and stabilization of zinc oxide nanoparticles. by this approach are quite stable and no visible changes were observed even after 6 months. These soluble elements could have acted as both reduction and stabilizing agents preventing the aggregation of nanoparticles in solution, extracellular biological synthesis of zinc oxide nanoparticles of size 36 nm.

Carbon abundances, major element chemistry, and mineralogy of hydrated interplanetary dust particles

NASA Technical Reports Server (NTRS)

Keller, L. P.; Thomas, K. L.; Mckay, D. S.

1993-01-01

Hydrated interplanetary dust particles (IDP's) comprise a major fraction of the interplanetary dust particles collected in the stratosphere. While much is known about the mineralogy and chemistry of hydrated IDP's, little is known about the C abundance in this class of IDP's, the nature of the C-bearing phases, and how the C abundance is related to other physical properties of hydrated IDP's. Bulk compositional data (including C and O) for 11 hydrated IDP's that were subsequently examined by the transition electron microscopy (TEM) to determine their mineralogy and mineral chemistry are reported. Our analysis indicates that these hydrated IDP's are strongly enriched in C relative to the most C-rich meteorites. The average abundance of C in these hydrated IDP's is 4X CI chondrite values. The bulk compositions (including C and O) of 11 hydrated IDP's were determined by thin-window, energy-dispersive x ray (EDX) spectroscopy of the uncoated IDP's on Be substrates in the scanning electron microscopy (SEM). As a check on our C measurements, one of the IDP's (L2006H5) was embedded in glassy S, and microtome thin sections were prepared and placed onto Be substrates. Thin-film EDX analyses of multiple thin sections of L2006H5 show good agreement with the bulk value determined in the SEM. Following EDX analysis, the mineralogy and mineral chemistry of each IDP was determined by analyzing ultramicrotome thin sections in a TEM equipped with an EDX spectrometer.

Synthesis and characterization of nano-hydroxyapatite using Sapindus Mukorossi extract

NASA Astrophysics Data System (ADS)

Subha, B.; Prasath, P. Varun; Abinaya, R.; Kavitha, R. J.; Ravichandran, K.

2015-06-01

Nano-Hydroxyapatite (HAP) powders were successfully synthesised by hydrothermal method using Sapindus Mukorossi extract as an additive. The structural and morphological analyses of thus synthesised powders were carried out using FT-IR, XRD and FESEM/EDX. The FT-IR spectra confirm the presence of phosphate and hydroxyl groups corresponding to HAP. The XRD analysis reveals the formation of HAP phase and found to reduce the crystallite size with addition of Sapindus Mukorossi extract. The morphology changes from sphere to flake shape by the influence of extract.

Lead (Pb2+) and copper (Cu2+) remediation from water using superparamagnetic maghemite (γ-Fe2O3) nanoparticles synthesized by Flame Spray Pyrolysis (FSP).

PubMed

Rajput, Shalini; Singh, Lok P; Pittman, Charles U; Mohan, Dinesh

2017-04-15

Superparamagnetic maghemite (γ-Fe 2 O 3 ) nanoparticles of controllable morphology were successfully synthesized using a flame spray pyrolysis (FSP) technique. Their physico-chemical properties, size, morphology, and surface chemistries were determined using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), selected area electron diffraction patterns (SAED), SEM-EDX, scanning electron microscopy (SEM), and pH ZPC (6.3). Elemental contents before and after adsorption were identified using energy dispersive X-ray fluorescence (ED-XRF), energy dispersive X-ray analysis (EDX) and elemental mapping. Surface area (S BET 79.35m 2 /g) and size distribution analyses were conducted using a surface area analyzer and dynamic light scattering (DLS), respectively. The magnetic moment (44.5 at 300K and 50.16 at 2K) was determined using a physical properties measurement system (PPMS). The first adsorption study using γ-Fe 2 O 3 nanoparticles synthesized by FSP to successfully remediate Pb 2+ and Cu 2+ from water is reported. Batch adsorption studies were carried out. An optimum pH of 5.0 was studied for Pb 2+ and Cu 2+ removal. Pb 2+ and Cu 2+ removal mechanisms by these maghemite nanoparticles were presented. The adsorption of Pb 2+ and Cu 2+ was highly pH-dependent. The metal ion uptake was mainly governed by electrostatic attractions. Sorption kinetic data followed the pseudo-second-order model. The Freundlich, Langmuir, Redlich-Peterson, Radke and Sips adsorption isotherm models were applied to interpret equilibrium data. The Freundlich and Langmuir isotherm equations best fit the respective equilibrium data for Pb 2+ and Cu 2+ . The maximum Langmuir adsorption capacities of these maghemite nanoparticles were 68.9mg/g at 45°C for Pb 2+ and 34.0mg/g at 25 °C for Cu 2+ . Thus, these maghemite nanoparticles made by FSP were readily prepared, characterized and showed promise for remediating heavy metal ions from aqueous solutions. Copyright © 2016 Elsevier Inc. All rights reserved.

Characterization of Chlorhexidine-Loaded Calcium-Hydroxide Microparticles as a Potential Dental Pulp-Capping Material

PubMed Central

Priyadarshini, Balasankar M.; Selvan, Subramanian T.; Narayanan, Karthikeyan; Fawzy, Amr S.

2017-01-01

This study explores the delivery of novel calcium hydroxide [Ca(OH)2] microparticles loaded with chlorhexidine (CHX) for potential dental therapeutic and preventive applications. Herein, we introduce a new approach for drug-delivery to deep dentin-surfaces in the form of drug-loaded microparticles. Unloaded Ca(OH)2 [Ca(OH)2/Blank] and CHX-loaded/Ca(OH)2 microparticles were fabricated by aqueous chemical-precipitation technique. The synthesized-microparticles were characterized in vitro for determination of surface-morphology, crystalline-features and thermal-properties examined by energy-dispersive X-ray scanning and transmission electron-microscopy (EDX-SEM/TEM), Fourier-transform infrared-spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA) and differential scanning-calorimetry (DSC). Time-related pH changes, initial antibacterial/biofilm-abilities and cytotoxicity of CHX-loaded/Ca(OH)2 microparticles were evaluated. Microparticles were delivered to dentin-surfaces with subsequent SEM examination of treated dentin-substrates. The in vitro and ex vivo CHX-release profiles were characterized. Ca(OH)2/Blank were hexagonal-shaped with highest z-average diameter whereas CHX-inclusion evidenced micro-metric spheres with distinguishable surface “rounded deposits” and a negative-shift in diameter. CHX:Ca(OH)2/50 mg exhibited maximum encapsulation-efficiency with good antibacterial and cytocompatible properties. SEM examination revealed an intact layer of microparticles on exposed dentin-surfaces with retention of spherical shape and smooth texture. Microparticles loaded on dentin-surfaces showed prolonged release of CHX indicating substantial retention on dentin-substrates. This study validated the inherent-applicability of this novel drug-delivery approach to dentin-surfaces using micro-metric CHX-loaded/Ca(OH)2 microparticles. PMID:28952538

SEM, EDX, Infrared and Raman spectroscopic characterization of the silicate mineral yuksporite

NASA Astrophysics Data System (ADS)

Frost, Ray L.; López, Andrés; Scholz, Ricardo; Theiss, Frederick L.; Romano, Antônio Wilson

2015-02-01

The mineral yuksporite (K,Ba)NaCa2(Si,Ti)4O11(F,OH)ṡH2O has been studied using the combination of SEM with EDX and vibrational spectroscopic techniques of Raman and infrared spectroscopy. Scanning electron microscopy shows a single pure phase with cleavage fragment up to 1.0 mm. Chemical analysis gave Si, Al, K, Na and Ti as the as major elements with small amounts of Mn, Ca, Fe and REE. Raman bands are observed at 808, 871, 930, 954, 980 and 1087 cm-1 and are typical bands for a natural zeolite. Intense Raman bands are observed at 514, 643 and 668 cm-1. A very sharp band is observed at 3668 cm-1 and is attributed to the OH stretching vibration of OH units associated with Si and Ti. Raman bands resolved at 3298, 3460, 3562 and 3628 cm-1 are assigned to water stretching vibrations.

Initial stages of microbiologically influenced tarnishing on titanium after 20 months of immersion in freshwater.

PubMed

Moreno, D A; Cano, E; Ibars, J R; Polo, J L; Montero, F; Bastidas, J M

2004-05-01

This paper studies the initial stages of iridescent tarnishes on titanium heat exchanger tubes in contact with running freshwater on the river Tagus in Spain for up to 20 months. Electrochemical impedance spectroscopy (EIS), scanning electron microscopy [(SEM with energy dispersive X-ray (EDX)] and X-ray photoelectron spectroscopy (XPS) in conjunction with argon-ion sputtering were the techniques used. The EIS data indicated a capacitive behavior, showing a semicircle that was better defined as the experimental time increased, indicating a decreasing tarnishing resistance of titanium. XPS and EDX results indicated that the main elements identified were calcium, phosphorus, nitrogen, and iron. The amount of these elements was higher on the tarnished titanium specimens than on the untarnished specimens. SEM analysis showed the presence of diatoms in the iridescent tarnishes on titanium tubes. Copyright 2003 Springer-Verlag

Simultaneous recovery of phosphorus and potassium as magnesium potassium phosphate from synthetic sewage sludge effluent.

PubMed

Nakao, Satoshi; Nishio, Takayuki; Kanjo, Yoshinori

2017-10-01

Bench-scale experiments were performed to investigate simultaneous recovery of phosphorus and potassium from synthetic sewage sludge effluent as crystals of magnesium potassium phosphate (MPP or struvite-(K), MgKPO 4 ·6H 2 O). The optimal pH of MPP formation was 11.5. A phosphorus level of at least 3 mM and K:P molar ratio over 3 were necessary to form MPP, which showed higher content rate of phosphorus and potassium in precipitate. MPP crystallization was confirmed by analysing the precipitates using a scanning electron microscope-energy dispersive X-ray spectroscopy (SEM-EDX) apparatus and an X-ray Diffractometer (XRD). Inhibition of MPP crystallization by iron and aluminium was confirmed by precipitation experiments and SEM-EDX analysis. Potassium ratio against magnesium in precipitate decreased for iron concentrations greater than over 0.2 mM and aluminium concentrations over 0.05 mM.

Silica Deposition on the Leaves of Mir- and Earth-Grown Super Dwarf Wheat

NASA Technical Reports Server (NTRS)

Campbell, William F.; Bubenheim, David L.; Salisbury, Frank B.; Bingham, Gail E.; McManus, William R.; Biesinger, H. D.; Strickland, D. T.; Levinskikh, Maragarita; Sytchev, Vladimir N.; Podolsky, Igor

2000-01-01

Scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) microanalysis were used to investigate the nature of crystals deposited on leaves of Mir- and Earth-grown Super Dwarf wheat (Triticum aestivum L.) plants. Leaves from these plants exhibited dense and uniformly distributed crystals on leaf abaxial surfaces when viewed by SEM. Young leaves showed that crystals initially accumulated around the stomata on the adaxial surface, but became more dense and uniformly distributed as the leaves aged. EDX microanalyses of the Balkanine (a nutrient charged clinoptilolite zeolite) medium in which the wheat plants were grown showed an elemental pattern similar to that observed on the wheat leaves. The absence of N and P in the Balkanine suggests that they were completely utilized by the plants. Only Si and O were evident in the drying agent, Sorb-it-Silica (trademark), and perhaps could have accounted for some of the Si observed on the plant tissue.

Synthesis and Raman scattering of GaN nanorings, nanoribbons and nanowires

NASA Astrophysics Data System (ADS)

Li, Z. J.; Chen, X. L.; Li, H. J.; Tu, Q. Y.; Yang, Z.; Xu, Y. P.; Hu, B. Q.

Low-dimensional GaN materials, including nanorings, nanoribbons and smooth nanowires have been synthesized by reacting gallium and ammonia using Ag particles as a catalyst on the substrate of MgO single crystals. They were characterized by field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). EDX, XRD indicated that the low-dimensional nanomaterials were wurtzite GaN. New features are found in Raman scatterings for these low-dimensional GaN materials, which are different from the previous observations of GaN materials.

Acaricidal, pediculicidal and larvicidal activity of synthesized ZnO nanoparticles using Momordica charantia leaf extract against blood feeding parasites.

PubMed

Gandhi, P Rajiv; Jayaseelan, C; Mary, R Regina; Mathivanan, D; Suseem, S R

2017-10-01

The aim of the present study was to evaluate the acaricidal, pediculicidal and larvicidal effect of synthesized zinc oxide nanoparticles (ZnO NPs) using Momordica charantia leaf extract against the larvae of Rhipicephalus (Boophilus) microplus, adult of Pediculus humanus capitis, and the larvae of Anopheles stephensi, Culex quinquefasciatus. The ZnO NPs were characterized by using UV, XRD, FTIR and SEM-EDX. The SEM image confirms that the synthesized nanoparticles were spherical in shape with a size of 21.32 nm. The results of GC-MS analysis indicates the presence of the major compound of Nonacosane (C 29 H 60 ) in the M. charantia leaf extract. Cattle tick, head lice and mosquito larvae were exposed to a varying concentrations of the synthesized ZnO NPs and M. charantia leaf extract for 24 h. Compared to the leaf aqueous extract, biosynthesized ZnO NPs showed higher toxicity against R. microplus, P. humanus capitis, An. stephensi, and Cx. Quinquefasciatus with the LC 50 values of 6.87, 14.38, 5.42, and 4.87 mg/L, respectively. The findings revealed that synthesized ZnO NPs possess excellent anti-parasitic activity. These results suggest that the green synthesized ZnO NPs has the potential to be used as an ideal ecofriendly approach for the control of R. microplus, P. humanus capitis and the mosquito larvae of An. Stephensi and Cx. quinquefasciatus. Copyright © 2017 Elsevier Inc. All rights reserved.

Novel high potential visible-light-active photocatalyst of CNT/Mo, S-codoped TiO2 hetero-nanostructure

NASA Astrophysics Data System (ADS)

Hamadanian, M.; Shamshiri, M.; Jabbari, V.

2014-10-01

The current study deals with synthesize of novel nanophotocatalysts of CNT/Mo,S-codoped TiO2 by reacting between titanium isopropoxide (Ti(OC3H7)4) and CNT in aqueous ammonia and subsequent calcining of hydrolysis of the products. The prepared catalysts were characterized by N2 adsorption-desorption measurements, XRD, SEM, TEM, EDX, FT-IR, and UV-vis DRS spectroscopy. SEM and TEM images exhibited uniform coverage of CNT with anatase TiO2 nanoclusters. It was also demonstrated that the presence of S and Mo within the TiO2 acts as electrons traps and prevents the charge recombination and also enables the TiO2 photocatalyst to be active in visible-light region. Moreover, the CNT/Mo,S-doped TiO2 nanohybrids has been proven to has a excellent photocatalytic performance in photodecomposition of Congored (CR), at which the rate of decomposition reaches 100% in only 20 and 30 min under UV and visible-light irradiation, respectively. The enhanced photocatalytic activity was ascribed to the synergetic effects of excellent electrical property of CNT and metal-non-metal codoping. Finally, which to best of our knowledge is done for the first time, we have demonstrated that Mo- and S-doped TiO2 decorated over CNT, or CNT/Mo,S-codoped TiO2, may have high potential applications in photocatalysis and environmental protection with superior catalytic activity under visible-light illumination.

Synthesis, characterization and effect of calcination temperature on phase transformation and photocatalytic activity of Cu,S-codoped TiO 2 nanoparticles

NASA Astrophysics Data System (ADS)

Hamadanian, M.; Reisi-Vanani, A.; Majedi, A.

2010-01-01

A novel copper and sulfur codoped TiO 2 photocatalyst was synthesized by modified sol-gel method using titanium(IV) isopropoxide, CuCl 2·2H 2O and thiourea as precursors. The samples were characterized by X-ray diffraction (XRD), diffuse reflectance spectroscopy (DRS), scanning electron microscopy equipped with energy dispersive X-ray micro-analysis (SEM-EDX), transmission electron microscopy (TEM) and Fourier transform infrared (FT-IR) analysis. The XRD results showed undoped and Cu,S-codoped TiO 2 nanoparticles only include anatase phase. Effect of calcination temperature showed rutile phase appears in 650 and 700 °C for undoped and 0.1% Cu,S-codoped TiO 2, respectively. The SEM analysis revealed the doping of Cu and S does not leave any change in morphology of the catalyst surface. The increase of copper doping enhanced "red-shift" in the UV-vis absorption spectra. The TEM images confirmed the dopants suppressed the growth of TiO 2 grains. The photocatalytic activity of samples was tested for degradation of methyl orange (MO) solutions. The results showed photocatalytic activity of the catalysts with 0.05% Cu,0.05% S and 0.1% Cu,0.05% S were higher than that of other catalysts under ultraviolet (UV) and visible irradiation, respectively. Because of synergetic effect of S and Cu, the Cu,S-codoped TiO 2 catalyst has higher activity than undoped and Cu or S doped TiO 2 catalysts.

Biomimetic formation of apatite on the surface of porous gelatin/bioactive glass nanocomposite scaffolds

NASA Astrophysics Data System (ADS)

Mozafari, Masoud; Rabiee, Mohammad; Azami, Mahmoud; Maleknia, Saied

2010-12-01

There have been several attempts to combine bioactive glasses (BaGs) with biodegradable polymers to create a scaffold material with excellent biocompatibility, bioactivity, biodegradability and toughness. In the present study, the nanocomposite scaffolds with compositions based on gelatin (Gel) and BaG nanoparticles in the ternary SiO 2-CaO-P 2O 5 system were prepared. In vitro evaluations of the nanocomposite scaffolds were performed, and for investigating their bioactive capacity these scaffolds were soaked in a simulated body fluid (SBF) at different time intervals. The scaffolds showed significant enhancement in bioactivity within few days of immersion in SBF solution. The apatite formation at the surface of the nanocomposite samples confirmed by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and X-ray powder diffraction (XRD) analyses. In vitro experiments with osteoblast cells indicated an appropriate penetration of the cells into the scaffold's pores, and also the continuous increase in cell aggregation on the bioactive scaffolds with increase in the incubation time demonstrated the ability of the scaffolds to support cell growth. The SEM observations revealed that the prepared scaffolds were porous with three dimensional (3D) and interconnected microstructure, pore size was 200-500 μm and the porosity was 72-86%. The nanocomposite scaffold made from Gel and BaG nanoparticles could be considered as a highly bioactive and potential bone tissue engineering implant.

Synthesis and Characterization of Hydrophobic Silica Thin Layer Derived from Methyltrimethoxysilane (MTMS)

NASA Astrophysics Data System (ADS)

Darmawan, Adi; Utari, Riyadini; Eka Saputra, Riza; Suhartana; Astuti, Yayuk

2018-01-01

This study investigated the synthesis and characterization of MTMS hydrophobic silica prepared by sol-gel method. In principle, silica xerogels and silica thin layer were obtained by reacting MTMS in ethanol solvent in some pH variations. The MTMS solution was used to modify the surface of the ceramic plate by dipcoating method to further be calcined at two different temperatures of 350°C and 500°C. The silica xerogels were analysed by FTIR, TGA-DSC and GSA to determine functional group characteristics, thermal properties and pore morphology respectively. Meanwhile, the silica thin layers were analysed their hydrophobic properties using water contact angle measurement and surface roughness determination using SEM. The results showed that the higher the pH used in the MTMS solution, the higher the resulting contact angle. The highest contact angle was obtained at pH 8.12 which reached 94.7° and 79.5° for silica thin layer calcined at 350°C and 500°C, respectively. The TGA results indicated that the methyl group survived up to 400°C and disappeared at 500°C which had implications on silica thin layer hydrophobic nature. GSA result exhibited that the silica xerogel had a close structure with a very low pore volume. While the SEM-EDX results displayed that the silica thin layer prepared at acidic pH had smoother surface morphology and became rough when prepared at an alkaline pH.

A novel study based on adaptive metal tolerance behavior in fungi and SEM-EDX analysis.

PubMed

Chen, Si Hui; Ng, Si Ling; Cheow, Yuen Lin; Ting, Adeline Su Yien

2017-07-15

Four fungal isolates: Simplicillium chinense (iso 9, accession no. KX425621), Penicillium simplicissimum (iso 10, KP713758), Trichoderma asperellum (iso 11, KP792512), and Coriolopsis sp. (1c3, KM403574) were subjected to a series of induced-tolerance training under high metal concentrations to determine if greater tolerance could be achieved from constant exposure to such conditions. Adaptive tolerance assay (Tolerance Index, TI) and Field-Emission Scanning Electron Microscopy with Energy Dispersive X-ray (SEM-EDX) characterized their metal tolerance. "Untrained" S. chinense, P. simplicissimum and T. asperellum showed tolerance towards 4000-4500ppm Al(III) (TI: 0.64-0.71), 1000ppm Cr(III) (0.52-0.83) and Pb(II) (0.32-0.88). With tolerance training, tolerance towards 2000-6000ppm Al(III), 500-3000ppm Pb(II) and 2000-3000ppm Cr(III) were achieved (TI: 0.01-0.82) compared to untrained cultures (0.00-0.59). In contrast, tolerance training for Coriolopsis sp. and P. simplicissimum was less successful, with TI values similar or lower than untrained cultures. SEM-EDX analysis proposed biosorption and bioaccumulation as mechanisms for metal removal. The latter was demonstrated with the removal of Cr(III) and Pb(II) by S. chinense (12.37 and 11.52mgg -1 , respectively) and T. asperellum (10.44 and 7.50mgg -1 ). Induced-tolerance training may render benefit in the long run, but this delicate approach is suggestively species and metal dependent. Copyright © 2017 Elsevier B.V. All rights reserved.

[The "silica" component in the PM10 of an urban site].

PubMed

De Berardis, Barbara; Incocciati, Emma; Massera, S; Gargaro, G; Paoletti, L

2007-01-01

In vivo and in vitro toxicological studies have shown that the aged fracturated crystalline silica, which is a component of airborne particulate, exerts an important inflammatory action on airways. The evaluation of the concentration level of airborne crystalline silica in an urban area is an important research subject in order to determine the exposure levels of the general population. The aim was to study the seasonal trend of the quartz (the most common form of crystalline silica) concentration levels in the particulate inhalable faction (PM10) in the urban area of Rome. PM10, sampled by a cascade impactor, was analysed by scanning electron microscopy, equipped with a thin-window system for X-ray microanalysis (SEM/EDX) for qualitative analysis. Parallely the concentration levels of quartz in the particulate were determined by X-ray diffractometry (XRD) for quantitative analysis, using the NIOSH 7500 method (NIOSH, 1994). From September 2004 to October 2005 the abundance of silica particles, evaluated by SEM/EDX was in the range 1.6/10.4%, with a concentration level of free crystalline silica in the range 0.25/2.87 microg/mi. The equivalent diameter of silica particles ranged from 0.3 to 10.5 mircom, moreover, more than 87% of particles showed a diameter less than 2.5 microm. The correlations between SEM/EDX and XRD data seem to suggest that the airborne silica particles in the urban location studied consisted mostly of crystalline silica. Moreover, the data suggest the existence of a significant contribution of silica particles due to southwest wind carrying a fine dust from the Sahara desert to Mediterranean Europe.

Gunshot residue testing in suicides: Part II: Analysis by inductive coupled plasma-atomic emission spectrometry.

PubMed

Molina, D Kimberley; Castorena, Joe L; Martinez, Michael; Garcia, James; DiMaio, Vincent J M

2007-09-01

Several different methods can be employed to test for gunshot residue (GSR) on a decedent's hands, including scanning electron microscopy with energy dispersive x-ray (SEM/EDX) and inductive coupled plasma-atomic emission spectrometry (ICP-AES). In part I of this 2-part series, GSR results performed by SEM/EDX in undisputed cases of suicidal handgun wounds were studied. In part II, the same population was studied, deceased persons with undisputed suicidal handgun wounds, but GSR testing was performed using ICP-AES. A total of 102 cases were studied and analyzed for caliber of weapon, proximity of wound, and the results of the GSR testing. This study found that 50% of cases where the deceased was known to have fired a handgun immediately prior to death had positive GSR results by ICP/AES, which did not differ from the results of GSR testing by SEM/EDX. Since only 50% of cases where the person is known to have fired a weapon were positive for GSR by either method, this test should not be relied upon to determine whether someone has discharged a firearm and is not useful as a determining factor of whether or not a wound is self-inflicted or non-self-inflicted. While a positive GSR result may be of use, a negative result is not helpful in the medical examiner setting as a negative result indicates that either a person fired a weapon prior to death or a person did not fire a weapon prior to death.

Calcification of Hydrophilic Acrylic Intraocular Lenses With a Hydrophobic Surface: Laboratory Analysis of 6 Cases.

PubMed

Gartaganis, Sotirios P; Prahs, Philipp; Lazari, Eftichia D; Gartaganis, Panos S; Helbig, Horst; Koutsoukos, Petros G

2016-08-01

To investigate the nature and characteristic features of deposits causing opacification of intraocular lenses (IOLs) based on the examination of clinical findings using scanning electron microscopy (SEM) and energy-dispersive x-ray spectroscopy (EDX) analysis. Retrospective, observational case series. This is a multicenter study of 6 hydrophilic acrylic IOLs (Lentis LS-502-1; Oculentis GmbH, Berlin, Germany) with a hydrophobic surface that were explanted from 5 patients because of opacification. Three patients had an uncomplicated phacoemulsification. One patient underwent combined phacoemulsification and pars plana vitrectomy for retinal detachment and later silicone oil endotamponade owing to redetachment. The last patient had a pars plana vitrectomy and silicone oil instillation combined with phacoemulsification for tractive retinal detachment and diabetic retinopathy. The explanted lenses were submitted to our laboratory and were examined by SEM and EDX in order to identify the morphologic features and the composition of the deposits. SEM and EDX analyses confirmed the presence of calcific deposits in the interior of the opacified hydrophilic IOLs, with a pattern showing the formation of lumps on the surface. The lumps were due to subsurface formation of calcium phosphate crystalline deposits. The crystallite clusters seemed to diffuse from the IOL interior to the surface. We demonstrated the calcification pattern of the hydrophilic IOL (Lentis LS-502-1) with a hydrophobic surface. Although hydrophilic acrylic lenses have a hydrophobic surface, the development of calcification is a possible threat initiating from the hydrophilic subsurface of the IOLs. Copyright © 2016 Elsevier Inc. All rights reserved.

Mechanical and interfacial characterization of laser welded Co-Cr alloy with different joint configurations

PubMed Central

Kokolis, John; Chakmakchi, Makdad; Theocharopoulos, Antonios; Prombonas, Anthony

2015-01-01

PURPOSE The mechanical and interfacial characterization of laser welded Co-Cr alloy with two different joint designs. MATERIALS AND METHODS Dumbbell cast specimens (n=30) were divided into 3 groups (R, I, K, n=10). Group R consisted of intact specimens, group I of specimens sectioned with a straight cut, and group K of specimens with a 45° bevel made at the one welding edge. The microstructure and the elemental distributions of alloy and welding regions were examined by an SEM/EDX analysis and then specimens were loaded in tension up to fracture. The tensile strength (TS) and elongation (ε) were determined and statistically compared among groups employing 1-way ANOVA, SNK multiple comparison test (α=.05) and Weibull analysis where Weibull modulus m and characteristic strength σο were identified. Fractured surfaces were imaged by a SEM. RESULTS SEM/EDX analysis showed that cast alloy consists of two phases with differences in mean atomic number contrast, while no mean atomic number was identified for welded regions. EDX analysis revealed an increased Cr and Mo content at the alloy-joint interface. All mechanical properties of group I (TS, ε, m and σο) were found inferior to R while group K showed intermediated values without significant differences to R and I, apart from elongation with group R. The fractured surfaces of all groups showed extensive dendritic pattern although with a finer structure in the case of welded groups. CONCLUSION The K shape joint configuration should be preferred over the I, as it demonstrates improved mechanical strength and survival probability. PMID:25722836

Kinetics of apatite formation on a calcium-silicate cement for root-end filling during ageing in physiological-like phosphate solutions.

PubMed

Gandolfi, Maria Giovanna; Taddei, Paola; Tinti, Anna; De Stefano Dorigo, Elettra; Rossi, Piermaria Luigi; Prati, Carlo

2010-12-01

The bioactivity of calcium silicate mineral trioxide aggregate (MTA) cements has been attributed to their ability to produce apatite in presence of phosphate-containing fluids. This study evaluated surface morphology and chemical transformations of an experimental accelerated calcium-silicate cement as a function of soaking time in different phosphate-containing solutions. Cement discs were immersed in Dulbecco's phosphate-buffered saline (DPBS) or Hank's balanced salt solution (HBSS) for different times (1-180 days) and analysed by scanning electron microscopy connected with an energy dispersive X-ray analysis (SEM-EDX) and micro-Raman spectroscopy. SEM-EDX revealed Ca and P peaks after 14 days in DPBS. A thin Ca- and P-rich crystalline coating layer was detected after 60 days. A thicker multilayered coating was observed after 180 days. Micro-Raman disclosed the 965-cm(-1) phosphate band at 7 days only on samples stored in DPBS and later the 590- and 435-cm(-1) phosphate bands. After 60-180 days, a layer approximately 200-900 μm thick formed displaying the bands of carbonated apatite (at 1,077, 965, 590, 435 cm(-1)) and calcite (at 1,088, 713, 280 cm(-1)). On HBSS-soaked, only calcite bands were observed until 90 days, and just after 180 days, a thin apatite-calcite layer appeared. Micro-Raman and SEM-EDX demonstrated the mineralization induction capacity of calcium-silicate cements (MTAs and Portland cements) with the formation of apatite after 7 days in DPBS. Longer time is necessary to observe bioactivity when cements are immersed in HBSS.

Characterization of As-polluted soils by laboratory X-ray-based techniques coupled with sequential extractions and electron microscopy: the case of Crocette gold mine in the Monte Rosa mining district (Italy).

PubMed

Allegretta, Ignazio; Porfido, Carlo; Martin, Maria; Barberis, Elisabetta; Terzano, Roberto; Spagnuolo, Matteo

2018-06-24

Arsenic concentration and distribution were studied by combining laboratory X-ray-based techniques (wavelength dispersive X-ray fluorescence (WDXRF), micro X-ray fluorescence (μXRF), and X-ray powder diffraction (XRPD)), field emission scanning electron microscopy equipped with microanalysis (FE-SEM-EDX), and sequential extraction procedure (SEP) coupled to total reflection X-ray fluorescence (TXRF) analysis. This approach was applied to three contaminated soils and one mine tailing collected near the gold extraction plant at the Crocette gold mine (Macugnaga, VB) in the Monte Rosa mining district (Piedmont, Italy). Arsenic (As) concentration, measured with WDXRF, ranged from 145 to 40,200 mg/kg. XRPD analysis evidenced the presence of jarosite and the absence of any As-bearing mineral, suggesting a high weathering grade and strong oxidative conditions. However, small domains of Fe arsenate were identified by combining μXRF with FE-SEM-EDX. SEP results revealed that As was mainly associated to amorphous Fe oxides/hydroxides or hydroxysulfates (50-80%) and the combination of XRPD and FE-SEM-EDX suggested that this phase could be attributed to schwertmannite. On the basis of the reported results, As is scarcely mobile, even if a consistent As fraction (1-3 g As/kg of soil) is still potentially mobilizable. In general, the proposed combination of laboratory X-ray techniques could be successfully employed to unravel environmental issues related to metal(loid) pollution in soil and sediments.

Quality assurance aspects of GSR analysis by SEM/EDX: a report of first-hand experiences

NASA Astrophysics Data System (ADS)

Charles, Sebastien; Dehan, Didier; Geusens, Nadia; Nys, Bart

2009-05-01

Like many forensic science labs, the Belgian National Institute of Forensic Science (NICC) is involved in a Quality Assurance program aiming towards an ISO17025 Accreditation. Since last year, a project is underway in the GSR lab to validate the method used in the analysis of GSR samples acquired from the hands of suspects by SEM/EDX. The project is well underway, and is planned to lead to accreditation for this technique by the start of 2010. The presentation will discuss several aspects of the functioning of the lab that have to be addressed when preparing for this accreditation. Some of these issues and problems are so involved that separate sub-projects were defined in order to provide a manageable solution. The following topics will be treated in detail: definition of the scope of the accreditation, the validation of the SEM/EDX method with respect to : accuracy, precision, reproducibility and robustness, and the documentation of the Chain of Custody (CoC) of the samples and their storage. One specific sub-project that will be discussed is the study of contamination monitoring in different relevant locations of the lab. Finally, as we have recently acquired a new microscope, the technical criteria we used in the acquisition study will be presented with a focus on their relevance in a QA context. We feel this discussion is informative, both for labs that are pursuing a formal accreditation in the future, and those that work already in such a context and are in the process of acquiring new equipment.

