Bulk substrate porosity verification by applying Monte Carlo modeling and Castaing's formula using energy-dispersive x-rays

NASA Astrophysics Data System (ADS)

Yung, Lai Chin; Fei, Cheong Choke; Mandeep, Jit Singh; Amin, Nowshad; Lai, Khin Wee

2015-11-01

The leadframe fabrication process normally involves additional thin-metal layer plating on the bulk copper substrate surface for wire bonding purposes. Silver, tin, and copper flakes are commonly adopted as plating materials. It is critical to assess the density of the plated metal layer, and in particular to look for porosity or voids underneath the layer, which may reduce the reliability during high-temperature stress. A fast, reliable inspection technique is needed to assess the porosity or void weakness. To this end, the characteristics of x-rays generated from bulk samples were examined using an energy-dispersive x-ray (EDX) detector to examine the porosity percentage. Monte Carlo modeling was integrated with Castaing's formula to verify the integrity of the experimental data. Samples with different porosity percentages were considered to test the correlation between the intensity of the collected x-ray signal and the material density. To further verify the integrity of the model, conventional cross-sectional samples were also taken to observe the porosity percentage using Image J software measurement. A breakthrough in bulk substrate assessment was achieved by applying EDX for the first time to nonelemental analysis. The experimental data showed that the EDX features were not only useful for elemental analysis, but also applicable to thin-film metal layer thickness measurement and bulk material density determination. A detailed experiment was conducted using EDX to assess the plating metal layer and bulk material porosity.

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.

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.

An in Vitro Evaluation of Remineralization Potential of Novamin(®) on Artificial Enamel Sub-Surface Lesions Around Orthodontic Brackets Using Energy Dispersive X-Ray Analysis (EDX).

PubMed

Mohanty, Pritam; Padmanabhan, Sridevi; Chitharanjan, Arun B

2014-11-01

To evaluate and compare the Ca/P ratio of enamel samples around the orthodontic brackets for time periods of 0, 2 and 10 days in two groups (control group and study group). Forty extracted teeth were randomly divided into control group and study group. All samples were demineralized and incubated in artificial saliva at 37°C for a period of 10 days after demineralization. During this phase the enamel samples in the study group were treated with remineralizing paste (NuproNusolution containing Novamin®-Dentsply) for 10 days. At the end of the incubation period, Ca/P ratios were analyzed for both the groupsby EDX analysis. Data obtained was subjected to statistical analysis using student t-test for paired samples and Student t- test for individual samples (p ≤ 0.05). It was found that the mean Ca/P ratio was significantly lower for the control group as compared to the study group (p-value < 0.05) after 10 d of incubation. Novamin(®) containing remineralization toothpaste showed significant remineralizing potential in inhibition of artificial enamel sub-surface lesion around bracket after 10 days of remineralization phase. EDX element analysis was found to be an efficient method to quantify the changes in mineral content of a sample during in vitro caries studies.

An in Vitro Evaluation of Remineralization Potential of Novamin® on Artificial Enamel Sub-Surface Lesions Around Orthodontic Brackets Using Energy Dispersive X-Ray Analysis (EDX)

PubMed Central

Padmanabhan, Sridevi; Chitharanjan, Arun B

2014-01-01

Objective: To evaluate and compare the Ca/P ratio of enamel samples around the orthodontic brackets for time periods of 0, 2 and 10 days in two groups (control group and study group). Materials and Methods: Forty extracted teeth were randomly divided into control group and study group. All samples were demineralized and incubated in artificial saliva at 37°C for a period of 10 days after demineralization. During this phase the enamel samples in the study group were treated with remineralizing paste (NuproNusolution containing Novamin®-Dentsply) for 10 days. At the end of the incubation period, Ca/P ratios were analyzed for both the groupsby EDX analysis. Data obtained was subjected to statistical analysis using student t-test for paired samples and Student t- test for individual samples (p ≤ 0.05). Results: It was found that the mean Ca/P ratio was significantly lower for the control group as compared to the study group (p-value < 0.05) after 10 d of incubation. Conclusion: Novamin® containing remineralization toothpaste showed significant remineralizing potential in inhibition of artificial enamel sub-surface lesion around bracket after 10 days of remineralization phase. EDX element analysis was found to be an efficient method to quantify the changes in mineral content of a sample during in vitro caries studies. PMID:25584326

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.

Composition Analysis of III-Nitrides at the Nanometer Scale: Comparison of Energy Dispersive X-ray Spectroscopy and Atom Probe Tomography.

PubMed

Bonef, Bastien; Lopez-Haro, Miguel; Amichi, Lynda; Beeler, Mark; Grenier, Adeline; Robin, Eric; Jouneau, Pierre-Henri; Mollard, Nicolas; Mouton, Isabelle; Monroy, Eva; Bougerol, Catherine

2016-12-01

The enhancement of the performance of advanced nitride-based optoelectronic devices requires the fine tuning of their composition, which has to be determined with a high accuracy and at the nanometer scale. For that purpose, we have evaluated and compared energy dispersive X-ray spectroscopy (EDX) in a scanning transmission electron microscope (STEM) and atom probe tomography (APT) in terms of composition analysis of AlGaN/GaN multilayers. Both techniques give comparable results with a composition accuracy better than 0.6 % even for layers as thin as 3 nm. In case of EDX, we show the relevance of correcting the X-ray absorption by simultaneous determination of the mass thickness and chemical composition at each point of the analysis. Limitations of both techniques are discussed when applied to specimens with different geometries or compositions.

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

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.

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.

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.

LIBS analysis of hydroxyapatite extracted from bovine bone for Ca/P ratio measurements

NASA Astrophysics Data System (ADS)

Tariq, Usman; Haider, Zuhaib; Hussain, Rafaqat; Tufail, Kashif; Ali, Jalil

2017-03-01

Hydroxyapatite has been extensively used as a potential biocompatible ceramic in many orhtopedic applications. Hydroxyapatite is one of the members of calcium phosphate family and been used extensively as a bone substitute. The mechanical properties of hydroxyapatite itself, ceramics and bone cements prepared from hydroxyapatite vary greatly with slight variation in its Ca/P ratio. At present EDX, XRD, XRF and ICP-OES are being used for the determination of Ca/P ratio in hydroxyapatite. These techniques require special sample preparation, may also use toxic chemicals and usually are not very fast in giving the measurements. We report LIBS as a rapid alternative technique for calculation of Ca/P ratio in hydroxyapatite extracted from bovine bone (BHA). Ca/P ratio in laboratory prepared HA is calculated using LIBS and the results are validated against EDX results Ca/P ratio of the hydroxyapatite was calculated as 1.54±0.19 using LIBS while 1.63±0.03 using EDX. Ca/P ratio calculated by LIBS and EDX and showed comparable results with a difference of 5.5%. Moreover, plasma temperature and the ratio of the calcium (ion) line to calcium (atomic) line did not show significant variation in plasma conditions during measurements. The present study has demonstrated that LIBS can also be used for the determination of Ca/P ratio of hydroxyapatite and other calcium phosphates. At the request of all authors of the paper, and with the agreement of the Proceedings Editor, an updated version of this article was published on 24 May 2017.

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.

A transmission electron microscopy study of CoFe2O4 ferrite nanoparticles in silica aerogel matrix using HREM and STEM imaging and EDX spectroscopy and EELS.

PubMed

Falqui, Andrea; Corrias, Anna; Wang, Peng; Snoeck, Etienne; Mountjoy, Gavin

2010-04-01

Magnetic nanocomposite materials consisting of 5 and 10 wt% CoFe2O4 nanoparticles in a silica aerogel matrix have been synthesized by the sol-gel method. For the CoFe2O4-10wt% sample, bright-field scanning transmission electron microscopy (BF STEM) and high-resolution transmission electron microscopy (HREM) images showed distinct, rounded CoFe2O4 nanoparticles, with typical diameters of roughly 8 nm. For the CoFe2O4-5wt% sample, BF STEM images and energy dispersive X-ray (EDX) measurements showed CoFe2O4 nanoparticles with diameters of roughly 3 +/- 1 nm. EDX measurements indicate that all nanoparticles consist of stoichiometric CoFe2O4, and electron energy-loss spectroscopy measurements from lines crossing nanoparticles in the CoFe2O4-10wt% sample show a uniform composition within nanoparticles, with a precision of at best than +/-0.5 nm in analysis position. BF STEM images obtained for the CoFe2O4-10wt% sample showed many "needle-like" nanostructures that typically have a length of 10 nm and a width of 1 nm, and frequently appear to be attached to nanoparticles. These needle-like nanostructures are observed to contain layers with interlayer spacing 0.33 +/- 0.1 nm, which could be consistent with Co silicate hydroxide, a known precursor phase in these nanocomposite materials.

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.

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 ...

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

Green Synthesis of Silver Nanoparticles Using an Aqueous Extract of Monotheca buxifolia (Flac.) Dcne

NASA Astrophysics Data System (ADS)

Anwar, Natasha; Khan, Abbas; Shah, Mohib; Anwar, Saad

2018-01-01

This study deals with the synthesis and physicochemical investigation of silver nanoparticles using an aqueous extract of Monotheca buxifolia (Flac.). On the treatment of aqueous solution of silver nitrate with the plant extract, silver nanoparticles were rapidly fabricated. The synthesized particles were characterized by using UV-visible spectrophotometry (UV), Fourier transform infrared spectroscopy (FTIR), Energy dispersive X-ray (EDX) and Scanning electron microscopy (SEM). The formation of AgNPs was confirmed by noting the change in colour through visual observations as well as via UV-Vis spectroscopy. UV-Vis spectrum of the aqueous medium containing silver nanoparticles showed an absorption peak at around 440 nm. FTIR was used to identify the chemical composition of silver nanoparticles and Ag-capped plant extract. The presence of elemental silver was also confirmed through EDX analysis. The SEM analysis of the silver nanoparticles showed that they have a uniform spherical shape with an average size in the range of 40-78 nm. This green system showed better capping and stabilizing agent for the fine particles. Further, in vitro the antioxidant activity of Monotheca buxifolia (Flac.) and Ag-capped with the plant was also evaluated using FeCl3/K3Fe (CN)6 essay.

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.

EDX-Element Analysis of the In Vitro Effect of Fluoride Oral Hygiene Tablets on Artificial Caries Lesion Formation and Remineralization in Human Enamel.

PubMed

Eggerath, J; Kremniczky, T; Gaengler, P; Arnold, W H

2011-01-01

Aim of this in-vitro-study was to assess the remineralization potential of a tooth cleaning tablet with different fluoride content quantitatively using EDX analysis.Twenty three caries free impacted third molars were examined; enamel surfaces were wax coated leaving two 3x4mm windows for exposure to demineralization/remineralization cycles. The teeth were randomly assigned to 4 groups of 5 control and 6 experimental teeth each. Demineralization by standardized HEC-gel, pH 4.7 at 37°C for 72h, was alternated by rinsing in remineralization solution, pH 7.0 at 37°C for 72h, total challenge time 432h. The negative control group N was treated during remineralization cycles with saline; positive control group P was treated with remineralization solution; experimental group D1 was exposed to remineralization solution containing Denttabs(®)-tablets with 1450 ppm F; experimental group D2 was exposed to remineralization solution and Denttabs(®)-tablets with 4350 ppm F. Each tooth was cut into serial sections and analyzed by scanning electron microscopy with EDX element analysis for assessment of the different zones of the lesions in 3 representative sections. Statistical analysis was based on the AVOVA test for repeated measurements and post hoc Bonferroni adjustment. The results showed a significantly higher Ca and P content in the body of the lesion in both fluoride treated groups compared to the controls. It can be concluded that higher concentrations of NaF may be more effective in remineralization of early advanced caries lesions.