Development of bimetal oxide doped multifunctional polymer nanocomposite for water treatment

NASA Astrophysics Data System (ADS)

Saxena, Swati; Saxena, Umesh

2016-08-01

Bimetal oxide doped polymer nanocomposite was developed using Alumina and Iron (III) Oxide as nanoparticles with Nylon 6, 6 and Poly (sodium-4-styrenesulphonate) as polymer matrix for removal of pollutants from water. The blend sample of polymers was prepared by well established solution blending technique and their nanocomposite samples were prepared through dispersion technique during the solution casting of blend sample. The fabricated composites were characterized adopting FTIR, XRD, FESEM and EDX techniques. XRD and FESEM were used for morphological characterization of nano phase, while FTIR and EDX analysis were adopted for characterization of chemical moieties in composites. In the study of pollutant removal capacities of prepared composites, 6 % nanocomposite provided the best results. It exhibited the maximum removal of all parameters. The removal of total alkalinity was 66.67 %, total hardness 42.85 %, calcium 66.67 %, magnesium 25 %, chloride 58.66 %, nitrate 34.78 %, fluoride 63.85 %, TDS 41.27 % and EC was up to the level of 41.37 % by this composite. The study is a step towards developing multifunctional, cost-effective polymer nanocomposites for water remediation applications.

X-ray diffraction, FTIR, UV-VIS and SEM studies on chromium (III) complexes

NASA Astrophysics Data System (ADS)

Mishra, Ashutosh; Dwivedi, Jagrati; Shukla, Kritika

2015-06-01

Five Chromium (III) complexes have been prepared using Schiff base ligands which derived from benzoin and five different amino acids (H2N-R). Samples were characterized by XRD, FTIR, UV-VIS and SEM method. X-Ray diffraction pattern analyzed that all chromium (III) complexes have hexagonal structure and crystalline, in nature, using Bruker D8 Advance instrument. Using VERTAX 70, FTIR spectroscopy reveals that Samples have (C=N), (C-O), (M-N) and (M-O) bonds in the range of 4000-400cm-1. UV-VIS spectroscopy give information that samples absorb the visible light which is in the range of 380-780nm. For this, Lambda 960 spectrometer used. SEM is designed for studying of the solid objects, using JEOL JSM 5600 instrument.

Investigation of Antibacterial and Fouling Resistance of Silver and Multi-Walled Carbon Nanotubes Doped Poly(Vinylidene Fluoride-co-Hexafluoropropylene) Composite Membrane

PubMed Central

Macevele, Lutendo E.; Moganedi, Kgabo L. M.; Magadzu, Takalani

2017-01-01

Composite membranes were successfully prepared using a phase-inversion method. The X-ray powder diffraction (XRD) and energy dispersive X-ray (EDX) profiles has confirmed formation of 4.8 wt % Ag/poly(vinylidene fluoride-co-hexafluoropropene) (PVDF-HFP), 3 wt % Ag-MWCNTs/PVDF-HFP (EDX surface composition of Ag nanoparticles) and 1.5 wt % MWCNTs/PVDF-HFP composite membranes. The MWCNTs crystallites are mainly encapsulated by a layer of PVDF-HFP, as evidenced by disappearance of graphitic peak. The scanning electron microscopy (SEM) images have depicted the formation of microporous structure, with few MWCNTs on the surface and strongly interacting with PVDF-HFP as demonstrated by thermogravimetric analysis (TGA), XRD and Fourier transform infrared (FTIR) data. The data indicated an increase in porosity, swellability and water content of the PVDF-HFP membrane with the addition of MWCNTs and/or Ag nanoparticles, showing an improved hydrophilicity. The 1.5 wt % MWCNTs/PVDF-HFP composite membrane showed good desalination and fouling resistance rates, which correlates with a low water contact angle. The combined effects of Ag nanoparticles and MWCNTs do not promote fouling resistance of PVDF-HFP membranes, as shown during NaCl microfiltration (this is linked with high water contact angle as compared to that of MWCNTs/PVDF-HFP composite). Both 1.5 wt % MWCNTs/PVDF-HFP and 3 wt % Ag-MWCNTs/PVDF-HFP composite membranes prevented the bacteria passing through the membrane (100% bacterial load reduction). The surface of 3 wt % Ag-MWCNTs/PVDF-HFP showed good bactericidal and non-leaching properties of the dopant materials (MWCNTs and Ag), as evidenced by bacterial growth on the edges of the membranes. PMID:28703740

Micro-abrasion package capture cell experiment on the trailing edge of LDEF: Impactor chemistry and whipple bumper shield efficiencies

NASA Technical Reports Server (NTRS)

Fitzgerald, Howard J.; Yano, Hajime

1995-01-01

Four of the eight available double layer microparticle capture cells, flown as the experiment A0023 on the trailing (West) face of LDEF, have been extensively studied. An investigation of the chemistry of impactors has been made using SEM/EDX techniques and the effectiveness of the capture cells as bumper shields has also been examined. Studies of these capture cells gave positive EDX results, with 53 percent of impact sites indicating the presence of some chemical residues, the predominant residue identified as being silicon in varying quantities.

Simultaneous production of oil enriched in ω-3 polyunsaturated fatty acids and biodiesel from fish wastes.

PubMed

Enascuta, Cristina Emanuela; Stepan, Emil; Bolocan, Ion; Bombos, Dorin; Calin, Catalina; Oprescu, Elena-Emilia; Lavric, Vasile

2018-05-01

The waste resulted from fish processing industries are discarded into the environment around the world, causing environmental pollution. The main problem of fish oil extracted from waste is the high content in free fatty acids (FFA) which decrease the yield in fatty acids esters during transesterification reactions. Therefore, to correct the fish-oil properties, a new environmentally friendly heterogeneous superacid catalyst (SO 4 2- /SnO 2 -ZrO 2 ) was tested in the esterification reaction of FFA with ethanol. The catalyst was characterized by different techniques (XRD, FT-IR, FT-IR of adsorbed pyridine, BET, SEM-EDX, TGA and acidity measurements). The reaction was found to follow a Langmuir-Hinshelwood (L-H) dual-site mechanism with the novelty that both Brönsted and Lewis acid centers participate equally in the esterification reaction. The pre-treated oil was subjected to transesterification reaction with ethanol over a heterogeneous base catalyst and then, the saturated and unsaturated fractions of fatty acid ethyl esters (FAEE) were separated using a vacuum rectification unit with falling film. The saturated content can be used as biofuel, while the unsaturated FAEE are further transesterified with glycerol in order to obtain oil with high content in polyunsaturated fatty acids (PUFA). A detailed study of the intrinsic kinetic process at the surface of the superacid catalyst and a thorough mathematical model of the fixed bed reactor were written and validated by an experimental program, designed according to the D-optimal methodology. Copyright © 2018 Elsevier Ltd. All rights reserved.

Biosynthesis of palladium nanoparticles by using Moringa oleifera flower extract and their catalytic and biological properties.

PubMed

Anand, K; Tiloke, C; Phulukdaree, A; Ranjan, B; Chuturgoon, A; Singh, S; Gengan, R M

2016-12-01

The biosynthesis of nanostructured biopalladium nanoparticles (PdNPs) from an aqueous solution of crystalline palladium acetate is reported. For the synthesised PdNPs in solution, an agroforest biomass waste petal of Moringa oleifera derived bis-phthalate was used as natural reducing and biocapping agents. Continuous absorption in the UV region and subsequent brown colour change confirmed the formation of PdNPs. A strong surface plasmon peak for PdNPs occurred at 460nm. PdNPs were characterized by SEM with EDX, FTIR, TEM and DLS. The chemical composition of the aqueous extract was determined by GC-MS coupled with FTIR and 1 NMR. The catalytic degradation effect by PdNPs on industrial organic toxic effluents p-nitrophenol (PNP) and methylene blue dye was monitored by UV Spectroscopy. On the other hand PdNPs catalysed the base mediated suzuki coupling reaction for biphenyl synthesis, in water. Moreover, PdNPs were found to be reusable catalysts. Toxicity studies of PdNPs showed that the death of brine shrimp to be <50%. Therefore, PdNPs displayed potential for further anticancer studies via tumour cell lines. The in vitro cytotoxicity evaluation of the extract capped nanoparticles was carried out using human lung carcinoma cells (A549) and peripheral lymphocytes normal cells by MTT cell viability assay. Also, PdNPs showed antibacterial activity against Enterococcus faecalis among the different tested strains, including Bacillus cereus, Staphylococcus aureus, Esherichia coli and Candida albicans, Candida utilis. Copyright © 2016 Elsevier B.V. All rights reserved.

Antibacterial efficacy of silver nanoparticles and ethyl acetate's metabolites of the potent halophilic (marine) bacterium, Bacillus cereus A30 on multidrug resistant bacteria.

PubMed

Arul, Dhayalan; Balasubramani, Govindasamy; Balasubramanian, Velramar; Natarajan, Thillainathan; Perumal, Pachiappan

2017-10-01

Bacteria are generally responsible for the prevalence of several diseases and pathogenic bacteria are showing increasing resistance to different antibacterials. During the present study an extremophilic bacterium-A30 isolated from the marine waters was characterized and evaluated against four multi-drug resistant (MDR) pathogens, viz; Methicillin-resistant Staphylococcus aureus (MRSA), Escherichia coli, Klebsiella pneumoniae, and Pseudomonas aeruginosa. The sensitivity pattern of the selected pathogens was tested with 31 antibiotics. Among the 47 marine microbial extracts tested on 4-MDR pathogens viz: Methicillin-resistant Staphylococcus aureus (MRSA), E. coli, K. pneumoniae and P. aeruginosa, only our strain A30 strain exhibited highest efficacy. This strain was subsequently subjected to 16S rDNA sequencing which confirmed its allocation as Bacillus cereus. Silver nanoparticle (AgNPs) synthesis and ethyl acetate extraction were performed using the supernatant of B. cereus. The synthesized AgNPs were characterized by UV-Visible, Fourier-transform infra-red (FT-IR), X-ray diffraction (XRD), Field emission-scanning electron microscopy (FE-SEM), energy dispersive X-ray spectroscopy (EDX), and Zeta potential analyses. The presence of functional groups and 13 bioactive components in the ethyl acetate extract were analyzed using FT-IR and gas chromatography-mass spectrometry (GC-MS). The synthesized of AgNPs and the ethyl acetate extract showed preponderant activity against P. aeruginosa and MRSA, respectively. The effects of AgNPs were significant when compared to ethyl acetate extract. Therefore, the halophilic bacterium, B. cereus mediated AgNPs could provide antibacterial applications in the biomedical industries.

SEM-EDX analysis in the source apportionment of particulate matter on Hypogymnia physodes lichen transplants around the Cu smelter and former mining town of Karabash, South Urals, Russia.

PubMed

Williamson, B J; Mikhailova, I; Purvis, O W; Udachin, V

2004-04-25

Scanning electron microscopy with energy-dispersive X-ray analysis (SEM-EDX) of particulate matter on lichen transplant thalli (Hypogymnia physodes) was assessed as a complementary technique to wet chemical analysis for source apportionment of airborne contaminants. Transplants (2 month exposure) stationed in the Cu smelter and former mining town of Karabash were compared with those from a control site 30 km south. Particulate matter in Karabash samples (715 analyses) showed higher levels of S, Pb, Cu, Sn and Zn compared with the control (598 analyses). Complex element associations among the particles confounded detailed mineralogical identifications, and therefore a simplified particle classification scheme was devised for source apportionment. Karabash samples contained high levels of particles classified as mining-related (MRP), and these were also identified in control samples, indicating wide spatial dispersion from the smelter and highlighting the sensitivity of the method. It was noted that MRP <2.5-microm diameter were poorly represented on lichen surfaces suggesting this may limit the usefulness of Hypogymnia transplants as proxies when assessing human health impacts from airborne particulates. Analyses of the lichen thallus surface (away from surface particulates) revealed high levels of Cu, Zn, Fe and Pb associated with organics in the Karabash samples compared with the control, with a proportionate loss of K, interpreted as being due to a stress-related increase in cell membrane permeability. This type of analysis may provide a novel SEM-EDX-based method for assessing lichen vitality. The techniques developed are presented and further implications of the study are discussed.

Analytical investigation of Mudéjar polychrome on the carpentry in the Casa de Pilatos palace in Seville using non-destructive XRF and complementary techniques

NASA Astrophysics Data System (ADS)

Garrote, M. A.; Robador, M. D.; Perez-Rodriguez, J. L.

2017-02-01

The pigments, execution technique and repainting used on the polychrome wood ceilings and doors in the Casa de Pilatos (Seville, Spain) were studied using portable X-ray fluorescence equipment. Cross-sections of small samples were also analysed by optical microscopy, SEM with EDX analysis, micro-Raman and micro-infrared spectroscopy and X-ray diffraction. These carpentry works are magnificent examples of the Mudéjar art made in Spain in the early 16th century. Portable X-ray fluorescence gave good information on the different components of the polychrome. The SEM-EDX study of the surfaces of small samples gave information on their components and also characterized the compounds that had been deposited or formed by environmental contamination or by the alteration of some pigments. The SEM-EDX study of cross-sections facilitated the characterization of all layers and pigments from the support to the most external layer. The following pigments were characterized: red (cinnabar/vermillion, lead oxide, iron oxides and orpiment/realgar), black (carbon black), white (white lead and titanium barium white), yellow-orange-red-brown (orpiment/realgar and iron oxides), green (chromium oxide), blue (indigo blue and ultramarine blue), and gilding (gold leaf on bole). False gold, bronze and brass were also found. The pigments were applied with the oil painting technique over a support layer that had been primed with animal glue. This support layer was gypsum in some cases and white lead in others. This study is essential to the polychrome conservation of the studied artwork, and it will help clarify uncertainties in the history and painting of Mudéjar art.

Analytical investigation of Mudéjar polychrome on the carpentry in the Casa de Pilatos palace in Seville using non-destructive XRF and complementary techniques.

PubMed

Garrote, M A; Robador, M D; Perez-Rodriguez, J L

2017-02-15

The pigments, execution technique and repainting used on the polychrome wood ceilings and doors in the Casa de Pilatos (Seville, Spain) were studied using portable X-ray fluorescence equipment. Cross-sections of small samples were also analysed by optical microscopy, SEM with EDX analysis, micro-Raman and micro-infrared spectroscopy and X-ray diffraction. These carpentry works are magnificent examples of the Mudéjar art made in Spain in the early 16th century. Portable X-ray fluorescence gave good information on the different components of the polychrome. The SEM-EDX study of the surfaces of small samples gave information on their components and also characterized the compounds that had been deposited or formed by environmental contamination or by the alteration of some pigments. The SEM-EDX study of cross-sections facilitated the characterization of all layers and pigments from the support to the most external layer. The following pigments were characterized: red (cinnabar/vermillion, lead oxide, iron oxides and orpiment/realgar), black (carbon black), white (white lead and titanium barium white), yellow-orange-red-brown (orpiment/realgar and iron oxides), green (chromium oxide), blue (indigo blue and ultramarine blue), and gilding (gold leaf on bole). False gold, bronze and brass were also found. The pigments were applied with the oil painting technique over a support layer that had been primed with animal glue. This support layer was gypsum in some cases and white lead in others. This study is essential to the polychrome conservation of the studied artwork, and it will help clarify uncertainties in the history and painting of Mudéjar art. Copyright © 2016 Elsevier B.V. All rights reserved.

Electrophoretic deposition of double-layer HA/Al composite coating on NiTi.

PubMed

Karimi, Esmaeil; Khalil-Allafi, Jafar; Khalili, Vida

2016-01-01

In order to improve the bioactivity of NiTi alloys, which are being known as the suitable materials for biomedical applications, numerous NiTi disks were electrophoretically coated by hetero-coagulated hydroxyapatite/aluminum composite coatings in three main voltages from suspensions with different Al concentrations. In this paper, the amount of Ni ions release and bioactivity of prepared samples as well as bonding strength of the coating to substrate were investigated. The surface characterization of the coating by XRD, EDX, SEM, and FTIR showed that HA particles bonded by Al particles. It caused the formation of a free crack coating on NiTi disks. Moreover, the bonding strength of HA/Al coatings to NiTi substrate were improved by two times as compared to that of the pure HA coatings. Immersing of coated samples in SBF for 1 week showed that apatite formation ability was improved on HA/Al composite coating and Ni ions release from the surface of composite coating decreased. These results induce the appropriate bioactivity and biocompatibility of the deposited HA/Al composite coatings on NiTi disks. Copyright © 2015 Elsevier B.V. All rights reserved.

Functionalized diamond nanopowder for phosphopeptides enrichment from complex biological fluids.

PubMed

Hussain, Dilshad; Najam-ul-Haq, Muhammad; Jabeen, Fahmida; Ashiq, Muhammad N; Athar, Muhammad; Rainer, Matthias; Huck, Christian W; Bonn, Guenther K

2013-05-02

Diamond is known for its high affinity and biocompatibility towards biomolecules and is used exclusively in separation sciences and life science research. In present study, diamond nanopowder is derivatized as Immobilized Metal Ion Affinity Chromatographic (IMAC) material for the phosphopeptides enrichment and as Reversed Phase (C-18) media for the desalting of complex mixtures and human serum profiling through MALDI-TOF-MS. Functionalized diamond nanopowder is characterized by Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) spectroscopy. Diamond-IMAC is applied to the standard protein (β-casein), spiked human serum, egg yolk and non-fat milk for the phosphopeptides enrichment. Results show the selectivity of synthesized IMAC-diamond immobilized with Fe(3+) and La(3+) ions. To comprehend the elaborated use, diamond-IMAC is also applied to the serum samples from gall bladder carcinoma for the potential biomarkers. Database search is carried out by the Mascot program (www.matrixscience.com) for the assignment of phosphorylation sites. Diamond nanopowder is thus a separation media with multifunctional use and can be applied to cancer protein profiling for the diagnosis and biomarker identification. Copyright © 2013 Elsevier B.V. All rights reserved.

Room temperature structural and dielectric studies of Pb(Fe0.585Nb0.25W0.165)O3 solid solution

NASA Astrophysics Data System (ADS)

Nagaraja, T.; Dadami, Sunanda T.; Angadi, Basavaraj

2018-05-01

The perovskite A(B'B''B''')O3 structure Pb(Fe0.585Nb0.25W0.165)O3 (PFNW) multiferroic material was synthesized by single step solid state reaction method. The single phase was achieved at low temperature with optimized synthesis parameters as calcination (700°C/2hr) and sintering (800 °C /3hr). Single phase was confirmed by room temperature (RT) X-ray diffraction (XRD). The scanning electron microscopy (SEM) shows the uniform distribution of grains throughout the surface of PFNW and the energy dispersive X-ray spectroscopy (EDX) confirms the exact elemental composition as that of the experimental. Fourier transform infrared spectroscopy (FTIR) exhibits two absorption bands at 602 cm-1 and 1385 cm-1 corresponds to the bending and stretching vibrations of metal oxides. RT dielectric studies (dielectric constant, tanδ, AC conductivity) exhibits maximum values at lower frequency region and decreases as the frequency increases. Thesingle semicircular arc in RT impedance spectra (Nyquist plot)indicatesthe contribution to the conductivity is from grains only. Hence PFNW is a potential candidate for near room temperature applications.

Adhesion of nitrile rubber to UV-assisted surface chemical modified PET fabric, part II: Interfacial characterization of MDI grafted PET

NASA Astrophysics Data System (ADS)

Razavizadeh, Mahmoud; Jamshidi, Masoud

2016-08-01

Fiber to rubber adhesion is an important subject in rubber industry. It is well known that surface treatment (i.e. physical, mechanical and chemical) is an effective method to improve interfacial bonding of fibers and/or fabrics to rubbers. UV irradiation is an effective method which has been used to increase fabric-rubber interfacial interactions. In this research UV assisted chemical modification of PET fabrics was used to increase PET to nitrile rubber (NBR) adhesion. Nitrile rubber is a perfect selection as fuel and oil resistant rubber. However it has weak bonding to PET fabric. For this purpose PET fabric was carboxylated under UV irradiation and then methylenediphenyl diisocyanate (MDI) was grafted on carboxylated PET. The chemical composition of the fabric before and after surface treatment was investigated by X-ray photoelectron spectroscopy (XPS). The sectional morphology of the experimental PET fibers and the interface between rubber compound and PET fabric was studied using scanning electron microscope (SEM). The morphology and structure of the product were analyzed by an energy dispersive X-ray spectrometer (EDX). FTIR-ATR and H NMR analysis were used to assess surface modifications on the PET irradiated fabrics.

Rapid biosynthesis of silver nanoparticles using Crotalaria verrucosa leaves against the dengue vector Aedes aegypti: what happens around? An analysis of dragonfly predatory behaviour after exposure at ultra-low doses.

PubMed

Murugan, Kadarkarai; Sanoopa, C P; Madhiyazhagan, Pari; Dinesh, Devakumar; Subramaniam, Jayapal; Panneerselvam, Chellasamy; Roni, Mathath; Suresh, Udaiyan; Nicoletti, Marcello; Alarfaj, Abdullah A; Munusamy, Murugan A; Higuchi, Akon; Kumar, Suresh; Perumalsamy, Haribalan; Ahn, Young-Joon; Benelli, Giovanni

2016-01-01

Aedes aegypti is a primary vector of dengue, a mosquito-borne viral disease infecting 50-100 million people every year. Here, we biosynthesised mosquitocidal silver nanoparticles (AgNP) using the aqueous leaf extract of Crotalaria verrucosa. The green synthesis of AgNP was studied by UV-vis spectroscopy, SEM, EDX and FTIR. C. verrucosa-synthesised AgNPs were toxic against A. aegypti larvae and pupae. LC50 of AgNP ranged from 3.496 ppm (I instar larvae) to 17.700 ppm (pupae). Furthermore, we evaluated the predatory efficiency of dragonfly nymphs, Brachydiplax sobrina, against II and III instar larvae of A. aegypti in an aquatic environment contaminated with ultra-low doses of AgNP. Under standard laboratory conditions, predation after 24 h was 87.5% (II) and 54.7% (III). In an AgNP-contaminated environment, predation was 91 and 75.5%, respectively. Overall, C. verrucosa-synthesised AgNP could be employed at ultra-low doses to reduce larval population of dengue vectors enhancing predation rates of dragonfly nymphs.

Propolis as a green corrosion inhibitor for bronze in weakly acidic solution

NASA Astrophysics Data System (ADS)

Varvara, Simona; Bostan, Roxana; Bobis, Otilia; Găină, Luiza; Popa, Florin; Mena, Vicente; Souto, Ricardo M.

2017-12-01

In the present work, the inhibitive action of natural propolis on bronze corrosion in a weakly acidic solution containing Na2SO4 and NaHCO3 at pH 5 was evaluated using multiscale electrochemical techniques, namely potentiodynamic polarization, electrochemical impedance spectroscopy and scanning vibrating electrode technique measurements. The major constituents of propolis were identified by HPLC. Surface characterization was performed by SEM-EDX and AFM analysis. Experiments were performed as a function of the propolis concentration and immersion time in the corrosive electrolyte. The obtained results showed that propolis presents good anticorrosive properties on bronze, acting as a mixed-type inhibitor, but its protective effectiveness is time-dependent. The highest inhibiting efficiency of 98.9% was obtained in the presence of 100 ppm propolis, after about 12 h of exposure to inhibitor-containing electrolyte through the stabilization of Cu2O on the bronze surface. The inhibitive properties of propolis on bronze corrosion are likely due to the adsorption of its main constituents (flavonoids and phenolic compounds), through the oxygen atoms in their functional groups and aromatic rings, which have been evidenced by FT-IR spectra. The adsorption of propolis on bronze was found to follow Langmuir adsorption isotherm.

Regular square planer bis-(4,4,4-trifluoro-1-(thiophen-2-yl)butane-1,3-dione)/copper(II) complex: Trans/cis-DFT isomerization, crystal structure, thermal, solvatochromism, hirshfeld surface and DNA-binding analysis

NASA Astrophysics Data System (ADS)

Hema, M. K.; Karthik, C. S.; Warad, Ismail; Lokanath, N. K.; Zarrouk, Abdelkader; Kumara, Karthik; Pampa, K. J.; Mallu, P.

2018-04-01

Trans-[Cu(O∩O)2] complex, O∩O = 4,4,4-trifluoro-1-(thiophen-2-yl)butane-1,3-dione was reported with high potential toward CT-DNA binder. The solved XRD-structure of complex indicated a perfect regular square-planer geometry around the Cu(II) center. The trans/cis-DFT-isomerization calculation supported the XRD seen in reflecting the trans-isomer as the kinetic-favor isomer. The desired complex structure was also characterized by conductivity measurement, CHN-elemental analyses, MS, EDX, SEM, UV-Vis., FT-IR, HAS and TG/DTG. The Solvatochromism behavior of the complex was evaluated using four different polar solvents. MPE and Hirshfeld surface analysis (HSA) come to an agreement that fluoride and thiophene protons atoms are with suitable electro-potential environment to form non-classical H-bonds of type CThsbnd H⋯F. The DNA-binding properties were investigated by viscosity tests and spectrometric titrations, the results revealed the complex as strong calf-thymus DNA binder. High intrinsic-binding constants value ∼1.8 × 105 was collected.

Photoluminescent and Thermoluminescent Studies of Dy3+ and Eu3+ Doped Y2O3 Phosphors.

PubMed

Verma, Tarkeshwari; Agrawal, Sadhana

2018-01-01

Eu 3+ doped and Dy 3+ codoped yttrium oxide (Y 2 O 3 ) phosphors have been prepared using solid-state reaction technique (SSR). The prepared phosphors were characterized by X-ray diffractometer (XRD), energy dispersive X-ray (EDX) spectroscopy, scanning electron microscopy (SEM) and Fourier transforms infrared spectroscopy (FTIR) techniques. Photoluminescence (PL) and Thermoluminescence (TL) properties were studied in detail. PL emission spectra were recorded for prepared phosphors under excitation wavelength 254 nm, which show a high intense peak at 613 nm for Y 2 O 3 :Dy 3+ , Eu 3+ (1:1.5 mol %) phosphor. The correlated color temperature (CCT) and CIE analysis have been performed for the synthesized phosphors. TL glow curves were recorded for Eu 3+ doped and Dy 3+ codoped phosphors to study the heating rate effect and dose response. The kinetic parameters were calculated using peak shape method for UV and γ exposures through computerized glow curve deconvolution (CGCD) technique. The phosphors show second order kinetics and activation energies varying from 5.823 × 10 - 1 to 18.608 × 10 - 1  eV.

A new analytical device incorporating a nitrogen doped lanthanum metal oxide with reduced graphene oxide sheets for paracetamol sensing.

PubMed

Ponnaiah, Sathish Kumar; Prakash, Periakaruppan; Vellaichamy, Balakumar

2018-06-01

The novel N-CeO 2 nanoparticles decorated on reduced graphene oxide (N-CeO 2 @rGO) composite has been synthesized by sonochemical method. The characterization of as prepared nanocomposite was intensely performed by UV-Vis, FT-IR, EDX, FE-SEM, HR-TEM, XRD, and TGA analysis. The synthesized nanomaterial was further investigated for its selective and sensitive sensing of paracetamol (PM) based on a N-CeO 2 @rGO modified glassy carbon electrode. A distinct and improved reversible redox peak of PM is obtained at N-CeO 2 @rGO nanocomposite compared to the electrodes modified with N-CeO 2 and rGO. It displays a very good performance with a wide linear range of 0.05-0.600 μM, a very low detection limit of 0.0098 μM (S/N = 3), a high sensitivity of 268 μA µM -1  cm -2 and short response time (<3 s). Also, the fabricated sensor shows a good sensibleness for the detection of PM in various tablet samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Extracellular synthesis of mycogenic silver nanoparticles by Cylindrocladium floridanum and its homogeneous catalytic degradation of 4-nitrophenol.

PubMed

Narayanan, Kannan Badri; Park, Hyun Ho; Sakthivel, Natarajan

2013-12-01

Green synthesis of extracellular mycogenic silver nanoparticles using the fungus, Cylindrocladium floridanum is reported. The synthesized mycogenic silver nanoparticles were characterized using UV-Vis absorption spectroscopy, X-ray diffraction (XRD), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM) techniques. The nanoparticles exhibit fcc structure with Bragg's reflections of (111), (200), (220) and (311) was evidenced by XRD pattern, high-resolution TEM lattice fringes and circular rings in selected-area electron diffraction (SAED) pattern. The morphology of nanoparticles was roughly spherical in shape with an average size of ca. 25 nm. From FTIR spectrum, it was found that the biomolecules with amide I and II band were involved in the stabilization of nanoparticles. These mycogenic silver nanoparticles exhibited the homogeneous catalytic potential in the reduction of pollutant, 4-nitrophenol (4-NP) to 4-aminophenol (4-AP) using sodium borohydride, which followed a pseudo-first-order kinetic model. Thus, the synthesis of metal nanoparticles using sustainable microbial approach opens up possibilities in the usage of mycogenic metal nanoparticles as catalysts in various chemical reactions. Copyright © 2013 Elsevier B.V. All rights reserved.

Loose nanofiltration membrane for dye/salt separation through interfacial polymerization with in-situ generated TiO2 nanoparticles

NASA Astrophysics Data System (ADS)

Zhang, Qi; Fan, Lin; Yang, Zhen; Zhang, Runnan; Liu, Ya-nan; He, Mingrui; Su, Yanlei; Jiang, Zhongyi

2017-07-01

In this study, a high flux nanofiltration (NF) membrane with hybrid polymer-nanoparticle active layer was fabricated by chemical crosslinking of piperazine (PIP) and 1, 3, 5-benzene tricarbonyl trichloride (TMC). An in-situ generated method was applied to deposit titanium dioxide (TiO2) nanoparticles uniformly on the membrane surface, leading to the enhancement of the surface hydrophilicity, roughness and relative surface area of the polyamide (PA) layer. The morphology of the modified membrane was investigated by scanning electron microscopy (SEM) and Atomic force microscopy (AFM), also energy dispersive X-ray microanalysis (EDX) was used to analyze the distribution of Ti element. Chemical structure was observed by Fourier transmission infrared attenuated total reflectance (FTIR-ATR) spectroscopy. Remarkably, the optimal water flux of the loose NF membrane was 65.0 Lm-2 h-1 bar-1 nearly 5 times as much as the pure PA membrane flux. The rejections of the loose NF membranes for dyes were almost all greater than 95.0%, while the rejection for sodium sulfate (Na2SO4) was only about 17.0%, which indicated that the modified membrane had an impressive potential application for dye desalination and purification.

Encapsulation and immobilization of papain in electrospun nanofibrous membranes of PVA cross-linked with glutaraldehyde vapor.

PubMed

Moreno-Cortez, Iván E; Romero-García, Jorge; González-González, Virgilio; García-Gutierrez, Domingo I; Garza-Navarro, Marco A; Cruz-Silva, Rodolfo

2015-01-01

In this paper, papain enzyme (E.C. 3.4.22.2, 1.6 U/mg) was successfully immobilized in poly(vinyl alcohol) (PVA) nanofibers prepared by electrospinning. The morphology of the electrospun nanofibers was characterized by scanning electron microscopy (SEM) and the diameter distribution was in the range of 80 to 170 nm. The presence of the enzyme within the PVA nanofibers was confirmed by infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDXS) analyses. The maximum catalytic activity was reached when the enzyme loading was 13%. The immobilization of papain in the nanofiber membrane was achieved by chemical crosslinking with a glutaraldehyde vapor treatment (GAvt). The catalytic activity of the immobilized papain was 88% with respect to the free enzyme. The crosslinking time by GAvt to immobilize the enzyme onto the nanofiber mat was 24h, and the enzyme retained its catalytic activity after six cycles. The crosslinked samples maintained 40% of their initial activity after being stored for 14 days. PVA electrospun nanofibers are excellent matrices for the immobilization of enzymes due to their high surface area and their nanoporous structure. Copyright © 2015. Published by Elsevier B.V.

Bio-solid-State processes for synthesis of Li-Fe-phosphate.

PubMed

Kim, Hyoung-Bum; Park, Byungno; Lee, Insung; Roh, Yul

2008-10-01

Lithium-Fe-phosphates have become of great interest as storage cathodes for rechargeable Li-batteries because of their high density, environmental friendliness, and safety. The objective of this study was to examine bio-solid-state synthesis of LiFePO4 by microbial processes at room temperature. The microbial reduction of Fe(III)-citrate using an organic carbon, glucose, as an electron donor in the presence of NaHPO4 and lithium that resulted in the formation of Li-substituted iron phosphate. Our studies showed that bacteria enriched from inter-tidal flat sediments, designated as Haejae-1, synthesized Li-substituted iron phosphate. Characterization by X-ray diffraction showed the reduction of Fe(III)-citrate in the presence of NaHPO4 and LiCl2 resulted in the precipitation of Li-substituted vivianite [Li(x)Fe(3-x)(PO4)2 x 8H2O]. SEM-EDX, FTIR, and ESCA analyses showed the chemical composition of the synthesized phases was Li, Fe, P, C, and O. Based on the chemical and physical structure of the mineral, the novel bio-nano-material may be potentially useful to the development of energy storage materials.

Microalgae associated Brevundimonas sp. MSK 4 as the nano particle synthesizing unit to produce antimicrobial silver nanoparticles

NASA Astrophysics Data System (ADS)

Rajamanickam, Karthic; Sudha, S. S.; Francis, Mebin; Sowmya, T.; Rengaramanujam, J.; Sivalingam, Periyasamy; Prabakar, Kandasamy

2013-09-01

The biosynthesis of silver nanoparticles and its antimicrobial property was studied using bacteria isolated from Spirulina products. Isolated bacteria were identified as Bacillus sp. MSK 1 (JX495945), Staphylococcus sp. MSK 2 (JX495946), Bacillus sp. MSK 3 (JX495947) and Brevundimonas sp. MSK 4 (JX495948). Silver nanoparticles (AgNPs) were synthesized using bacterial culture filtrate with AgNO3. The initial syntheses of Ag nanoparticles were characterized by UV-vis spectrophotometer (by measuring the color change to intense brown). Fourier Transform Infrared Spectroscopy (FTIR) study showed evidence that proteins are possible reducing agents and Energy-dispersive X-ray (EDX) study showing the metal silver as major signal. The structure of AgNPs was determined by Scanning electron microscopy (SEM) and X-ray diffraction (XRD). Synthesized Ag nanoparticles with an average size of 40-65 nm have antimicrobial property against human pathogens like Proteus vulgaris, Salmonella typhi, Vibrio cholera, Streptococcus sp., Bacillus subtilis, Staphylococcus aureus, and Escherichia coli. Among the isolates Brevundimonas sp. MSK 4 alone showed good activity in both synthesis of AgNPs and antimicrobial activity. This work demonstrates the possible use of biological synthesized silver nanoparticles to combat the drug resistant problem.

Effective degradation of rhodamine B by electro-Fenton process, using ferromagnetic nanoparticles loaded on modified graphite felt electrode as reusable catalyst: in neutral pH condition and without external aeration.

PubMed

Tian, Jiangnan; Zhao, Jixiang; Olajuyin, Ayobami Matthew; Sharshar, Moustafa Mohamed; Mu, Tingzhen; Yang, Maohua; Xing, Jianmin

2016-08-01

Polytetrafluoroethylene/ferromagnetic nanoparticle/carbon black (PTFE/MNP/CB)-modified graphite felt (GF) was successfully applied as cathode for the mineralization of rhodamine B (RhB) in electro-Fenton (EF) process. The modified cathode showed high decolorization efficiency for RhB solution even in neutral pH condition and without external aeration, achieving nearly complete decolorization and 89.52 % total organic carbon (TOC) removal after 270-min oxidation with the MNP load 1.2 g at 50 A/m(2). Moreover, the operational parameters (current density, MNP load, initial pH, and airflow rate) were optimized. After that, adsorption isotherm was also conducted to compare the absorption quantity of CB and carbon nanotube (CNT). Then, the surface morphologies of MNPs were characterized by transmission electron microscope (TEM), energy-dispersive X-ray detector (EDX), and Fourier transform infrared spectroscopy (FTIR); and the modified cathode was characterized by SEM and contact angle. Finally, the stability and reusability of modified cathode were tested. Result uncovered that the PTFE/MNP/CB-modified cathode has the potential for industrial application and the solution after treatment was easily biodegradable.

Novel symmetrical coralloid Cu 3D superstructures: Solid-state synthesis from a Cu-carboxylate MOF and their in-situ thermal conversion

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chen Lingyun, E-mail: lychen@cqu.edu.c; Shen Yongming; Bai Junfeng, E-mail: bjunfeng@nju.edu.c

2009-08-15

We describe here a one-step solid-state process for the synthesis of metal three-dimensional (3D) superstructures from a metal-organic framework (MOF). Novel symmetrical coralloid Cu 3D superstructures with surface interspersed with clusters of Cu nanoparticles were successfully synthesized by thermolysis of the [Cu{sub 3}(btc){sub 2}] (btc=benzene-1,3,5-tricarboxylato) MOF in a one-end closed horizontal tube furnace (OCTF). The obtained products were characterized by TGA, FT-IR, XRD, EDX, SEM, TEM, HRTEM and SAED. Different reaction conditions were discussed. Furthermore, the synthesized Cu samples were converted into CuO microstructures by in-situ calcination in the air. In addition, the possible formation mechanism was also proposed. Thismore » method is a simple and facile route, which builds a direct linkage between metal-carboxylate MOF crystals and metal nano- or microstructures and also opens a new application field of MOFs. - Graphical abstract: Novel symmetrical coralloid Cu 3D superstructures were synthesized by thermolysis of the [Cu{sub 3}(btc){sub 2}] (btc=benzene-1,3,5-tricarboxylato) MOF microcrystals in a one-end closed horizontal tube furnace (OCTF).« less

Synthesis and characterization of TiO2 loaded cashew nut shell activated carbon and photocatalytic activity on BG and MB dyes under sunlight radiation.

PubMed

Ragupathy, S; Raghu, K; Prabu, P

2015-03-05

Synthesis of titanium dioxide (TiO2) nanoparticles and TiO2 loaded cashew nut shell activated carbon (TiO2/CNSAC) had been undertaken using sol-gel method and their application in BG and MB dyes removal under sunlight radiation has been investigated. The synthesized photocatalysts were characterized by X-ray diffraction analysis (XRD), Fourier infra-red spectroscopy (FT-IR), UV-Vis-diffuse reflectance spectroscopy (DRS) and scanning electron microscopy (SEM) with energy dispersive X-ray analysis (EDX). The various experimental parameters like amount of catalyst, contact time for efficient dyes degradation of BG and MB were concerned in this study. Activity measurements performed under solar irradiation has shown good results for the photodegradation of BG and MB in aqueous solution. It was concluded that the higher photocatalytic activity in TiO2/CNSAC was due to parameters like band-gap, number of hydroxyl groups, surface area and porosity of the catalyst. The kinetic data were also described by the pseudo-first-order and pseudo-second-order kinetic models. Copyright © 2014 Elsevier B.V. All rights reserved.

Development of electrochemical folic acid sensor based on hydroxyapatite nanoparticles

NASA Astrophysics Data System (ADS)

Kanchana, P.; Sekar, C.

2015-02-01

We report the synthesis of hydroxyapatite (HA) nanoparticles (NPs) by a simple microwave irradiation method and its application as sensing element for the precise determination of folic acid (FA) by electrochemical method. The structure and composition of the HA NPs characterized using XRD, FTIR, Raman and XPS. SEM and EDX studies confirmed the formation of elongated spherical shaped HA NPs with an average particle size of about 34 nm. The HA NPs thin film on glassy carbon electrode (GCE) were deposited by drop casting method. Electrocatalytic behavior of FA in the physiological pH 7.0 was investigated by cyclic voltammetry (CV), linear sweep voltammetry (LSV) and chronoamperometry. The fabricated HA/GCE exhibited a linear calibration plot over a wide FA concentration ranging from 1.0 × 10-7 to 3.5 × 10-4 M with the detection limit of 75 nM. In addition, the HA NPs modified GCE showed good selectivity toward the determination of FA even in the presence of a 100-fold excess of ascorbic acid (AA) and 1000-fold excess of other common interferents. The fabricated biosensor exhibits good sensitivity and stability, and was successfully applied for the determination of FA in pharmaceutical samples.

Kinetic research on dechlorinating dichlorobenzene in aqueous system by nano-scale nickel/iron loaded with CMC/NFC hydrogel.

PubMed

Wan, Xiao-Fang; Guo, Congbao; Liu, Yu; Chai, Xin-Sheng; Li, Youming; Chen, Guangxue

2018-03-01

In this study, we reported on the nano-scale nickel/iron particles loaded in carboxymethyl/nanofibrillated cellulose (CMC/NFC) hydrogel for the dechlorination of o-dichlorobenzene (DCB) in aqueous solution. The biodegradable hydrogel may provide an ideal supporting material for fastening the bimetallic nano-scale particles, which was examined and characterized by TEM, SEM-EDX, FT-IR and BET. The performance of the selected bimetallic particles was evaluated by conducting the dechlorination of DCB in the solution under different reaction conditions (e.g., pH, dosage of nickel/iron nanoparticles and temperature). The results showed that about 70% of DCB could be dechlorinated at 20 °C in 8 h, which indicated that the immobilized reactive material had a high reduction activity when Ni/Fe loading dosage in the hydrogel (18 wt%) was considered. Moreover, the reduction behavior agreed to the pseudo-first order reaction, in which the dechlorination rate was irrelative to the pH aqueous solution. A kinetic model for predicting the concentration of DCB during the reduction reaction was established based on the experimental data. Copyright © 2017 Elsevier Ltd. All rights reserved.

Fabrication of multicolor fluorescent polyvinyl alcohol through surface modification with conjugated polymers by oxidative polymerization

NASA Astrophysics Data System (ADS)

Hai, Thien An Phung; Sugimoto, Ryuichi

2018-06-01

A simple method for the preparation of multicolor polyvinyl alcohol (PVA) by chemical oxidative polymerization is introduced. The PVA surface was successfully modified with conjugated polymers composed of 3-hexylthiophene (3HT) and fluorene (F). The incorporation of the 3HT/F copolymer onto the PVA surface was confirmed by Fourier-transform infrared (FT-IR), ultraviolet-visible (UV-vis), and fluorescence spectroscopies, X-ray diffraction (XRD), as well as thermogravimetric analysis (TGA), contact angle, and field-emission scanning electron microscopy (FE-SEM) coupled with energy dispersive X-ray (EDX) analysis. Different 3HT/F ratios on the PVA surface result in optical properties that include multicolor-emission and absorption behavior. The color of the resultant (3HT/F)-g-PVA shifted from red to blue, and the quantum yield increased with increasing F content. The surface hydrophobicity of the modified PVA increased significantly through grafting with the conjugated polymers, with the water contact angle increasing by 30° compared to pristine PVA. The PVA XRD peaks were less intense following surface modification. Thermogravimetric analyses reveal that the thermal stability of the PVA decreases as a result of grafting with the 3HT/F copolymers.

Chitosan-doped-hybrid/TiO2 nanocomposite based sol-gel coating for the corrosion resistance of aluminum metal in 3.5% NaCl medium.

PubMed

J, Balaji; M G, Sethuraman

2017-11-01

The study outlines the role of chitosan, a biopolymer on corrosion behavior of Hy/nano-TiO 2 based sol-gel coating over aluminum metal. In this study organic-inorganic hybrid sols were synthesized through hydrolysis and condensation of 3-glycidoxypropyltrimethoxy silane (GPTMS), tetraethoxysilane (TEOS) and titanium (IV) isopropoxide (TIP) in acidic solution. Chitosan was doped into sol-gel matrix and self-assembled over aluminum substrate. The resultant chitosan-doped-Hy/nano-TiO 2 sol-gel coating was characterized by Fourier Transform Infrared (FT-IR) spectra, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM) and Energy-Dispersive X-ray Spectroscopy (EDX) analyses. The as-tailored aluminum substrate was evaluated for corrosion resistance in neutral medium. The protection ability of these coatings was evaluated by electrochemical impedance studies (EIS) and potentiodynamic polarization (PP) measurements in 3.5% NaCl medium. The EIS and PP results showed that chitosan-doped- Hy/nano-TiO 2 sol-gel coating exhibited better protection from corrosion than the undoped Hy/TiO 2 nanocomposite coating. Copyright © 2017 Elsevier B.V. All rights reserved.

Effect of solvents on the extraction of natural pigments and adsorption onto TiO2 for dye-sensitized solar cell applications

NASA Astrophysics Data System (ADS)

Al-Alwani, Mahmoud A. M.; Mohamad, Abu Bakar; Kadhum, Abd. Amir H.; Ludin, Norasikin A.

2015-03-01

Nine solvents, namely, n-hexane, ethanol, acetonitrile, chloroform, ethyl-ether, ethyl-acetate, petroleum ether, n-butyl alcohol, and methanol were used to extract natural dyes from Cordyline fruticosa, Pandannus amaryllifolius and Hylocereus polyrhizus. To improve the adsorption of dyes onto the TiO2 particles, betalain and chlorophyll dyes were mixed with methanol or ethanol and water at various ratios. The adsorption of the dyes mixed with titanium dioxide (TiO2) was also observed. The highest adsorption of the C.fruticosa dye mixed with TiO2 was achieved at ratio 3:1 of methanol: water. The highest adsorption of P.amaryllifolius dye mixed with TiO2 was observed at 2:1 of ethanol: water. H.polyrhizus dye extracted by water and mixed with TiO2 demonstrated the highest adsorption among the solvents. All extracted dye was adsorbed onto the surface of TiO2 based on Fourier Transform Infrared Spectroscopy (FTIR) analysis. The inhibition of crystallinity of TiO2 was likewise investigated by X-ray analysis. The morphological properties and composition of dyes were analyzed via SEM and EDX.

Improvement in the water retention characteristics of sandy loam soil using a newly synthesized poly(acrylamide-co-acrylic acid)/AlZnFe2O4 superabsorbent hydrogel nanocomposite material.

PubMed

Shahid, Shaukat Ali; Qidwai, Ansar Ahmad; Anwar, Farooq; Ullah, Inam; Rashid, Umer

2012-08-03

The use of some novel and efficient crop nutrient-based superabsorbent hydrogel nanocomposites (SHNCs), is currently becoming increasingly important to improve the crop yield and productivity, due to their water retention properties. In the present study a poly(Acrylamide-co-acrylic acid)/AlZnFe2O4 superabsorbent hydrogel nanocomposite was synthesized and its physical properties characterized using Energy Dispersive X-ray (EDX), FE-SEM and FTIR spectroscopic techniques. The effects of different levels of SHNC were studied to evaluate the moisture retention properties of sandy loam soil (sand 59%, silt 21%, clay 19%, pH 7.4, EC 1.92 dS/m). The soil amendment with 0.1, 0.2, 0.3 and 0.4 w/w% of SHNC enhanced the moisture retention significantly at field capacity compared to the untreated soil. Besides, in a separate experiment, seed germination and seedling growth of wheat was found to be notably improved with the application of SHNC. A delay in wilting of seedlings by 5-8 days was observed for SHNC-amended soil, thereby improving wheat plant growth and establishment.

Development of Processing Techniques for Advanced Thermal Protection Materials

NASA Technical Reports Server (NTRS)

Selvaduray, Guna; Cox, Michael; Srinivasan, Vijayakumar

1997-01-01

Thermal Protection Materials Branch (TPMB) has been involved in various research programs to improve the properties and structural integrity of the existing aerospace high temperature materials. Specimens from various research programs were brought into the analytical laboratory for the purpose of obtaining and refining the material characterization. The analytical laboratory in TPMB has many different instruments which were utilized to determine the physical and chemical characteristics of materials. Some of the instruments that were utilized by the SJSU students are: Scanning Electron Microscopy (SEM), Energy Dispersive X-ray analysis (EDX), X-ray Diffraction Spectrometer (XRD), Fourier Transform-Infrared Spectroscopy (FTIR), Ultra Violet Spectroscopy/Visible Spectroscopy (UV/VIS), Particle Size Analyzer (PSA), and Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES). The above mentioned analytical instruments were utilized in the material characterization process of the specimens from research programs such as: aerogel ceramics (I) and (II), X-33 Blankets, ARC-Jet specimens, QUICFIX specimens and gas permeability of lightweight ceramic ablators. In addition to analytical instruments in the analytical laboratory at TPMB, there are several on-going experiments. One particular experiment allows the measurement of permeability of ceramic ablators. From these measurements, physical characteristics of the ceramic ablators can be derived.

Synthesis and characterization of Ni NPs-doped silica-titania nanocomposites: structural, optical and photocatalytic properties

NASA Astrophysics Data System (ADS)

Islam, S.; Bidin, N.; Osman, S. S.; Krishnan, G.; Salim, A. A.; Riaz, S.; Suan, L. P.; Naseem, S.; Sanagi, M. M.

2017-01-01

The synthesis of Ni-doped silica-titania nanocomposite is performed by sol-gel method. The samples prior and after heat treatment at 300 °C for 1 h are characterized by analytical instrumental techniques. FE-SEM and AFM results indicate the regular morphology with low surface roughness without any cracks. EDX analysis verifies the formation of nanocomposites. XRD of the films reveals crystalline titania phases after annealing at 300 °C. The FTIR confirms the bond linkage between silica, titania and nickel molecules. High surface area 155 m2/g, pore volume of 0.2 cm3/g and pore diameter of 48.10 Å are obtained after heat treatment. The magnetic results show that the composite content is reminiscent of ferromagnetic hysteresis loop, with remanence magnetization Mr of 45.35 and 13.20 emu/g for both samples. The organic dye phenol red is used for the evaluation of photocatalytic activity of the synthesized magnetic material. The homogeneous surface morphology, crystalline nature, good solubility of magnetic nanoparticles into the silica-titania matrix show that the Ni/SiO2-TiO2 magnetic photocatalyst can be efficient and reusable.

Ultrasonic degradation of aqueous phenolsulfonphthalein (PSP) in the presence of nano-Fe/H2O2.

PubMed

Ayanda, Olushola S; Nelana, Simphiwe M; Naidoo, Eliazer B

2018-10-01

In this study, nano iron (nano-Fe) was successfully synthesized by sodium borohydride reduction of ferric chloride solution to enhance the ultrasonic degradation of phenolsulfonphthalein (PSP). The nano-Fe was characterized by scanning electron microscopy - energy dispersive spectroscopy (SEM-EDX), transmission electron microscopy (TEM), powder X-ray diffraction (XRD), attenuated total reflection - Fourier transform infrared spectroscopy (ATR-FTIR), and Brunauer, Emmett and Teller (BET) surface area determination. Experimental results demonstrated that a combined ultrasonic/nano-Fe/H 2 O 2 system was more effective for PSP removal in combination than they were individually and there was a significant difference between the combined and single processes. The ultrasonic/nano-Fe/H 2 O 2 degradation follows the Langmuir-Hinshelwood (L-H) kinetic model. The addition of nano-Fe and H 2 O 2 to the ultrasonic reactor greatly accelerated the degradation of PSP (25 mg/L) from 12.5% up to 96.5%. These findings indicated that ultrasonic degradation in the presence of nano-Fe and H 2 O 2 is a promising and efficient technique for the elimination of emerging micropollutants from aqueous solution. Copyright © 2018 Elsevier B.V. All rights reserved.

Photocatalytic activity against azo dye and cytotoxicity on MCF-7 cell lines of zirconium oxide nanoparticle mediated using leaves of Lagerstroemia speciosa.

PubMed

Sai Saraswathi, V; Santhakumar, K

2017-04-01

Metal oxide nanoparticles are gaining interest in recent years. The present paper explains about the green synthesis of zirconium oxide nanoparticles (ZrO NPs) mediated from the leaves of Lagerstroemia speciosa. The prepared ZrO NPs were characterized by UV-vis spectroscopy, FT-IR, X-ray diffraction analysis (XRD), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray spectroscopy (EDX) and Thermogravimetric Analysis (TGA). The photocatalytic activity of ZrO NPs was studied for azo dye by exposing to sunlight. The azo dye was degraded up to 94.58%. Also the ZrO NPs were studied for in vitro cytotoxicity activity against breast cancer cell lines-MCF-7 and evaluated by MTT assay. The cell morphological changes were recorded by light microscope. The cells viability was seen at 500μg/mL when compared against control. Hence the research highlights, that the method was simple, eco-friendly towards environment by phytoremediation activity of the azo dye and cytotoxicity activity against MCF-7 cell lines. Hence the present paper may help to further explore the metal nanoparticle for its potential applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Advancement in conductive cotton fabrics through in situ polymerization of polypyrrole-nanocellulose composites.

PubMed

Hebeish, A; Farag, S; Sharaf, S; Shaheen, Th I

2016-10-20

Current research was undertaking with a view to innovate a new approach for development of conductive - coated textile materials through coating cotton fabrics with nanocellulose/polypyrrole composites. The study was designed in order to have a clear understanding of the role of nanocellulose as well as modified composite thereof under investigation. It is anticipated that incorporation of nanocellulose in the pyrrole/cotton fabrics/FeCl3/H2O system would form an integral part of the composites with mechanical, electrical or both properties. Three different nanocellulosic substrates are involved in the oxidation polymerization reaction of polypyrrole (Ppy) in presence of cotton fabrics. Polymerization was subsequently carried out by admixing at various ratios of FeCl3 and pyrrole viz. Ppy1, Ppy2 and pp3. The conductive, mechanical and thermal properties of cotton fabrics coated independently with different nanocellulose/polypyrrole were investigated. FTIR, TGA, XRD, SEM and EDX were also used for further characterization. Results signify that, the conductivity of cotton fabrics increases exponentially with increasing the dose of pyrrole and oxidant irrespective of nanocellulose substrate used. While, the mechanical properties of cotton fabrics are not significantly affected by the oxidant treatment. Copyright © 2016 Elsevier Ltd. All rights reserved.

Electrophoretic deposition of gentamicin-loaded bioactive glass/chitosan composite coatings for orthopaedic implants.

PubMed

Pishbin, Fatemehsadat; Mouriño, Viviana; Flor, Sabrina; Kreppel, Stefan; Salih, Vehid; Ryan, Mary P; Boccaccini, Aldo R

2014-06-11

Despite their widespread application, metallic orthopaedic prosthesis failure still occurs because of lack of adequate bone-bonding and the incidence of post-surgery infections. The goal of this research was to develop multifunctional composite chitosan/Bioglass coatings loaded with gentamicin antibiotic as a suitable strategy to improve the surface properties of metallic implants. Electrophoretic deposition (EPD) was applied as a single-step technology to simultaneously deposit the biopolymer, bioactive glass particles, and the antibiotic on stainless steel substrate. The microstructure and composition of the coatings were characterized using SEM/EDX, XRD, FTIR, and TGA/DSC, respectively. The in vitro bioactivity of the coatings was demonstrated by formation of hydroxyapatite after immersion in simulated body fluid (SBF) in a short period of 2 days. High-performance liquid chromatography (HPLC) measurements indicated the release of 40% of the loaded gentamicin in phosphate buffered saline (PBS) within the first 5 days. The developed composite coating supported attachment and proliferation of MG-63 cells up to 10 days. Moreover, disc diffusion test showed improved bactericidal effect of gentamicin-loaded composite coatings against S. aureus compared to control non-gentamicin-loaded coatings.

Quinone-formaldehyde polymer as an active material in Li-ion batteries

NASA Astrophysics Data System (ADS)

Pirnat, Klemen; Mali, Gregor; Gaberscek, Miran; Dominko, Robert

2016-05-01

A benzoquinone polymer is synthesized by the polymerisation of hydrobenzoquinone and formaldehyde, followed by oxidation process using a hydrogen peroxide to convert hydroquinone to quinone. As prepared materials are characterized with FTIR, 1H-13C CPMAS NMR, pyrolysis coupled with gas chromatography (GC) and mass spectrometer (MS), TGA-MS analysis, EDX, elemental analysis, XRD, SEM and TEM microscopies and BET nitrogen adsorption. The benzoquinone polymer shows an excellent electrochemical performance when used as a positive electrode material in Li-ion secondary batteries. Using an electrolyte consisting 1 M bis(trifluoromethane)-sulfonimide lithium salt dissolved in 1,3-dioxolane and dimethoxyethane in a vol. ratio 1:1 (1 M LiTFSI/DOL + DME = 1:1) a stable capacity close to 150 mAh/g can be obtained. Compared to other electroactive materials based on benzoquinones it has a supreme capacity stability and is prepared by a simple synthesis using easily accessible starting materials. Further improvements in the capacity value (up to the theoretical value of 406 mAh/g) can be foreseen by achieving a higher degree of oxidation and by modification of polymerization process to enhance the electronic and ionic conductivity.

Innovative Linear Low Density Polyethylene Nanocomposite Films Reinforced with Organophilic Layered Double Hydroxides: Fabrication, Morphology and Enhanced Multifunctional Properties.

PubMed

Xie, Jiazhuo; Wang, Haijun; Wang, Zhou; Zhao, Qinghua; Yang, Yuechao; Waterhouse, Geoffrey I N; Hao, Lei; Xiao, Zihao; Xu, Jing

2018-01-08

Herein, we reported the successful development of novel nanocomposite films based on linear low density polyethylene (LLDPE) with enhanced anti-drop, optical, mechanical, thermal and water vapor barrier properties by introducing organophilic layered double hydroxides (OLDHs) nanosheets. OLDHs loadings were varied from 0-6 wt.%. Structural analyses using the Fourier transform infrared spectrum (FT-IR), X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) indicated that the OLDHs nanosheets were homogeneously dispersed with an ordered alignment in the LLDPE matrix. The LLDPE film containing 2 wt.% OLDHs (denoted as OLDHs-2) showed the optimal mechanical, thermal and water vapor barrier properties, whilst the anti-drop and optical performance of the films improved with increasing OLDHs content. The enhanced antidrop properties of the composite films relative to pristine LLDPE can be expected to effectively reduce agricultural losses to disease when the films are applied as agricultural films, whilst the superior light transmittance and water-retaining properties of the composite films will boost agricultural production. Results presented suggest that multifunctional LLDPE/OLDHs nanocomposites show great promise as low cost agricultural plastic films.

Ag/CuO nanoparticles prepared from a novel trinuclear compound [Cu(Imdz)4(Ag(CN)2)2] (Imdz = imidazole) by a pyrolysis display excellent antimicrobial activity

NASA Astrophysics Data System (ADS)

Adhikary, Jaydeep; Das, Balaram; Chatterjee, Sourav; Dash, Sandeep Kumar; Chattopadhyay, Sourav; Roy, Somenath; Chen, Jeng-Wei; Chattopadhyay, Tanmay

2016-06-01

One copper and two silver containing one hetero tri-nuclear precursor compound [Cu(Imdz)4(Ag(CN)2)2] (1) (Imdz = Imidazole) has been synthesized and characterized by single crystal X-ray diffraction. Simple pyrolysis of the complex at 550 °C for 4 h afforded Ag/CuO nanoparticles (NPs). The synthesized nanoparticles were characterized by ultraviolet-visible (UV-Vis), Fourier transform infrared (FT-IR), X-ray powder diffraction (XRPD), dynamic light scattering (DLS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive X-ray (EDX) and X-ray photo electron spectroscopy (XPS). Staphylococcus aureus (S. aureus) and Escherichia coli (E. coli) have been employed as model microbial species to study the anti-microbial activity of the synthesized NPs. The NPs showed potent anti-microbial activity evidenced from the Minimum Inhibitory Concentration (MIC) and Minimum Bactericidal Concentration (MBC) values. Very high level of cell uptake and then generation of reactive oxygen species (ROS) are the origin of such strong antimicrobial activity for the NPs. However, the cytotoxicity level of the NPs towards normal human cell is very low.

Biosynthesis of silver nanoparticles using ethanolic petals extract of Rosa indica and characterization of its antibacterial, anticancer and anti-inflammatory activities

NASA Astrophysics Data System (ADS)

Manikandan, Ramar; Manikandan, Beulaja; Raman, Thiagarajan; Arunagirinathan, Koodalingam; Prabhu, Narayanan Marimuthu; Jothi Basu, Muthuramalingam; Perumal, Muthulakshmi; Palanisamy, Subramanian; Munusamy, Arumugam

2015-03-01

The present study was aimed at biosynthesis of silver nanoparticles (AgNPs) using ethanolic extract of rose (Rosa indica) petals and testing their potential antibacterial activity using selective human pathogenic microbes, anticancer activity using human colon adenocarcinoma cancer cell line HCT 15 as well as anti-inflammatory activity using rat peritoneal macrophages in vitro. The biologically synthesized AgNPs were also characterized by UV-visible spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), energy-dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). The characterized AgNPs showed an effective antibacterial activity against Gram negative (Escherichia coli, Klebsiella pneumoniae) than Gram positive (Streptococcus mutans, Enterococcus faecalis) bacteria. MTT assay, analysis of nuclear morphology, mRNA expression of Bcl-2, Bax and protein expression of caspase 3 as well as 9, indicated potential anticancer activity. In addition, green synthesized AgNPs also attenuated cytotoxicity, nuclear morphology and free radical generation (O2- and NO) by rat peritoneal macrophages in vitro. The results of our study show the potential green synthesis of silver nanoparticles in mitigating their toxicity while retaining their antibacterial activities.

The behaviour of selected yttrium containing bioactive glass microspheres in simulated body environments.

PubMed

Cacaina, D; Ylänen, H; Simon, S; Hupa, M

2008-03-01

The study aims at the manufacture and investigation of biodegradable glass microspheres incorporated with yttrium potentially useful for radionuclide therapy of cancer. The glass microspheres in the SiO2-Na2O-P2O5-CaO-K2O-MgO system containing yttrium were prepared by conventional melting and flame spheroidization. The behaviour of the yttrium silicate glass microspheres was investigated under in vitro conditions using simulated body fluid (SBF) and Tris buffer solution (TBS), for different periods of time, according to half-life time of the Y-90. The local structure of the glasses and the effect of yttrium on the biodegradability process were evaluated by Fourier Transform Infrared (FT-IR) spectroscopy and Back Scattered Electron Imaging of Scanning Electron Microscopy (BEI-SEM) equipped with Energy Dispersive X-ray (EDX) analysis. UV-VIS spectrometry and Inductively Coupled Plasma Mass Spectrometry (ICP-MS) was used for analyzing the release behaviour of silica and yttrium in the two used solutions. The results indicate that the addition of yttrium to a bioactive glass increases its structural stability which therefore, induced a different behaviour of the glasses in simulated body environments.

Characterisation and sintering of nanophase hydroxyapatite synthesised by a species of Serratia

NASA Astrophysics Data System (ADS)

LSammons, R.; Thackray, A. C.; Medina Ledo, H.; Marquis, P. M.; Jones, I. P.; Yong, P.; Macaskie, L. E.

2007-12-01

The bacterium Serratia sp. NCIMB40259, which grows as a biofilm on polymeric, glass and metal substrates, produces extracellular crystals of hydroxyapatite (HA) by enzymatic cleavage of β-glycerophosphate in the presence of calcium chloride. Following growth on polyurethane foam, biomineralisation and subsequent sintering, an HA scaffold is formed whose three-dimensional architecture replicates that of the foam and the biofilm. Serratia HA was characterised using X-ray diffraction (XRD), Fourier Transform Infra-Red Spectroscopy (FTIR), energy dispersive X-ray analysis (EDX) scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED). The nascent, unsintered material consisted mainly of calcium-deficient HA (CDHA) with a Ca/P ratio of 1.61+/- 0.06 and crystal size (TEM) of 50 +/- 10nm length. ED of unsintered crystals and crystals sintered at 600° C showed resolvable ring (unsintered) or dot (600° C) patterns ascribed to (0002), (1122) and (0006) planes of crystalline HA. Material sintered at 1200° C consisted of needle-like crystals of length range 54-111nm (XRD) with lattice parameters of a = 9.441 Å and c = 6.875 Å, consistent with HA.

Chemical form analysis of reaction products in Cs-adsorption on stainless steel by means of HAXPES and SEM/EDX

NASA Astrophysics Data System (ADS)

Kobata, M.; Okane, T.; Nakajima, K.; Suzuki, E.; Ohwada, K.; Kobayashi, K.; Yamagami, H.; Osaka, M.

2018-01-01

In this study, for the understandings of Cesium (Cs) adsorption behavior on structure materials in severe accidents in a light water nuclear reactor, the chemical state of Cs and its distribution on the surface of SUS304 stainless steel (SS) with different Si concentrations was investigated by hard X-ray photoelectron spectroscopy (HAXPES) and scanning electron microscope/energy dispersive X-ray spectroscopy (SEM/EDX). As a result, it was found that Cs is selectively adsorbed at the site where Si distributes with a high concentration. CsFeSiO4 is the dominant Cs products in case of low Si content, while Cs2Si2O5 and Cs2Si4O9 are formed in addition to CsFeSiO4 in case of high Si content. The chemical forms of the Cs compounds produced in the adsorption process on the SS surface have a close correlation with the concentration and chemical states of Si originally included in SS.

Microwave assisted synthesis and characterization of barium titanate nanoparticles for multi layered ceramic capacitor applications.

PubMed

Thirumalai, Sundararajan; Shanmugavel, Balasivanandha Prabu

2011-01-01

Barium titanate is a common ferroelectric electro-ceramic material having high dielectric constant, with photorefractive effect and piezoelectric properties. In this research work, nano-scale barium titanate powders were synthesized by microwave assisted mechano-chemical route. Suitable precursors were ball milled for 20 hours. TGA studies were performed to study the thermal stability of the powders. The powders were characterized by XRD, SEM and EDX Analysis. Microwave and Conventional heating were performed at 1000 degrees C. The overall heating schedule was reduced by 8 hours in microwave heating thereby reducing the energy and time requirement. The nano-scale, impurity-free and defect-free microstructure was clearly evident from the SEM micrograph and EDX patterns. LCR meter was used to measure the dielectric constant and dielectric loss values at various frequencies. Microwave heated powders showed superior dielectric constant value with low dielectric loss which is highly essential for the fabrication of Multi Layered Ceramic Capacitors.