EDX-Element Analysis of the In Vitro Effect of Fluoride Oral Hygiene Tablets on Artificial Caries Lesion Formation and Remineralization in Human Enamel

PubMed Central

Eggerath, J; Kremniczky, T; Gaengler, P; Arnold, W.H

2011-01-01

Aim of this in-vitro-study was to assess the remineralization potential of a tooth cleaning tablet with different fluoride content quantitatively using EDX analysis. Twenty three caries free impacted third molars were examined; enamel surfaces were wax coated leaving two 3x4mm windows for exposure to demineralization/remineralization cycles. The teeth were randomly assigned to 4 groups of 5 control and 6 experimental teeth each. Demineralization by standardized HEC-gel, pH 4.7 at 37°C for 72h, was alternated by rinsing in remineralization solution, pH 7.0 at 37°C for 72h, total challenge time 432h. The negative control group N was treated during remineralization cycles with saline; positive control group P was treated with remineralization solution; experimental group D1 was exposed to remineralization solution containing Denttabs®-tablets with 1450 ppm F; experimental group D2 was exposed to remineralization solution and Denttabs®-tablets with 4350 ppm F. Each tooth was cut into serial sections and analyzed by scanning electron microscopy with EDX element analysis for assessment of the different zones of the lesions in 3 representative sections. Statistical analysis was based on the AVOVA test for repeated measurements and post hoc Bonferroni adjustment. The results showed a significantly higher Ca and P content in the body of the lesion in both fluoride treated groups compared to the controls. It can be concluded that higher concentrations of NaF may be more effective in remineralization of early advanced caries lesions. PMID:21687564

Chemical Species, Micromorphology, and XRD Fingerprint Analysis of Tibetan Medicine Zuotai Containing Mercury

PubMed Central

Li, Cen; Yang, Hongxia; Xiao, Yuancan; Zhandui; Sanglao; Wang, Zhang; Ladan, Duojie; Bi, Hongtao

2016-01-01

Zuotai (gTso thal) is one of the famous drugs containing mercury in Tibetan medicine. However, little is known about the chemical substance basis of its pharmacodynamics and the intrinsic link of different samples sources so far. Given this, energy dispersive spectrometry of X-ray (EDX), scanning electron microscopy (SEM), atomic force microscopy (AFM), and powder X-ray diffraction (XRD) were used to assay the elements, micromorphology, and phase composition of nine Zuotai samples from different regions, respectively; the XRD fingerprint features of Zuotai were analyzed by multivariate statistical analysis. EDX result shows that Zuotai contains Hg, S, O, Fe, Al, Cu, and other elements. SEM and AFM observations suggest that Zuotai is a kind of ancient nanodrug. Its particles are mainly in the range of 100–800 nm, which commonly further aggregate into 1–30 μm loosely amorphous particles. XRD test shows that β-HgS, S8, and α-HgS are its main phase compositions. XRD fingerprint analysis indicates that the similarity degrees of nine samples are very high, and the results of multivariate statistical analysis are broadly consistent with sample sources. The present research has revealed the physicochemical characteristics of Zuotai, and it would play a positive role in interpreting this mysterious Tibetan drug. PMID:27738409

Chemical Species, Micromorphology, and XRD Fingerprint Analysis of Tibetan Medicine Zuotai Containing Mercury.

PubMed

Li, Cen; Yang, Hongxia; Du, Yuzhi; Xiao, Yuancan; Zhandui; Sanglao; Wang, Zhang; Ladan, Duojie; Bi, Hongtao; Wei, Lixin

2016-01-01

Zuotai ( gTso thal ) is one of the famous drugs containing mercury in Tibetan medicine. However, little is known about the chemical substance basis of its pharmacodynamics and the intrinsic link of different samples sources so far. Given this, energy dispersive spectrometry of X-ray (EDX), scanning electron microscopy (SEM), atomic force microscopy (AFM), and powder X-ray diffraction (XRD) were used to assay the elements, micromorphology, and phase composition of nine Zuotai samples from different regions, respectively; the XRD fingerprint features of Zuotai were analyzed by multivariate statistical analysis. EDX result shows that Zuotai contains Hg, S, O, Fe, Al, Cu, and other elements. SEM and AFM observations suggest that Zuotai is a kind of ancient nanodrug. Its particles are mainly in the range of 100-800 nm, which commonly further aggregate into 1-30  μ m loosely amorphous particles. XRD test shows that β -HgS, S 8 , and α -HgS are its main phase compositions. XRD fingerprint analysis indicates that the similarity degrees of nine samples are very high, and the results of multivariate statistical analysis are broadly consistent with sample sources. The present research has revealed the physicochemical characteristics of Zuotai , and it would play a positive role in interpreting this mysterious Tibetan drug.

Synthesis, characterizations and anti-bacterial activities of pure and Ag doped CdO nanoparticles by chemical precipitation method

NASA Astrophysics Data System (ADS)

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

2015-02-01

In the present study, synthesized pure and Ag (1%, 2%, and 3%) doped Cadmium Oxide (CdO) nanoparticles by chemical precipitation method. Then, the synthesized products were characterized by thermo gravimetric-differential thermal analysis (TG-DTA), X-ray diffraction (XRD) analysis, Fourier transform infrared (FT-IR) spectroscopy, Ultra violet-Vis diffused reflectance spectroscopy (UV-Vis-DRS), Scanning electron microscopy (SEM), Energy dispersive X-rays (EDX) spectroscopy, and anti-bacterial activities, respectively. The transition temperatures and phase transitions of Cd(OH)2 to CdO at 400 °C was confirmed by TG-DTA analysis. The XRD patterns show the cubic shape and average particle sizes are 21, 40, 34, and 37 nm, respectively for pure and Ag doped samples. FT-IR study confirmed the presence of CdO and Ag at 677 and 459 cm-1, respectively. UV-Vis-DRS study shows the variation on direct and indirect band gaps. The surface morphologies and elemental analysis have been confirmed from SEM and with EDX. In addition, the synthesized products have been characterized by antibacterial activities against Gram-positive and negative bacteria. Further, the present investigation suggests that CdO nanoparticles have the great potential applications on various industrial and medical fields of research.

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.

Quantitative determination of occupation sites of trace Co substituted for multiple Fe sites in M-type hexagonal ferrite using statistical beam-rocking TEM-EDXS analysis.

PubMed

Ohtsuka, Masahiro; Muto, Shunsuke; Tatsumi, Kazuyoshi; Kobayashi, Yoshinori; Kawata, Tsunehiro

2016-04-01

The occupation sites and the occupancies of trace dopants in La/Co co-doped Sr-M-type ferrite, SrFe12O19, were quantitatively and precisely determined by beam-rocking energy-dispersive X-ray spectroscopy (EDXS) on the basis of electron-channeling effects. Because the Co atoms, in particular, should be partially substituted for the five crystallographically inequivalent sites, which could be key parameters in improving the magneto-crystalline anisotropy, it is difficult yet intriguing to discover their occupation sites and occupancies without using the methods of large-scale facilities, such as neutron diffraction and synchrotron radiation. In the present study, we tackled this problem by applying an extended statistical atom location by channeling enhanced microanalysis method, using conventional transmission electron microscopy, EDXS and dynamical electron elastic/inelastic scattering theories. The results show that the key occupation sites of Co were the 2a, 4f1 and 12k sites. The quantified occupancies of Co were consistent with those of the previous study, which involved a combination of neutron diffraction and extended X-ray absorption fine structure analysis, as well as energetics considerations based on by first-principles calculations. © The Author 2015. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

Mineral content changes in bone associated with damage induced by the electron beam.

PubMed

Bloebaum, Roy D; Holmes, Jennifer L; Skedros, John G

2005-01-01

Energy-dispersive x-ray (EDX) spectroscopy and backscattered electron (BSE) imaging are finding increased use for determining mineral content in microscopic regions of bone. Electron beam bombardment, however, can damage the tissue, leading to erroneous interpretations of mineral content. We performed elemental (EDX) and mineral content (BSE) analyses on bone tissue in order to quantify observable deleterious effects in the context of (1) prolonged scanning time, (2) scan versus point (spot) mode, (3) low versus high magnification, and (4) embedding in poly-methylmethacrylate (PMMA). Undemineralized cortical bone specimens from adult human femora were examined in three groups: 200x embedded, 200x unembedded, and 1000x embedded. Coupled BSE/EDX analyses were conducted five consecutive times, with no location analyzed more than five times. Variation in the relative proportions of calcium (Ca), phosphorous (P), and carbon (C) were measured using EDX spectroscopy, and mineral content variations were inferred from changes in mean gray levels ("atomic number contrast") in BSE images captured at 20 keV. In point mode at 200x, the embedded specimens exhibited a significant increase in Ca by the second measurement (7.2%, p < 0.05); in scan mode, a small and statistically nonsignificant increase (1.0%) was seen by the second measurement. Changes in P were similar, although the increases were less. The apparent increases in Ca and P likely result from decreases in C: -3.2% (p < 0.05) in point mode and -0.3% in scan mode by the second measurement. Analysis of unembedded specimens showed similar results. In contrast to embedded specimens at 200x, 1000x data showed significantly larger variations in the proportions of Ca, P, and C by the second or third measurement in scan and point mode. At both magnifications, BSE image gray level values increased (suggesting increased mineral content) by the second measurement, with increases up to 23% in point mode. These results show that mineral content measurements can be reliable when using coupled BSE/EDX analyses in PMMA-embedded bone if lower magnifications are used in scan mode and if prolonged exposure to the electron beam is avoided. When point mode is used to analyze minute regions, adjustments in accelerating voltages and probe current may be required to minimize damage.

Physical examination, magnetic resonance image, and electrodiagnostic study in patients with lumbosacral disc herniation or spinal stenosis.

PubMed

Lee, Jung Hwan; Lee, Sang-Ho

2012-10-01

To compare the clinical implications of electro-diagnostic study with those of magnetic resonance imaging in patients with lumbosacral intervertebral herniated disc or spinal stenosis. Retrospective study of clinical data. Patients with lumbosacral intervertebral herniated disc or spinal stenosis, diagnosed by clinical assessment and magnetic resonance imaging (MRI), were selected. A total of 753 patients (437 with lumbosacral intervertebral herniated disc and 316 with spinal stenosis) were included in the study. Clinical data for electrodiagnostic study (EDX)and MRI were compared and the sensitivity and specificity of these studies were evaluated. Among all subjects, 267 had radiculopathy on EDX (EDX (+)) and 486 no radiculopathy (EDX(-)). Furthermore, 391 had root compression on MRI (MRI (+)) and 362 no root compression on MRI (MRI (-)). Patients with radioculopathy on EDX (+) showed a significantly higher visual analogue scale score for radiating pain and a higher Oswestry Disability Index than those with negative findings by EDX (-) in the total subjects group and the lumbosacral intervertebral herniated disc subgroup, and there was a trend toward higher Oswestry Disability Index in the spinal stenosis subgroup. Although patients with radioculopathy on root compression on MRI (+) also had a higher visual analogue scale for radiating pain than patients with negative findings by MRI (-) in the total subjects group and the lumbosacral intervertebral herniated disc subgroup, no significant difference was seen in the Oswestry Disability Index. EDX revealed a significant correlation with muscle weakness in the total subjects group and the lumbosacral intervertebral herniated disc subgroup, and trends toward muscle weakness in the spinal stenosis subgroup, whereas there was no such significant correlation for MRI findings in any group. Electrodiagnostic study had a higher specificity in terms of physical examination data than MRI, in spite of its lower sensitivity. Electrodiagnostic study was significantly more correlated with clinical data, especially leg muscle weakness and functional status, and showed a higher specificity than MRI in patients with lumbosacral intervertebral herniated disc or spinal stenosis.

Elemental composition and structural characteristics of as-received TriTaniumTM orthodontic archwire

NASA Astrophysics Data System (ADS)

Ilievska, I.; Petrov, V.; Mihailov, V.; Karatodorov, S.; Andreeva, L.; Zaleski, A.; Mikli, V.; Gueorgieva, M.; Petrova, V.; Stoyanova-Ivanova, A.