Characterization of morphology and composition of inorganic fillers in dental alginates.

PubMed

Guiraldo, Ricardo Danil; Berger, Sandrine Bittencourt; Consani, Rafael Leonardo Xediek; Consani, Simonides; de Carvalho, Rodrigo Varella; Lopes, Murilo Baena; Meneghel, Luciana Lira; da Silva, Fabiane Borges; Sinhoreti, Mário Alexandre Coelho

2014-01-01

Energy dispersive X-ray spectroscopy microanalysis (EDX), scanning electron microscopy (SEM), and Archimedes' Principle were used to determine the characteristics of inorganic filler particles in five dental alginates, including Cavex ColorChange (C), Hydrogum 5 (H5), Hydrogum (H), Orthoprint (O), and Jeltrate Plus (JP). The different alginate powders (0.5 mg) were fixed on plastic stubs (n = 5) and sputter coated with carbon for EDX analysis, then coated with gold, and observed using SEM. Volume fractions were determined by weighing a sample of each material in water before and after calcining at 450(°)C for 3 h. The alginate materials were mainly composed of silicon (Si) by weight (C-81.59%, H-79.89%, O-78.87%, H5-77.95%, JP-66.88%, wt). The filler fractions in volume (vt) were as follows: H5-84.85%, JP-74.76%, H-70.03%, O-68.31%, and C-56.10%. The tested materials demonstrated important differences in the inorganic elemental composition, filler fraction, and particle morphology.

Progress toward Synthesis and Characterization of Rare-Earth Nanoparticles

NASA Astrophysics Data System (ADS)

Romero, Dulce G.; Ho, Pei-Chun; Attar, Saeed; Margosan, Dennis

2010-03-01

Magnetic nanoparticles exhibit interesting phenomena, such as enhanced magnetization and reduced magnetic ordering temperature (i.e. superparamagnetism), which has technical applications in industry, including magnetic storage, magnetic imaging, and magnetic refrigeration. We used the inverse micelle technique to synthesize Gd and Nd nanoparticles given its potential to control the cluster size, amount of aggregation, and prevent oxidation of the rare-earth elements. Gd and Nd were reduced by NaBH4 from the chloride salt. The produced clusters were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive X-ray spectroscopy (EDX). The results from the XRD show that the majority of the peaks match those of the surfactant, DDAB. No peaks of Gd were observed due to excess surfactant or amorphous clusters. However, the results from the SEM and EDX indicate the presence of Gd and Nd in our clusters microscopically, and current synthesized samples contain impurities. We are using liquid-liquid extraction method to purify the sample, and the results will be discussed.

SEM and EDX Study of Stainless Steels, Suggested as Human Body Implants

NASA Astrophysics Data System (ADS)

Simitchiiska, R. N.; Ivanova, D.; Fachikov, L.

2018-06-01

The most important requirement for any material used as an implant is to be biocompatible and not to cause undesirable effects in the human body. Corrosion of implants is included in the topic of biocompatibility because it is a determining factor in their sustainability and seamless fulfillment of their functional purpose. The work presents the results obtained in the comparative study of two austenitic stainless steels (Cr18Ni9 and Cr18Mn12N) in two models of artificial saliva, accepted as environments for testing the corrosion behavior of materials for these aims. The nature of the corrosion attack, the composition of the corrosion products at 37°C and the pH 5.5 and pH 6.75 of the model media were determined using physical methods such as SEM and EDX of investigation and analysis. It was found that Cr18Mn12N steel (0.61 % N), exhibits higher corrosion resistance.

Nanosilver microalgae biosynthesis: cell appearance based on SEM and EDX methods

NASA Astrophysics Data System (ADS)

Pancasakti Kusumaningrum, Hermin; Zainuri, Muhammad; Marhaendrajaya, Indras; Subagio, Agus

2018-05-01

Microbial contamination has caused public health problems in the world population. This problem has spurred the development of methods to overcome and prevent microbial invasion. The extensive use of antibiotics has facilitated the continued emergence and spread of resistant organisms. Synthesized of silver nanoparticle (AgNPs) on microalgae Chlorella pyrenoidosa offer environmentally safe antimicrobial agent. The present study is focused on the biosynthesis of AgNPs using microalgae C. pyrenoidosa. The research methods was conducted by insertion of nanosilver particle into microalgae cells with and without agitation to speed up the process of formation nanosilver microalgae. The formation of microalgae SNP was analyzes by UV-Vis spectrophotometer, Scanning Electron Micrograph (SEM) and Energy-dispersive X-ray spectroscopy (EDX) methods. The research result showed that nanosilver microalgae biosynthesis using the agitation treatment was exhibited better performance in particle insertion and cell stability, comparing with no agitation treatment. However, synthesis of nanosilver microalgae tend to reduce the cell size.

Production of gold nanoparticles by electrode-respiring Geobacter sulfurreducens biofilms

PubMed Central

Tanzil, Abid H.; Sultana, Sujala T.; Saunders, Steven R.; Dohnalkova, Alice C.; Shi, Liang; Davenport, Emily; Ha, Phuc; Beyenal, Haluk

2017-01-01

The goal of this work was to synthesize gold nanoparticles (AuNPs) using electrode-respiring Geobacter sulfurreducens biofilms. We found that AuNPs are generated in the extracellular matrix of Geobacter biofilms and have an average particle size of 20 nm. The formation of AuNPs was verified using TEM, FTIR and EDX. We also found that the extracellular substances extracted from electrode-respiring G. sulfurreducens biofilms reduce Au3+ to AuNPs. From FTIR spectra, it appears that reduced sugars were involved in the bioreduction and synthesis of AuNPs and that amine groups acted as the major biomolecules involved in binding. PMID:27866628

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bernard, Laetitia, E-mail: laetitia.bernard@empa.ch; Leemann, Andreas

In this study, the potential of time-of-flight secondary ion mass spectrometry (ToF-SIMS) for the application in cement-based materials is assessed in combination and comparison with scanning electron microscopy (SEM) and energy dispersive X-ray (EDX). Mortar, concrete and samples from model systems providing products formed by the alkali–silica reaction (ASR) were studied. ToF-SIMS provides qualitative data on alkalis in cases where EDX reaches its limits in regard to detectable concentration, lateral resolution and atomic number of the elements. Due to its high in-depth resolution of a few atomic monolayers, thin layers of reaction products can be detected on the surfaces andmore » chemically analyzed with ToF-SIMS. Additionally, it delivers information on the molecular conformation within the ASR product, its hydrogen content and its isotope ratios, information not provided by EDX. Provided the samples are carefully prepared, ToF-SIMS opens up new possibilities in the analysis of cement-based materials.« less

Ionic liquid-impregnated activated carbon for biohydrogen purification in an adsorption unit

NASA Astrophysics Data System (ADS)

Yusuf, N. Y.; Masdar, M. S.; Isahak, W. N. R. W.; Nordin, D.; Husaini, T.; Majlan, E. H.; Rejab, S. A. M.; Chew, C. L.

2017-06-01

Biological methods for hydrogen production (biohydrogen) are known as energy intensive and can be operated at ambient temperature and pressure; however, consecutive productions such as purification and separation processes still remain challenging in the industry. Various techniques are used to purify and separate hydrogen. These techniques include the use of sorbents/solvents, membranes and cryogenic distillation. In this study, carbon dioxide (CO2) was purified and separated from biohydrogen to produce high purity hydrogen gas. CO2 capture was studied using the activated carbon (AC) modified with the ionic liquid (IL) choline chloride as adsorbent. The physical and chemical properties of the adsorbents were characterized through XRD, FTIR, SEM-EDX, TGA, and BET analyses. The effects of IL loading, flow rate, temperature, and gas mixture were also investigated based on the absorption and desorption of CO2. The CO2 level in the biohydrogen composition was analyzed using a CO2 gas analyzer. The SEM image indicated that the IL homogeneously covered the AC surface. High IL dispersion inlet enhanced the capability of the adsorbent to capture CO2 gas. The thermal stability and presence of the functionalized group of ILs on AC were analyzed by TGA and FTIR techniques, respectively. CO2 adsorption experiments were conducted using a 1 L adsorber unit. Hence, adsorption technologies exhibit potential for biohydrogen purification and mainly affected by adsorbent ability and operating parameters. This research presents an improved biohydrogen technique based on adsorption technology with novel adsorbents. Two different types of commercial CO2 adsorbents were used in the experiment. Results show that the IL/AC exhibited properties suitable for CO2 adsorption. The IL/AC sample presented a high CO2 uptake of 30 wt. % IL when treated at 30 °C for 6 h under a flow rate of 1 L/min. The presence of IL increased the selectivity of CO2 removal during the adsorption process. This IL/AC can be regenerated for several times without any significant loss in the performance.

Efficacy of Modified Bioactive Glass for Dentin Remineralization and Obstruction of Dentinal Tubules.

PubMed

Saffarpour, Mahshid; Mohammadi, Maryam; Tahriri, Mohammadreza; Zakerzadeh, Azadeh

2017-07-01

This study assessed the efficacy of modified bioactive glass (MBG) for dentin remineralization and obstruction of dentinal tubules. Thirty-six dentin discs were made from 20 third molars and were stored in 12% lactic acid solution for two weeks to induce demineralization. The samples were divided into three groups (n=12): 1- BG, 2- BG modified with 5% strontium (Sr) and 3- BG modified with 10% Sr. After applying the BG, the samples were stored in artificial saliva for 7, 14 and 21 days. Attenuated Total Reflection-Fourier Transform Infrared Spectroscopy (ATR-FTIR), X-ray Diffraction (XRD) analysis, Scanning Electron Microscopy (SEM), and Energy-Dispersive X-ray (EDX) analysis were used to assess remineralization. Also, 6 dentin discs were divided into three groups of BG, BG modified with 5% Sr and BG modified with 10% Sr, to examine tubular occlusion. The discs were etched using 0.5M of EDTA for two minutes and were stored in artificial saliva for 7 days. Changes in dentin surface morphology were evaluated under SEM. Group 3 showed high rates of remineralization at days 7 and 14, although the rate decreased at day 21. Group 2 exhibited high rates of remineralization at days 7, 14 and 21. Dentinal tubules were partially occluded by BG and BG modified with 5% Sr, while they were almost completely obstructed after the use of BG modified with 10% Sr. Strontium increases remineralization. Addition of 10% Sr to BG enhances apatite formation; however, the apatite dissolves over time. Addition of 5% Sr to BG stabilizes the apatite lattice and increases the remineralization.

Phase identification and morphology study of hematite (Fe2O3) with sintering time varitions

NASA Astrophysics Data System (ADS)

Yazirin, Cepi; Puspitasari, Poppy; Sasongko, Muhammad Ilman Nur; Tsamroh, Dewi Izzatus; Risdanareni, Puput

2017-09-01

Iron oxide has been the interest of many studies due to its applications in various scientific and industrial fields including in environment, corrosion, soil science, and exhaust emissions. Iron oxide (Fe2O3) has potential applications in catalytic reactions in electronic devices such as semiconductors, paint formulations, and lithium rechargeable batteries. Fe2O3 can be synthesized through the process of stirring, decomposition of organic iron, sol-gel, combustion, and evaporating solvents. Most of the methods used involve several steps and take a long time. The aim of this research was to investigate the phase and morphology characterization of iron oxide (Fe2O3) powder with solvent ethylene glycol after being sintered for 1 hour, 2 hours and 3 hours. The characterization tools utilized were XRD, SEM-EDX, and FTIR. The results of XRD analysis showed that the Fe2O3 sintered for 1 hour had the smallest crystallite size with a diameter of 21.05 nm. In the XRD test, the beam of X-ray was shot directly at the grain being tested. The results of SEM analysis showed thatthe Fe2O3 sintered for 1 hour produced the best result due to its crystallite size of 12.36 nm and hada shape of homogeneous nanosphere; the duration of sintering indeed had a great influence on the grain size of iron oxide (Fe2O3). In addition, the results of the elemental composition analysis indicate that the longer the sintering process, the higher the concentration of O but the lower the Fe.

Structural, magnetic and electronic structure properties of Co doped ZnO nanoparticles

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kumar, Shalendra, E-mail: shailuphy@gmail.com; School of Materials Science and Engineering, Changwon National University, Changwon, Gyeongnam 641-773; Song, T.K., E-mail: tksong@changwon.ac.kr

Highlights: • XRD and HR-TEM results show the single phase nature of Co doped ZnO nanoparticles. • XMCD and dc magnetization results indicate the RT-FM in Co doped ZnO nanoparticles. • Co L{sub 3,2} NEXAFS spectra infer that Co ions are in 2+ valence state. • O K edge NEXAFS spectra show that O vacancy increases with Co doping in ZnO. - Abstract: We reported structural, magnetic and electronic structure studies of Co doped ZnO nanoparticles. Doping of Co ions in ZnO host matrix has been studied and confirmed using various methods; such as X-ray diffraction (XRD), field emission scanningmore » electron microscopy (FE-SEM), energy dispersed X-ray (EDX), high resolution transmission electron microscopy (HR-TEM), Fourier transform infrared spectroscopy (FT-IR), near edge X-ray absorption fine structure (NEXAFS) spectroscopy, magnetic hysteresis loop measurements and X-ray magnetic circular dichroism (XMCD). From the XRD and HR-TEM results, it is observed that Co doped ZnO nanoparticles have single phase nature with wurtzite structure and exclude the possibility of secondary phase formation. FE-SEM and TEM micrographs show that pure and Co doped nanoparticles are nearly spherical in shape. O K edge NEXAFS spectra indicate that O vacancies increase with Co doping. The Co L{sub 3,2} edge NEXAFS spectra revealed that Co ions are in 2+ valence state. DC magnetization hysteresis loops and XMCD results clearly showed the intrinsic origin of temperature ferromagnetism in Co doped ZnO nanoparticles.« less

Co(II), Ni(II), Cu(II) and Zn(II) complexes of tridentate ONO donor Schiff base ligand: Synthesis, characterization, thermal, non-isothermal kinetics and DFT calculations

NASA Astrophysics Data System (ADS)

Kusmariya, Brajendra S.; Mishra, A. P.

2017-02-01

We report here four mononuclear Co(II), Ni(II), Cu(II) and Zn(II) coordination compounds of general formula [M(L)2] {L = dcp; M = CoII, CuII & ZnII} and [M(L)(H2O)]·H2O {L = dcp; M = NiII} derived from tridentate 2,4-dichloro-6-{[(3-chloro-2-hydroxy-5-nitrophenyl)imino]methyl}phenol (dcp) ligand. These compounds were synthesized and characterized by elemental analysis, FT-IR, uv-vis, 1H NMR, molar conductance, magnetic moment, thermal, PXRD and SEM-EDX. The Powder X-ray Diffraction patterns and SEM analyses showed the crystalline nature of synthesized compounds. The peak broadening was explained in terms of crystallite size and the lattice strain using Scherrer and Williamson-Hall method. Thermogravimetric analysis was performed to determine the thermal stability of synthesized compounds under nitrogen atmosphere up to 820 K at 10 Kmin-1 heating rate. The kinetic and thermodynamic parameters of thermal decomposition were calculated using Coats-Redfern (C-R), Piloyan-Novikova (P-N) and Horowitz-Metzger (H-M) methods assuming first order degradation. The calculated optical band gap values of complexes were found to be in semiconducting range. To support the experimental findings, and derive some fruitful information viz. frequency calculations, HOMO-LUMO, energy gap (ΔE), molecular electrostatic potential (MEP), spin density, absorption spectra etc.; theoretical calculations by means of DFT and TD-DFT at B3LYP level were incorporated.

A Golden Drachma From Bruttia: Counterfeit Money Revealed By Scanning Electron Microscopy and Cathodoluminescence.

NASA Astrophysics Data System (ADS)

Pingitore, Valentino; Barberio, Marianna; Oliva, Antonino; Noce, Nicoletta; Gattuso, Caterina; Davoli, Mariano

Diagnostic studies performed on an ancient coin are presented in order to find if the coin is authentic or is a coinage proof. Our investigation includes Scanning Electron Microscopy - Energy Dispersive X-ray (SEM-EDX) and Cathodoluminescence (CL). The coin is a Drachma representing on the obverse the portrait of Poseidon and, on the reverse the figure of Anfitrite riding a seahorse while Eros is shooting an arrow. The coin is well known in the numismatic studies and originals can also be found in Catanzaro, Naples or Milan museums. The EDX analysis, executed on narrow points of the surface, revealed Pb and Cu as main components of the coin on both sides: 51% of Pb and 35% of Cu their weight and surprisingly on both sides traces of gold was found. The maximum dimensions and the percentage in weight of the small revealed gold spots were respectively on the order of 20 μm and 95%. At the same time luminescence emission induced by electron bombardment (CL) on these spots was executed. This analysis confirmed SEM results, though the presence of Au was more evident than in SEM analysis. In fact CL analysis showed a little presence of Au throughout the sample surface.

Investigation on by-products of bioenergy systems (anaerobic digestion and gasification) as potential crop nutrient using FTIR, XRD, SEM analysis and phyto-toxicity test.

PubMed

Kataki, Sampriti; Hazarika, Samarendra; Baruah, D C

2017-07-01

Success and acceptability of the bio energy conversion technology to a large extent depend upon management of the inevitable by-products generated during the conversion process. By-products can be considered favourable as organic fertilizer as they retain nutrients with varying composition depending upon input biomass. However, characteristics of these heterogeneous resources with respect to feedstock and processing conditions have to be assessed to state on their agricultural and environmental benefits. Therefore, 3 types of anaerobic digestion by-products (digestate) from surplus biomass viz. cow dung, Ipomoea carnea:cow dung (60:40 dry weight basis) and rice straw:green gram stover:cow dung (30:30:40 dry weight basis) and one gasification by-product (biochar) from rice husk are considered to understand the fertilizer prospects. Considering 3 potential application options, digestate from each feedstock option was further processed as separated solid, separated liquid and ash from solid digestates. Thus, a total of 10 by-products were investigated for understanding their prospects as fertilizer using Fourier Transform Infrared Spectroscopy (FTIR), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Energy Dispersive X ray Spectroscopy (EDX) and phyto-toxicity test to have a broad insight in terms of their organic, mineral, elemental composition, morphological feature and potential phyto-toxicity. In general, irrespective of origin of feedstock, solid digestate, ash digestate and char showed similarity in terms of composition of functional groups with some degree of variation in relative content as reflected by FTIR analysis. Dominance of organic functional groups in separated solid digestates compared to liquid fraction indicated the former as favourable organic amendments. Quartz was the prevalent mineral phase in all separated solid, ash digestate and rice husk char. Digestates in ash phase represent more concentrated plant nutrient source with higher content of K, Ca, P, Na and Mg than their respective solid phase. Application of ash digestates and char is likely to improve adsorptive capacity of soil for water and nutrient due to presence of relatively uniformly distributed porous particles. Liquid fraction of Ipomoea digestates exhibited inhibitory effect on seed germination of greengram (Vigna radiate) with significant reduction of germination index. Inhibitory effects of by-products were found to correlate negatively with their electrical conductivity and ammonia-nitrogen content. Understanding on spectroscopic, morphological and phytotoxic properties of different application options of bioenergy by-products would be useful for assessment of their appropriate use in agriculture. Copyright © 2017 Elsevier Ltd. All rights reserved.

IDENTIFICATION OF POSSIBLE SOURCES OF PARTICULATE MATTER IN THE PERSONAL CLOUD USING SEM/EDX

EPA Science Inventory

The United States Environmental Protection Agency (U.S. EPA) conducted the Baltimore Particulate Matter (PM) Epidemiology-Exposure Study of the Elderly during the summer of 1998. The study design included PM2.5 samples obtained from elderly (65+ years of age) retirement facility ...

Gold nanoparticles: sonocatalytic synthesis using ethanolic extract of Andrographis paniculata and functionalization with polycaprolactone-gelatin composites

NASA Astrophysics Data System (ADS)

Babu, Punuri Jayasekhar; Saranya, Sibyala; Sharma, Pragya; Tamuli, Ranjan; Bora, Utpal

2012-09-01

Gold nanoparticles (AuNPs) were synthesized by sonication using ethanolic leaf extract of Andrographis paniculata. We investigated the optimum parameters for AuNP synthesis and functionalization with polycaprolactone-gelatin (PCL-GL) composites. The AuNPs were characterized with various biophysical techniques such as TEM, XRD, FT-IR and EDX spectroscopy. TEM images showed that nanoparticles were spherical in shape with a size range from 5 to 75 nm. EDX analysis revealed the presence of molecular oxygen and carbon on the surface of AuNPs. The synthesized AuNPs were tested for their effect on HeLa (human cervical cancer) and MCF-7 (human breast cancer) cell lines and found to be nontoxic and biocompatible, which are potential carriers for hydrophobic drugs.

Effective coating of titania nanoparticles with alumina via atomic layer deposition

NASA Astrophysics Data System (ADS)

Azizpour, H.; Talebi, M.; Tichelaar, F. D.; Sotudeh-Gharebagh, R.; Guo, J.; van Ommen, J. R.; Mostoufi, N.

2017-12-01

Alumina films were deposited on titania nanoparticles via atomic layer deposition (ALD) in a fluidized bed reactor at 180 °C and 1 bar. Online mass spectrometry was used for real time monitoring of effluent gases from the reactor during each reaction cycle in order to determine the optimal dosing time of precursors. Different oxygen sources were used to see which oxygen source, in combination with trimethyl aluminium (TMA), provides the highest alumina growth per cycle (GPC). Experiments were carried out in 4, 7 and 10 cycles using the optimal dosing time of precursors. Several characterization methods, such as high resolution transmission electron microscopy (HRTEM), Brunauer-Emmett-Teller (BET), energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared (FTIR), X-ray diffraction (XRD) and instrumental neutron activation analysis (INAA), were conducted on the products. Formation of the alumina film was confirmed by EDX mapping and EDX line profiling, FTIR and TEM. When using either water or deuterium oxide as the oxygen source, the thickness of the alumina film was greater than that of ozone. The average GPC measured by TEM for the ALD of TMA with water, deuterium oxide and ozone was about 0.16 nm, 0.15 nm and 0.11 nm, respectively. The average GPC calculated using the mass fraction of aluminum from INAA was close to those measured from TEM images. Excess amounts of precursors lead to a higher average growth of alumina film per cycle due to insufficient purging time. XRD analysis demonstrated that amorphous alumina was coated on titania nanoparticles. This amorphous layer was easily distinguished from the crystalline core in the TEM images. Decrease in the photocatalytic activity of titania nanoparticles after alumina coating was confirmed by measuring degradation of Rhodamine B by ultraviolet irradiation.

Microscopic and Metallurgical Aspects of the Space Shuttle Columbia Accident Investigation and Reconstruction

NASA Technical Reports Server (NTRS)

McDaniels, Steven J.

2004-01-01

The Space Shuttle Columbia was descending for a landing at the Kennedy Space Center (KSC) on February 1, 2003. Approximately 20 minutes prior to touchdown, the Columbia began disintegrating over the western United States; the majority of debris eventually impacted in eastern Texas and western Louisiana. A monumental effort eventually recovered approximately 84,000 pieces of debris, approximately 38% of the Orbiter's original dry weight. The debris was transported to KSC, where the items were catalogued and evaluated. Critical areas of interest, such as the left and right leading edge surfaces and the underside of the ship, were placed upon a grid to aid in the reconstruction. Items of interest included metallic structures, reinforced carbon-carbon composites, and ceramic heat insulation tiles. Many of the leading edge elements had re-solidified metallic deposits spattered on them. These deposits became known as slag and were one of the main focuses of the investigation. In order to help determine the sequence of events inside the left wing during the accident, the slag's composition, layering order, and directionality of deposition were studied. A myriad of analytical tests were performed in an attempt to ascertain the compositional and depositional characteristics of selected slag deposits, including the ordering of deposited layers within each individual slag deposit harvested. Initially, Scanning Electron Microscopy and Energy Dispersive X-Ray Spectroscopy (SEM/EDX) were performed to quickly characterize the overall composition of individual slag deposits: SEM utilizes a narrowlyfocused high-energy electron beam impinging upon a specimen. The incident beam excites and liberates lower energy secondary electrons, which are detected and analyzed, providing a visual representation of the sample's surface topography. EDX also relies on an incident electron beam, except an EDX unit measures X-ray energies generated by the impinging beam. Each element generates a unique X-ray signature; the EDX detector measures these discreet energies. EDX actually penetrates approximately 2 microns into the bulk of the sample. However, random examination of various portions of slag, coupled with the semiquantitative nature of the SEM/EDX analysis, did not yield convincingly pertinent data. Therefore, X-ray dot mapping was conducted, which provided more understandable data, both in terms of slag layering and composition. An X-ray dot map is generated by performing numerous EDX scans for individual elements, then compiling the scans in a visual representation. Eventually, specimens consisting of not only the slag, but of the adjacent RCC substrate as well were cross-sectioned. X-Ray dot mapping of the materialographicallymounted and -polished cross- sections provided a visual representation of both the layering sequence and compositional characteristics of the slag. Contemporaneously, Electron Spectroscopy for Chemical Analysis/X-Ray Photoelectron Spectroscopy (ESCA/XPS) and powdered X-Ray Diffraction (XRD) were performed to further characterize the deposits and to attempt to identify what, if any, compounds were present. The ESCA/XPS analysis allowed the analyst to "sputter" into the sample with an electron gun, aiding in the identification of the layering sequence. XPS uses photons, rather than electrons, which impinge upon the surface of the sample. XPS measures the electrons emitted from within the first 5 nm of the sample's surface. The XRD measures the scatter angles of incident X-rays; the angle and intensity of scatter depend upon the crystalline structure of the pulverized sample. XRD is considered a qualitative rather than quantitative technique. ESCA/XPS revealed that the final layer to deposit was predominantly carbonaceous. XRD was successful in identifying specific compounds, such as Al 2O3, Al and/or Al3 21SiO47, mullite (3(Al2)O3 -SiO2), and nickel-aluminides. Eventually, Electron MicroProbe Analysis (EMPA) was conducted on the marialographically-prepared cross- sections of selected slag deposits. Microprobe combines SEM and Wavelength Dispersive X-Ray Spectroscopy (WDS), and, like EDX, uses a narrowly-focused high-energy electron beam impinging upon a specimen to elicit, in the case of EPMA, characteristic X-rays with specific wavelengths. This quantitative, analytical tool proved the most useful in determining depositional layering and composition of the slag deposits. This information was utilized in verifying the location of the breach in the left leading edge of the wing of the Columbia.

Sorption isotherms, kinetic and optimization process of amino acid proline based polymer nanocomposite for the removal of selected textile dyes from industrial wastewater.

PubMed

Raghunath, Sharista; Anand, K; Gengan, R M; Nayunigari, Mithil Kumar; Maity, Arjun

2016-12-01

In this article, adsorption and kinetic studies were carried out on three textile dyes, namely Reactive Blue 222 (RB 222), Reactive Red 195 (RR 195) and Reactive Yellow 145 (RY 145). The dyes studied in a mixture were adsorbed under various conditions onto PRO-BEN, a bentonite modified with a new cationic proline polymer (l-proline-epichlorohydrin polymer). The proline polymer was characterized by 1 H NMR, Fourier transform infrared spectroscopy (FT-IR), dynamic light scattering (DLS) and TEM. The PRO-BEN composite was characterized by FT-IR, dynamic light scattering (DLS) (zeta potential), TEM imaging, SEM/EDX and X-ray photoelectron spectroscopy (characterize the binding energy). During adsorption studies, factors involving pH, temperature, the initial concentrations of the dyes and the quantity of PRO-BEN used during adsorption were established. The results revealed that the adsorption mechanism was categorized by the Langmuir type 1 isotherm. The adsorption data followed the pseudo-second order kinetic model. The intraparticle diffusion model indicated that adsorption did not only depend on the intraparticle diffusion of the dyes. The thermodynamic parameters verified that the adsorption process was spontaneous and exothermic. The Gibbs free energy values indicated that physisorption had occurred. Successful adsorption of dyes from an industrial effluent was achieved. Desorption studies concluded that PRO-BEN desorbed the dyes better than alumina. This can thereby be viewed as a recyclable remediation material. The PRO-BEN composite could be a cost efficient alternative towards the removal of organic dyes in wastewater treatment. Copyright © 2016 Elsevier B.V. All rights reserved.

Adsorption of nucleotides on biomimetic apatite: The case of adenosine 5⿲ triphosphate (ATP)

NASA Astrophysics Data System (ADS)

Hammami, Khaled; El-Feki, Hafed; Marsan, Olivier; Drouet, Christophe

2016-01-01

ATP is a well-known energy supplier in cells. The idea to associate ATP to pharmaceutical formulations/biotechnological devices to promote cells activity by potentially modulating their microenvironment thus appears as an appealing novel approach. Since biomimetic nanocrystalline apatites have shown great promise for biomedical applications (bone regeneration, cells diagnostics/therapeutics, ⿦), thanks to a high surface reactivity and an intrinsically high biocompatibility, the present contribution was aimed at exploring ATP/apatite interactions. ATP adsorption on a synthetic carbonated nanocrystalline apatite preliminarily characterized (by XRD, FTIR, Raman, TG-DTA and SEM-EDX) was investigated in detail, pointing out a good agreement with Sips isothermal features. Adsorption characteristics were compared to those previously obtained on monophosphate nucleotides (AMP, CMP), unveiling some specificities. ATP was found to adsorb effectively onto biomimetic apatite: despite smaller values of the affinity constant KS and the exponential factor m, larger adsorbed amounts were reached for ATP as compared to AMP for any given concentration in solution. m < 1 suggests that the ATP/apatite adsorption process is mostly guided by direct surface bonding rather than through stabilizing intermolecular interactions. Although standard οGads ° was estimated to only ⿿4 kJ/mol, the large value of Nmax led to significantly negative effective οGads values down to ⿿33 kJ/mol, reflecting the spontaneous character of adsorption process. Vibrational spectroscopy data (FTIR and Raman) pointed out spectral modifications upon adsorption, confirming chemical-like interactions where both the triphosphate group of ATP and its nucleic base were involved. The present study is intended to serve as a basis for future research works involving ATP and apatite nanocrystals/nanoparticles in view of biomedical applications (e.g. bone tissue engineering, intracellular drug delivery, ⿦).

Preparation and characterization of NiW-nHA composite catalyst for hydrocracking

NASA Astrophysics Data System (ADS)

Zhou, Gang; Hou, Yongzhao; Liu, Lei; Liu, Hongru; Liu, Can; Liu, Jing; Qiao, Huiting; Liu, Wenyong; Fan, Yubo; Shen, Shituan; Rong, Long

2012-11-01

The synthesis, characterization and catalytic capability of the NiW-nano-hydroxyapatite (NiW-nHA) composite were investigated in this paper. The NiW-nHA catalyst was prepared by a co-precipitation method. Then Fourier transform infrared (FT-IR) spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD) and energy dispersive spectroscopy (EDX) were used to analyze this material. In addition, the catalytic capacity of the NiW-nHA composite was also examined by FT-IR and gas chromatography (GC). The results of FT-IR analysis indicated that Ni, W and nHA combined closely. TEM observation revealed that this catalyst was needle shaped and the crystal retained a nanometer size. XRD data also suggested that a new phase of CaWO4 appeared and the lattice parameters of nHA changed in this system. nHA was the carrier of metals. The rates of Ni/W-loading were 73.24% and 65.99% according to the EDX data, respectively. Furthermore, the conversion of 91.88% Jatropha oil was achieved at 360 °C and 3 MPa h-1 over NiW-nHA catalyst. The straight chain alkanes ranging from C15 to C18 were the main components in the production. The yield of C15-C18 alkanes was up to 83.56 wt%. The reaction pathway involved hydrocracking of the C&z.dbd;C bonds of these triglycerides from Jatropha oil. This paper developed a novel non-sulfided catalyst to obtain a ``green biofuel'' from vegetable oil.

Surface modification of an aluminum alloy by electron beam introducing TiCN nanoparticles

NASA Astrophysics Data System (ADS)

Kolev, M.; Dimitrova, R.; Parshorov, St.; Valkov, St.; Lazarova, R.; Petrov, P.

2018-03-01

TiCN nanopowder deposited in an appropriate way on the surface of an AlSi12Cu2NiMg substrate was incorporated in the matrix using an electron beam technology. The samples were studied by means of light microscopy, SEM, and EDX; their microhardness was also determined. The formation was found of a uniform and dense coating with a thickness of 7 – 10 μgm with a good adherence to the substrate. A modified zone appeared under the coating with a thickness of 100 – 150 μgm containing dendrites of an α-solid solution and a fine eutectic between them, as well as primary silicon crystals. The microhardness of this modified zone was up to 2.4 times higher than that of the matrix. The results of SEM and EDX studies revealed unambiguously the presence of titanium in the coating and in the zones below it. Obviously, the electron beam treatment resulted in the TiCN nanoparticles penetrating into the coating and the substrate immediately below the coating.