2018-03-01

Orthodontic archwires are among the most important devices of fixed orthodontic therapy. Many types of archwires are made available on the market by various manufacturers with different elemental composition and structural characteristics. Knowing this information is important when choosing a suitable archwire for a particular stage of orthodontic treatment. The aim of our study is to characterize a new type orthodontic archwires (TriTaniumTM, American Orthodontics) before their placement in the oral cavity. To achieve the aim, we used modern methods for determining their elemental composition and structural characteristics: laser-induced plasma spectroscopy (LIBS), X-ray diffraction analysis (XRD), scanning electronic microscopy (SEM), energy dispersive X-ray spectroscopy (EDX) and differential scanning calorimetry (DSC). The results obtained from the qualitative elemental analysis by LIBS and the quantitative elemental analysis by EDX showed that Ni and Ti are the main elements in the archwire studied. The room-temperature XRD patterns showed peaks typical for a Ni-Ti alloy with an austenite-type structure. Monitoring the phase transitions by means of DSC measurements in the temperature range from –50 °C to +50 °C, we showed that in TriTaniumTM archwires, besides the austenite to martensite transition, there exists a rhombohedral intermediate phase (R phase). This study will be useful in assisting orthodontists in applying appropriate nickel-titanium orthodontic archwires in the clinical practice.

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.

Direct observation of the core/double-shell architecture of intense dual-mode luminescent tetragonal bipyramidal nanophosphors

NASA Astrophysics Data System (ADS)

Kim, Su Yeon; Jeong, Jong Seok; Mkhoyan, K. Andre; Jang, Ho Seong

2016-05-01

Highly efficient downconversion (DC) green-emitting LiYF4:Ce,Tb nanophosphors have been synthesized for bright dual-mode upconversion (UC) and DC green-emitting core/double-shell (C/D-S) nanophosphors--Li(Gd,Y)F4:Yb(18%),Er(2%)/LiYF4:Ce(15%),Tb(15%)/LiYF4--and the C/D-S structure has been proved by extensive scanning transmission electron microscopy (STEM) analysis. Colloidal LiYF4:Ce,Tb nanophosphors with a tetragonal bipyramidal shape are synthesized for the first time and they show intense DC green light via energy transfer from Ce3+ to Tb3+ under illumination with ultraviolet (UV) light. The LiYF4:Ce,Tb nanophosphors show 65 times higher photoluminescence intensity than LiYF4:Tb nanophosphors under illumination with UV light and the LiYF4:Ce,Tb is adapted into a luminescent shell of the tetragonal bipyramidal C/D-S nanophosphors. The formation of the DC shell on the core significantly enhances UC luminescence from the UC core under irradiation of near infrared light and concurrently generates DC luminescence from the core/shell nanophosphors under UV light. Coating with an inert inorganic shell further enhances the UC-DC dual-mode luminescence by suppressing the surface quenching effect. The C/D-S nanophosphors show 3.8% UC quantum efficiency (QE) at 239 W cm-2 and 73.0 +/- 0.1% DC QE. The designed C/D-S architecture in tetragonal bipyramidal nanophosphors is rigorously verified by an energy dispersive X-ray spectroscopy (EDX) analysis, with the assistance of line profile simulation, using an aberration-corrected scanning transmission electron microscope equipped with a high-efficiency EDX. The feasibility of these C/D-S nanophosphors for transparent display devices is also considered.Highly efficient downconversion (DC) green-emitting LiYF4:Ce,Tb nanophosphors have been synthesized for bright dual-mode upconversion (UC) and DC green-emitting core/double-shell (C/D-S) nanophosphors--Li(Gd,Y)F4:Yb(18%),Er(2%)/LiYF4:Ce(15%),Tb(15%)/LiYF4--and the C/D-S structure has been proved by extensive scanning transmission electron microscopy (STEM) analysis. Colloidal LiYF4:Ce,Tb nanophosphors with a tetragonal bipyramidal shape are synthesized for the first time and they show intense DC green light via energy transfer from Ce3+ to Tb3+ under illumination with ultraviolet (UV) light. The LiYF4:Ce,Tb nanophosphors show 65 times higher photoluminescence intensity than LiYF4:Tb nanophosphors under illumination with UV light and the LiYF4:Ce,Tb is adapted into a luminescent shell of the tetragonal bipyramidal C/D-S nanophosphors. The formation of the DC shell on the core significantly enhances UC luminescence from the UC core under irradiation of near infrared light and concurrently generates DC luminescence from the core/shell nanophosphors under UV light. Coating with an inert inorganic shell further enhances the UC-DC dual-mode luminescence by suppressing the surface quenching effect. The C/D-S nanophosphors show 3.8% UC quantum efficiency (QE) at 239 W cm-2 and 73.0 +/- 0.1% DC QE. The designed C/D-S architecture in tetragonal bipyramidal nanophosphors is rigorously verified by an energy dispersive X-ray spectroscopy (EDX) analysis, with the assistance of line profile simulation, using an aberration-corrected scanning transmission electron microscope equipped with a high-efficiency EDX. The feasibility of these C/D-S nanophosphors for transparent display devices is also considered. Electronic supplementary information (ESI) available: XRD patterns, PL and PLE spectra, SEM and HR-TEM images, PL decay times, photographs showing the transparent nanophosphor solutions and their dual-mode luminescence, and additional EDX data. See DOI: 10.1039/c5nr05722a

[Simultaneous determination of multiple elements in airborne particulate samples by X-ray fluorescence spectrometry].

PubMed

Takada, T; Hitosugi, M; Kadowaki, T; Kudo, M

1983-07-01

An energy dispersive X-ray fluorescence spectrometer (EDX) has been applied to determine multielements in the workplace air. The standards for X-ray fluorescence analysis were prepared by the chelate precipitation method on polyvinyl chloride (PVC) membrane filter. And, the specimens were prepared to deposit various metal compounds of different chemical forms by the suspension method on PVC membrane filter, and they were determined with EDX and atomic absorption spectrometer (AAS). The results obtained were as follows. Though there is a difference by each element, an amount less than 3 microgram/cm2 per unit area makes it possible to undergo multielement analysis, that is, is has no influence on fine particle effect (particle size; under 5 microns). Then, effects of the X-ray intensity by different chemical forms are negligible. At the presence the neighboring element and other elements this technique showed greater precision by carrying out on corrective treatment, etc. The coefficient of variation of this technique was in the range of 2.5-6.5% at DDTC-Cu of 0.5-5.0 micrograms/cm2, with the limit of detection for As : 0.002 microgram/cm2, Zn : 0.003 microgram/cm2, Pb : 0.003 microgram/cm2, Cu : 0.004 microgram/cm2, Ni : 0.003 microgram/cm2, Fe : 0.005 microgram/cm2, Mn : 0.008 microgram/cm2, Cr : 0.013 microgram/cm2, respectively. Aerosols collected at the workplace were analyzed with EDX and AAS, and the obtained results showed good agreement with such regression line as y = 1.04 chi + 0.04, the coefficient of correlation being r = 0.995. From these results, this technique was found to be a very excellent method for monitoring of multielements in the workplace air.

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.

Multi-color electron microscopy by element-guided identification of cells, organelles and molecules.

PubMed

Scotuzzi, Marijke; Kuipers, Jeroen; Wensveen, Dasha I; de Boer, Pascal; Hagen, Kees C W; Hoogenboom, Jacob P; Giepmans, Ben N G

2017-04-07

Cellular complexity is unraveled at nanometer resolution using electron microscopy (EM), but interpretation of macromolecular functionality is hampered by the difficulty in interpreting grey-scale images and the unidentified molecular content. We perform large-scale EM on mammalian tissue complemented with energy-dispersive X-ray analysis (EDX) to allow EM-data analysis based on elemental composition. Endogenous elements, labels (gold and cadmium-based nanoparticles) as well as stains are analyzed at ultrastructural resolution. This provides a wide palette of colors to paint the traditional grey-scale EM images for composition-based interpretation. Our proof-of-principle application of EM-EDX reveals that endocrine and exocrine vesicles exist in single cells in Islets of Langerhans. This highlights how elemental mapping reveals unbiased biomedical relevant information. Broad application of EM-EDX will further allow experimental analysis on large-scale tissue using endogenous elements, multiple stains, and multiple markers and thus brings nanometer-scale 'color-EM' as a promising tool to unravel molecular (de)regulation in biomedicine.

Multi-color electron microscopy by element-guided identification of cells, organelles and molecules

PubMed Central

Scotuzzi, Marijke; Kuipers, Jeroen; Wensveen, Dasha I.; de Boer, Pascal; Hagen, Kees (C.) W.; Hoogenboom, Jacob P.; Giepmans, Ben N. G.

2017-01-01

Cellular complexity is unraveled at nanometer resolution using electron microscopy (EM), but interpretation of macromolecular functionality is hampered by the difficulty in interpreting grey-scale images and the unidentified molecular content. We perform large-scale EM on mammalian tissue complemented with energy-dispersive X-ray analysis (EDX) to allow EM-data analysis based on elemental composition. Endogenous elements, labels (gold and cadmium-based nanoparticles) as well as stains are analyzed at ultrastructural resolution. This provides a wide palette of colors to paint the traditional grey-scale EM images for composition-based interpretation. Our proof-of-principle application of EM-EDX reveals that endocrine and exocrine vesicles exist in single cells in Islets of Langerhans. This highlights how elemental mapping reveals unbiased biomedical relevant information. Broad application of EM-EDX will further allow experimental analysis on large-scale tissue using endogenous elements, multiple stains, and multiple markers and thus brings nanometer-scale ‘color-EM’ as a promising tool to unravel molecular (de)regulation in biomedicine. PMID:28387351

The green synthesis of fine particles of gold using an aqueous extract of Monotheca buxifolia (Flac.)

NASA Astrophysics Data System (ADS)

Anwar, Natasha; Khan, Abbas; Shah, Mohib; Azam, Andaleeb; Zaman, Khair; Parven, Zahida

2016-12-01

This study deals with the synthesis and physicochemical investigation of gold nanoparticles using an aqueous extract of Monotheca buxifolia (Flac.). On the treatment of aqueous solution of tetrachloroauric acid with the plant extract, gold nanoparticles were rapidly fabricated. The synthesized particles were characterized by UV-Vis spectrophotometry (UV), Fourier transform infrared spectroscopy (FTIR), energy dispersive X-ray (EDX) and Scanning electron microscopy (SEM). The formation of AuNPs was confirmed by noting the change in color through visual observations as well as via UV-Vis spectroscopy. UV‒Vis spectrum of the aqueous medium containing gold nanoparticles showed an absorption peak at around 540 nm. FTIR was used to identify the chemical composition of gold nanoparticles and Au-capped plant extract. The presence of elemental gold was also confirmed through EDX analysis. SEM analysis of the gold nanoparticles showed that they have a uniform spherical shape with an average size in the range of 70-78 nm. This green system showed to be better capping and stabilizing agent for the fine particles. Further, the antioxidant activity of Monotheca buxifolia (Flac.) extract and Au-capped with the plant extract was also evaluated using FeCl3/K3[Fe(CN)]6 in vitro assay.

Surface modification of AISI H13 tool steel by laser cladding with NiTi powder

NASA Astrophysics Data System (ADS)

Norhafzan, B.; Aqida, S. N.; Chikarakara, E.; Brabazon, D.

2016-04-01

This paper presents laser cladding of NiTi powder on AISI H13 tool steel surface for surface properties enhancement. The cladding process was conducted using Rofin DC-015 diffusion-cooled CO2 laser system with wavelength of 10.6 µm. NiTi powder was pre-placed on H13 tool steel surface. The laser beam was focused with a spot size of 90 µm on the sample surface. Laser parameters were set to 1515 and 1138 W peak power, 18 and 24 % duty cycle and 2300-3500 Hz laser pulse repetition frequency. Hardness properties of the modified layer were characterized by Wilson Hardness tester. Metallographic study and chemical composition were conducted using field emission scanning electron microscope and energy-dispersive X-ray spectrometer (EDXS) analysis. Results showed that hardness of NiTi clad layer increased three times that of the substrate material. The EDXS analysis detected NiTi phase presence in the modified layer up to 9.8 wt%. The metallographic study shows high metallurgical bonding between substrate and modified layer. These findings are significant to both increased hardness and erosion resistance of high-wear-resistant components and elongating their lifetime.

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.

[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.

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

Coordinated EDX and micro-Raman analysis of presolar silicon carbide: A novel, nondestructive method to identify rare subgroup SiC

NASA Astrophysics Data System (ADS)

Liu, Nan; Steele, Andrew; Nittler, Larry R.; Stroud, Rhonda M.; De Gregorio, Bradley T.; Alexander, Conel M. O'D.; Wang, Jianhua

2017-12-01

We report the development of a novel method to nondestructively identify presolar silicon carbide (SiC) grains with high initial 26Al/27Al ratios (>0.01) and extreme 13C-enrichments (12C/13C ≤ 10) by backscattered electron-energy dispersive X-ray (EDX) and micro-Raman analyses. Our survey of a large number of presolar SiC demonstrates that (1) 80% of core-collapse supernova and putative nova SiC can be identified by quantitative EDX and Raman analyses with >70% confidence; (2) 90% of presolar SiC are predominantly 3C-SiC, as indicated by their Raman transverse optical (TO) peak position and width; (3) presolar 3C-SiC with 12C/13C ≤ 10 show lower Raman TO phonon frequencies compared to mainstream 3C-SiC. The downward shifted phonon frequencies of the 13C-enriched SiC with concomitant peak broadening are a natural consequence of isotope substitution. 13C-enriched SiC can therefore be identified by micro-Raman analysis; (4) larger shifts in the Raman TO peak position and width indicate deviations from the ideal 3C structure, including rare polytypes. Coordinated transmission electron microscopy analysis of one X and one mainstream SiC grain found them to be of 6H and 15R polytypes, respectively; (5) our correlated Raman and NanoSIMS study of mainstream SiC shows that high nitrogen content is a dominant factor in causing mainstream SiC Raman peak broadening without significant peak shifts; and (6) we found that the SiC condensation conditions in different stellar sites are astonishingly similar, except for X grains, which often condensed more rapidly and at higher atmospheric densities and temperatures, resulting in a higher fraction of grains with much downward shifted and broadened Raman TO peaks.

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

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.

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.

Defective enamel ultrastructure in diabetic rodents.

PubMed

Atar, M; Atar-Zwillenberg, D R; Verry, P; Spornitz, U M

2004-07-01

We investigated six different types of diabetic rodents. Four expressed a genetic obesity resulting in diabetes. One developed diabetes induced by a diet-dependent obesity, and one with genetic diabetes received anti-diabetic medication. The tooth samples were examined under a scanning electron microscope and with an energy dispersive microanalysis (EDX). The electron micrographs showed severe, varying degrees of damage within the six different diabetic animal types, such as irregular crystallite deposition and prism perforations in genetically obese animals compared to less-disordered prism structures in diet-dependent obesity. Anti-diabetic medication resulted in normal enamel ultrastructure. The EDX analysis revealed a reduction in the amount of calcium and phosphorus in all regions affected by diabetes. Based on these animal studies, we suggest that both juvenile diabetes type I (in infants) and adult diabetes type II (in pregnant mothers, affecting the developing foetus) may affect the normal development of teeth in humans.

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.

Orthogonal identification of gunshot residue with complementary detection principles of voltammetry, scanning electron microscopy, and energy-dispersive X-ray spectroscopy: sample, screen, and confirm.

PubMed

O'Mahony, Aoife M; Samek, Izabela A; Sattayasamitsathit, Sirilak; Wang, Joseph

2014-08-19

Field-deployable voltammetric screening coupled with complementary laboratory-based analysis to confirm the presence of gunshot residue (GSR) from the hands of a subject who has handled, loaded, or discharged a firearm is described. This protocol implements the orthogonal identification of the presence of GSR utilizing square-wave stripping voltammetry (SWSV) as a rapid screening tool along with scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) to confirm the presence of the characteristic morphology and metal composition of GSR particles. This is achieved through the judicious modification of the working electrode of a carbon screen-printed electrode (CSPE) with carbon tape (used in SEM analysis) to fix and retain a sample. A comparison between a subject who has handled and loaded a firearm and a subject who has had no contact with GSR shows the significant variations in voltammetric signals and the presence or absence of GSR-consistent particles and constituent metals. This initial electrochemical screening has no effect on the integrity of the metallic particles, and SEM/EDX analysis conducted prior to and postvoltammetry show no differences in analytical output. The carbon tape is instrumental in retaining the GSR sample after electrochemical analysis, supported by comparison with orthogonal detection at a bare CSPE. This protocol shows great promise as a two-tier detection system for the presence of GSR from the hands of a subject, whereby initial screening can be conducted rapidly onsite by minimally trained operators; confirmation can follow at the same substrate to substantiate the voltammetric results.

Acute-onset chronic inflammatory demyelinating polyneuropathy: An electrodiagnostic study.

PubMed

Anadani, Mohammad; Katirji, Bashar

2015-11-01

Acute-onset chronic inflammatory demyelinating polyneuropathy (A-CIDP) is an increasingly recognized CIDP subtype. Differentiating A-CIDP from Guillain-Barré syndrome (GBS) is challenging but important, because there are different treatment outcomes. We report 3 patients with A-CIDP who were initially diagnosed with severe GBS but were later confirmed to have CIDP based on their clinical course and electrodiagnostic (EDx) studies. We also report on the long-term treatment of these patients and review the literature on EDx studies in this syndrome. Three patients were initially diagnosed with GBS and responded to treatment. However, all 3 had arrest in improvement or deterioration during their rehabilitation phases. EDx studies showed prominent demyelinating changes many months after the initial presentation. All responded very well to immunotherapy. Although several features may suggest the diagnosis of A-CIDP at initial presentation, close follow-up of GBS patients during the recovery phase is also needed for accurate diagnosis. EDx studies may distinguish patients with A-CIDP from GBS patients. © 2015 Wiley Periodicals, Inc.

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.

A standards-based method for compositional analysis by energy dispersive X-ray spectrometry using multivariate statistical analysis: application to multicomponent alloys.

PubMed

Rathi, Monika; Ahrenkiel, S P; Carapella, J J; Wanlass, M W

2013-02-01

Given an unknown multicomponent alloy, and a set of standard compounds or alloys of known composition, can one improve upon popular standards-based methods for energy dispersive X-ray (EDX) spectrometry to quantify the elemental composition of the unknown specimen? A method is presented here for determining elemental composition of alloys using transmission electron microscopy-based EDX with appropriate standards. The method begins with a discrete set of related reference standards of known composition, applies multivariate statistical analysis to those spectra, and evaluates the compositions with a linear matrix algebra method to relate the spectra to elemental composition. By using associated standards, only limited assumptions about the physical origins of the EDX spectra are needed. Spectral absorption corrections can be performed by providing an estimate of the foil thickness of one or more reference standards. The technique was applied to III-V multicomponent alloy thin films: composition and foil thickness were determined for various III-V alloys. The results were then validated by comparing with X-ray diffraction and photoluminescence analysis, demonstrating accuracy of approximately 1% in atomic fraction.

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.

Analysis of Multilayer Devices for Superconducting Electronics by High-Resolution Scanning Transmission Electron Microscopy and Energy Dispersive Spectroscopy

DOE PAGES

Missert, Nancy; Kotula, Paul G.; Rye, Michael; ...

2017-02-15

We used a focused ion beam to obtain cross-sectional specimens from both magnetic multilayer and Nb/Al-AlOx/Nb Josephson junction devices for characterization by scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX). An automated multivariate statistical analysis of the EDX spectral images produced chemically unique component images of individual layers within the multilayer structures. STEM imaging elucidated distinct variations in film morphology, interface quality, and/or etch artifacts that could be correlated to magnetic and/or electrical properties measured on the same devices.

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.

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.

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.

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.

Magnesium-Aluminum-Zirconium Oxide Amorphous Ternary Composite: A Dense and Stable Optical Coating

NASA Technical Reports Server (NTRS)

Sahoo, N. K.; Shapiro, A. P.

1998-01-01

In the present work, the process parameter dependent optical and structural properties of MgO-Al(2)O(3)-ZrO(2) ternary mixed-composite material have been investigated. Optical properties were derived from spectrophotometric measurements. The surface morphology, grain size distributions, crystallographic phases and process dependent material composition of films have been investigated through the use of Atomic Force Microscopy (AFM), X-ray diffraction analysis and Energy Dispersive X- ray (EDX) analysis. EDX analysis made evident the correlation between the optical constants and the process dependent compositions in the films. It is possible to achieve environmentally stable amorphous films with high packing density under certain optimized process conditions.

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.

A transmission electron microscopy study of Fe-Co alloy nanoparticles in silica aerogel matrix using HREM, EDX, and EELS.

PubMed

Falqui, Andrea; Corrias, Anna; Gass, Mhairi; Mountjoy, Gavin

2009-04-01

Magnetic nanocomposite materials consisting of 5.5 wt% Fe-Co alloy nanoparticles in a silica aerogel matrix, with compositions Fe(x)Co(1-x) of x = 0.50 and 0.67, have been synthesized by the sol-gel method. The high-resolution transmission electron microscopy images show nanoparticles consisting of single crystal grains of body-centered cubic Fe-Co alloy, with typical crystal grain diameters of approximately 4 and 7 nm for Fe(0.5)Co(0.5) and Fe(0.67)Co(0.33) samples, respectively. The energy dispersive X-ray (EDX) spectra summed over areas of the samples gave compositions Fe(x)C(o1-x) with x = 0.48 +/- 0.06 and 0.68 +/- 0.05. The EDX spectra obtained with the 1.5 nm probe positioned at the centers of approximately 20 nanoparticles gave slightly lower concentrations of Fe, with means of x = 0.43 +/- 0.01 and x = 0.64 +/- 0.02, respectively. The Fe(0.5)Co(0.50) sample was studied using electron energy loss spectroscopy (EELS), and EELS spectra summed over whole nanoparticles gave x = 0.47 +/- 0.06. The EELS spectra from analysis profiles of nanoparticles show a distribution of Fe and Co that is homogeneous, i.e., x = 0.5, within a precision of at best +/-0.05 in x and +/-0.4 nm in position. The present microscopy results have not shown the presence of a thin layer of iron oxide, but this might be at the limit of detectability of the methods.