Rapid extra-/intracellular biosynthesis of gold nanoparticles by the fungus Penicillium sp.

NASA Astrophysics Data System (ADS)

Du, Liangwei; Xian, Liang; Feng, Jia-Xun

2011-03-01

In this work, the fungus Penicillium was used for rapid extra-/intracellular biosynthesis of gold nanoparticles. AuCl4 - ions reacted with the cell filtrate of Penicillium sp. resulting in extracellular biosynthesis of gold nanoparticles within 1 min. Intracellular biosynthesis of gold nanoparticles was obtained by incubating AuCl4 - solution with fungal biomass for 8 h. The gold nanoparticles were characterized by means of visual observation, UV-Vis absorption spectroscopy, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDX). The extracellular nanoparticles exhibited maximum absorbance at 545 nm in UV-Vis spectroscopy. The XRD spectrum showed Bragg reflections corresponding to the gold nanocrystals. TEM exhibited the formed spherical gold nanoparticles in the size range from 30 to 50 nm with an average size of 45 nm. SEM and TEM revealed that the intracellular gold nanoparticles were well dispersed on the cell wall and within the cell, and they are mostly spherical in shape with an average diameter of 50 nm. The presence of gold was confirmed by EDX analysis.

Determination of precursor sites for pitting corrosion of polycrystalline titanium by using different techniques

DOE Office of Scientific and Technical Information (OSTI.GOV)

Garfias-Mesias, L.F.; Alodan, M.; James, P.I.

1998-06-01

Scanning electrochemical microscopy (SECM) in ferrocyanide and bromide solutions was used to locate active sites (pitting precursors) on polycrystalline Ti where oxidation of Br{sup {minus}} and Fe(CN){sub 6}{sup 4{minus}} was possible. Analysis of the electrochemically active sites was done by using electron microscopy (SEM), energy dispersive X-ray analysis (EDX), atomic force microscopy (AFM), and in situ confocal laser scanning microscopy (CLSM). In most cases, the active sites were found to be associated with particles (inclusions) which contained mainly Al and Si; however, some other areas not associated with particles were also found to be active. Although the size of themore » inclusions was normally smaller than 20 {micro}m, as revealed by SEM and AFM imaging, in some cases larger particles were also found. Pitting corrosion tests in bromide solution at potentials above 1.5 V{sub SCE} followed by EDX analysis inside the pits and in situ CLSM observation, confirmed that most of the localized attack started in the areas where particles had been located.« less

Laser engravings as reason for mechanical failure of titanium-alloyed total hip stems.

PubMed

Kluess, Daniel; Steinhauser, Erwin; Joseph, Micheal; Koch, Ursula; Ellenrieder, Martin; Mittelmeier, Wolfram; Bader, Rainer

2015-07-01

Two revisions of broken β-titanium total hip stems had to be performed in our hospital after 2 and 4 years in situ. Since both fractures were located at the level of a laser engraving, a failure analysis was conducted. Both retrieved hip stems were disinfected and collected in our retrieval database after patient's signed agreement. Each fragment was macroscopically photographed. Fracture surfaces were analyzed using scanning electron microscopy (SEM). Quantification of element content was conducted using energy dispersive X-ray (EDX) analysis. Both stems show fatigue fracture, as displayed by the lines of rest on the fracture surface. The origin of fracture was identified directly at the laser engraving of the company logo at both stems by means of SEM. The EDX analysis showed an oxygen level beneath the laser engraving about twice as high as in the substrate, causing material embrittlement. Laser engravings need to be reduced to a minimum of necessary information, and should be placed at locations with minimum mechanical load. Biomechanical analyses are recommended to identify less loaded areas in implant components to avoid such implant failures.

Characterization of Morphology and Composition of Inorganic Fillers in Dental Alginates

PubMed Central

Guiraldo, Ricardo Danil; Berger, Sandrine Bittencourt; Consani, Rafael Leonardo Xediek; Consani, Simonides; de Carvalho, Rodrigo Varella; Lopes, Murilo Baena; Meneghel, Luciana Lira; da Silva, Fabiane Borges; Sinhoreti, Mário Alexandre Coelho

2014-01-01

Energy dispersive X-ray spectroscopy microanalysis (EDX), scanning electron microscopy (SEM), and Archimedes' Principle were used to determine the characteristics of inorganic filler particles in five dental alginates, including Cavex ColorChange (C), Hydrogum 5 (H5), Hydrogum (H), Orthoprint (O), and Jeltrate Plus (JP). The different alginate powders (0.5 mg) were fixed on plastic stubs (n = 5) and sputter coated with carbon for EDX analysis, then coated with gold, and observed using SEM. Volume fractions were determined by weighing a sample of each material in water before and after calcining at 450°C for 3 h. The alginate materials were mainly composed of silicon (Si) by weight (C—81.59%, H—79.89%, O—78.87%, H5—77.95%, JP—66.88%, wt). The filler fractions in volume (vt) were as follows: H5—84.85%, JP—74.76%, H—70.03%, O—68.31%, and C—56.10%. The tested materials demonstrated important differences in the inorganic elemental composition, filler fraction, and particle morphology. PMID:25165690

Mapping chemical elements on the surface of orthodontic appliance by SEM-EDX

PubMed Central

Mikulewicz, Marcin; Wołowiec, Paulina; Michalak, Izabela; Chojnacka, Katarzyna; Czopor, Wojciech; Berniczei-Royko, Adam; Vegh, Andras; Gedrange, Thomas

2014-01-01

Background During orthodontic treatment, the various elements that constitute the fixed appliance undergo different processes. As a result of a change of the surface, elution/coverage of metals on the surface can be observed in the process of corrosion/passivation. Material/Methods Scanning electron microscopy with an energy-dispersive X-ray analytical system (SEM-EDX) was used to analyze the composition of stainless steel elements of orthodontic fixed appliances (before and after orthodontic treatment), to obtain the composition of the surface of the elements. The analyzed elements were: brackets (Victory Series APC PLUS 022, 3M Unitek, Monrovia, CA, USA); wires (0.017×0.025, 3M Unitek, Monrovia, CA, USA); and bands (37+, 3M Unitek, Monrovia, CA, USA). Results The results showed a decrease of chromium and iron contribution to the surface, with increase of oxygen content in used vs. new elements of the appliance. Conclusions Our results confirm the formation of oxides (passivation layer) on the surface of stainless steel as a result of the presence of the orthodontic appliance in patients’ oral cavities. PMID:24857929

Mapping chemical elements on the surface of orthodontic appliance by SEM-EDX.

PubMed

Mikulewicz, Marcin; Wołowiec, Paulina; Michalak, Izabela; Chojnacka, Katarzyna; Czopor, Wojciech; Berniczei-Royko, Adam; Vegh, Andras; Gedrange, Thomas

2014-05-25

During orthodontic treatment, the various elements that constitute the fixed appliance undergo different processes. As a result of a change of the surface, elution/coverage of metals on the surface can be observed in the process of corrosion/passivation. Scanning electron microscopy with an energy-dispersive X-ray analytical system (SEM-EDX) was used to analyze the composition of stainless steel elements of orthodontic fixed appliances (before and after orthodontic treatment), to obtain the composition of the surface of the elements. The analyzed elements were: brackets (Victory Series APC PLUS 022, 3M Unitek, Monrovia, CA, USA); wires (0.017×0.025, 3M Unitek, Monrovia, CA, USA); and bands (37+, 3M Unitek, Monrovia, CA, USA). The results showed a decrease of chromium and iron contribution to the surface, with increase of oxygen content in used vs. new elements of the appliance. Our results confirm the formation of oxides (passivation layer) on the surface of stainless steel as a result of the presence of the orthodontic appliance in patients' oral cavities.

Femtosecond laser ablation of cemented carbides: properties and tribological applications

NASA Astrophysics Data System (ADS)

Dumitru, G.; Romano, V.; Weber, H. P.; Gerbig, Y.; Haefke, H.; Bruneau, S.; Hermann, J.; Sentis, M.

Laser ablation with fs laser pulses was performed in air on cobalt cemented tungsten carbide by means of a Ti : sapphire laser (800 nm, 100 fs). Small and moderate fluences (2, 5, 10 J/cm2) and up to 5×104 pulses per irradiated spot were used to drill holes with aspect ratios up to 10. Cross-section cuts from laser-irradiated samples were produced and they were analysed with optical microscopy and SEM. EDX analyses were carried out on selected zones. Quasi-cylindrical holes were found for 2 J/cm2, whereas for 5 and 10 J/cm2 irregular shapes (lobes, bottoms wider than hole entrances) were found to occur after a given number of incident pulses. Layers with modified structure were evidenced at pore walls. SEM revealed a denser structure, while EDX analyses showed uniform and almost similar contents of W, C, and Co in these layers. As a direct application, patterning of coated WC-Co was carried out with 2 J/cm2 and 100 pulses per pore. The resulted surfaces were tribologically tested and these tests revealed an improved friction and wear behaviour.

Photoelectrochemical Performance of TiO2/Ti Electrode for Organic Compounds

NASA Astrophysics Data System (ADS)

Maulidiyah, M.; Wijawan, I. B. P.; Wibowo, D.; Aladin, A.; Hamzah, B.; Nurdin, M.

2018-05-01

Photoelectrochemical performance of TiO2/Ti electrode was investigated by using organic compounds. The TiO2/Ti electrode was prepared by anodic oxidation at a potential bias of 25 V for 4 h then calcined for 450 °C to obtain the anatase polymorph. Subsequently, it was characterized by X-Ray Diffraction (XRD) and Scanning Electron Microscope-Energy Dispersive X-ray (SEM-EDX). The XRD pattern showed that TiO2 has anatase phase as confirmed by 2θ peaks at 37.93° 63.00°, and 83.00°. Using SEM-EDX data the TiO2 layer was formed on Ti plate with the composition of Ti (4.5 keV) and O (0.5 keV) elements. Furthermore, the photoelectrochemical sensing on the three organic compounds (ascorbic acid, glucose, and titan yellow) with the electrolyte addition showed that the linearity of TiO2/Ti electrode were 0.937, 0.968, and 0.938, meanwhile without the electrolyte were 0.998, 0.989, and 0.923, respectively.

Effects of laser-aided circumferential supracrestal fiberotomy on root surfaces.

PubMed

Lee, Ji-Won; Park, Ki-Ho; Chung, Jong-Hyuk; Kim, Su-Jung

2011-11-01

To evaluate and compare the effects of circumferential supracrestal fiberotomy in vivo (using diode, CO(2), and Er∶YAG lasers) on the morphology and chemical composition of the root surface. Forty healthy premolar teeth, intended for extraction for orthodontic reasons, were used in this study. Root surfaces were treated using different laser methods, as follows: (1) control; (2) Er∶YAG laser (2.94 µm, 100 mJ, 10 Hz); (3) diode laser (808 nm, 1.2 W, continuous wave); and (4) CO(2) laser (10.6 µm, 3 W, continuous wave). Subsequently, the teeth were removed and subjected to scanning electron microscopic (SEM) examination and energy dispersive x-ray (EDX) spectrometric analysis. SEM analysis indicated that no thermal changes, including melting or carbonization, were observed following the lasing procedures. EDX analysis showed that the laser procedures resulted in similar mineral contents (weight % of calcium and phosphate) as compared to those in the control group. Based on these findings, we concluded that laser-aided procedures, when used at appropriate laser settings, preserve the original morphology and chemical composition of cementum.

Analysis of particulates on tape lift samples

NASA Astrophysics Data System (ADS)

Moision, Robert M.; Chaney, John A.; Panetta, Chris J.; Liu, De-Ling

2014-09-01

Particle counts on tape lift samples taken from a hardware surface exceeded threshold requirements in six successive tests despite repeated cleaning of the surface. Subsequent analysis of the particle size distributions of the failed tests revealed that the handling and processing of the tape lift samples may have played a role in the test failures. In order to explore plausible causes for the observed size distribution anomalies, scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), and time-of-flight secondary ion mass spectrometry (ToF-SIMS) were employed to perform chemical analysis on collected particulates. SEM/EDX identified Na and S containing particles on the hardware samples in a size range identified as being responsible for the test failures. ToF-SIMS was employed to further examine the Na and S containing particulates and identified the molecular signature of sodium alkylbenzene sulfonates, a common surfactant used in industrial detergent. The root cause investigation suggests that the tape lift test failures originated from detergent residue left behind on the glass slides used to mount and transport the tape following sampling and not from the hardware surface.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Chandraboss, V.L.; Natanapatham, L.; Karthikeyan, B.

Graphical abstract: The hetero-junctions that are formed between the ZnO and the Bi provide an internal electric field that facilitates separation of the electron-hole pairs and induces faster carrier migration. Thus they often enhanced photocatalytic reaction. - Highlights: • Bi-doped ZnO nanocomposite material was prepared by precipitation method. • Characterized by XRD, HR-SEM with EDX, UV–visible DRS and FT-RAMAN analysis. • Bi-doped ZnO nanocomposite material was used to photodegradation of Congo red. • Mechanism and photocatalytic effect of nanocomposite material have been discussed. - Abstract: Bismuth (Bi)-doped ZnO nanocomposite material was prepared by precipitation method with doping precursors of bismuthmore » nitrate pentahydrate and oxalic acid, characterized by X-ray diffraction (XRD), High Resolution-Scanning Electron Microscopy (HR-SEM) with Energy Dispersive X-ray (EDX) analysis, UV–visible Diffuse Reflectance Spectroscopy (UV–visible DRS) and Fourier Transform-Raman (FT-RAMAN) analysis. The enhanced photocatalytic activity of the Bi-doped ZnO is demonstrated through photodegradation of Congo red under UV-light irradiation. The mechanism of photocatalytic effect of Bi-doped ZnO nanocomposite material has been discussed.« less

Mechanistic understanding and performance of biosorption of metal ions by grapefruit peel using FTIR spectroscopy, kinetics and adsorption isotherms modeling, alkali and alkaline metal displacement and EDX analysis

USDA-ARS?s Scientific Manuscript database

The performance and mechanism of the sorptive removal of Ni2+ and Zn2+ from aqueous solution using grapefruit peel (GFP) as a new sorbent was investigated. The sorption process was fast, equilibrium was established in 60 min. The equilibrium process was described well by the Langmuir isotherm model,...

Characterization of size-resolved urban haze particles collected in summer and winter at Taiyuan City, China using quantitative electron probe X-ray microanalysis

NASA Astrophysics Data System (ADS)

Geng, Hong; Jin, Chun-Song; Zhang, Dong-Peng; Wang, Shu-Rong; Xu, Xiao-Tian; Wang, Xu-Ran; Zhang, Yuan; Wu, Li; Ro, Chul-Un

2017-07-01

The aim of the study is to characterize the size-resolved urban haze particles and investigate their modification in morphology and composition in summer and winter using the semi-quantitative electron probe X-ray microanalysis (EPMA) based on both scanning and transmission electron microscopies equipped with ultrathin-window energy dispersive X-ray spectrometers (SEM-EDX and TEM-EDX). The haze and non-haze particles were collected through a seven-stage May cascade impactor on Dec. 29-30, 2009 and Jan. 8-9 and July 11-14, 2010 in Taiyuan, a typical inland city in the North China Plain. Approximately 3752 atmospheric particles in the size ranges of 4-2 μm, 2-1 μm, 1-0.5 μm, and 0.5-0.25 μm in aerodynamic diameter were measured and identified according to their secondary electron or TEM images and elemental atomic concentrations calculated through a Monte Carlo simulation program. Results show that on the haze days many reacted or aged mineral dust particles were encountered, in which the sulfate-containing ones outnumbered the nitrate-containing ones in the winter samples while it was on the contrary in the summer samples, suggesting different haze formation and evolution mechanisms in summer and winter. Furthermore, in the haze events (especially in summer), many CNOS-rich particles, likely mixtures of water-soluble organic carbon with (NH4)2SO4 or NH4HSO4, were observed not only in the submicron but also in the super-micron fractions. The simultaneous observation of the fresh and aged CNOS-rich particles in the same SEM or TEM images implied that the status and components of secondary particles were complicated and changeable. The significant increase of both elemental concentration ratios of [N]/[S] and [C]/[S] in the aged ones compared to the fresh ones indicated that NH4NO3 and secondary organic matter were likely absorbed onto (NH4)2SO4 or NH4HSO4 particles and mixed with them. K-rich, Fe-rich, and heavy metal-containing particles in TEM-EDX measurement were detected more in the winter haze samples than in the summer ones, suggesting that they tend to be smaller in size and mainly derive from anthropogenic biomass burning and coal combustion. It was concluded that the combined use of SEM-EDX and TEM-EDX can identify both submicron and super-micron urban haze particles in a straightforward way and trace their modifications in size, shape, mixing state, and chemical compositions in different seasons, helping address their evolution processes and hazards on human health.

Sol-gel synthesis, phase composition, morphological and structural characterization of Ca10(PO4)6(OH)2: XRD, FTIR, SEM, 3D SEM and solid-state NMR studies

NASA Astrophysics Data System (ADS)

Kareiva, Simonas; Klimavicius, Vytautas; Momot, Aleksandr; Kausteklis, Jonas; Prichodko, Aleksandra; Dagys, Laurynas; Ivanauskas, Feliksas; Sakirzanovas, Simas; Balevicius, Vytautas; Kareiva, Aivaras

2016-09-01

Aqueous sol-gel chemistry route based on ammonium-hydrogen phosphate as the phosphorus precursor, calcium acetate monohydrate as source of calcium ions, and 1,2-ethylendiaminetetraacetic acid (EDTA), or 1,2-diaminocyclohexanetetracetic acid (DCTA), or tartaric acid (TA), or ethylene glycol (EG), or glycerol (GL) as complexing agents have been used to prepare calcium hydroxyapatite (Ca10(PO4)6(OH)2, CHAp). The phase transformations, composition, and structural changes in the polycrystalline samples were studied by infrared spectroscopy (FTIR), X-ray powder diffraction analysis (XRD), and scanning electron microscopy (SEM). The local short-range (nano- and mezo-) scale effects in CHAp were studied using solid-state NMR spectroscopy. The spatial 3D data from the SEM images of CHAp samples obtained by TA, EG and GL sol-gel routes were recovered for the first time to our knowledge.

Trace elements in chondritic stratospheric particles - Zinc depletion as a possible indicator of atmospheric entry heating

NASA Technical Reports Server (NTRS)

Flynn, G. J.; Sutton, S. R.

1992-01-01

Major-element abundances in 11 C, C?, and TCA cosmic dust particles have been measured using SEM and TEM energy dispersive X-ray (EDX) systems. The Fe/Ni ratio, when coupled with major element abundances, appears to be a useful discriminator of cosmic particles. Three particles classified as C?, but having Fe/Ni peak height ratios similar to those measured on the powdered Allende meteorite sample in their HSC EDX spectra, exhibit chondritic minor-/trace-element abundance patterns, suggesting they are extraterrestrial. The one particle classified as C-type, but without detectable Ni in its JSC EDX spectrum, exhibits an apparently nonchondritic minor-/trace-element abundance pattern. A class of particles that are chondritic except for large depletions in the volatile elements Zn and S has been identified. It is likely that these particles condensed with a C1 abundance pattern and that Zn and S were removed by some subsequent process.

Coating of Bio-mimetic Minerals-Substituted Hydroxyapatite on Surgical Grade Stainless Steel 316L by Electrophoretic Deposition for Hard tissue Applications

NASA Astrophysics Data System (ADS)

Govindaraj, Dharman; Rajan, Mariappan

2018-02-01

Third-era bio-implant materials intend to empower particular live cell reactions at the atomic level, these materials represented with a resorbable and biocompatibility that bodies recuperate once they have been embedded. Necessitate to decrease expenses in public health services has required the utilization of surgical grade stainless steel (SS 316L) as the most inexpensive choice for orthodontic and orthopaedic implants. 316L SS is one of the broadly used implant biomaterials in orthodontic and orthopaedic surgeries. Yet, frequently those discharge for toxic metal ions is confirm from the implants and hence a second surgery is required will remove those implant material. One approach to managing the discharge of toxic metal ions is to coat the implant substance with bio-mimetic minerals in hydroxyapatite (HA). Bio-mimetic minerals such as magnesium (Mg), strontium (Sr), also zinc (Zn) were revealed with animate bone growth furthermore restrain bone resorption both in vitro and in vivo. The present work deals with the electrophoretic deposition (EPD) for multi minerals substituted hydroxyapatite (M-HA) on the surface treated 316L SS under distinctive temperatures (27°C, (room temperature), 60 and 80°C). The resultant coatings were characterized by FT-IR, XRD, SEM-EDX, adhesion strength and leach out analysis.

Kinetic and isotherm studies of bisphenol A adsorption onto orange albedo(Citrus sinensis): Sorption mechanisms based on the main albedo components vitamin C, flavones glycosides and carotenoids.

PubMed

Kamgaing, Theophile; Doungmo, Giscard; Melataguia Tchieno, Francis Merlin; Gouoko Kouonang, Jimmy Julio; Mbadcam, Ketcha Joseph

2017-07-03

Orange albedo and its adsorption capacity towards bisphenol A (BPA) were studied. Adsorption experiments were conducted in batch mode at 25-55°C. Scanning electron microscopy (SEM), Energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) and Fourier transform infrared (FTIR) spectroscopy were used to characterise the biosorbent. The effects of various parameters including adsorption time, equilibrium pH, adsorbent dosage and initial adsorbate concentration were investigated. The optimum contact time and pH for the removal of BPA were 60 min and 2, respectively. It was found that the adsorption isotherms best matched the Freundlich model, the adsorption of BPA being multilayer and that of the albedo surface heterogeneous. From the kinetic studies, it was found that the removal of BPA best matched the pseudo-second order kinetic model. An adsorption mechanism based on the albedo surface molecules is proposed and gives a good account of π-π interactions and hydrogen bonding. Orange albedo, with a maximum BPA loading capacity of 82.36 mg g -1 (significantly higher than that of most agricultural residues), is a good candidate for BPA adsorption in aqueous media.

The novel synthesis of magnetically chitosan/carbon nanotube composites and their catalytic applications.

PubMed

Zarnegar, Zohre; Safari, Javad

2015-04-01

Chitosan-modified magnetic carbon nanotubes (CS-MCNTs) were synthesized and were investigated by FT-IR, EDX, FE-SEM, elemental analysis, XRD, VSM and TGA. In order to synthesize the CS-MCNTs composites, Fe3O4 decorated carbon nanotubes (CNTs-Fe3O4) were modified with a silica layer by the ammonia-catalysed hydrolysis of tetraethyl orthosilicate (CNTs-Fe3O4@SiO2). Then, CS-MCNTs were successfully grafted on the surface of CNTs-Fe3O4@SiO2via a suspension cross-linking method. The CS-MCNT was found to be an excellent heterogeneous catalyst for the synthesis of 1,4-dihydropyridines (DHPs). The attractive advantages of the present process include short reaction times, milder and cleaner conditions, higher purity and yields, easy isolation of products, easier work-up procedure and lower generation of waste or pollutions. This catalyst was easily separated by an external magnet and the recovered catalyst was reused several times without any significant loss of activity. A combination of the advantages of CNTs, chitosan and magnetic nanoparticles provides an important methodology for carrying out catalytic transformations. Therefore, this method provides a green and much improved protocol over the existing methods. Copyright © 2015 Elsevier B.V. All rights reserved.

Cu (II) binded chitosan/Fe3O4 nanocomomposite as a new biosorbent for efficient and selective removal of phosphate.

PubMed

Zavareh, Siamak; Behrouzi, Zahra; Avanes, Armen

2017-08-01

The aim of this study was to develop a chitosan-based magnetic adsorbent for selective and effective removal of phosphate from aqueous solutions. For this purpose, Cu-chitosan/Fe 3 O 4 nanocomposite was prepared using a facile method and characterized. The prepared adsorbent exhibited more porous surface with higher specific area compared to neat chitosan based on SEM and BET studies. The FTIR and EDX studies indicated the presence of Cu(II) bonded to the adsorbent surface. Crystalline properties of the adsorbent were also studied using XRD. Experimental isotherm data were fitted to nonlinear forms of Langmuir and Freunlich models. The maximum capacity for the modified adsorbent was calculated to be 88mg P 2 O 5 /g, much higher than that for neat chitosan and chitosan/Fe 3 O 4 according to the Langmuir isotherm. The adsorption by the modified adsorbent had fast kinetics and obeyed pseudo-second-order kinetic model. Interestingly, the maximum removal efficiency for the modified adsorbent was observed in neutral pH values, pHs of natural waters. A high selectivity against natural waters common anions as well as good regeneration ability was obtained for the introduced adsorbent. Copyright © 2017 Elsevier B.V. All rights reserved.

Plasma-surface modification vs air oxidation on carbon obtained from peach stone: Textural and chemical changes and the efficiency as adsorbents

NASA Astrophysics Data System (ADS)

De Velasco Maldonado, Paola S.; Hernández-Montoya, Virginia; Montes-Morán, Miguel A.

2016-10-01

Carbons were prepared from peach stones (Prunus persica) using different carbonization temperatures (600, 800 and 1000 °C). A selected sample was modified by oxidation using conventional oxidation techniques (thermal treatment in air atmosphere) and with cold oxygen plasma oxidation, under different conditions. Samples were characterized using elemental analysis, FT-IR spectroscopy, nitrogen adsorption isotherms at -196 °C, SEM/EDX analysis, potentiometric titration and XPS analysis. Carbons with and without oxidation were employed in the adsorption of Pb2+ in aqueous solution. Results obtained indicated that the materials with high contents of acidic oxygen groups were more efficient in the removal of Pb2+, values as high as approx. 40 mg g-1 being obtained for the best performing carbon. Textural properties of the original, un-oxidized carbon were significantly altered only after oxidation under air atmosphere at 450 °C. On the other hand, the samples oxidized with plasma show little changes in the textural parameters and a slight increase in the specific surface was observed for the sample treated at high RF power (100 W). Additionally, a significant increment of the oxygen content was observed for the plasma oxidized samples, as measured by XPS.

One pot synthesis of chitosan grafted quaternized resin for the removal of nitrate and phosphate from aqueous solution.

PubMed

Banu, H Thagira; Meenakshi, Sankaran

2017-11-01

The present study deals with the synthesis of chitosan quaternized resin for efficient removal of nitrate and phosphate from aqueous solution. The resin was characterized with FTIR, SEM with EDX and XRD. Batch method was carried out to optimize various parameters such as contact time, initial concentration of nitrate and phosphate, dosage, pH, co-anions and temperature on the adsorption capacity of the adsorbent. The adsorption process illustrated that the Freundlich isotherm and the pseudo-second order are the best fitted models for the sorption of both anions. The respective negative values of ΔH° and ΔG° revealed that the adsorption of both the anions were exothermic and spontaneous. The removal efficiency of nitrate and phosphate on chitosan quaternized resin were 78% and 90% respectively with 0.1g of adsorbent and the initial concentration as 100mg/L. Nitrate and phosphate anions adsorbed effectively on chitosan quaternized resin by replacing Cl - ions from quaternary site through electrostatic attraction as well as ion-exchange mechanism. Hydrogen bonding also played important role in adsorption process. Even after 7th regeneration cycle the adsorbent retained its adsorption capacity as 23.7mg/g and 30.4mg/g for both nitrate and phosphate respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Hierarchical structured Sm2O3 modified CuO nanoflowers as electrode materials for high performance supercapacitors

NASA Astrophysics Data System (ADS)

Zhang, Xiaojuan; He, Mingqian; He, Ping; Liu, Hongtao; Bai, Hongmei; Chen, Jingchao; He, Shaoying; Zhang, Xingquan; Dong, Faqing; Chen, Yang

2017-12-01

By a simple and cost effective chemical precipitation-hydrothermal method, novel hierarchical structured Sm2O3 modified CuO nanoflowers are prepared and investigated as electrode materials for supercapacitors. The physical properties of prepared materials are characterized by XRD, FE-SEM, EDX and FTIR techniques. Furthermore, electrochemical performances of prepared materials are investigated by cyclic voltammetry, galvanostatic charge/discharge and electrochemical impedance spectrum in 1.0 M KOH electrolyte. The resulting Sm2O3 modified CuO based electrodes exhibit obviously enhanced capacitive properties owing to the unique nanostructures and strong synergistic effects. It is worth noting that the optimized SC-3 based electrode exhibits the best electrochemical performances in all prepared electrodes, including higher specific capacitance (383.4 F g-1 at 0.5 A g-1) and good rate capability (393.2 F g-1 and 246.3 F g-1 at 0.3 A g-1 and 3.0 A g-1, respectively), as well as excellent cycling stability (84.6% capacitance retention after 2000 cycles at 1.0 A g-1). The present results show that Sm2O3 is used as a promising modifier to change the morphology and improve electrochemical performances of CuO materials.

Solid State Reaction Synthesis of Si-HA as Potential Biomedical Material: An Endeavor to Enhance the Added Value of Indonesian Mineral Resources

NASA Astrophysics Data System (ADS)

Hartatiek; Yudyanto; Ratnasari, S. D.; Windari, R. Y.; Hidayat, N.

2017-05-01

In recent years, one of the most prominently investigated materials is hydroxyapatite (HA). It is because of its excellent properties for medical applications, essentially related to orthopedic. Also, the introduction of other materials to HA becomes another research focus of many leading scientists. In this present study, silicon with various concentrations was introduced, by means of solid state reaction route, to HA forming Si-HA. The crystal structure properties of the as-prepared samples were evaluated by X-ray diffractometer (XRD). Fourier Transform Infra Red (FTIR) spectroscopy data collection and analysis were done to investigate the functional groups within the samples. The microstructural characteristics as well as elemental mapping of the samples were captured by scanning electron microscopy and energy dispersive x-ray spectroscopy (SEM-EDX). Vickers hardness test was also conducted to investigate the hardness properties of the samples. Furthermore, in vitro characterization-based bio resorbability of the samples in a simulated body fluid were also described. This study revealed that Indonesian limestone can be utilized as the raw material for synthesizing HA. The silicon has been successfully incorporated into phosphate site of the HA crystal. Conclusively, the Si-HA reported in this study shows good bioresorbability characteristic.

Facile synthesis of 2-D Cu doped WO3 nanoplates with structural, optical and differential anti cancer characteristics

NASA Astrophysics Data System (ADS)

Mehmood, Faisal; Iqbal, Javed; Gul, Asma; Ahmed, Waqqar; Ismail, M.

2017-04-01

Simple chemical co-precipitation method has been employed to synthesize two dimensional copper (Cu) doped tungsten oxide (WO3) nanoplates. A numbers of characterization techniques have been used to investigate their structural, optical and biocompatible anti cancer properties. The XRD results have confirmed the monoclinic crystal structure of WO3 nanoplates, and also successful doping of Cu ions into the WO3 crystal lattice. The presence of functional groups and chemical bonding have been verified through FTIR and Raman spectroscopy. The SEM images demonstrate that both undoped and Cu doped WO3 samples have squares plate like morphology. The EDX spectra confirm the presence of Cu, W and O ions. Diffuse reflectance spectroscopy (DRS) analysis has revealed a substantial red-shift in the absorption edge and a decrease in the band gap energy of nanoplates with Cu doping. Photoluminescence spectroscopy has been used to study the presence of defects like oxygen vacancies. Furthermore, the differential cytotoxic properties of Cu doped WO3 samples have been evaluated against human breast (MCF-7) and liver (Hep-2) cancer cells with ectocervical epithelial (HECE) healthy cells. The present findings confirm that the Cu doped WO3 nanoplates can be used as an efficient biocompatible anti cancer agent.

Surface sodium lignosulphonate-immobilized sawdust particle as an efficient adsorbent for capturing Hg2+ from aqueous solution.

PubMed

Gao, Shan; Luo, Tiantian; Zhou, Qi; Luo, Wenjun; Li, Haifeng; Jing, Luru

2018-05-01

In this work, the soluble sodium lignosulphonate (LS Na ) molecules were successfully grafted onto the surface of pine sawdust (PSD) particles to obtain an efficient adsorbent (PSD-LS) for removing Hg 2+ from wastewater. In advance, the surface of sawdust particles were carboxymethylated by chloroacetic acid, the LS Na would be anchored on the surface by a heterogeneous esterification reaction occurred between the hydroxyl of LS Na and carboxyl on PSD surface. The resultant product (PSD-LS) exhibited a good adsorption performance for Hg 2+ with adsorption capacity up to 164.77 mg/g and it was characterized by scanning electron microscope (SEM), energy dispersive X-ray diffraction (EDX), Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The effects of pH, contact time, adsorption temperature and initial concentration on the adsorption of Hg 2+ were investigated. Results showed that the pseudo-second-order kinetics and Langmuir isotherm model could describe the adsorption process better. In addition, the composite adsorbent has outstanding reusability with high and stable desorption rates under several continuous cycle. These findings suggested that PSD-LS was a potential adsorbent to remove hazardous metal ions from wastewater. Copyright © 2018 Elsevier Inc. All rights reserved.

Obtaining and characterization of La0.8Sr0.2CrO3 perovskite by the combustion method

NASA Astrophysics Data System (ADS)

Morales Rivera, A. M.; Gómez Cuaspud, J. A.; López, E. Vera

2017-01-01

This research is focused on the synthesis and characterization of a perovskite oxide based on La0.8Sr0.2CrO3 system by the combustion method. The material was obtained in order to contribute to analyse the effect of synthesis route in the obtaining of advanced anodic materials for solid oxide fuel cells (SOFC). The obtaining of solid was achieved starting from corresponding nitrate dissolutions, which were polymerized by temperature effect in presence of citric acid. The solid precursor as a foam citrate was characterized by infrared (FTIR) and ultraviolet (UV) spectroscopy, confirming the effectiveness in synthesis process. The solid was calcined in oxygen atmosphere at 800°C and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive of X-ray spectroscopy (EDX) and solid state impedance spectroscopy (IS). Results confirm the obtaining of an orthorhombic solid with space group Pnma (62) and cell parameters a=5.4590Å, b=7.7310Å and c=5.5050Å. At morphological level the solid showed a heterogeneous distribution with an optimal correspondence with proposed and obtained stoichiometry. The electrical characterization, confirm a semiconductor behaviour with a value of 2.14eV Band-gap according with previous works.

Nafion/lead nitroprusside nanoparticles modified carbon ceramic electrode as a novel amperometric sensor for L-cysteine.

PubMed

Razmi, H; Heidari, H

2009-05-01

This work describes the electrochemical and electrocatalytic properties of carbon ceramic electrode (CCE) modified with lead nitroprusside (PbNP) nanoparticles as a new electrocatalyst material. The structure of deposited film on the CCE was characterized by energy dispersive X-ray (EDX), Fourier transform infrared (FTIR), and scanning electron microscopy (SEM). The cyclic voltammogram (CV) of the PbNP modified CCE showed two well-defined redox couples due to [Fe(CN)5NO](3-)/[Fe(CN)5NO](2-) and Pb(IV)/Pb(II) redox reactions. The modified electrode showed electrocatalytic activity toward the oxidation of L-cysteine and was used as an amperometric sensor. Also, to reduce the fouling effect of L-cysteine and its oxidation products on the modified electrode, a thin film of Nafion was coated on the electrode surface. The sensor response was linearly changed with L-cysteine concentration in the range of 1 x 10(-6) to 6.72 x 10(-5)mol L(-1) with a detection limit (signal/noise ratio [S/N]=3) of 0.46 microM. The sensor sensitivity was 0.17 microA (microM)(-1), and some important advantages such as simple preparation, fast response, good stability, interference-free signals, antifouling properties, and reproducibility of the sensor for amperometric determination of L-cysteine were achieved.

Synthesis of the Novel Type of Bimodal Ceramic Nanowires from Polymer and Composite Fibrous Mats

PubMed Central

Matysiak, Wiktor

2018-01-01

The purpose of this paper was to produce SiO2 and TiO2 nanowires via the electrospinning process from a polyvinylpyrrolidone (PVP)/Tetraethyl orthosilicate (TEOS)/Titanium (IV) butoxide (TNBT)/dimethylformamide (DMF) and ethanol (EtOH) solution. The as-obtained nanofibers were calcined at temperatures ranging from 400 °C to 600 °C in order to remove the organic phase. The one-dimensional ceramic nanostructures were studied using a scanning electron microscope (SEM) and a transmission electron microscope (TEM) to analyze the influence of the used temperature on the morphology and structures of the obtained ceramic nanomaterials. In order to examine the chemical structure of the nanowires, energy dispersive spectrometry (EDX) and Fourier-Transform Infrared spectroscopy (FTIR) were used. The optical property analysis was performed on the basis of UV-Vis spectra of absorbance as a function of the wavelength. Using the modified Swanepoel method, which the authors proposed and the recorded absorbance spectra allowed to determine the banded refractive index n, real n′ and imaginary k part of the refractive index as a function of the wavelength, complex dielectric permeability ε, and real and imaginary part εr and εi of the dielectric permeability as a function of the radiation energy of the produced ceramic nanowires. PMID:29558456

Utilization of Cocoa Peel as Biosorbent for Oil and Color Removal in Palm Oil Mill Effluent (POME)

NASA Astrophysics Data System (ADS)

Pandia, S.; Hutagalung, A. T.; Siahaan, A. D.

2018-01-01

The aim of this study is to discover the effectiveness of cocoa peel as biosorbents for oil and color removal in POME. This study used biosorbent from cocoa peel with variation of particle size which passed through 70 mesh, 100 mesh, and 120 mesh and was activated with the ratio of biosorbent and 0,6 M HNO3 of 1:2, 1:4, and 1:6 (m/v). The adsorption process was carried out using biosorbent with the highest iodine number in varying biosorbent mass and contact time. The highest iodine number was 596,684 mg/g and obtained at particle size 120 mesh and the ratio of biosorbent : HNO3 as 1 : 4. The resulting biosorbents were analyzed for their characterization, such as vapor content, ash content, and volatile matter, including FT-IR and SEM-EDX. The POME were analyzed for their oil and color content, using gravimetric method and UV-Vis spectrophotometry. The best removal is were 80,88% for oil and 83.45% for color at 1.5 g biosorbent mass and 3 h contact time. The resullt for oil removal was close to the standard of Indonesian Environment Minister for oil in effluent. Also the adsorption of oil and color behaves as a pseudo-second-order kinetic models.

Preparation of TiO2/(TiO2-V2O5)/polypyrrole nanocomposites and a study on catalytic activities of the hybrid materials under UV/Visible light and in the dark

NASA Astrophysics Data System (ADS)

Piewnuan, C.; Wootthikanokkhan, J.; Ngaotrakanwiwat, P.; Meeyoo, V.; Chiarakorn, S.

2014-11-01

Hybrid metal oxides/polymer nanocomposites, namely TiO2/(TiO2-V2O5)/polypyrrole (PPy), were synthesized via in situ polymerization. Structures of the products were characterized by SEM-EDX, XRD, and FTIR techniques. The light absorbance and band gap energy values of the materials were evaluated by UV/Visible spectroscopy. The catalytic activity of the materials was determined from a degradation of methylene blue. It was found that, regardless of the polymerization time, the absorbance of TiO2/(TiO2-V2O5)/PPy was greater than those of TiO2/PPy and the neat TiO2, respectively. This was in accordance with the decrease in the band gap energy of the materials. The catalytic activity of TiO2/(TiO2-V2O5) was also observed in the dark. After polymerization, the catalytic activity of nanocomposite under UV/Visible light and in the dark was compromised. The above effects are discussed in the light of the energy storage ability of V2O5 and capability of the polymer in acting as a binder for the system.

Facile low-temperature one-step synthesis of pomelo peel biochar under air atmosphere and its adsorption behaviors for Ag(I) and Pb(II).

PubMed

Zhao, Tuo; Yao, Ying; Li, Danrong; Wu, Feng; Zhang, Cunzhong; Gao, Bin

2018-05-29

This study prepared a novel low-cost surface functionalized carbon adsorbent (PPC) from biomass waste (pomelo peel) through a facile low-temperature (250 °C) one-step method under regular air atmosphere. The adsorption performance and mechanism of the carbon material for Ag(I) and Pb(II) were investigated by a range of sorption experiments and characterizations including SEM, EDX, XRD and FTIR. Sorption experimental results suggested that PPC had high adsorption capacities of 137.4 and 88.7 mg/g for Ag(I) and Pb(II), respectively, with adsorbent dosage of 2 g/L at unadjusted solution pH and room temperature (23 ± 1 °C). The characterization results indicated high-efficiency removal of the heavy metals by PPC was attributed to the strong chemical adsorption involving that Ag(I) ions were reduced as metallic Ag particles by oxygenic functional groups and Pb(II) ions were precipitated as Pb 5 (PO 4 ) 3 OH crystals by phosphorous functional groups on the carbon surfaces. This study provides the possibility of synthesis high-efficient adsorbent using economic and environmental-friendly approach with low energy consumption. Copyright © 2018 Elsevier B.V. All rights reserved.

Magnetic activated carbon-Fe3O4 nanocomposites--synthesis and applications in the removal of acid yellow dye 17 from water.

PubMed

Ranjithkumar, V; Hazeen, A Nizarul; Thamilselvan, M; Vairam, S

2014-07-01

In this work, synthesis of activated carbon-Fe3O4 composites using activated carbon and iron benzoate/oxalate precursors by simple pyrolytic method and its utility for the removal of acid yellow dye from water are presented. Iron carboxylates held up into the pores of carbon dissociate at their decomposition temperatures form dispersed Fe3O4 nanoparticles in carbon matrix. The composites were characterized by FTIR, PXRD, SEM, TEM, EDX and magnetization measurements. The size of the nano iron oxides are in the range of 21-33 nm formed from iron benzoate precursor and 6-11 nm from iron oxalate precursor. The oxides are magnetic and their saturation magnetization in the range of 0.08-0.16 emu/g and Coercivity (H(c)) 474-600, being lower and higher than that of bare bulk Fe3O4 are due to the nano size of oxides. Composites find application in the removal of acid yellow dye 17 from the synthetic aqueous solution at pH 5. The adsorption data are found to fit well for Langmuir adsorption isotherm. Kinetics data of adsorption of dyes indicate that the adsorption follows pseudo-second order kinetic model.

Development of electrochemical folic acid sensor based on hydroxyapatite nanoparticles.

PubMed

Kanchana, P; Sekar, C

2015-02-25

We report the synthesis of hydroxyapatite (HA) nanoparticles (NPs) by a simple microwave irradiation method and its application as sensing element for the precise determination of folic acid (FA) by electrochemical method. The structure and composition of the HA NPs characterized using XRD, FTIR, Raman and XPS. SEM and EDX studies confirmed the formation of elongated spherical shaped HA NPs with an average particle size of about 34 nm. The HA NPs thin film on glassy carbon electrode (GCE) were deposited by drop casting method. Electrocatalytic behavior of FA in the physiological pH 7.0 was investigated by cyclic voltammetry (CV), linear sweep voltammetry (LSV) and chronoamperometry. The fabricated HA/GCE exhibited a linear calibration plot over a wide FA concentration ranging from 1.0×10(-7) to 3.5×10(-4) M with the detection limit of 75 nM. In addition, the HA NPs modified GCE showed good selectivity toward the determination of FA even in the presence of a 100-fold excess of ascorbic acid (AA) and 1000-fold excess of other common interferents. The fabricated biosensor exhibits good sensitivity and stability, and was successfully applied for the determination of FA in pharmaceutical samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Sequestration of toxic Pb(II) ions by chemically treated rubber (Hevea brasiliensis) leaf powder.

PubMed

Kamal, Megat Hanafiah Megat Ahmad; Azira, Wan Mat Khalir Wan Khaima; Kasmawati, Mohamed; Haslizaidi, Zakaria; Saime, Wan Ngah Wan

2010-01-01

Rubber leaf powder (an agricultural waste) was treated with potassium permanganate followed by sodium carbonate and its performance in the removal of Pb(II) ions from aqueous solution was evaluated. The interactions between Pb(II) ions and functional groups on the adsorbent surface were confirmed by Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscopy (SEM) coupled with X-ray energy dispersive spectroscopy (EDX). The effects of several important parameters which can affect adsorption capacity such as pH, adsorbent dosage, initial lead concentration and contact time were studied. The optimum pH range for lead adsorption was 4-5. Even at very low adsorbent dosage of 0.02 g, almost 100% of Pb(II) ions (23 mg/L) could be removed. The adsorption capacity was also dependent on lead concentration and contact time, and relatively a short period of time (60-90 min) was required to reach equilibrium. The equilibrium data were analyzed with Langmuir, Freundlich and Dubinin-Radushkevich isotherms. Based on Langmuir model, the maximum adsorption capacity of lead was 95.3 mg/g. Three kinetic models including pseudo first-order, pseudo second-order and Boyd were used to analyze the lead adsorption process, and the results showed that the pseudo second-order fitted well with correlation coefficients greater than 0.99.

Preparation and characterization of magnetic allylamine modified graphene oxide-poly(vinyl acetate-co-divinylbenzene) nanocomposite for vortex assisted magnetic solid phase extraction of some metal ions.

PubMed

Khan, Mansoor; Yilmaz, Erkan; Sevinc, Basak; Sahmetlioglu, Ertugrul; Shah, Jasmin; Jan, Muhammad Rasul; Soylak, Mustafa

2016-01-01

Magnetic allylamine modified graphene oxide-poly(vinyl acetate-co-divinylbenzene) (MGO-DVB-VA) was synthesized and used for magnetic solid phase extraction of Pb(II), Cd(II), Cu(II), Ni(II) and Co(II) prior to their determination by flame atomic absorption spectroscopy. The adsorbent surface functional group was characterized by using FT-IR and Raman spectroscopy. XRD pattern was used to determine the layers of GO. Surface morphology and elemental composition of the adsorbent were evaluated by using SEM and EDX analysis. Various parameters, effecting adsorption efficiency like initial solution pH, adsorbent dose, type and volume of eluent, volume of sample and diverse ions effects were optimized. The preconcentration factor (PF) is 40 for all the metals and the limits of detection for Pb, Cd, Cu, Ni and Co are in the range of 0.37-2.39 µg L(-1) and relative standard deviation below 3.1%. The method was validated by using the method for certified reference materials (Tobacco Leaves (INCT-OBTL-5), Tomato Leaves (1573a), Certified Water (SPS-ww2) and Certified Water (TMDA 64-2)). The method was successfully applied for natural water and food samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Fabrication and physico-mechanical properties of thin magnetron sputter deposited silver-containing hydroxyapatite films

NASA Astrophysics Data System (ADS)

Ivanova, A. A.; Surmeneva, M. A.; Tyurin, A. I.; Pirozhkova, T. S.; Shuvarin, I. A.; Prymak, O.; Epple, M.; Chaikina, M. V.; Surmenev, R. A.

2016-01-01

As a measure of the prevention of implant associated infections, a number of strategies have been recently applied. Silver-containing materials possessing antibacterial activity as expected might have wide applications in orthopedics and dentistry. The present work focuses on the physico-chemical characterization of silver-containing hydroxyapatite (Ag-HA) coating obtained by radio frequency (RF) magnetron sputtering. Mechanochemically synthesized Ag-HA powder (Ca10⿿xAgx(PO4)6(OH)2⿿x, x = 1.5) was used as a precursor for sputtering target preparation. Morphology, composition, crystallinity, physico-mechanical features (Young's modulus and nanohardness) of the deposited Ag-HA coatings were investigated. The sputtering of the nanostructured multicomponent target at the applied process conditions allowed to deposit crystalline Ag-HA coating which was confirmed by XRD and FTIR data. The SEM results revealed the formation of the coating with the grain morphology and columnar cross-section structure. The EDX analysis confirmed that Ag-HA coating contained Ca, P, O and Ag with the Ca/P ratio of 1.6 ± 0.1. The evolution of the mechanical properties allowed to conclude that addition of silver to HA film caused increase of the coating nanohardness and elastic modulus compared with those of pure HA thin films deposited under the same deposition conditions.

Arsanilic acid modified superparamagnetic iron oxide nanoparticles for Purification of alkaline phosphatase from hen's egg yolk.

PubMed

Farzi-Khajeh, Hamed; Safa, Kazem D; Dastmalchi, Siavoush

2017-09-01

Recent studies of magnetic carrier technology have focused on its applications in separation and purification technologies, due to easy separation of the target from the reaction medium by applying an external magnetic field. In the present study, Fe 3 O 4 superparamagnetic nanoparticles were prepared to utilize a chemical co-precipitation method, then the surfaces of the nanoparticles were modified with arsanilic acid derivatives which were used as the specific nanocarriers for the affinity purification of alkaline phosphatase from the hen's egg yolk. The six different types of magnetic nanocarriers with varied lengths of the linkers were obtained. All samples were characterized step by step and validated using FTIR, SEM, EDX, VSM and XRD analysis methods As the results were shown, the use of inflexible tags with long linkers on the surface of the nanocarrier could lead to better results for separation of alkaline phosphatase from the hen's egg yolk with 76.2% recovery and 1361.7-fold purification. The molecular weight of the purified alkaline phosphatase was estimated to be 68kDa by SDS-PAGE. The results of this study showed that the novel magnetic nanocarriers were capable of purifying alkaline phosphatase in a practically time and cost effective way. Copyright © 2017 Elsevier B.V. All rights reserved.

Multilayer adsorption of Cu(II) and Cd(II) over Brazilian Orchid Tree (Pata-de-vaca) and its adsorptive properties

NASA Astrophysics Data System (ADS)

Jorgetto, Alexandre de O.; da Silva, Adrielli C. P.; Wondracek, Marcos H. P.; Silva, Rafael I. V.; Velini, Edivaldo D.; Saeki, Margarida J.; Pedrosa, Valber A.; Castro, Gustavo R.

2015-08-01

Through very simple and inexpensive processes, pata-de-vaca leaves were turned into a powder and applied as an adsorbent for the uptake of Cu(II) and Cd(II) from water. The material was characterized through SEM, EDX, FTIR and surface area measurement. The material had its point of zero charge determined (5.24), and its adsorption capacity was evaluated as a function of time, pH and metal concentration. The material presented fast adsorption kinetics, reaching adsorption equilibrium in less than 5 min and it had a good correlation with the pseudo-second order kinetic model. Optimum pH for the adsorption of Cu(II) and Cd(II) were found to be in the range from 4 to 5, approximately. In the experiment as a function of the analyte concentration, analogously to gas adsorption, the material presented a type II isotherm, indicating the formation of multilayers for both species. Such behavior was explained with basis in the alternation between cations and anions over the material's surface, and the maximum adsorption capacity, considering the formation of the multilayers were found to be 0.238 mmol L-1 for Cu(II) and 0.113 mmol L-1 for Cd(II).

Synthesis, crystal structure, characterizations and magnetic study of a novel two-dimensional iron fluoride

NASA Astrophysics Data System (ADS)

Bouketaya, Sabrine; Smida, Mouna; Abdelbaky, Mohammed S. M.; Dammak, Mohamed; García-Granda, Santiago

2018-06-01

A new hybrid compound formulated as [Fe3F8(H2O)2](Am2TAZ)2 (Am2TAZ= 3,5-diamino-1,2,4-triazole) was prepared under hydrothermal conditions. The crystal structure was solved by single-crystal X-ray diffraction and the bulk was characterized by thermal analyses (TG-MS), vibrational spectroscopy (FTIR, Raman), Ultraviolet-visible spectroscopy (UV-Vis), and scanning electron microscopy (SEM-EDX). It crystallizes in the triclinic system space group P 1 ̅ with unit cell parameters a= 7.100(2) Å, b= 7.658(2) Å, c= 8.321(2) Å, α = 107.330(20)°, β = 111.842(18)°, γ = 93.049(17)°, Z = 1 and V= 394.01(17) Å3. The studied X-ray crystal structure shows the two oxidation states for iron atoms (Fe2+, Fe3+) and generates a 2D inorganic network, built up of inorganic layers constructed from infinite inorganic chains running along a axis. In fact, these chains are connected via (Fe3+(3)F6) octahedral. OW-H…F and N-H…F hydrogen bonds, making up the whole 3D network, are strongly linked in the layers. Magnetization measurements were performed, exhibiting the paramagnetic feature of the studied compound above 150 K.

Biosynthesis of silver nanoparticles using ethanolic petals extract of Rosa indica and characterization of its antibacterial, anticancer and anti-inflammatory activities.

PubMed

Manikandan, Ramar; Manikandan, Beulaja; Raman, Thiagarajan; Arunagirinathan, Koodalingam; Prabhu, Narayanan Marimuthu; Jothi Basu, Muthuramalingam; Perumal, Muthulakshmi; Palanisamy, Subramanian; Munusamy, Arumugam

2015-03-05

The present study was aimed at biosynthesis of silver nanoparticles (AgNPs) using ethanolic extract of rose (Rosa indica) petals and testing their potential antibacterial activity using selective human pathogenic microbes, anticancer activity using human colon adenocarcinoma cancer cell line HCT 15 as well as anti-inflammatory activity using rat peritoneal macrophages in vitro. The biologically synthesized AgNPs were also characterized by UV-visible spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR), energy-dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). The characterized AgNPs showed an effective antibacterial activity against Gram negative (Escherichia coli, Klebsiella pneumoniae) than Gram positive (Streptococcus mutans, Enterococcus faecalis) bacteria. MTT assay, analysis of nuclear morphology, mRNA expression of Bcl-2, Bax and protein expression of caspase 3 as well as 9, indicated potential anticancer activity. In addition, green synthesized AgNPs also attenuated cytotoxicity, nuclear morphology and free radical generation (O2(-) and NO) by rat peritoneal macrophages in vitro. The results of our study show the potential green synthesis of silver nanoparticles in mitigating their toxicity while retaining their antibacterial activities. Copyright © 2014 Elsevier B.V. All rights reserved.

Robust Synthesis of Ciprofloxacin-Capped Metallic Nanoparticles and Their Urease Inhibitory Assay.

PubMed

Nisar, Muhammad; Khan, Shujaat Ali; Qayum, Mughal; Khan, Ajmal; Farooq, Umar; Jaafar, Hawa Z E; Zia-Ul-Haq, Muhammad; Ali, Rashid

2016-03-25

The fluoroquinolone antibacterial drug ciprofloxacin (cip) has been used to cap metallic (silver and gold) nanoparticles by a robust one pot synthetic method under optimized conditions, using NaBH₄ as a mild reducing agent. Metallic nanoparticles (MNPs) showed constancy against variations in pH, table salt (NaCl) solution, and heat. Capping with metal ions (Ag/Au-cip) has significant implications for the solubility, pharmacokinetics and bioavailability of fluoroquinolone molecules. The metallic nanoparticles were characterized by several techniques such as ultraviolet visible spectroscopy (UV), atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and energy dispersive X-ray (EDX) methods. The nanoparticles synthesized using silver and gold were subjected to energy dispersive X-ray tests in order to show their metallic composition. The NH moiety of the piperazine group capped the Ag/Au surfaces, as revealed by spectroscopic studies. The synthesized nanoparticles were also assessed for urease inhibition potential. Fascinatingly, both Ag-cip and Au-cip NPs exhibited significant urease enzyme inhibitory potential, with IC50 = 1.181 ± 0.02 µg/mL and 52.55 ± 2.3 µg/mL, compared to ciprofloxacin (IC50 = 82.95 ± 1.62 µg/mL). MNPs also exhibited significant antibacterial activity against selected bacterial strains.

The effect of addition of PTFE or urea on luminescence response of copper-doped lithium tetraborate

NASA Astrophysics Data System (ADS)

Iskandar, Ferry; Fajri, Annisa; Nuraeni, Nunung; Stavila, Erythrina; Aimon, Akfiny H.; Nuryadin, Bebeh W.

2018-04-01

Lithium tetraborate (Li2B4O7) is a promising material for application in personal dosimetry due to its tissue equivalent properties. The addition of copper as a dopant in Li2B4O7 is known to increase the sensitivity for both photoluminescent (PL) and thermoluminescent (TL) emission. Therefore, in this paper, synthesis of Li2B4O7:Cu is reported. The optimum synthesis condition was achieved using the solution-assisted method, followed by calcination at 700 °C for 2 h. The addition of 0.1 wt% Cu resulted in the highest PL and TL emissions. Further investigation of the influence of polytetrafluoroethylene (PTFE) or urea addition on the luminescence response of Li2B4O7:Cu is described. All samples were characterized by x-ray diffraction (XRD), attenuated total reflectance-Fourier transform infrared (ATR-FTIR) spectrometry, photoluminescence spectrofluorophotometer, thermoluminescence reader, scanning electron microscopy (SEM), and energy dispersive x-ray (EDX) spectroscopy. The addition of PTFE decreased the PL emission of the Li2B4O7:Cu but slightly increased its TL emission. Meanwhile, the addition of urea increased the luminescence emission for both PL and TL of the Li2B4O7:Cu.

Adsorption of Pb2+ ions on novel ternary nanocomposite of tin, iron and titania

NASA Astrophysics Data System (ADS)

Rehman, Mahfooz ur; Rehman, Wajid; Waseem, Muhammad; Haq, Sirajul; Hussain Shah, Khizar; Kang, Peng

2018-02-01

In this study, ternary nanocomposite (TNC) was synthesized by microemulsion method by taking Sn, Ti and Fe in (1:1:1) molar ratio. The BET surface area and pore size were measured by nitrogen adsorption method. The morphological features of TNC like particle size, elemental percentage and crystallite size were studied by scanning electron microscopy (SEM), energy dispersive x-rays (EDX) and x-rays diffraction (XRD) respectively, whereas the surface functional groups were detected by Fourier Transform Infrared (FTIR) spectroscopy. The crystallite size was found to be 11 nm, calculated from FWHM of diffraction peak with relative intensity 100%. For the thermal stability of TNC, thermogravimetric analysis (TGA) was performed. Batch adsorption tests were used for the removal of Pb2+ ions from aqueous solutions. The maximum adsorption capacity in this study was found to be 79.56 mg g-1 at 40 °C which is promising than the values reported in the literature. Based on the regression coefficient (r 2), the adsorption data was found well fitted to the Langmuir as compared to Freundlich model. The exchange of a single proton with every Pb2+ ion was calculated. Thermodynamic parameters were indicative for the sorption process to be endothermic and spontaneous.

Fast enhancement on hydrophobicity of poplar wood surface using low-pressure dielectric barrier discharges (DBD) plasma

NASA Astrophysics Data System (ADS)

Chen, Weimin; Zhou, Xiaoyan; Zhang, Xiaotao; Bian, Jie; Shi, Shukai; Nguyen, Thiphuong; Chen, Minzhi; Wan, Jinglin

2017-06-01

The hydrophilicity of woody products leads to deformation and cracks, which greatly limits its applications. Low-pressure dielectric barrier discharge (DBD) plasma using hexamethyldisiloxane was applied in poplar wood surface to enhance the hydrophobicity. The chemical properties, micro-morphology, and contact angles of poplar wood surface before and after plasma treatment were investigated by attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR), x-ray photoelectron spectroscopy (XPS), scanning electron microscope and energy dispersive analysis of X-ray (SEM-EDX), atomic force microscopy (AFM), and optical contact angle measurement (OCA). Moreover, tinfoil film was used as the base to reveal the enhancement mechanism. The results showed that hexamethyldisiloxane monomer is first broken into several fragments with active sites and hydrophobic chemical groups. Meanwhile, plasma treatment results in the formation of free radicals and active sites in the poplar wood surface. Then, the fragments are reacted with free radicals and incorporated into the active sites to form a network structure based on the linkages of Si-O-Si and Sisbnd Osbnd C. Plasma treatment also leads to the formation of acicular nano-structure in poplar wood surface. These facts synergistically enhance the hydrophobicity of poplar wood surface, demonstrating the dramatically increase in the equilibrium contact angle by 330%.

Green in-situ synthesized silver nanoparticles embedded in bacterial cellulose nanopaper as a bionanocomposite plasmonic sensor.

PubMed

Pourreza, Nahid; Golmohammadi, Hamed; Naghdi, Tina; Yousefi, Hossein

2015-12-15

Herein, we introduce a new strategy for green, in-situ generation of silver nanoparticles using flexible and transparent bacterial cellulose nanopapers. In this method, adsorbed silver ions on bacterial cellulose nanopaper are reduced by the hydroxyl groups of cellulose nanofibers, acting as the reducing agent producing a bionanocomposite "embedded silver nanoparticles in transparent nanopaper" (ESNPs). The fabricated ESNPs were investigated and characterized by field emission scanning electron microscopy (FE-SEM), UV-visible spectroscopy (UV-vis), Fourier-transform infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA) and energy-dispersive X-ray spectroscopy (EDX). The important parameters affecting the ESNPs were optimized during the fabrication of specimens. The resulting ESNPs were used as a novel and sensitive probe for the optical sensing of cyanide ion (CN(-)) and 2-mercaptobenzothiazole (MBT) in water samples with satisfactory results. The change in surface plasmon resonance absorption intensity of ESNPs was linearly proportional to the concentration in the range of 0.2-2.5 µg mL(-1) and 2-110 µg mL(-1) with a detection limit of 0.012 µg mL(-1) and 1.37 µg mL(-1) for CN(-) and MBT, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

Improved separation and antifouling properties of thin-film composite nanofiltration membrane by the incorporation of cGO

NASA Astrophysics Data System (ADS)

Li, Hongbin; Shi, Wenying; Du, Qiyun; Zhou, Rong; Zhang, Haixia; Qin, Xiaohong

2017-06-01

Poly(piperazine amide) composite nanofiltration (NF) membranes were modified through the incorporation of carboxylated graphene oxide (cGO) in the polyamide layer during the interfacial polymerization (IP) process on the polysulfone (PSF)/nonwoven fabric (NWF) ultrafiltration (UF) substrate membrane surface. The composition and morphology of the prepared NF membrane surface were determined by means of ATR-FTIR, SEM-EDX and AFM. The effects of cGO contents on membrane hydrophilicity, separation performance and antifouling properties were investigated through Water Contact Angle (WCA) analysis, the permeance and three-cycle fouling measurements. The growth model of cGO-incorporated polyamide thin-film was proposed. Compared to the original NF membranes, the surface hydrophilicity, water permeability, salt rejection and antifouling properties of the cGO-incorporated NF membrane had all improved. When cGO content was 100 ppm, the MgSO4 rejection of composite NF membrane reached a maximum value of 99.2% meanwhile membrane obtained an obvious enhanced water flux (81.6 L m-2 h-1, at 0.7 MPa) which was nearly three times compared to the virginal NF membrane. The cGO-incorporated NF membrane showed an excellent selectivity of MgSO4 and NaCl with the rejection ratio of MgSO4/NaCl of approximately 8.0.

Exploration of zwitterionic cellulose acetate antifouling ultrafiltration membrane for bovine serum albumin (BSA) separation.

PubMed

Liu, Yang; Huang, Haitao; Huo, Pengfei; Gu, Jiyou

2017-06-01

This study focused on the preparation of a new kind of membrane material, zwitterionic cellulose acetate (ZCA), via a three-step procedure consist of oxidization, Schiff base and quaternary amination reaction, and the fabrication of antifouling ZCA ultrafiltration membrane by the non-solvent-induced phase separation method (NIPS). The morphologies, surface chemical structures and compositions of the obtained CA and ZCA membranes were thoroughly characterized by field emission scanning electron microscopy (FE-SEM) with energy dispersive X-ray (EDX) spectroscopy, Fourier transform infrared spectroscopy (FTIR) and X-ray photoelectron spectroscopy (XPS), respectively. Meanwhile, the thermal stability, porosity and average pore size of two investigated membranes were also studied. As a result, the ZCA membrane displayed significantly improved hydrophilicity and water permeability compared with those of the reference CA membrane, despite a slight decrease in the protein rejection ratio. According to the cycle ultrafiltration performance of bovine serum albumin (BSA) solution and protein adsorption experiment, ZCA membrane exhibited better flux recovery property and fouling resistant ability, especially irreversible fouling resistant ability, suggesting superior antifouling performance. This new approach gives polymer-based membrane a long time life and excellent ultrafiltration performance, and seems promising for potential applications in the protein separation. Copyright © 2017 Elsevier Ltd. All rights reserved.

Synergistic enhancement in photocatalytic performance of Ce (IV) and Cr (III) co-substituted magnetite nanoparticles loaded on reduced graphene oxide sheets.

PubMed

Rad, Tannaz Sadeghi; Khataee, Alireza; Rahim Pouran, Shima

2018-05-24

Effective utilization of visible-light by a photocatalyst is of great significance in photocatalytic processes. Herein, magnetite structure was modified by co-incorporation of Ce 4+ and Cr 3+ cations, and deposition on reduced graphene oxide sheets. The as-prepared Fe 2.8 Cr 0.2 O 4 #rGO and Fe 2.5 Cr 0.2 Ce 0.3 O 4 #rGO nanocomposites were characterized by XRD, SEM, X-ray Dot mapping, EDX, BET, DRS, XPS, FT-IR and VSM techniques and assessed for their photocatalytic performance under visible light irradiation for treatment of methylene blue. The results confirmed the central role of the incorporated Cr and Ce in improving the photocatalytic performance of magnetite through enhanced light harvesting, and the role of Ce 3+ /Ce 4+ redox pair, and rGO sheets in extending the life span of photo-induced e - /h + . Moreover, the influence of enhancers and scavengers were evaluated and oxidation path and generated byproducts were estimated. The results established the Fe 2.5 Cr 0.2 Ce 0.3 O 4 #rGO nanocomposite as a visible-light-driven photocatalyst for effective degradation of recalcitrant compounds. Copyright © 2018 Elsevier Inc. All rights reserved.