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

Dental Enamel Irradiated with Infrared Diode Laser and Photo-Absorbing Cream: Part 2—EDX Study

PubMed Central

dos Santos, Edson Aparecido Pereira; Soares, Luís Eduardo Silva; do Espírito Santo, Ana Maria; Martin, Airton Abrahão; Duarte, Danilo Antônio; Pacheco-Soares, Cristina; Brugnera, Aldo

2009-01-01

Abstract Objective: The effects of laser-induced compositional changes on the enamel were investigated by energy-dispersive X-ray fluorescence spectrometry (μ-EDX). After cariogenic challenge, we administered treatment of low-level infrared diode laser and a photo-absorbing cream (used to intensify the superficial light absorption). Background Data: Dental caries is considered the most prevalent oral disease. A simple and noninvasive caries preventive regimen is treating tooth enamel with a laser, either alone or in combination with fluoride, which reduces enamel solubility and dissolution rates. High power lasers are still not widely used in private practice. Low-power near-infrared lasers may be an alternative approach. Energy-dispersive μ-EDX is a versatile and nondestructive spectroscopic technique that allows for a qualitative and quantitative elemental analysis of inorganic enamel components, such as calcium and phosphorus. Materials and Methods: Twenty-four extracted or exfoliated caries-free deciduous molars were divided into six groups: 1) control group (CTR-no treatment); 2) infrared laser treatment (L) (λ = 810 nm, 100 mW/cm2, 90 sec, 4.47 J/cm2, 9 J); 3) infrared laser irradiation and photo-absorbing agent (CL); 4) photo-absorbing agent alone (C); 5) infrared laser irradiation and fluoridated photo-absorbing agent (FCL); and 6) fluoridated photo-absorbing agent alone (FC). Samples were analyzed using μ-EDX after two sets of treatments and pH cycling cariogenic challenges. Results: The CL group showed statistically significant increases in calcium and phosphorus (wt%) compared with the CTR group. The Ca/P ratio was similar in the FCL and CTR groups. There was a significant laser-induced reduction compared with the CTR group, and there was a possible modification of the organic balance content in enamel treated with laser and cream. Conclusion: μ-EDX may be able to detect compositional changes in mineral phases of lased enamel under cariogenic challenge. Our results suggest that with a combined laser and photo-absorbing agent (CL) treatment, there was a possible disorganization of organic content in the tooth enamel with hydroxyapatite crystal reordering and reorganization. PMID:19878028

Dental enamel irradiated with infrared diode laser and photo-absorbing cream: part 2--EDX study.

PubMed

de Sant'Anna, Giselle Rodrigues; dos Santos, Edson Aparecido Pereira; Soares, Luís Eduardo Silva; do Espírito Santo, Ana Maria; Martin, Airton Abrahão; Duarte, Danilo Antônio; Pacheco-Soares, Cristina; Brugnera, Aldo

2009-10-01

The effects of laser-induced compositional changes on the enamel were investigated by energy-dispersive X-ray fluorescence spectrometry (micro-EDX). After cariogenic challenge, we administered treatment of low-level infrared diode laser and a photo-absorbing cream (used to intensify the superficial light absorption). Dental caries is considered the most prevalent oral disease. A simple and noninvasive caries preventive regimen is treating tooth enamel with a laser, either alone or in combination with fluoride, which reduces enamel solubility and dissolution rates. High power lasers are still not widely used in private practice. Low-power near-infrared lasers may be an alternative approach. Energy-dispersive micro-EDX is a versatile and nondestructive spectroscopic technique that allows for a qualitative and quantitative elemental analysis of inorganic enamel components, such as calcium and phosphorus. Twenty-four extracted or exfoliated caries-free deciduous molars were divided into six groups: 1) control group (CTR-no treatment); 2) infrared laser treatment (L) (lambda = 810 nm, 100 mW/cm(2), 90 sec, 4.47 J/cm(2), 9 J); 3) infrared laser irradiation and photo-absorbing agent (CL); 4) photo-absorbing agent alone (C); 5) infrared laser irradiation and fluoridated photo-absorbing agent (FCL); and 6) fluoridated photo-absorbing agent alone (FC). Samples were analyzed using micro-EDX after two sets of treatments and pH cycling cariogenic challenges. The CL group showed statistically significant increases in calcium and phosphorus (wt%) compared with the CTR group. The Ca/P ratio was similar in the FCL and CTR groups. There was a significant laser-induced reduction compared with the CTR group, and there was a possible modification of the organic balance content in enamel treated with laser and cream. micro-EDX may be able to detect compositional changes in mineral phases of lased enamel under cariogenic challenge. Our results suggest that with a combined laser and photo-absorbing agent (CL) treatment, there was a possible disorganization of organic content in the tooth enamel with hydroxyapatite crystal reordering and reorganization.

Allochthonous Addition of Meteoritic Organics to the Lunar Regolith

NASA Technical Reports Server (NTRS)

Thomas-Keprta, K. L.; Clemett, S.; Ross, D. K.; Le, L.; Rahman, Z.; McKay, D. S.; Gibson, E. K.; Gonzalez, C.

2013-01-01

Preparation of lunar samples 74220,861 was discussed in detail in [3, 4]. Our analysis sequence was as follows: optical microscopy, UV fluorescence imaging, -Raman, FESEM-EDX imaging and mapping, FETEMEDX imaging and mapping of a Focused Ion Beam (FIB) extracted section, and NanoSIMs analysis. We observed fluffytextured C-rich regions of interest (ROI) on three different volcanic glass beads. Each ROI was several m2 in size and fluoresced when exposed to UV. Using FESEM/EDX, the largest ROI measured 36 m and was located on an edge of a plateau located on the uppermost surface of the bead. The ROI was covered on one edge by a siliceous filament emanating from the plateau surface indicating it was attached to the bead while on the Moon. EDX mapping of the ROI shows it is composed primarily of heterogeneously distributed C. Embedded with the carbonaceous phase are localized concentrations of Si, Fe, Al and Ti indicating the presence of glass and/or minerals grains. -Raman showed strong D- and G-bands and their associated second order bands; intensity and location of these bands indicates the carbonaceous matter is structurally disorganized. A TEM thin section was extracted from the surface of a glass bead using FIB microscopy. High resolution TEM imaging and selected area electron diffraction demonstrate the carbonaceous layer to be amorphous; it lacked any long or short range order characteristic of micro- or nanocrystalline graphite. Additionally TEM imaging also revealed the presence of submicron mineral grains, typically < 50 nm in size, dispersed within the carbonaceous layer. NanoSIMs data will be presented and discussed at the meeting. Given the noted similarities between the carbonaceous matter present on 74220 glass beads and meteoritic kerogen, we suggest the allochthonous addition of meteoritic organics as the most probable source for the C-rich ROIs.

Errors in quantitative backscattered electron analysis of bone standardized by energy-dispersive x-ray spectrometry.

PubMed

Vajda, E G; Skedros, J G; Bloebaum, R D

1998-10-01

Backscattered electron (BSE) imaging has proven to be a useful method for analyzing the mineral distribution in microscopic regions of bone. However, an accepted method of standardization has not been developed, limiting the utility of BSE imaging for truly quantitative analysis. Previous work has suggested that BSE images can be standardized by energy-dispersive x-ray spectrometry (EDX). Unfortunately, EDX-standardized BSE images tend to underestimate the mineral content of bone when compared with traditional ash measurements. The goal of this study is to investigate the nature of the deficit between EDX-standardized BSE images and ash measurements. A series of analytical standards, ashed bone specimens, and unembedded bone specimens were investigated to determine the source of the deficit previously reported. The primary source of error was found to be inaccurate ZAF corrections to account for the organic phase of the bone matrix. Conductive coatings, methylmethacrylate embedding media, and minor elemental constituents in bone mineral introduced negligible errors. It is suggested that the errors would remain constant and an empirical correction could be used to account for the deficit. However, extensive preliminary testing of the analysis equipment is essential.

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

Missert, Nancy; Kotula, Paul G.; Rye, Michael

We used a focused ion beam to obtain cross-sectional specimens from both magnetic multilayer and Nb/Al-AlOx/Nb Josephson junction devices for characterization by scanning transmission electron microscopy (STEM) and energy dispersive X-ray spectroscopy (EDX). An automated multivariate statistical analysis of the EDX spectral images produced chemically unique component images of individual layers within the multilayer structures. STEM imaging elucidated distinct variations in film morphology, interface quality, and/or etch artifacts that could be correlated to magnetic and/or electrical properties measured on the same devices.

The Synthesis of Silicon Carbide in Rhombohedral Form with Different Chemicals

NASA Astrophysics Data System (ADS)

KARİPER, İ. AFŞIN

2017-06-01

This study describes the attempt at producing silicon carbide using a simpler and less costly method. Within the study, XRD, EDX, and FTIR analyses were performed to determine the structural properties of the product, and SEM analyses were used to identify its surface properties. The characteristics such as porosity and surface area were determined through BET analysis. The starting reagents were compared with the product using FTIR analysis, whereas the product was compared with a sample of SiC procured from a supplier who manufactures high-purity products through BET analysis. In EDX analysis, approximately 72 pct Si and 28 pct C were identified. The vibrational peaks of the synthesized product (characteristics Si-C bonds) were observed at around 1076 cm-1 (FTIR analysis). At the same time, the outcomes were compared with major publications in the literature.

The in vitro effect of fluoridated milk in a bacterial biofilm--enamel model.

PubMed

Arnold, Wolfgang H; Forer, Stefan; Heesen, Joerg; Yudovich, Keren; Steinberg, Doron; Gaengler, Peter

2006-07-01

The purpose of this study was to investigate the effect of milk and fluoridated milk on bacterially induced caries-like lesions. Extracted impacted human molars were cut in half and covered with a varnish leaving a 4*4 mm window. The samples were coated with biofilm of S. sobrinus and were further divided into three experimental groups of S. sobrinus, S. sobrinus and milk and S. sobrinus and fluoridated milk. As negative controls served teeth incubated in saline. Of twenty tooth halves serial ground sections were cut through the lesions and investigated with polarization light microscopy (PLM) and scanning electron microscopy (SEM) and EDX element analysis. The PLM photographs were used for 3D reconstruction, volumetric assessment and determination of the extension of the lesion zones. Of eight tooth halves the biofilm on the enamel surface was studied with SEM and EDX element analysis. Volumetric assessment showed a statistically significant difference in the volume of the body of the lesion and the translucent zone between the milk group and fluoridated milk group. Quantitative element analysis demonstrated significant differences between sound enamel and the superficial layer in the fluoridated milk group. The biofilm on the enamel surface showed an increased Ca content in the milk group and fluoridated milk group. Milk as a common nutrient seems to play a complex role in in-vitro biofilm--enamel interactions stimulating bacterial demineralization on one hand, and, as effective fluoride carrier, inhibits caries-like demineralization.

The study and characteristics of ZnO/CdS nanocomposite and its application on nanoantibacterial activities

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

Ali, Tinku; Tripathi, P.; Ahammed, Nashiruddin

We have studied the structural and optical properties of ZnO/CdS nanocomposite and its application on nanoantibacterial activities. In this paper, we have used X-ray diffraction, Transmission electron microscope (TEM) and Energy dispersive X-ray spectroscopy (EDX) techniques in order to know about the structural and optical properties of synthesized ZnO/CdS nanocomposite. After TEM and EDX analysis it has been confirmed that the shape of this nanocomposite is hexagonal and it has no impurity. The optical absorption spectra of pure ZnO and ZnO/CdS nanocomposite have been presented by UV-Visible Spectrometer and the estimated band gap from absorption peak has been found tomore » be 3.36 and 3.74 eV respectively. Antibacterial activity of ZnO/CdS nanocomposite was evaluated by using standard zone of inhibition (ZOI) microbiology assay. The synthesized ZnO/CdS showed promising antibacterial activity against Staphylococcus aureus in dose dependent manner.« less

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.

Spectroscopic studies on sidewall carboxylic acid functionalization of multi-walled carbon nanotubes with valine

NASA Astrophysics Data System (ADS)

Deborah, M.; Jawahar, A.; Mathavan, T.; Dhas, M. Kumara; Benial, A. Milton Franklin

2015-03-01

The valine functionalized multi-walled carbon nanotubes (MWCNTS) were prepared and characterized by using XRD, UV-Vis, FT-IR, EPR, SEM, and EDX, spectroscopic techniques. The enhanced XRD peak (0 0 2) intensity was observed for valine functionalized MWCNTs compared with oxidized MWCNTs, which is likely due to sample purification by acid washing. UV-Vis study shows the formation of valine functionalized MWCNTs. FT-IR study confirms the presence of functional groups of oxidized MWCNTs and valine functionalized MWCNTs. The ESR line shape analysis indicates that the observed EPR line shape is a Gaussian line shape. The g-values indicate that the systems are isotropic in nature. The morphology study was carried out for oxidized MWCNTs and valine functionalized MWCNTs by using SEM. The EDX spectra revealed that the high purity of oxidized MWCNTs and valine functionalized MWCNTs. The functionalization has been chosen because, functionalization of CNTs with amino acids makes them soluble and biocompatible. Thus, they have potential applications in the field of biosensors and targeted drug delivery.