Synthesis and characterization of mangenese(III) porphyrin supported on imidazole modified chloromethylated MIL-101(Cr): A heterogeneous and reusable catalyst for oxidation of hydrocarbons with sodium periodate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zadehahmadi, Farnaz; Tangestaninejad, Shahram, E-mail: stanges@sci.ui.ac.ir; Moghadam, Majid, E-mail: moghadamm@sci.ui.ac.ir

2014-10-15

In the present work, chloromethylated MIL-101(Cr) modified with imidazole, Im-MIL-101, was applied as a support for immobilizing of tetraphenylporphyrinatomangenese(III) chloride. The imidazole-bound MIL-101, Im-MIL-101, not only used as support for immobilization of manganese porphyrin but also applied as a heterogeneous axial base. The Mn(TPP)Cl@Im-MIL-101 catalyst was characterized by UV–vis, FT-IR, X-ray diffraction (XRD), N{sub 2} adsorption, field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray (EDX), elemental analysis and inductively coupled plasma (ICP) methods. The catalytic activity of this new catalytic system was investigated in the alkene epoxidation and alkane hydroxylation using NaIO{sub 4} as an oxidant in CH{sub 3}CN/H{submore » 2}O at room temperature. This heterogeneous catalyst is highly efficient, stable and reusable in the oxidation of hydrocarbons. - Highlights: • MIL-101 was modified by covalent post synthetic modification. • Mn(TPP)Cl was anchored to imidazole modified MIL-101 by covalent attachment. • A heterogeneous catalyst was prepared. • The catalyst was used for epoxidation of alkenes and hydroxylation of alkanes. • The catalyst was reusable.« less

Microalgae associated Brevundimonas sp. MSK 4 as the nano particle synthesizing unit to produce antimicrobial silver nanoparticles.

PubMed

Rajamanickam, Karthic; Sudha, S S; Francis, Mebin; Sowmya, T; Rengaramanujam, J; Sivalingam, Periyasamy; Prabakar, Kandasamy

2013-09-01

The biosynthesis of silver nanoparticles and its antimicrobial property was studied using bacteria isolated from Spirulina products. Isolated bacteria were identified as Bacillus sp. MSK 1 (JX495945), Staphylococcus sp. MSK 2 (JX495946), Bacillus sp. MSK 3 (JX495947) and Brevundimonas sp. MSK 4 (JX495948). Silver nanoparticles (AgNPs) were synthesized using bacterial culture filtrate with AgNO3. The initial syntheses of Ag nanoparticles were characterized by UV-vis spectrophotometer (by measuring the color change to intense brown). Fourier Transform Infrared Spectroscopy (FTIR) study showed evidence that proteins are possible reducing agents and Energy-dispersive X-ray (EDX) study showing the metal silver as major signal. The structure of AgNPs was determined by Scanning electron microscopy (SEM) and X-ray diffraction (XRD). Synthesized Ag nanoparticles with an average size of 40-65 nm have antimicrobial property against human pathogens like Proteus vulgaris, Salmonella typhi, Vibrio cholera, Streptococcus sp., Bacillus subtilis, Staphylococcus aureus, and Escherichia coli. Among the isolates Brevundimonas sp. MSK 4 alone showed good activity in both synthesis of AgNPs and antimicrobial activity. This work demonstrates the possible use of biological synthesized silver nanoparticles to combat the drug resistant problem. Copyright © 2013 Elsevier B.V. All rights reserved.

Surface modification of polypropylene mesh devices with cyclodextrin via cold plasma for hernia repair: Characterization and antibacterial properties

NASA Astrophysics Data System (ADS)

Sanbhal, Noor; Mao, Ying; Sun, Gang; Xu, Rui Fang; Zhang, Qian; Wang, Lu

2018-05-01

Light weight polypropylene (PP) mesh is the most widely used implant among all other synthetic meshes for hernia repair. However, infection is the complication associated to all synthetic meshes after hernia repair. Thus, to manage mesh related infection; antibacterial drug is generally loaded to surgical implants to supply drug locally in mesh implanted site. Nevertheless, PP mesh restricts the loading of antibacterial drug at operated area due to its low wettability. The aim of this study was to introduce a novel antimicrobial PP mesh modified with β-cyclodextrine (CD) and loaded with antimicrobial agent for infection prevention. A cold oxygen plasma treatment was able to activate the surfaces of polypropylene fibers, and then CD was incorporated onto the surfaces of PP fibers. Afterward, triclosan, as a model antibacterial agent, was loaded into CD cavity to provide desired antibacterial functions. The modified polypropylene mesh samples CD-Tric-1, CD-Tric-3 exhibited excellent inhibition zone and continuous antibacterial efficacy against E. coli and S. aureus up to 6 and 7 days respectively. Results of AFM, SEM, FTIR and antibacterial tests evidenced that oxygen plasma process is necessary to increase chemical connection between CD molecules and PP fibers. The samples were also characterized by using EDX, XRD, TGA, DSC and water contact angle.

Bioleaching of manganese by Aspergillus sp. isolated from mining deposits.

PubMed

Mohanty, Sansuta; Ghosh, Shreya; Nayak, Sanghamitra; Das, Alok Prasad

2017-04-01

A comprehensive study on fungus assisted bioleaching of manganese (Mn) was carried out to demonstrate Mn solubilization of collected low grade ore from mining deposits of Sanindipur, Odisha, India. A native fungal strain MSF 5 was isolated and identified as Aspergillus sp. by Inter Transcribed Spacer (ITS) sequencing. The identified strain revealed an elevated tolerance ability to Mn under varying optimizing conditions like initial pH (2, 3, 4, 5, 6, 7), carbon sources (dextrose, sucrose, fructose and glucose) and pulp density (2%, 3%, 4%, 5% and 6%). Bioleaching studies carried out under optimized conditions of 2% pulp density of Mn ore at pH 6, temperature 37 °C and carbon dosage (dextrose) resulted with 79% Mn recovery from the ore sample within 20 days. SEM-EDX characterization of the ore sample and leach residue was carried out and the micrographs demonstrated porous and coagulated precipitates scattered across the matrix. The corresponding approach of FTIR analysis regulating the Mn oxide formation shows a distinctive peak of mycelium cells with and without treated Mn, resulting with generalized vibrations like MnO x stretching and CH 2 stretch. Thus, our investigation endeavors' the considerate possible mechanism involved in fungal surface cells onto Mn ore illustrating an alteration in cellular Mn interaction. Copyright © 2016 Elsevier Ltd. All rights reserved.

Synthesis of antibacterial surfaces by plasma grafting of zinc oxide based nanocomposites onto polypropylene.

PubMed

de Rancourt, Yoann; Couturaud, Benoit; Mas, André; Robin, Jean Jacques

2013-07-15

Antibacterial polymer surfaces were designed using ZnO nanoparticles as a bactericide. Mineral encapsulated nanoparticles were grafted onto activated polymer surfaces through their shells. Polypropylene (PP) surfaces were treated using an innovative process coupling core-shell technology and plasma grafting, well-known techniques commonly used to obtain active surfaces for biomedical applications. First, ZnO nanoparticles were encapsulated by (co)polymers: poly(acrylic acid) (PAA) or a poly(methyl methacrylate-co-methacrylic acid) copolymer [P(MMA-MA)]. Second, PP substrates were activated using plasma treatment. Finally, plasma-treated surfaces were immersed in solutions containing the encapsulated nanoparticles dispersed in an organic solvent and allowed to graft onto it. The presence of nanoparticles on the substrates was demonstrated using Fourier-Transform Infrared Spectroscopy (FTIR) analysis, Scanning Electron Microspcopy (SEM)/Energy-Dispersive X-ray (EDX), and Atomic Force Microscopy (AFM) studies. Indeed, the ZnO-functionalized substrates exhibited an antibacterial response in Escherichia coli adhesion tests. Moreover, this study revealed that, surprisingly, native ZnO nanoparticles without any previous functionalization could be directly grafted onto polymeric surfaces through plasma activation. The antibacterial activity of the resulting sample was shown to be comparable to that of the other samples. Copyright © 2013 Elsevier Inc. All rights reserved.

Detection of oxygen species generated by WO{sub 3} modification fullerene/TiO{sub 2} in the degradation of 1,5-diphenyl carbazide

DOE Office of Scientific and Technical Information (OSTI.GOV)

Meng, Ze-Da; Department of Advanced Materials Science and Engineering, Hanseo University, Seosan-si, Chungnam-do 356-706; Zhu, Lei

2014-08-15

Highlights: • Reactive oxygen species were detected through oxidation reaction from DPCI to DPCO. • Generated reactive oxygen species and hydroxyl radicals can be analysed by DPCI degradation. • C{sub 60} have good effect in photo/ultrasonic degradation process. • Enhanced adsorption capacity can increase the degradation effect. • Photocatalytic activity attributed to photo-absorption effect by C{sub 60} and cooperative effect of WO{sub 3} and TiO{sub 2}. - Abstract: In the present work, powders with different relative mole ratios of WO{sub 3}-fullerene/TiO{sub 2} were irradiated by visible light and ultrasonic. The composite obtained was characterized by BET surface area measurements, X-raymore » diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), fourier transform infrared (FT-IR), transmission electron microscopy (TEM) and UV–vis analysis. A methylene blue (MB) solution under visible light and ultrasonic irradiation was used to determine the catalytic activity. The generation of reactive oxygen species were detected through the oxidation reaction from 1,5-diphenyl carbazide (DPCI) to 1,5-diphenyl carbazone (DPCO). Finally, we performed experiments to find the optimum relative mole ratio of fullerene for the degradation of MB.« less

Photocatalytic properties of amine functionalized Bi2Sn2O7/rGO nanocomposites

NASA Astrophysics Data System (ADS)

Gnanamoorthy, G.; Muthamizh, S.; Sureshbabu, K.; Munusamy, S.; Padmanaban, A.; Kaaviya, A.; Nagarajan, R.; Stephen, A.; Narayanan, V.

2018-07-01

The binary metal oxide nanomaterials are having applications in various fields like sensors, optics, electrocatalyst and photocatalyst so on. Bi2Sn2O7 with pyrochlore structure is having low band gap energy; hence it is utilized in battery storage and gas sensor applications. In the present work, we have made an attempt to synthesis amine-functionalized Bi2Sn2O7/rGO nanocomposites by a thermal decomposition method and in-situ method; the synthesized nanocomposites were confirmed by XRD, FT-IR and Raman analysis. The AF-Bi2Sn2O7/rGO nanocomposites morphology was confirmed by FE-SEM along with EDX spectroscopy, we obtained different flowers and nest-like morphology. The pure and composite material band gap energy is decreases from 2.6 eV to 1.6 eV. All three nanomaterials Bi2Sn2O7, AF-Bi2Sn2O7, AF-Bi2Sn2O7/rGO nanocomposites (AF-amine functionalized) were utilized for the photocatalytic degradation of methylene blue dye under visible light irradiation. AF-Bi2Sn2O7/rGO nanocomposite showed an excellent photocatalytic activity than pure Bi2Sn2O7 and AF- Bi2Sn2O7.

Utilization Chitosan-p-t-Butylcalix[4]Arene for Red MX 8B Adsorbent

NASA Astrophysics Data System (ADS)

Handayani, D. S.; Kusumaningsih, T.; Hak, L. A.

2017-02-01

Adsorption of Procion Red MX 8B using chitosan dan chitosan-linked p-t-butylcalix[4]arene has been done. The research aimed to understand the adsorption of Procion Red MX 8B using chitosan p-t-butylcalix[4]arene compared to ordinary chitosan. The research was conducted in a batch process varying in pH, contact time and initial concentration of the Procion Red MX 8B. The amount of dye adsorbed was determined using UV-Vis spectrophotometer and the adsorben was characterized using FTIR and SEM-EDX spectrophotometer. The result showed that the optimum condition was achieved when the pH was set at 4, contact time 135 minutes and initial concentration at 200 ppm. The kinetic analysis showed that the adsorption followed Ho kinetic model and pseudo second order with the adsorption rate constant was 3.69×10-3 g/mg.minute and 2.03×10-3 g/mg.minute. The isotherm analysis showed that the adsorption process tend to occur following the Langmuir model with maximum capacity for chitosan and chitosan-linked p-t-butylcalix[4]arene 136.09 mg/g and 147.35 mg/g respectively. The adsorption energy of chitosan and chitosan-linked p-t-butylcalix[4]arene at 30.53 kJ/mole and 33.65 kJ/mole.

Novel synthesis of silver nanoparticles using Bauhinia variegata: a recent eco-friendly approach for mosquito control.

PubMed

Govindarajan, Marimuthu; Rajeswary, Mohan; Veerakumar, Kaliyan; Muthukumaran, Udaiyan; Hoti, S L; Mehlhorn, Heinz; Barnard, Donald R; Benelli, Giovanni

2016-02-01

Mosquito vectors are responsible for transmitting diseases such as malaria, dengue, chikungunya, Japanese encephalitis, dengue, and lymphatic filariasis. The use of synthetic insecticides to control mosquito vectors has caused physiological resistance and adverse environmental effects, in addition to high operational cost. Biosynthesis of silver nanoparticles has been proposed as an alternative to traditional control tools. In the present study, green synthesis of silver nanoparticles (AgNPs) using aqueous leaf extract of Bauhinia variegata by reduction of Ag(+) ions from silver nitrate solution has been investigated. The bioreduced silver nanoparticles were characterized by UV–visible spectrophotometry, Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray analysis (EDX), and X-ray diffraction analysis (XRD). Leaf extract and synthesized AgNPs were evaluated against the larvae of Anopheles subpictus, Aedes albopictus, and Culex tritaeniorhynchus. Compared to aqueous extract, synthesized AgNPs showed higher toxicity against An. subpictus, Ae. albopictus, and Cx. tritaeniorhynchus with LC50 and LC90 values of 41.96, 46.16, and 51.92 μg/mL and 82.93, 89.42, and 97.12 μg/mL, respectively. Overall, this study proves that B. variegata is a potential bioresource for stable, reproducible nanoparticle synthesis and may be proposed as an efficient mosquito control agent.

Chlorhexidine-calcium phosphate nanoparticles - Polymer mixer based wound healing cream and their applications.

PubMed

Viswanathan, Kaliyaperumal; Monisha, P; Srinivasan, M; Swathi, D; Raman, M; Dhinakar Raj, G

2016-10-01

In this work, we developed a wound healing cream composed of two different polymers, namely chitosan and gelatin with chlorhexidine along with calcium phosphate nanoparticles. The physicochemical properties of the prepared cream were investigated based on SEM, EDX, Raman, FTIR and the results indicated that the cream contained gelatin, chitosan, calcium phosphate nanoparticles and chlorhexidine. The maximum swelling ratio studies indicated that the ratio was around of 52±2.2 at pH7.4 and the value was increased in acidic and alkaline pH. The antimicrobial activity was tested against bacteria and the results indicated that, both chlorhexidine and the hybrid cream devoid of chlorhexidine exhibited antimicrobial activity but the chlorhexidine impregnated cream showed three fold higher antimicrobial activity than without chlorhexidine. In vivo wound healing promoting activities of hybrid cream containing 0.4mg/L chlorhexidine were evaluated on surgically induced dermal wounds in mice. The results indicated that the cream with incorporated chlorhexidine significantly enhanced healing compared with the control samples. For the field validations, the veterinary clinical animals were treated with the cream and showed enhanced healing capacity. In conclusion, a simple and efficient method for design of a novel wound healing cream has been developed for veterinary applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Chromatographic matrix based on hydrogel-coated reticulated polyurethane foams, prepared by gamma irradiation

NASA Astrophysics Data System (ADS)

Sánchez, Mirna L.; Giménez, Claudia Y.; Delgado, Juan F.; Martínez, Leandro J.; Grasselli, Mariano

2017-12-01

Novel chromatographic materials for protein purification with high adsorption capacity and fouling resistance are highly demanded to improve downstream processes. Here, we describe a novel adsorptive material based on reticulated polyurethane foam (rPUF) coated with a functional hydrogel layer. rPUF provides physical rigidity through its macroscopic structure, whereas the hydrogel layer provides capacity to adsorb proteins by specific interactions. The hydrogel coating process was performed by the dip-coating method, using a polyvinyl alcohol (PVA) solution. The PVA hydrogel was linked to the rPUF material by using a radiation-induced crosslinking process in aqueous ethanol solution. The ethanol in the solvent mixture allowed a balance between PVA swelling and PVA dissolution during the irradiation step. The resulting material showed higher thermal stability than the non-irradiated one. In addition, a simultaneous radiation-induced grafting polymerization (SRIGP) was done by simple addition of glycidyl methacrylate monomer into the irradiation solution. In a further step, sulfonic ligands were included specifically in the hydrogel layer, which contained around 200% of PVA respect to the original rPUF. Materials were characterized by FT-IR, thermogravimetric analysis, SEM microscopy and EDX analysis. The cation-exchange rPUF material was functionally characterized by the Langmuir isotherm and a dynamic adsorption experiment to analyze the chromatographic properties for protein purification processes.

Upcycling of polypropylene waste by surface modification using radiation-induced grafting

NASA Astrophysics Data System (ADS)

Hassan, Muhammad Inaam ul; Taimur, Shaista; Yasin, Tariq

2017-11-01

In this work, upcycling of polypropylene waste into amidoxime functionalized polypropylene adsorbent was studied using radiation-induced grafting technique. Polypropylene waste (PPw) was resulted from accelerated thermal ageing of polypropylene (PP). Bulk grafting of acrylonitrile (AN) onto PPw was achieved by simultaneous radiation grafting method using gamma rays. Degree of grafting of AN on PPw is affected by absorbed dose and dose rate. The acrylonitrile groups of grafted PPw were chemically converted into amidoxime functionality. Both the acrylonitrile-grafted PP waste and its amidoxime product were investigated by FTIR, XRD, SEM-EDX and TGA techniques. The prepared amidoxime adsorbent with amidoxime group density of 8.06 mmol/g was used for removal of copper ions from aqueous solutions. The effects of various physicochemical conditions such as: solution pH, adsorbent content, initial metal ion concentration and time on adsorption were studied to maximize adsorption of metal ion. Pseudo-first-order, pseudo-second-order and intra-particle diffusion models were applied to study the kinetics of adsorption. Maximum Langmuir adsorption capacity of 208.3 mg/g at pH 5.0 with optimum contact time of 120 min was observed. Utilization of PP waste and its comparable adsorption capacity with existing radiation grafted polymer-based adsorbents provide a new, cheap and cost effective system.

Bio-active glass air-abrasion has the potential to remove resin composite restorative material selectively

NASA Astrophysics Data System (ADS)

Milly, Hussam; Andiappan, Manoharan; Thompson, Ian; Banerjee, Avijit

2014-06-01

The aims of this study were to assess: (a) the chemistry, morphology and bioactivity of bio-active glass (BAG) air-abrasive powder, (b) the effect of three air-abrasion operating parameters: air pressure, powder flow rate (PFR) and the abrasive powder itself, on the selective removal of resin composite and (c) the required "time taken". BAG abrasive particles were characterised using scanning electron microscopy-energy dispersive X-ray spectrometry (SEM-EDX) and Fourier-transform infrared spectroscopy (FTIR). Standardised resin composite restorations created within an enamel analogue block (Macor™) in vitro, were removed using air-abrasion undersimulated clinical conditions. 90 standardised cavities were scanned before and after resin composite removal using laser profilometry and the volume of the resulting 3D images calculated. Multilevel linear model was used to identify the significant factors affecting Macor™ removal. BAG powder removed resin composite more selectively than conventional air-abrasion alumina powder using the same operating parameters (p < 0.001) and the effect of altering the unit's operating parameters was significant (p < 0.001). In conclusion, BAG powder is more efficient than alumina in the selective removal of resin composite particularly under specific operating parameters, and therefore may be recommended clinically as a method of preserving sound enamel structure when repairing and removing defective resin composite restorations.

Synthesis and Characterization of AlCl3 Impregnated Molybdenum Oxide as Heterogeneous Nano-Catalyst for the Friedel-Crafts Acylation Reaction in Ambient Condition.

PubMed

Jadhav, Arvind H; Chinnappan, Amutha; Hiremath, Vishwanath; Seo, Jeong Gil

2015-10-01

Aluminum trichloride (AlCl3) impregnated molybdenum oxide heterogeneous nano-catalyst was prepared by using simple impregnation method. The prepared heterogeneous catalyst was characterized by powder X-ray diffraction, FT-IR spectroscopy, solid-state NMR spectroscopy, SEM imaging, and EDX mapping. The catalytic activity of this protocol was evaluated as heterogeneous catalyst for the Friedel-Crafts acylation reaction at room temperature. The impregnated MoO4(AlCl2)2 catalyst showed tremendous catalytic activity in Friedel-Crafts acylation reaction under solvent-free and mild reaction condition. As a result, 84.0% yield of acyl product with 100% consumption of reactants in 18 h reaction time at room temperature was achieved. The effects of different solvents system with MoO4(AlCl2)2 catalyst in acylation reaction was also investigated. By using optimized reaction condition various acylated derivatives were prepared. In addition, the catalyst was separated by simple filtration process after the reaction and reused several times. Therefore, heterogeneous MoO4(AlCl2)2 catalyst was found environmentally benign catalyst, very convenient, high yielding, and clean method for the Friedel-Crafts acylation reaction under solvent-free and ambient reaction condition.

SBA-15/hydrotalcite nanocomposite as an efficient support for the immobilization of heteropolyacid: A triply-hybrid catalyst for the synthesis of 2-amino-4H-pyrans in water

NASA Astrophysics Data System (ADS)

Sadjadi, Samahe; Heravi, Majid M.; Zadsirjan, Vahideh; Farzaneh, Vahid

2017-12-01

To circumvent the high solubility and low surface area of heteropolyacid and in attempt to develop a bi-functional heterogeneous catalyst for promoting organic transformations, heteropolyacid was embedded in functionalized SBA-15 and subsequently hybridized with layered double hydroxide. The catalyst could be considered as a bi-functional catalyst with both acidic and basic properties. The acidic properties emerged from the SBA-15 and heteropolyacid component while layered double hydroxide render the catalyst basic. The catalyst was characterized by using SEM/EDX, FT-IR, XRD, ICP-AES, BET and elemental mapping analysis. The catalytic activity of the catalyst was studied for promoting one-pot three-component condensation of aromatic aldehydes, malononitrile or ethyl cyanoacetate and C-H activated acidic molecules in aqueous media for the synthesis of 2-amino-4H-pyran derivatives. The catalyst exhibited high catalytic activity, which was superior to the previously reported ones. Moreover, the reusability of the catalyst was excellent and the leaching of heteropolyacid was dramatically suppressed. High yields, short reaction times, eco-friendly conditions, simplicity of the procedure, reusability of the catalyst and broad substrate scope are the merits of this protocol.

Histological observation on dental hard tissue irradiated by ultrashort-pulsed laser

NASA Astrophysics Data System (ADS)

Uchizono, Takeyuki; Awazu, Kunio; Igarashi, Akihiro; Kato, Junji; Hirai, Yoshito

2006-04-01

In the field of dentistry, effectiveness of USPL irradiation is researched because USPL has less thermal side effect to dental hard tissue. In this paper, we observed morphological change and optical change of dental hard tissue irradiated by USPL for discussing the safety and effectiveness of USPL irradiation to dental hard tissues. Irradiated samples were crown enamel and root dentin of bovine teeth. Lasers were Ti:sapphire laser, which had pulse duration (P d)of 130 fsec and pulse repetition rate (f) of 1kHz and wavelength (l) of 800nm, free electron laser (FEL), which had P d of 15 μsec and f of 10Hz and wavelength of 9.6μm, and Er:YAG laser, which had P d of 250 μsec and f of 10Hz and wavelength of 2.94μm. After laser irradiation, the sample surfaces and cross sections were examined with SEM and EDX. The optical change of samples was observed using FTIR. In SEM, the samples irradiated by USPL had sharp and accurate ablation with no crack and no carbonization. But, in FEL and Er:YAG laser, the samples has rough ablation with crack and carbonization. It was cleared that the P/Ca ratio of samples irradiated by USPL had same value as non-irradiated samples. There was no change in the IR absorption spectrum between samples irradiated by USPL and non-irradiated sample. But, they of samples irradiated by FEL and Er:YAG laser, however, had difference value as non-irradiated samples. These results showed that USPL might be effective to ablate dental hard tissue without thermal damage.

Efficacy of Modified Bioactive Glass for Dentin Remineralization and Obstruction of Dentinal Tubules

PubMed Central

Saffarpour, Mahshid; Tahriri, Mohammadreza; Zakerzadeh, Azadeh

2017-01-01

Objectives: This study assessed the efficacy of modified bioactive glass (MBG) for dentin remineralization and obstruction of dentinal tubules. Materials and Methods: Thirty-six dentin discs were made from 20 third molars and were stored in 12% lactic acid solution for two weeks to induce demineralization. The samples were divided into three groups (n=12): 1- BG, 2- BG modified with 5% strontium (Sr) and 3- BG modified with 10% Sr. After applying the BG, the samples were stored in artificial saliva for 7, 14 and 21 days. Attenuated Total Reflection-Fourier Transform Infrared Spectroscopy (ATR-FTIR), X-ray Diffraction (XRD) analysis, Scanning Electron Microscopy (SEM), and Energy-Dispersive X-ray (EDX) analysis were used to assess remineralization. Also, 6 dentin discs were divided into three groups of BG, BG modified with 5% Sr and BG modified with 10% Sr, to examine tubular occlusion. The discs were etched using 0.5M of EDTA for two minutes and were stored in artificial saliva for 7 days. Changes in dentin surface morphology were evaluated under SEM. Results: Group 3 showed high rates of remineralization at days 7 and 14, although the rate decreased at day 21. Group 2 exhibited high rates of remineralization at days 7, 14 and 21. Dentinal tubules were partially occluded by BG and BG modified with 5% Sr, while they were almost completely obstructed after the use of BG modified with 10% Sr. Conclusions: Strontium increases remineralization. Addition of 10% Sr to BG enhances apatite formation; however, the apatite dissolves over time. Addition of 5% Sr to BG stabilizes the apatite lattice and increases the remineralization. PMID:29285031

Sorption Studies and Characterization of As (III) Adsorption over Developed Iron-Biochar Composites from Water.

NASA Astrophysics Data System (ADS)

Singh, P.; Mohan, D.

2016-12-01

Problem related to arsenic occurrence in groundwater has caused severe threat to human health in worldwide. Thus there is an increasing demand to find the chemistry and plausible mechanism of arsenic adsorption while remediating it from water. In present study iron-biochar composites are synthesised using agricultural waste materials. The rice husk iron-biochar composite (RIBC) and wheat husk iron-biochar composite (WIBC) were characterised and utilised for As (III) remediation from aqueous solution. The rice husk (RIBC) and wheat husk (WIBC) iron biochar composites were characterised. XPS, FT-IR, and XRD, were studied to analyse their elemental composition and functional group identification. While SEM, TEM, SEM-EDX were conducted to study their surface chemistry, mineralogy, porosity and crystallinity etc. Batch sorption studies were conducted for both rice husk (RIBC) and wheat husk (WIBC) iron-biochar composites to find sorption efficiency. Maximum As (III) adsorption was achieved in pH range 6-8 for both iron-biochar composites. Kinetic studies were conducted to establish the mechanism of As (III) adsorption at different dose and time. Optimum dose of 2g/L and 1g/L were reported for rice husk (RIBC) and wheat husk (WIBC) iron-biochar composites respectively. Electrostatic forces developed between arsenites and iron hydroxyl surface developed over the surface may have caused the removal of As (III). Significant amount of oxygen containing groups have been revealed through studies. Higher As (III) adsorption capacities were obtained for both iron-biochar composites to measure the amount of surface sites. Furthermore, various adsorption models are used to find the monolayer adsorption capacity. These findings suggest that developed iron-biochar composites may be used to remediate As (III) from contaminated water.

Multi-technical analysis as a tool to investigate structural species in the "replica" of First Mass in Brazil painting by Sebastião Vieira Fernandes

NASA Astrophysics Data System (ADS)

Costa, Thiago G.; Ritcher, Fabio A.; de M. Correia, Marcelino D.; Escorteganha, Márcia R.; Santiago, Alina G.; Gonçalves, Samantha; Spudeit, Daniel A.; Micke, Gustavo A.; Miranda, Fábio S.

2016-09-01

Constituent materials of the painting ;Primeira Missa no Brasil; by Sebastião Vieira Fernandes, which belongs to the Historical Museum of Santa Catarina, were analyzed by using imaging through UV-induced visible luminescence, FTIR, μ-FTIR, EDX and GC-MS with the aim of characterizing the materials and correlating them with Victor Meirelles' pigment elemental analysis reported in the literature. The images obtained under ultraviolet light showed alterations in the painting's aging process and instances of possible repainting confirmed by μ-FTIR, where characteristic bands of barium sulfate were identified. EDS analyses showed that there is a correlation between the elemental composition of pigments used by Meirelles and Fernandes, especially for lead, associated with lead white and proven by FTIR, used for giving a light tone to the paint, and found in all the analyzed samples. The GC-MS results revealed the presence of the mixture of linseed and animal oil as the main binding components with the predominance of palmitic, stearic, oleic, and linolenic acids.

Laser-induced Multi-energy Processing in Diamond Growth

DTIC Science & Technology

2012-05-01

microscopy (SEM) and energy dispersive X - ray (EDX) measurements, Drs. Yi Liu and Shah Valloppilly from Nebraska Center for Materials and Nanoscience...NCMN) at UNL for help on X - Ray diffraction (XRD) measurements, and Professor Steve W. Martin and Dr. Young Sik Kim from the Department of Material...spectroscopy and X - ray diffraction ................... 62 4.4 Conclusions

Acetone sensor based on zinc oxide hexagonal tubes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hastir, Anita, E-mail: anitahastir@gmail.com; Singh, Onkar, E-mail: anitahastir@gmail.com; Anand, Kanika, E-mail: anitahastir@gmail.com

2014-04-24

In this work hexagonal tubes of zinc oxide have been synthesized by co-precipitation method. For structural, morphological, elemental and optical analysis synthesized powders were characterized by using x-ray diffraction, field emission scanning microscope, EDX, UV-visible and FTIR techniques. For acetone sensing thick films of zinc oxide have been deposited on alumina substrate. The fabricated sensors exhibited maximum sensing response towards acetone vapour at an optimum operating temperature of 400°C.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kulawik, K., E-mail: kulawik@agh.edu.pl; Buffat, P.A., E-mail: philippe.buffat@epfl.ch; Ecole Polytechnique Fédérale de Lausanne, CIME, Station 12, CH-1015 Lausanne Switzerland

Microstructural characterization of Inconel 718 superalloy after three different heat treatment variants was performed by electron microscopy and electron tomography techniques, taking advantage of recent development in quantitative electron microscopy. Distribution maps of the chemical elements, collected by ChemiSTEM™ EDX system, offer a clear contrast between γ′, γ″, and the γ matrix. It was found that the γ′ phase contains mainly Ni, Al, and Ti, while the γ″ phase contains Ni, Nb, and Ti. Thus application of the Al and Nb STEM–EDX elemental maps enables identification and size measurements of γ′ and γ″ nanoparticles. 3D morphology of γ′ and γ″more » precipitates was examined by electron microscopy and FIB–SEM tomography. Employed methods revealed that in all three heat treatment variants the γ′ particles are almost spheroidal while the γ″ precipitates are mainly elongated-disc shaped. However, the precipitate sizes differed for each variant contributing to differences in the yield strength. Tomographic images were used for estimation of the volume fraction of the both strengthening phases. - Highlights: • ChemiSTEM™ EDX elemental maps bring a fast mean to differentiate γ′ and γ″ particles. • Such maps enable for the explicit size measurements of γ′ and γ″ nanoparticles. • Explicit γ′ and γ″ phases total volume fraction was measured employing FIB–SEM. • γ′/γ″ co-precipitates and sandwich-like γ′/γ″/γ′ particles were present. • HRSTEM-HAADF imaging revealed atomic columns of the γ′/γ″ co-precipitates.« less

Molecularly Imprinted Polymers Chitosan-Glutaraldehyde for Monosodium Glutamate

NASA Astrophysics Data System (ADS)

Mulyasuryani, Ani; Haryanto, Edi; Sulistyarti, Hermin; Rumhayati, Barlah

2018-01-01

Chitosan has been used as a functional monomer in the synthesis of molecularly imprinted polymers (MIP) for monosodium glutamate (MSG). MIP is made from a mixture of 5 g chitosan, 50 mg glutaraldehyde and 2 g MSG, MIP is formed as flakes and beads. MIPs are identified by the FTIR spectrum, SEM image and their adsorption capabilities. MIP flakes and beads have no structural differences if they are based on FTIR or SEM spectra, but MIP adsorption capacity of beads higher than flakes. Adsorption capacity of MIP flakes is 548 mg/g and MIP beads 627 mg/g.

Morphological and ultrastructural comparative analysis of bone tissue after Er:YAG laser and surgical drill osteotomy.