Chemical analysis of superconducting phase in K-doped picene

NASA Astrophysics Data System (ADS)

Kambe, Takashi; Nishiyama, Saki; Nguyen, Huyen L. T.; Terao, Takahiro; Izumi, Masanari; Sakai, Yusuke; Zheng, Lu; Goto, Hidenori; Itoh, Yugo; Onji, Taiki; Kobayashi, Tatsuo C.; Sugino, Hisako; Gohda, Shin; Okamoto, Hideki; Kubozono, Yoshihiro

2016-11-01

Potassium-doped picene (K3.0picene) with a superconducting transition temperature (T C) as high as 14 K at ambient pressure has been prepared using an annealing technique. The shielding fraction of this sample was 5.4% at 0 GPa. The T C showed a positive pressure-dependence and reached 19 K at 1.13 GPa. The shielding fraction also reached 18.5%. To investigate the chemical composition and the state of the picene skeleton in the superconducting sample, we used energy-dispersive x-ray (EDX) spectroscopy, MALDI-time-of-flight (MALDI-TOF) mass spectroscopy and x-ray diffraction (XRD). Both EDX and MALDI-TOF indicated no contamination with materials other than K-doped picene or K-doped picene fragments, and supported the preservation of the picene skeleton. However, it was also found that a magnetic K-doped picene sample consisted mainly of picene fragments or K-doped picene fragments. Thus, removal of the component contributing the magnetic quality to a superconducting sample should enhance the volume fraction.

Preliminary study of the biomechanical behavior and physical characteristics of tantalum (Ta)-coated prostheses.

PubMed

Duan, Yonghong; Liu, Lie; Wang, Ling; Guo, Fei; Li, Haoping; Shi, Lei; Li, Mao; Yin, Dayu; Jiang, Chi; Zhu, Qingsheng

2012-03-01

Use of Ta biomaterials in medicine started in the middle of the last century. The good biocompatibility and chemical stability, and the unique physical characteristics of Ta metal have resulted in many possible developments of Ta biomaterials. In this study, histopathological observation, histomorphometric analysis, scanning electron microscope (SEM) observation, energy-dispersive X-ray spectroscopy (EDX) analysis, biomechanical testing, and examination of the coating's mechanical strength have been used to evaluate the value of clinical application of Ta-coated prostheses prepared by a plasma-spraying process. Histopathological observation has demonstrated that the periprosthetic new bone tissues tightly and stably adhere to the Ta coating after the implantation, with no signs of loosening. Early after implantation, there is no significant difference in periprosthetic bone volume and ultimate shear strength between Ta-coated and Ti-coated prostheses (P > 0.05). EDX analysis suggests that the ultimate shear stress does not damage Ta coating. Mechanical strength testing shows that the adhesive strength and Vicker's surface hardness (HV) of the Ta coating are significantly higher than those of the Ti coating (P < 0.01). Ta coating has good stability and bone biocompatibility; the extraordinary physical characteristics of Ta coating have great significance in maintaining prosthetic stability and surface porosity after implantation.

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.

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.

Investigation of high temperature corrosion behavior on 304L austenite stainless steel in corrosive environments

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

Sahri, M. I.; Othman, N. K.; Samsu, Z.

2014-09-03

In this work, 304L stainless steel samples were exposed at 700 °C for 10hrs in different corrosive environments; dry oxygen, molten salt, and molten salt + dry oxygen. The corrosion behavior of samples was analyzed using weight change measurement technique, optical microscope (OM) and Scanning Electron Microscope (SEM) equipped with Energy Dispersive X-ray (EDX). The existence phases of corroded sample were determined using X-ray Diffraction (XRD). The lowest corrosion rate was recorded in dry oxygen while the highest was in molten salt + dry oxygen environments with the value of 0.0062 mg/cm{sup 2} and −13.5225 mg/cm{sup 2} respectively. The surfacemore » morphology of sample in presence of salt mixture showed scale spallation. Oxide scales of Fe{sub 3}O{sub 4}, Fe{sub 2}O{sub 3} were the main phases developed and detected by XRD technique. Cr{sub 2}O{sub 3} was not developed in every sample as protective layers but chromate-rich oxide was developed. The cross-section analysis found the oxide scales were in porous, thick and non-adherent that would not an effective barrier to prevent from further degradation of alloy. EDX analysis also showed the Cr-element was low compared to Fe-element at the oxide scale region.« less

Biosynthesis of silver nanoparticles using a probiotic Bacillus licheniformis Dahb1 and their antibiofilm activity and toxicity effects in Ceriodaphnia cornuta.

PubMed

Shanthi, Sathappan; Jayaseelan, Barbanas David; Velusamy, Palaniyandi; Vijayakumar, Sekar; Chih, Cheng Ta; Vaseeharan, Baskaralingam

2016-04-01

In the present study, we synthesized and characterized a probiotic Bacillus licheniformis cell free extract (BLCFE) coated silver nanoparticles (BLCFE-AgNPs). These BLCFE-AgNPs were characterized by UV-visible spectrophotometer, XRD, EDX, FTIR, TEM and AFM. A strong surface plasmon resonance centered at 422 nm in UV-visible spectrum indicates the formation of AgNPs. The XRD spectrum of silver nanoparticles exhibited 2θ values corresponding to the silver nanocrystal. TEM and AFM showed the AgNPs were spherical in shape within the range of 18.69-63.42 nm and the presence of silver was confirmed by EDX analysis. Light and Confocal Laser Scanning Microscope (CLSM) images showed a weak adherence and disintegrated biofilm formation of Vibrio parahaemolyticus Dav1 treated with BLCFE-AgNPs compared to control. This result suggests that BLCFE-AgNps may be used for the control of biofilm forming bacterial populations in the biomedical field. In addition, acute toxicity results concluded that BLCFE-AgNPs were less toxic to the fresh water crustacean Ceriodaphnia cornuta (50 μg/ml) when compared to AgNO3 (22 μg/ml). This study also reports a short term analysis (24 h) of uptake and depuration of BLCFE-AgNPs in C. cornuta. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

Unique local bone tissue characteristics in iliac crest bone biopsy from adolescent idiopathic scoliosis with severe spinal deformity

PubMed Central

Wang, Zhiwei; Chen, Huanxiong; Yu, Y. Eric; Zhang, Jiajun; Cheuk, Ka-Yee; Ng, Bobby K. W.; Qiu, Yong; Guo, X. Edward; Cheng, Jack C. Y.; Lee, Wayne Y. W.

2017-01-01

Adolescent idiopathic scoliosis is a complex disease with unclear etiopathogenesis. Systemic and persistent low bone mineral density is an independent prognostic factor for curve progression. The fundamental question of how bone quality is affected in AIS remains controversy because there is lack of site-matched control for detailed analysis on bone-related parameters. In this case-control study, trabecular bone biopsies from iliac crest were collected intra-operatively from 28 severe AIS patients and 10 matched controls with similar skeletal and sexual maturity, anthropometry and femoral neck BMD Z-score to control confounding effects. In addition to static histomorphometry, micro-computed tomography (μCT) and real time-PCR (qPCR) analyses, individual trabecula segmentation (ITS)-based analysis, finite element analysis (FEA), energy dispersive X-ray spectroscopy (EDX) were conducted to provide advanced analysis of structural, mechanical and mineralization features. μCT and histomorphometry showed consistently reduced trabecular number and connectivity. ITS revealed predominant change in trabecular rods, and EDX confirmed less mineralization. The structural and mineralization abnormality led to slight reduction in apparent modulus, which could be attributed to differential down-regulation of Runx2, and up-regulation of Spp1 and TRAP. In conclusion, this is the first comprehensive study providing direct evidence of undefined unique pathological changes at different bone hierarchical levels in AIS. PMID:28054655

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

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.

The antiestrogen endoxifen protects rat liver mitochondria from permeability transition pore opening and oxidative stress at concentrations that do not affect the phosphorylation efficiency

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

Ribeiro, Mariana P.C.; Silva, Filomena S.G.; Santos, Armanda E.

2013-02-15

Endoxifen (EDX) is a key active metabolite of tamoxifen (TAM) with higher affinity and specificity to estrogen receptors that also inhibits aromatase activity. It is safe and well tolerated by healthy humans, but its use requires toxicological characterization. In this study, the effects of EDX on mitochondria, the primary targets for xenobiotic-induced toxicity, were monitored to clarify its potential side effects. EDX up to 30 nmol/mg protein did not affect the mitochondrial oxidative phosphorylation. At 50 nmol EDX/mg protein, EDX decreased the ADP phosphorylation rate and a partial collapse of mitochondrial membrane potential (Δψ), that parallels a state 4 stimulation,more » was observed. As the stimulation of state 4 was not inhibited by oligomycin and 50 nmol EDX/mg protein caused a slight decrease in the light scattering of mitochondria, these data suggest that EDX promotes membrane permeabilization to protons, whereas TAM at the same concentration induced mitochondrial membrane disruption. Moreover, EDX at 10 nmol/mg protein prevented and reversed the Ca{sup 2+}-induced depolarization of ΔΨ and the release of mitochondrial Ca{sup 2+}, similarly to cyclosporine A, indicating that EDX did not affect Ca{sup 2+} uptake, but directly interfered with the proteins of the mitochondrial permeability transition (MPT) megacomplex, inhibiting MPT induction. At this concentration, EDX exhibited antioxidant activity that may account for the protective effect against MPT pore opening. In conclusion, EDX within the range of concentrations reached in tissues did not significantly damage the bioenergetic functions of mitochondria, contrarily to the prodrug TAM, and prevented the MPT pore opening and the oxidative stress in mitochondria, supporting that EDX may be a less toxic drug for women with breast carcinoma. - Highlights: ► Mitochondria are important targets of Endoxifen. ► Endoxifen prevents mitochondrial permeability transition. ► Endoxifen prevents oxidative stress in mitochondria. ► Endoxifen slightly affects mitochondrial bioenergetics in comparison with tamoxifen. ► Endoxifen is a key active metabolite of tamoxifen relevant in cancer therapy.« less

Quantitative analysis of a brass alloy using CF-LIBS and a laser ablation time-of-flight mass spectrometer

NASA Astrophysics Data System (ADS)

Ahmed, Nasar; Abdullah, M.; Ahmed, Rizwan; Piracha, N. K.; Aslam Baig, M.

2018-01-01

We present a quantitative analysis of a brass alloy using laser induced breakdown spectroscopy, energy dispersive x-ray spectroscopy (EDX) and laser ablation time-of-flight mass spectrometry (LA-TOF-MS). The emission lines of copper (Cu I) and zinc (Zn I), and the constituent elements of the brass alloy were used to calculate the plasma parameters. The plasma temperature was calculated from the Boltzmann plot as (10 000  ±  1000) K and the electron number density was determined as (2.0  ±  0.5)  ×  1017 cm-3 from the Stark-broadened Cu I line as well as using the Saha-Boltzmann equation. The elemental composition was deduced using these techniques: the Boltzmann plot method (70% Cu and 30% Zn), internal reference self-absorption correction (63.36% Cu and 36.64% Zn), EDX (61.75% Cu and 38.25% Zn), and LA-TOF (62% Cu and 38% Zn), whereas, the certified composition is (62% Cu and 38% Zn). It was observed that the internal reference self-absorption correction method yields analytical results comparable to that of EDX and LA-TOF-MS.