PubMed

Panduric, Dragana Gabric; Juric, Ivona Bago; Music, Svetozar; Molčanov, Krešimir; Sušic, Mato; Anic, Ivica

2014-07-01

The purpose of this study was to analyze morphological, chemical, and crystallographic changes of bone tissue after osteotomy performed with an erbium:yttrium-aluminium-garnet (Er:YAG) laser and a low speed pilot drill. Bone blocks were prepared from porcine ribs, and on each block, two tunnel preparations were performed using the Er:YAG laser (pulse energy: 1000 mJ, pulse duration: 300 μs, pulse repetition rate: 20 Hz) or the low-speed surgical pilot drill. The morphological changes of the cortical and the spongious surface of the tunnel preparations were analyzed under the field emission scanning electron microscopy (FE-SEM) at low and high resolution. The distribution and the level of chemical elements in the treated surfaces were evaluated by qualitative and semiquantitative energy dispersive x-ray analysis (SEM-EDX). Diffraction x-ray analysis was used to detect any differences and thermally induced modifications of hydroxyapatite crystals. FE-SEM revealed sharp edges of the Er:YAG preparations, with empty intertrabecular spaces and no signs of carbonization. In the drill group, the surface of the preparations was smooth, completely covered with smear layer and microcracks, and with hairy-like irregularities on the edges. SEM-EDX analysis did not reveal any differences in the number of specific chemical elements between the laser and the drill group. There were no thermally induced modifications of hydroxyapatite crystal structure in the bone tissue in either group. The Er:YAG laser ablation did not cause any chemical or crystallographic changes of the bone tissue. Compared with the drill, Er:YAG laser created well-defined edges of the preparations, and cortical bone had no smear layer.

Application of biocompatible magnetite nanoparticles for the removal of arsenic and copper from water

NASA Astrophysics Data System (ADS)

Iconaru, S. L.; Beuran, M.; Turculet, C. S.; Negoi, I.; Teleanu, G.; Prodan, A. M.; Motelica-Heino, M.; Guégan, R.; Ciobanu, C. S.; Jiga, G.; Predoi, Daniela

2018-02-01

The progress of nanotechnology made possible the use of nanomaterials as adsorbents and magnetic iron oxides represents one of the first generations of nanoscale materials used in environment technologies [1]. A systematic characterization of commercial magnetite (Fe3O4) is presented in this research. The commercial (Fe3O4) magnetic adsorbents were characterized by various characterizations methods such as X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray analysis (EDX). This study was also focused on the study of adsorption isotherms and the kinetics evaluation. X-ray studies indicated that As3+ and Cu2+ removed by Fe3O4 did not seem to alter the structure of Fe3O4 but they were highlighted in the EDX analysis. In addition, the SEM studies were consistent with the XRD results. The rate of adsorption of contaminants, in contaminated solutions decreases when the amount of contaminant increases in all experiments performed. The results revealed that Fe3O4 nanoparticles are promising candidates which could be used as sorbents for the removal of arsenic from the marine environment, for site remediation and groundwater treatment.

Multifunctional AgNPs@Wool: colored, UV-protective and antioxidant functional textiles

NASA Astrophysics Data System (ADS)

Shabbir, Mohd; Mohammad, Faqeer

2018-02-01

Nanomaterials have great impact on textile industry for multifunctional and smart clothing as per the need of present, and further, green nanotechnology is the current hotspot of research and industrial developments. Silver nanoparticles (AgNPs) are synthesized (in situ) by using natural compounds of plant extracts (naphthoquinones, phenolics/flavonoids, polyphenols) as reducing or stabilizing agents, and simultaneously deposited on wool fabric for coloration, UV protection and antioxidant properties. UV-visible spectroscopy is used to monitor the route of biosynthesis of nanoparticles and transmission electron microscopy for morphological characteristics of synthesized AgNPs. Spherical and almost oval-shaped AgNPs were synthesized by naphthoquinones, polyphenols and flavonoids, respectively. Scanning electron microscopy (SEM) coupled with energy dispersive X-ray (EDX) spectroscopy, X-ray diffraction pattern (XRD) and Fourier transform infrared spectroscopy were used for the AgNPs@Wool fabrics characterization. SEM-EDX analysis and XRD patterns confirmed the successful deposition of silver nanoparticles on wool. Coloration characteristics in terms of color strength (K/S) and CIEL*a*b*c*h° values, UV protection abilities in terms of UV transmittance and UV protection factor, and % antioxidant activity of AgNPs@Wool are suggestive of good-to-excellent results.

Genotoxic effect of Pb and Cd on in vitro cultures of Sphagnum palustre: An evaluation by ISSR markers.

PubMed

Sorrentino, Maria Cristina; Capozzi, Fiore; Giordano, Simonetta; Spagnuolo, Valeria

2017-08-01

In the present work, the genotoxic effect of cadmium and lead supplied in a laboratory trial, was investigated for the first time in the moss Sphagnum palustre, by ISSR molecular markers. A total of 169 reproducible bands were obtained with 12 primers, ten of which gave polymorphisms (i.e., appearance/disappearance of bands), indicating a clear genotoxic effect induced by the metals. Both metals induced a decrease of the genome template stability in a dose dependent manner. At concentration >10 -5 Cd also induced a general toxic effect in S. palustre, leading to chlorophyll degradation and moss death. Moreover, we followed the fate of supplied heavy metals into the moss tissue by SEM-EDX to see if they entered the cells. SEM-EDX observations on moss cultures treated with equimolar concentrations of the two metals showed that most Pb precipitated in form of particles on moss surface, while Cd did not aggregate in particles and was not found on moss surface. In light of these findings, we concluded that probably Pb induced a genotoxic effect at lower intracellular concentrations than Cd. Copyright © 2017 Elsevier Ltd. All rights reserved.

Combined effect of pulse electron beam treatment and thin hydroxyapatite film on mechanical features of biodegradable AZ31 magnesium alloy

NASA Astrophysics Data System (ADS)

Surmeneva, M. A.; Tyurin, A. I.; Teresov, A. D.; Koval, N. N.; Pirozhkova, T. S.; Shuvarin, I. A.; Surmenev, R. A.

2015-11-01

The morphology, elemental, phase composition, nanohardness, and Young's modulus of the hydroxyapatite (HA) coating deposited via radio frequency (RF) magnetron sputtering onto the AZ31 surface were investigated by atomic force microscopy (AFM), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), and nanoindentationtechniques. The calcium phosphate (Ca/P) molar ratio of the HA coating deposited via RF-magnetron sputtering onto AZ31 substrates according to EDX was 1.57+0.03. The SEM experiments revealed significant differences in the morphology of the HA film deposited on untreated and treated with the pulsed electron beam (PEB) AZ31 substrate. Nanoindentation studies demonstrated significant differences in the mechanical responses of the HA film deposited on the initial and PEB-modified AZ31 substrates. The nanoindentation hardness and the Young's modulus of the HA film on the magnesium alloy modified using the PEB treatment were higher than that of the HA layer on the untreated substrate. Moreover, the HA film fabricated onto the PEB-treated surface was more resistant to plastic deformation than the same film on the untreated AZ31 surface.

Surface martensitization of Carbon steel using Arc Plasma Sintering

NASA Astrophysics Data System (ADS)

Wahyudi, Haris; Dimyati, Arbi; Sebayang, Darwin

2018-03-01

In this paper new technology of surface structure modification of steel by short plasma exposure in Arc Plasma Sintering (APS) device is presented. APS is an apparatus working based on plasma generated by DC pulsed current originally used for synthesizing materials via sintering and melting. Plasma exposure in APS was applied into the specimens for 1 and 3 seconds which generate temperature approximately about 1300-1500°C. The SUP9, pearlitic carbon steel samples were used. The hardness, hardening depth and microstructure of the specimens have been investigated by Vickers micro hardness test and Scanning Electron Microscopy (SEM) supported by Energy Dispersive X-Ray Spectroscopy (EDX). The results have showed that the mechanical property was significantly improved due to the formation of single martensitic structures as identified by SEM. The hardness of treated surface evaluated by Vickers hardness test showed significant improvement nearly three time from 190 VHN before to 524 VHN after treatment. Furthermore, EDX confirmed that the formation of martensite layer occurred without altering its composition. The APS also produced uniform hardened layer up to 250 μm. The experiment has demonstrated that arc plasma process was successfully improved the mechanical properties of steel in relatively very short time.

In vivo surface analysis of titanium and stainless steel miniplates and screws.

PubMed

Matthew, I R; Frame, J W; Browne, R M; Millar, B G

1996-12-01

This study was undertaken to characterize the surfaces of Champy titanium and stainless steel miniplates and screws that had been used to stabilize fractures of the mandible in an animal model. Miniplates and screws were retrieved at 4, 12, and 24 weeks after surgery. Low-vacuum scanning electron microscopy (SEM) of autoclaved unused (control) and test miniplates from the same production batches was undertaken. Energy-dispersive X-ray (EDX) analysis was used to identify compositional variations of the miniplate surface, and Vickers hardness testing was performed. At autopsy, clinical healing of all fractures was noted. SEM analysis indicated no perceptible difference in the surface characteristics of the miniplates at all time intervals. Aluminium and silicon deposits were identified by EDX analysis over the flat surfaces. There was extensive damage to some screw heads. It is concluded that there were no significant changes in the surface characteristics of miniplates retrieved up to 24 weeks after implantation in comparison with controls. Damage to the screws during insertion due to softness of the materials may render their removal difficult. There was no evidence to support the routine removal of titanium or stainless steel miniplates because of surface corrosion up to 6 months after implantation.

Measuring Mass-Based Hygroscopicity of Atmospheric Particles through in situ Imaging

DOE Office of Scientific and Technical Information (OSTI.GOV)

Piens, Dominique` Y.; Kelly, Stephen T.; Harder, Tristan

Quantifying how atmospheric particles interact with water vapor is critical for understanding the effects of aerosols on climate. We present a novel method to measure the mass-based hygroscopicity of particles while characterizing their elemental and carbon functional group compositions. Since mass-based hygroscopicity is insensitive to particle geometry, it is advantageous for probing the hygroscopic behavior of atmospheric particles, which can have irregular morphologies. Combining scanning electron microscopy with energy dispersive X-ray analysis (SEM/EDX), scanning transmission X-ray microscopy (STXM) analysis, and in situ STXM humidification experiments, this method was validated using laboratory-generated, atmospherically relevant particles. Then, the hygroscopicity and elemental compositionmore » of 15 complex atmospheric particles were analyzed by leveraging quantification of C, N, and O from STXM, and complementary elemental quantification from SEM/EDX. We found three types of hygroscopic responses, and correlated high hygroscopicity with Na and Cl content. The mixing state determined for 158 particles broadly agreed with those of the humidified particles, indicating the potential to infer the atmospheric hygroscopic behavior from a selected subset of particles. These methods offer unique quantitative capabilities to characterize and correlate the hygroscopicity and chemistry of individual submicron atmospheric particles.« less

Inhibition effect of fatty amides with secondary compound on carbon steel corrosion in hydrodynamic condition

NASA Astrophysics Data System (ADS)

Ibrahim, I. M.; Jai, J.; Daud, M.; Hashim, Md A.

2018-03-01

The inhibition effect demonstrates an increase in the inhibition performance in presence of a secondary compound in the inhibited solution. This study introduces fatty amides as corrosion inhibitor and oxygen scavenger, namely, sodium sulphite as a secondary compound. The main objective is to determine the synergistic inhibition effect of a system by using fatty amides together with sodium sulphite in hydrodynamic condition. The synergistic inhibition of fatty amides and sodium sulphite on corrosion of carbon steel in 3.5 wt% sodium chloride solution had been studied using linear polarization resistance method and scanning electron microscope (SEM) with energy dispersive X-ray spectroscopy (EDX). Electrochemical measurement was carried out using rotating cylinder electrode at different flow regimes (static, laminar, transition and turbulent). Linear polarization resistance experiments showed the changes in polarization resistance when the rotation speed increased. It found that, by addition of fatty amides together with sodium sulphite in test solution, the inhibition efficiency increased when rotation speed increased. The results collected from LPR experiment correlated with results from SEM-EDX. The results showed inhibition efficiency of system was enhanced when fatty amides and oxygen scavengers were present together.

Deposition of magnesium nitride thin films on stainless steel-304 substrates by using a plasma focus device

NASA Astrophysics Data System (ADS)

Ramezani, Amir Hoshang; Habibi, Maryam; Ghoranneviss, Mahmood

2014-08-01

In this research, for the first time, we synthesize magnesium nitride thin films on 304-type stainless steel substrates using a Mather-type (2 kJ) plasma focus (PF) device. The films of magnesium nitride are coated with different number of focus shots (like 15, 25 and 35) at a distance of 8 cm from the anode tip and at 0° angular position with respect to the anode axis. For investigation of the structural properties and surface morphology of magnesium nitride films, we utilized the X-ray diffractometer (XRD), atomic force microscopy (AFM) and scanning electron microscopy (SEM) analysis, respectively. Also, the elemental composition is characterized by energy-dispersive X-ray (EDX) analysis. Furthermore, Vicker's microhardness is used to study the mechanical properties of the deposited films. The results show that the degree of crystallinity of deposited thin films (from XRD), the average size of particles and surface roughness (from AFM), crystalline growth of structures (from SEM) and the hardness values of the films depend on the number of focus shots. The EDX analysis demonstrates the existence of the elemental composition of magnesium in the deposited samples.

Optical and magnetic properties of Co-doped CuO flower/plates/particles-like nanostructures.

PubMed

Basith, N Mohamed; Vijaya, J Judith; Kennedy, L John; Bououdina, M; Hussain, Shamima

2014-03-01

In this study, pure and Co-doped CuO nanostructures (0.5, 1.0, 1.5, and 2.0 at wt% of Co) were synthesized by microwave combustion method. The prepared samples were characterized by X-ray diffraction (XRD), high resolution scanning electron microscopy (HR-SEM), energy dispersive X-ray analysis (EDX), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) spectroscopy and vibrating sample magnetometry (VSM). Powder X-ray diffraction patterns refined by the Rietveld method indicated the formation of single-phase monoclinic structure. The surface morphology and elemental analysis of Co-doped CuO nanostructures were studied by using HR-SEM and EDX. Interestingly, the morphology was found to change considerably from nanoflowers to nanoplates then to nanoparticles with the variation of Co concentration. The optical band gap calculated using DRS was found to be 2.1 eV for pure CuO and increases up to 3.4 eV with increasing cobalt content. Photoluminescence measurements also confirm these results. The magnetic measurements indicated that the obtained nanostructures were ferromagnetic at room temperature with an optimum value of saturation magnetization at 1.0 wt.% of Co-doped CuO, i.e., 970 micro emu/g.

Poly(vinylpyrrolidone) coated iron nanoparticles in polar aprotic solvent.

PubMed

Ban, Zhihui; Cushing, Brian L; O'Connor, Charles J

2008-04-01

Poly(vinylpyrrolidone) (PVP) coated iron nanoparticles which show well-defined core-shell structures have been successfully synthesized in a polar aprotic solvent. In this approach, PVP was employed not as capping agent, but as coating polymer directly applied to the metallic (iron) core nanoparticles. The morphologies, structures, compositions and magnetic properties of the products were investigated by transmission electron microscopy (TEM), X-ray powder diffraction (XRD), energy dispersive X-ray spectroscopy (EDXS), SQUID magnetometry and FTIR spectroscopy.

New airtight transfer box for SEM experiments: Application to lithium and sodium metals observation and analyses.

PubMed

Stephant, Nicolas; Grissa, Rabeb; Guillou, Fanch; Bretaudeau, Mickaël; Borjon-Piron, Yann; Guillet, Jacques; Moreau, Philippe

2018-04-18

The surface of some materials reacts very quickly on contact with air, either because it is oxidized or because it gets humidity from the air. For the sake of original surface observation by scanning electron microscopy (SEM), we conceived an airtight transfer box to keep the samples under vacuum from the place of manufacturing to the SEM chamber. This object is designed to fit in all the models of SEM including those provided with an airlock chamber. The design is voluntarily simplified to allow the manufacturing of the object by a standard mechanical workshop. The transfer box can be easily opened by gravity inside the SEM and allows the preservation of the best vacuum inside, before opening. SEM images and energy dispersive spectroscopy (EDX) analyses of metallic lithium and sodium samples are presented prior and after exposure to the air. X-ray Photoelectron Spectroscopy (XPS) analyses of all samples are also discussed in order to investigate the chemical environments of the detected elements. Copyright © 2018 Elsevier Ltd. All rights reserved.

A new member of troglobitic Carychiidae, Koreozospeum nodongense gen. et sp. n. (Gastropoda, Eupulmonata, Ellobioidea) is described from Korea.

PubMed

Jochum, Adrienne; Prozorova, Larisa; Sharyi-Ool, Mariana; Páll-Gergely, Barna

2015-01-01

A new genus of troglobitic Carychiidae Jeffreys, 1830 is designated from Nodong Cave, North Chungcheong Province, Danyang, South Korea. This remarkable find represents a great range extension and thus, a highly distant distribution of troglobitic Carychiidae in Asia. The Zospeum-like, carychiid snails were recently included, without a formal description, in records documenting Korean malacofauna. The present paper describes Koreozospeum Jochum & Prozorova, gen. n. and illustrates the type species, Koreozospeum nodongense Lee, Prozorova & Jochum, sp. n. using novel Nano-CT images, including a video, internal shell morphology, SEM and SEM-EDX elemental compositional analysis of the shell.

Cellulose nanofibrils (CNF) filled boron nitride (BN) nanocomposites

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sulaiman, Hanisah Syed; Hua, Chia Chin; Zakaria, Sarani

In this study, nanocomposite using cellulose nanofibrils filled with different percentage of boron nitride (CNF-BN) were prepared. The objective of this research is to study the effect of different percentage of BN to the thermal conductivity of the nanocomposite produced. The CNF-BN nanocomposite were characterization by FT-IR, SEM and thermal conductivity. The FT-IR analysis of the CNF-BN nanocomposite shows all the characteristic peaks of cellulose and BN present in all samples. The dispersion of BN in CNF were seen through SEM analysis. The effect of different loading percentage of BN to the thermal conductivity of the nanocomposite were also investigated.

Sol gel method for synthesis of semiconducting ferrite and the study of FTIR, DTA, SEM and CV

NASA Astrophysics Data System (ADS)

Alva, Sagir; Hua, Tang Ing; Kalmar Nizar, Umar; Wahyudi, Haris; Sundari, Rita

2018-03-01

In this study, a sol gel method using citric acid as anionic surfactant is used for synthesis of magnesium ferrite. Calcinations of magnesium ferrite at temperature (300°C, 600°C and 800°C) have been conducted after sol gel process. Characterization study of the prepared magnesium ferrite related to calcinations using Fourier transform infrared spectrometry (FTIR), Differential thermogravic analysis (DTA), and Scanning electron microscope (SEM) has been discussed. The study of Cyclic voltammetry (CV) of the prepared magnesium ferrite has been examined to assay the semiconducting behavior of magnesium ferrite in relation to its electrochemical behavior.

Preparation, characterization and conductivity study of nitro-mercurated styrene butadiene rubber/silver doped zinc oxide nanocomposites

NASA Astrophysics Data System (ADS)

Anilkumar, T.; Naik, Adarsh Ajith; Ramesan, M. T.

2017-06-01

Here we report the preparation of nitromercurated styrene butadiene rubber (NMSBR)/silver doped zinc oxide nanocomposite by inexpensive and ecofriendly two roll mill mixing. The composites were characterized by UV, FTIR, XRD, SEM, TGA and conductivity measurements. UV and FTIR spectrum indicated the interfacial interaction between the polymer and nanoparticles.XRD and SEM images showed the uniform arrangement of nanoparticles within the macromolecular chain. TGA study indicated the better thermal resistance of the composite. The dielectric properties and AC conductivity ofnanocomposites were much greater than nitromercurated SBR and they may be used as multifunctional materials for nanoelectronic devices.

Preparation, characterization, dielectric properties and diffusion studies of styrene butadiene rubber (SBR)/manganous tungstate (MnWO4) nanocomposites

NASA Astrophysics Data System (ADS)

Jasna, V. C.; Ramesan, M. T.

2017-06-01

Nanocomposites based on SBR with different content of manganous tungstate nanoparticles were prepared and characterized by FTIR, UV-visible spectroscopy, XRD, SEM, TGA, DSC and impedance analysis. The interaction between nanoparticles and the elastomer was clear from the shift in peaks of UV and FTIR. XRD and SEM analysis showed the uniform arrangement of nanoparticles in SBR matrix. Glass transition temperature, thermal stability and dielectric properties of composites were enhanced by the addition of nanoparticles. Sorption studies of nanocomposites were done in aromatic solvents at different temperature. Sorption data obtained were used to estimate the thermodynamic properties.

Parts, Materials, and Processes Control Program for Expendable Launch Vehicles

DTIC Science & Technology

2015-07-31

burn-in, electrical tests (DWV, room and hot IR, partial discharge when in corona region); perform DPA with SEM/EDX analysis of dielectric...life test; x-ray and vicinal illumination inspection; electrical tests (DWV, room and hot IR, partial discharge when in corona region) Termination...defects; proper voltage derating. Partial discharge testing, corona inception testing up to 60% of rated voltage; CSAM screening; voltage burn

Characterization of Fine Airborne Particulate Collected in Tokyo and Major Atmospheric Emission Sources by Using Single Particle Measurement of SEM-EDX

NASA Astrophysics Data System (ADS)

Sato, K.; Iijima, A.; Furuta, N.

2008-12-01

In our long-term monitoring of size-classified Airborne Particulate Matter (APM) in Tokyo since 1995, it had been demonstrated that toxic elements such as As, Se, Cd, Sb and Pb were extremely enriched in fine APM (PM2.5). However, in that study, total sampled APM on a filter was digested with acids, and thus only averaged elemental composition in fine APM could be obtained. One of the effective methods to determine the origin of APM is single particle measurement by using SEM-EDX. By using characteristic shapes observed by SEM and marker elements contained in APM measured by EDX, detailed information for source identification can be obtained. In this study, fine APM (PM2.5) was collected at various locations such as roadside, diesel vehicle exhaust, a heavy oil combustion plant and a waste incineration plant as well as ambient atmosphere in Tokyo, and characteristics of fine particles that will be utilized for identification of emission sources are elucidated. Fine particles can be classified into 3 main characteristic shape groups; edge-shaped, cotton-like and spherical. Shape of particles collected in a heavy oil combustion plant and a waste incineration plant was mostly spherical, and these particles may be associated with thermal process. Diesel exhaust particles were predominantly cotton-like which may consist of coagulated nano-sized particles. Most of brake abrasion dusts were edge-shaped, which may be associated with mechanical abrasion of brake pads. In the elemental analysis of fine particles, high concentrations of Sb, Cu, Ti and Ba were detected in brake abrasion dusts. Since these elements are major constituents of brake pads, these can be used for marker elements of brake abrasion dusts. High concentration of C was detected in diesel exhaust particles and oil combustion particles, and thus C can be used for marker elements of their origin. Furthermore, high concentrations of C, Ca and K were detected in fly ash from a waste incineration plant, which may be associated with emission from biomass combustion.

Physical properties of nanostructured CeO2 thin films grown by SILAR method

NASA Astrophysics Data System (ADS)

Khan, Ishaque Ahmed; Belkhedkar, M. R.; Salodkar, R. V.; Ubale, A. U.

2018-05-01

Nanostructured CeO2 thin films have been deposited by Successive Ionic Layer Adsorption and Reaction (SILAR) method onto glass substrate using (CeNO3)3 6H2O and NaOH as cationic and anionic precursors respectively. The structural and morphological characterizations were carried out by means of X-ray diffraction, FTIR, FESEM and EDX studies. The highly resistive (1010 Ω cm) semiconducting CeO2 film exhibits 2.95 eV optical band gap.

Evidence of ammonium ion-exchange properties of natural bentonite and application to ammonium detection.

PubMed

Zazoua, A; Kazane, I; Khedimallah, N; Dernane, C; Errachid, A; Jaffrezic-Renault, N

2013-12-01

Ammonium exchange with hybrid PVC-bentonite (mineral montmorillonite clay) thin film was revealed using FTIR spectroscopy, EDX, cyclic voltammetry and electrochemical impedance spectroscopy. The effect of ammonium exchange on the charge transfer resistance of PVC-bentonite hybrid thin film was attributed to a modification of the intersheet distance and hydration of bentonite crystals. The obtained impedimetric ammonium sensor shows a linear range of detection from 10(-4)M to 1M and a detection limit around 10(-6)M. © 2013.

Magnetic graphene coated inorganic-organic hybrid nanocomposite for enhanced preconcentration of selected pesticides in tomato and grape.

PubMed

Rashidi Nodeh, Hamid; Sereshti, Hassan; Gaikani, Hamid; Kamboh, Muhammad Afzal; Afsharsaveh, Zahra

2017-08-04

The new magnetic graphene based hybrid silica-N-[3-(trimethoxysilyl)propyl]ethylenediamine (MG@SiO 2 -TMSPED) nanocomposite was synthesized via sol-gel process, and used as an effective adsorbent in magnetic solid phase extraction (MSPE) of three selected pesticides followed by gas chromatography micro-electron capture detection (GC-μECD). The adsorbent was characterized using Fourier transform-infrared spectroscopy (FT-IR), Brunauer-Emmett-Teller (BET), Barrett-Joyner-Halenda (BJH), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy dispersive X-ray spectroscopy (EDXS) techniques. The analytical validity of the developed method was evaluated under optimized conditions and the following figures of merit were obtained: linearity, 1-20μgkg -1 with good determination coefficients (R 2 =0.995-0.999); limits of detection (LODs), 0.23-0.30μgkg -1 (3×SD/m, n=3); and limits of quantitation (LOQ), 0.76-1.0μgkg -1 (10×SD/m, n=3). The precision (RSD%) of the proposed MSPE method was studied based on intra-day (3.43-8.83%, n=3) and inter-day (6.68-8.37%, n=12) precisions. Finally, the adsorbent was applied to determination of pesticides in tomato and grape samples and good recoveries were obtained in the range from 82 to 113% (RSDs 5.1-8.1%, n=3). Copyright © 2017 Elsevier B.V. All rights reserved.

Efficient removal of atrazine from aqueous solutions using magnetic Saccharomyces cerevisiae bionanomaterial.

PubMed

Wu, Xin; He, Huijun; Yang, William L; Yu, Jiaping; Yang, Chunping

2018-06-17

A novel bionanomaterial comprising Saccharomyces cerevisiae (S. cerevisiae) and Fe 3 O 4 nanoparticles encapsulated in a sodium alginate-polyvinyl alcohol (SA-PVA) matrix was synthesized for the efficient removal of atrazine from aqueous solutions. The effects of the operating parameters, nitrogen source, and glucose and Fe 3+ contents on atrazine removal were investigated, and the intermediates were detected by gas chromatography-mass spectrometry (GC-MS). In addition, the synthesized Fe 3 O 4 particles were characterized by XRD, EDX, HR-TEM, FTIR, and hysteresis loops, and the bionanomaterial was characterized by SEM. The results showed that the maximum removal efficiency of 100% was achieved at 28 °C, a pH of 7.0, and 150 rpm with an initial atrazine concentration of 2.0 mg L -1 and that the removal efficiency was still higher than 95.53% even when the initial atrazine concentration was 50 mg L -1 . Biodegradation was demonstrated to be the dominant removal mechanism for atrazine because atrazine was consumed as the sole carbon source for S. cerevisiae. The results of GC-MS showed that dechlorination, dealkylation, deamination, isomerization, and mineralization occurred in the process of atrazine degradation, and thus, a new degradation pathway was proposed. These results indicated that this bionanomaterial has great potential for the bioremediation of atrazine-contaminated water.

Iron and iron oxide nanoparticles are highly toxic to Culex quinquefasciatus with little non-target effects on larvivorous fishes.

PubMed

Murugan, Kadarkarai; Dinesh, Devakumar; Nataraj, Devaraj; Subramaniam, Jayapal; Amuthavalli, Pandiyan; Madhavan, Jagannathan; Rajasekar, Aruliah; Rajan, Mariappan; Thiruppathi, Kulandhaivel Palani; Kumar, Suresh; Higuchi, Akon; Nicoletti, Marcello; Benelli, Giovanni

2018-04-01

The control of filariasis vectors has been enhanced in several areas, but there are main challenges, including increasing resistance to insecticides and lack of cheap and eco-friendly products. The toxicity of iron (Fe 0 ) and iron oxide (Fe 2 O 3 ) nanoparticles has been scarcely investigated yet. We studied the larvicidal and pupicidal activity of Fe 0 and Fe 2 O 3 nanoparticles against Culex quinquefasciatus. Fe 0 and Fe 2 O 3 nanoparticles produced by green (using a Ficus natalensis aqueous extract) and chemical nanosynthesis, respectively, were analyzed by UV-Vis spectrophotometry, FT-IR spectroscopy, XRD analysis, SEM, and EDX assays. In larvicidal and pupicidal experiments on Cx. quinquefasciatus, LC 50 of Fe 0 nanoparticles ranged from 20.9 (I instar larvae) to 43.7 ppm (pupae) and from 4.5 (I) to 22.1 ppm (pupae) for Fe 2 O 3 nanoparticles synthesized chemically. Furthermore, the predation efficiency of the guppy fish, Poecilia reticulata, after a single treatment with sub-lethal doses of Fe 0 and Fe 2 O 3 nanoparticles was magnified. Overall, this work provides new insights about the toxicity of Fe 0 and Fe 2 O 3 nanoparticles against mosquito vectors; we suggested that green and chemical fabricated nano-iron may be considered to develop novel and effective pesticides.

Characterization of bacterial diversity associated with calcareous deposits and drip-waters, and isolation of calcifying bacteria from two Colombian mines.

PubMed

García G, Mariandrea; Márquez G, Marco Antonio; Moreno H, Claudia Ximena

2016-01-01

Bacterial carbonate precipitation has implications in geological processes and important biotechnological applications. Bacteria capable of precipitating carbonates have been isolated from different calcium carbonate deposits (speleothems) in caves, soil, freshwater and seawater around the world. However, the diversity of bacteria from calcareous deposits in Colombia, and their ability to precipitate carbonates, remains unknown. In this study, conventional microbiological methods and molecular tools, such as temporal temperature gradient electrophoresis (TTGE), were used to assess the composition of bacterial communities associated with carbonate deposits and drip-waters from two Colombian mines. A genetic analysis of these bacterial communities revealed a similar level of diversity, based on the number of bands detected using TTGE. The dominant phylogenetic affiliations of the bacteria, determined using 16S rRNA gene sequencing, were grouped into two phyla: Proteobacteria and Firmicutes. Within these phyla, seven genera were capable of precipitating calcium carbonates: Lysinibacillus, Bacillus, Strenotophomonas, Brevibacillus, Methylobacterium, Aeromicrobium and Acinetobacter. FTIR and SEM/EDX were used to analyze calcium carbonate crystals produced by isolated Acinetobacter gyllenbergii. The results showed that rhombohedral and angular calcite crystals with sizes of 90μm were precipitated. This research provides information regarding the presence of complex bacterial communities in secondary carbonate deposits from mines and their ability to precipitate calcium carbonate from calcareous deposits of Colombian mines. Copyright © 2015 Elsevier GmbH. All rights reserved.

Hierarchical nanostructures of copper(II) phthalocyanine on electrospun TiO(2) nanofibers: controllable solvothermal-fabrication and enhanced visible photocatalytic properties.

PubMed

Zhang, Mingyi; Shao, Changlu; Guo, Zengcai; Zhang, Zhenyi; Mu, Jingbo; Cao, Tieping; Liu, Yichun

2011-02-01

In the present work, 2,9,16,23-tetranitrophthalocyanine copper(II) (TNCuPc)/TiO(2) hierarchical nanostructures were successfully fabricated by a simple combination method of electrospinning technique and solvothermal processing. Scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) spectroscopy, X-ray diffraction (XRD), UV-vis diffuse reflectance (DR), Fourier transform infrared spectrum (FT-IR), X-ray photoelectron spectroscopy (XPS), and thermal gravimetric and differential thermal analysis (TG-DTA) were used to characterize the as-synthesized TNCuPc/TiO(2) hierarchical nanostructures. The results showed that the secondary TNCuPc nanostructures were not only successfully grown on the primary TiO(2) nanofibers substrates but also uniformly distributed without aggregation. By adjusting the solvothermal fabrication parameters, the TNCuPc nanowires or nanoflowers were facilely fabricated, and also the loading amounts of TNCuPc could be controlled on the TNCuPc/TiO(2) hierarchical nanostructural nanofibers. And, there might exist the interaction between TNCuPc and TiO(2). A possible mechanism for the formation of TNCuPc/TiO(2) hierarchical nanostructures was suggested. The photocatalytic studies revealed that the TNCuPc/TiO(2) hierarchical nanostructures exhibited enhanced photocatalytic efficiency of photodegradation of Rhodamine B (RB) compared with the pure TNCuPc or TiO(2) nanofibers under visible-light irradiation.