Investigation of the nanoscale two-component ZnS-ZnO heterostructures by means of HR-TEM and X-ray based analysis

NASA Astrophysics Data System (ADS)

Pankin, I. A.; Polozhentsev, O. E.; Soldatov, M. A.; Bugaev, A. L.; Tsaturyan, A.; Lomachenko, K. A.; Guda, A. A.; Budnyk, A. P.; Lamberti, C.; Soldatov, A. V.

2018-06-01

This article is devoted to the spectroscopic characterization of ZnS-ZnO nanoscale heterostructures synthesized by the microwave-assisted solvothermal method. The synthesized samples were investigated by means of X-ray powder diffraction (XRPD), high energy resolution fluorescence detected X-ray absorption near-edge-structure (HERFD-XANES) spectroscopy, valence-to-core X-ray emission spectroscopy (VtC-XES) and high resolution transmission electron microscopy (HR-TEM) as well as energy dispersive X-ray spectroscopy (EDX). The average crystallite size estimated by the broadening of XRPD peaks increases from 2.7 nm to 3.7 nm in the temperature range from 100 °C to 150 °C. HR-TEM images show that nanoparticles are arranged in aggregates with the 60-200 nm size. Theoretical estimation shows that the systems synthesized at higher temperatures more prone to the agglomeration. The full profile Reitveld analysis of XRPD data reveals the formation of hexagonal zinc sulfide structure, whereas electron diffraction data reveal also the formation of cubic zinc sulfide and claim the polymorphous character of the system. High energy resolution Zn K-edge XANES data unambiguously demonstrate the presence of a certain amount of the zinc oxide which is likely to have an amorphous structure and could not be detected by XRPD. Qualitative analysis of XANES data allows deriving ZnS/ZnO ratio as a function of synthesis temperature. EDX analysis depicts homogeneous distribution of ZnS and amorphous ZnO phases across the conglomerates. A complementary element-selective valence to core X-ray emission spectroscopy evidences formation of two-component system and confirms estimations of ZnS/ZnO fractions obtained by linear combination fit of XANES data.

The usefulness of electrodiagnostic studies in the diagnosis and management of neuromuscular disorders.

PubMed

Lindstrom, Heather; Ashworth, Nigel L

2018-03-13

This study seeks to evaluate the usefulness of electrodiagnostic (EDX) studies in terms of the patient's diagnosis and subsequent management and to identify patient groups in which EDX is particularly useful. The records of new patients referred to a single tertiary hospital EDX laboratory during 1 calendar year were reviewed to determine whether results of EDX studies led to a changed diagnosis and/or management plan. Logistic regression was used to determine whether any factors were associated with changed diagnosis or management. Results of EDX studies led to a change in diagnosis and a confirmation in diagnosis in 51.5% and 46.5% of the cases, respectively. Results of EDX studies led to a change in the management plan in 63.4% of all cases. The diagnosis and management plan were more likely to be changed in older patients and patients referred in hospital. EDX studies seem useful for confirming or changing the diagnosis and in guiding management in patients with suspected neuromuscular disorders. Muscle Nerve, 2018. © 2018 Wiley Periodicals, Inc.

An Aspergillus aculateus strain was capable of producing agriculturally useful nanoparticles via bioremediation of iron ore tailings.

PubMed

Bedi, Ankita; Singh, Braj Raj; Deshmukh, Sunil K; Adholeya, Alok; Barrow, Colin J

2018-06-01

Mining waste such as iron ore tailing is environmentally hazardous, encouraging researchers to develop effective bioremediation technologies. Among the microbial isolates collected from iron ore tailings, Aspergillus aculeatus (strain T6) showed good leaching efficiency and produced iron-containing nanoparticles under ambient conditions. This strain can convert iron ore tailing waste into agriculturally useful nanoparticles. Fourier-transform Infrared Spectroscopy (FT-IR analysis) established the at the particles are protein coated, with energy dispersive X-ray Spectroscopy (EDX analysis) showing strong signals for iron. Transmission Electron Microscopy (TEM analysis) showed semi-quasi spherical particles having average size of 15 ± 5 nm. These biosynthesized nanoparticles when tested for their efficacy on seed emergence activity of mungbean (Vigna radiata) seeds, and enhanced plant growth at 10 and 20 ppm. Copyright © 2018 Elsevier Ltd. All rights reserved.

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

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.

Spectroscopic studies on sidewall carboxylic acid functionalization of multi-walled carbon nanotubes with valine.

PubMed

Deborah, M; Jawahar, A; Mathavan, T; Dhas, M Kumara; Benial, A Milton Franklin

2015-03-15

The valine functionalized multi-walled carbon nanotubes (MWCNTS) were prepared and characterized by using XRD, UV-Vis, FT-IR, EPR, SEM, and EDX, spectroscopic techniques. The enhanced XRD peak (002) intensity was observed for valine functionalized MWCNTs compared with oxidized MWCNTs, which is likely due to sample purification by acid washing. UV-Vis study shows the formation of valine functionalized MWCNTs. FT-IR study confirms the presence of functional groups of oxidized MWCNTs and valine functionalized MWCNTs. The ESR line shape analysis indicates that the observed EPR line shape is a Gaussian line shape. The g-values indicate that the systems are isotropic in nature. The morphology study was carried out for oxidized MWCNTs and valine functionalized MWCNTs by using SEM. The EDX spectra revealed that the high purity of oxidized MWCNTs and valine functionalized MWCNTs. The functionalization has been chosen because, functionalization of CNTs with amino acids makes them soluble and biocompatible. Thus, they have potential applications in the field of biosensors and targeted drug delivery. Copyright © 2014 Elsevier B.V. All rights reserved.

Trace element content and magnetic properties of commercial HOPG samples studied by ion beam microscopy and SQUID magnetometry

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

Spemann, D., E-mail: spemann@uni-leipzig.de; Esquinazi, P., E-mail: esquin@physik.uni-leipzig.de; Setzer, A.

In this study, the impurity concentration and magnetic response of nine highly oriented pyrolytic graphite (HOPG) samples with different grades and from different providers were determined using ion beam microscopy and SQUID magnetometry. Apart from sideface contaminations in the as-received state, bulk contamination of the samples in most cases consists of disk-shaped micron-sized particles made of Ti and V with an additional Fe contamination around the grain perimeter. The saturation magnetization typically increases with Fe concentration, however, there is no simple correlation between Fe content and magnetic moment. The saturation magnetization of one, respectively six, out of nine samples clearlymore » exceeds the maximum contribution from pure Fe or Fe{sub 3}C. For most samples the temperature dependence of the remanence decreases linearly with T – a dependence found previously for defect-induced magnetism (DIM) in HOPG. We conclude that apart from magnetic impurities, additional contribution to the ferromagnetic magnetization exists in pristine HOPG in agreement with previous studies. A comparative study between the results of ion beam microscopy and the commonly used EDX analysis shows clearly that EDX is not a reliable method for quantitative trace elemental analysis in graphite, clarifying weaknesses and discrepancies in the element concentrations given in the recent literature.« less

Metallurgical and electrochemical characterization of contemporary silver-based soldering alloys.

PubMed

Ntasi, Argyro; Al Jabbari, Youssef; Mueller, Wolf Dieter; Eliades, George; Zinelis, Spiros

2014-05-01

To investigate the microstructure, hardness, and electrochemical behavior of four contemporary Ag-based soldering alloys used for manufacturing orthodontic appliances. The Ag-based alloys tested were Dentaurum Universal Silver Solder (DEN), Orthodontic Solders (LEO), Ortho Dental Universal Solder (NOB), and Silver Solder (ORT). Five disk-shaped specimens were produced for each alloy, and after metallographic preparation their microstructural features, elemental composition, and hardness were determined by scanning electron microscopy with energy-dispersive X-ray (EDX) microanalysis, X-ray diffraction (XRD) analysis, and Vickers hardness testing. The electrochemical properties were evaluated by anodic potentiodynamic scanning in 0.9% NaCl and Ringer's solutions. Hardness, corrosion current (Icorr), and corrosion potential (Ecorr) were statistically analyzed by one-way analysis of variance and Tukey test (α=.05). EDX analysis showed that all materials belong to the Ag-Zn-Cu ternary system. Three different mean atomic contrast phases were identified for LEO and ORT and two for DEN and NOB. According to XRD analysis, all materials consisted of Ag-rich and Cu-rich face-centered cubic phases. Hardness testing classified the materials in descending order as follows: DEN, 155±3; NOB, 149±3; ORT, 141±4; and LEO, 136±8. Significant differences were found for Icorr of NOB in Ringer's solution and Ecorr of DEN in 0.9% NaCl solution. Ag-based soldering alloys demonstrate great diversity in their elemental composition, phase size and distribution, hardness, and electrochemical properties. These differences may anticipate variations in their clinical performance.

Electron microprobe analysis and histochemical examination of the calcium distribution in human bone trabeculae: a methodological study using biopsy specimens from post-traumatic osteopenia

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

Obrant, K.J.; Odselius, R.

1984-01-01

Energy dispersive X-ray microanalysis (EDX) (or electron microprobe analysis) of the relative intensity for calcium in different bone trabeculae from the tibia epiphysis, and in different parts of one and the same trabecula, was performed on 3 patients who had earlier had a fracture of the ipsilateral tibia-diaphysis. The variation in intensity was compared with the histochemical patterns obtained with both the Goldner and the von Kossa staining techniques for detecting calcium in tissues. Previously reported calcium distribution features, found to be typical for posttraumatic osteopenia, such as striated mineralization patterns in individual trabeculae and large differences in mineralization levelmore » between different trabeculae, could be verified both by means of the two histochemical procedures and from the electron microprobe analysis. A pronounced difference was observed, however, between the two histochemical staining techniques as regards their sensitivity to detect calcium. To judge from the values obtained from the EDX measurements, the sensitivity of the Goldner technique should be more than ten times higher than that of von Kossa. The EDX measurements gave more detailed information than either of the two histochemical techniques: great variations in the intensity of the calcium peak were found in trabeculae stained as unmineralized as well as mineralized.« 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 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.

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.

NETL's Energy Data Exchange (EDX) - a coordination, collaboration, and data resource discovery platform for energy science

NASA Astrophysics Data System (ADS)

Rose, K.; Rowan, C.; Rager, D.; Dehlin, M.; Baker, D. V.; McIntyre, D.

2015-12-01

Multi-organizational research teams working jointly on projects often encounter problems with discovery, access to relevant existing resources, and data sharing due to large file sizes, inappropriate file formats, or other inefficient options that make collaboration difficult. The Energy Data eXchange (EDX) from Department of Energy's (DOE) National Energy Technology Laboratory (NETL) is an evolving online research environment designed to overcome these challenges in support of DOE's fossil energy goals while offering improved access to data driven products of fossil energy R&D such as datasets, tools, and web applications. In 2011, development of NETL's Energy Data eXchange (EDX) was initiated and offers i) a means for better preserving of NETL's research and development products for future access and re-use, ii) efficient, discoverable access to authoritative, relevant, external resources, and iii) an improved approach and tools to support secure, private collaboration and coordination between multi-organizational teams to meet DOE mission and goals. EDX presently supports fossil energy and SubTER Crosscut research activities, with an ever-growing user base. EDX is built on a heavily customized instance of the open source platform, Comprehensive Knowledge Archive Network (CKAN). EDX connects users to externally relevant data and tools through connecting to external data repositories built on different platforms and other CKAN platforms (e.g. Data.gov). EDX does not download and repost data or tools that already have an online presence. This leads to redundancy and even error. If a relevant resource already has an online instance, is hosted by another online entity, EDX will point users to that external host either using web services, inventorying URLs and other methods. EDX offers users the ability to leverage private-secure capabilities custom built into the system. The team is presently working on version 3 of EDX which will incorporate big data analytical capabilities amongst other advanced features.

Process-Parameter-Dependent Optical and Structural Properties of ZrO2MgO Mixed-Composite Films Evaporated from the solid Solution

NASA Technical Reports Server (NTRS)

Sahoo, N. K.; Shapiro, A. P.

1998-01-01

The process-parameter-dependent optical and structural properties of ZrO2MgO mixed-composite material have been investigated. Optical properties were derived from spectrophotometric measurements. By use of atomic force microscopy, x-ray diffraction analysis, and energy-dispersive x-ray (EDX) analysis, the surface morphology, grain size distributions, crystallographic phases, and process-dependent material composition of films have been investigated. EDX analysis made evident the correlation between the oxygen enrichment in the films prepared at a high level of oxygen pressure and the very low refractive index. Since oxygen pressure can be dynamically varied during a deposition process, coatings constructed of suitable mixed-composite thin films can benefit from continuous modulation of the index of refraction. A step modulation approach is used to develop various multilayer-equivalent thin-film devices.

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.

Calcium to phosphate ratio measurements in calcium phosphates using LIBS

NASA Astrophysics Data System (ADS)

Tariq, U.; Haider, Z.; Chaudhary, K.; Hussain, R.; Ali, J.

2018-05-01

In this study, we report the measurement of Ca/P ratio of hydroxyapatite using LIBS. Hydroxyapatite was prepared by wet chemical precipitation method with different stoichiometric ratios of Ca and P (1.5, 1.6, 1.67, 1.70, 1.80). Samples were then pelletized using KBr as a binder under a hydraulic press. Samples were irradiated with a laser beam and corresponding spectra were recorded. Spectra were further analyzed to calculate the Ca/P ratio which was then compared with the EDX for validation. LIBS results showed promise with a deviation of < 5% with the Stoichiometric ratios and EDX results.

Distal Predominance of Electrodiagnostic Abnormalities in Early Stage Amyotrophic Lateral Sclerosis.

PubMed

Shayya, Luay; Babu, Suma; Pioro, Erik P; Li, Jianbo; Li, Yuebing

2018-05-09

We compare the electrodiagnostic (EDX) yield of limb muscles in revealing lower motor neuron (LMN) dysfunction by electromyography (EMG) in early stage amyotrophic lateral sclerosis (ALS). Single-site retrospective review Results: This study includes 122 consecutive patients with possible ALS as defined by revised El Escorial Criteria. Distal limb muscles show more frequent EMG abnormalities than proximal muscles. EDX yield is higher in the limb where weakness begins and when clinical signs of LMN dysfunction are evident. Adoption of Awaji criteria increases the yield of EMG positive segments significantly in the cervical (p<0.0005) and lumbosacral regions (P<0.0001), and upgrades 19 patients into probable and 1 patient into definite categories. Electromyographic abnormalities are distal limb-predominant in early stage ALS. A redefinition of an EDX-positive cervical or lumbosacral segment, with an emphasis on distal limb muscles, may result in an earlier ALS diagnosis. This article is protected by copyright. All rights reserved. © 2018 Wiley Periodicals, Inc.

Investigation of radiation-induced free radicals and luminescence properties in fresh pomegranate fruits.

PubMed

Shahbaz, Hafiz M; Akram, Kashif; Ahn, Jae-Jun; Kwon, Joong-Ho

2013-05-01

Radiation-induced free radicals and luminescence properties were investigated in γ-irradiated (0-3 kGy) pomegranate ( Punica granatum L.) fruits. Photostimulated luminescence (PSL) analysis showed limited applicability, and only 3 kGy-irradiated pomegranates showed positive PSL values (>5000 PCs). Thermoluminescence (TL) glow curve features, such as intensity and the presence of maximum glow peak in radiation-specific temperature range (150-250 °C), provided definite proof of irradiation, and the TL ratios (TL1/TL2) also confirmed the reliability of TL results. Scanning electron microscopy energy dispersive X-ray (SEM-EDX) analysis of the separated minerals showed that feldspar and quartz minerals were responsible for the luminescence properties. Radiation-induced cellulose radicals were detected in the seeds and rinds by ESR analysis. The ESR results were better in freeze-dried samples than in alcohol-extracted ones. A positive correlation was found between the ESR and TL signal intensities and irradiation doses; however, the most promising detection of the irradiation status was possible through TL analysis.

Type 1 diabetes mellitus effects on dental enamel formation revealed by microscopy and microanalysis.

PubMed

Silva, Bruna Larissa Lago; Medeiros, Danila Lima; Soares, Ana Prates; Line, Sérgio Roberto Peres; Pinto, Maria das Graças Farias; Soares, Telma de Jesus; do Espírito Santo, Alexandre Ribeiro

2018-03-01

Type 1 diabetes mellitus (T1DM) largely affects children, occurring therefore at the same period of deciduous and permanent teeth development. The aim of this work was to investigate birefringence and morphology of the secretory stage enamel organic extracellular matrix (EOECM), and structural and mechanical features of mature enamel from T1DM rats. Adult Wistar rats were maintained alive for a period of 56 days after the induction of experimental T1DM with a single dose of streptozotocin (60 mg/kg). After proper euthanasia of the animals, fixed upper incisors were accurately processed, and secretory stage EOECM and mature enamel were analyzed by transmitted polarizing and bright field light microscopies (TPLM and BFLM), energy-dispersive x-ray (EDX) analysis, scanning electron microscopy (SEM), and microhardness testing. Bright field light microscopies and transmitted polarizing light microscopies showed slight morphological changes in the secretory stage EOECM from diabetic rats, which also did not exhibit statistically significant alterations in birefringence brightness when compared to control animals (P > .05). EDX analysis showed that T1DM induced statistically significant little increases in the amount of calcium and phosphorus in outer mature enamel (P < .01) with preservation of calcium/phosphorus ratio in that structure (P > .05). T1DM also caused important ultrastructural alterations in mature enamel as revealed by SEM and induced a statistically significant reduction of about 13.67% in its microhardness at 80 μm from dentin-enamel junction (P < .01). This study shows that T1DM may disturb enamel development, leading to alterations in mature enamel ultrastructure and in its mechanical features. © 2017 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

Study on the Synergetic Fire-Retardant Effect of Nano-Sb₂O₃ in PBT Matrix.

PubMed

Niu, Lei; Xu, Jianlin; Yang, Wenlong; Ma, Jiqiang; Zhao, Jinqiang; Kang, Chenghu; Su, Jiaqiang

2018-06-22

Nano-Sb₂O₃ has excellent synergistic flame-retardant effects. It can effectively improve the comprehensive physical and mechanical properties of composites, reduce the use of flame retardants, save resources, and protect the environment. In this work, nanocomposites specimens were prepared by the melt-blending method. The thermal stability, mechanical properties, and flame retardancy of a nano-Sb₂O₃⁻brominated epoxy resin (BEO)⁻poly(butylene terephthalate) (PBT) composite were analyzed, using TGA and differential scanning calorimetry (DSC), coupled with EDX analysis, tensile testing, cone calorimeter tests, as well as scanning electron microscopy (SEM) and flammability tests (limiting oxygen index (LOI), UL94). SEM observations showed that the nano-Sb₂O₃ particles were homogeneously distributed within the PBT matrix, and the thermal stability of PBT was improved. Moreover, the degree of crystallinity and the tensile strength were improved, as a result of the superior dispersion and interfacial interactions between nano-Sb₂O₃ and PBT. At the same time, the limiting oxygen index and flame-retardant grade were increased as the nano-Sb₂O₃ content increased. The results from the cone calorimeter test showed that the peak heat release rate (PHRR), total heat release rate (THR), peak carbon dioxide production (PCO₂P), and peak carbon monoxide production (PCOP) of the nanocomposites were obviously reduced, compared to those of the neat PBT matrix. Meanwhile, the SEM⁻energy dispersive spectrometry (EDX) analysis of the residues indicated that a higher amount of C element was left, thus the charring layer of the nanocomposites was compact. This showed that nano-Sb₂O₃ could promote the degradation and charring of the PBT matrix, improving thermal stability and flame retardation.

Application of STEM characterization for investigating radiation effects in BCC Fe-based alloys

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

Parish, Chad M.; Field, Kevin G.; Certain, Alicia G.

2015-04-20

This paper provides a general overview of advanced scanning transmission electron microscopy (STEM) techniques used for characterization of irradiated BCC Fe-based alloys. Advanced STEM methods provide the high-resolution imaging and chemical analysis necessary to understand the irradiation response of BCC Fe-based alloys. The use of STEM with energy dispersive x-ray spectroscopy (EDX) for measurement of radiation-induced segregation (RIS) is described, with an illustrated example of RIS in proton- and self-ion irradiated T91. Aberration-corrected STEM-EDX for nanocluster/nanoparticle imaging and chemical analysis is also discussed, and examples are provided from ion-irradiated oxide dispersion strengthened (ODS) alloys. In conclusion, STEM techniques for void,more » cavity, and dislocation loop imaging are described, with examples from various BCC Fe-based alloys.« less

Carbon protrusions on PTFE surface prepared by ion irradiation and chemical defluorination

NASA Astrophysics Data System (ADS)

Kobayashi, T.; Iwaki, M.

2006-01-01

A surface of PTFE was covered with small protrusions by ion-beam irradiation. In this study, we converted PTFE protrusions into carbon protrusions by a defluorination (carbonization) process using sodium vapor. The morphology, composition and structure were analyzed by SEM-EDX, Raman spectroscopy and TEM. The irradiated PTFE sheets were packed in evacuated glass tubes with a sodium block and kept at 473 K for 2-48 h. The samples were then rinsed in HCl and distilled water to remove NaF precipitates. The EDX measurement showed that the NaF precipitates were completely removed by washing, and the percentage of carbon atoms was controlled from 60% to 99% by the treatment. Raman spectra showed that graphite structures grow during the defluorination process. TEM micrographs showed that the protrusions have a bubble structure and are covered with a thin wall. The carbonized protrusions were conductive and grew perpendicular to the substrate.

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).

Scanning Electron Microscopy Investigation of a Sample Depth Profile Through the Martian Meteorite Nakhla

NASA Technical Reports Server (NTRS)

Toporski, Jan; Steele, Andrew; Westall, Frances; McKay, David S.

2000-01-01

The ongoing scientific debate as to whether or not the Martian meteorite ALH84001 contained evidence of possible biogenic activities showed the need to establish consistent methods to ascertain the origin of such evidence. To distinguish between terrestrial organic material/microbial contaminants and possible indigenous microbiota within meteorites is therefore crucial. With this in mind a depth profile consisting of four samples from a new sample allocation of Martian meteorite Nakhla was investigated using scanning electron microscopy (SEM) and energy dispersive X-ray analysis. SEM imaging of freshly broken fractured chips revealed structures strongly recent terrestrial microorganisms, in some cases showing evidence of active growth. This conclusion was supported by EDX analysis, which showed the presence of carbon associated with these structures, we concluded that these structures represent recent terrestrial contaminants rather than structures indigenous to the meteorite. Page

International Conference of Defects in Semiconductors (19th), ICDS, Held in Aveiro, Portugal on July 21-25, 1997, Pt. 3

DTIC Science & Technology

1998-01-23

2 1 ■1 WWW .; 0 100 200 300 400 0 100 200 300 400 0 100 200 300 400 co (Mrad/s) Fig. 1 Characteristic EFG corresponding to type II...results for 1/T -» 0. Materials Science Forum Vols. 258-263 1355 ent, and the quasi-Fermi level, eF, is pinned to the DX level position, eDX . eB...denoted by E plus index. For single electron processes, s = E). The pressure dependence of eDX is shown by squares in Fig. 4. The dashed line shows the

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.

Microbial synthesis of Flower-shaped gold nanoparticles.

PubMed

Singh, Priyanka; Kim, Yeon Ju; Wang, Chao; Mathiyalagan, Ramya; Yang, Deok Chun

2016-09-01

The shape of nanoparticles has been recognized as an important attribute that determines their applicability in various fields. The flower shape (F-shape) has been considered and is being focused on, because of its enhanced properties when compared to the properties of the spherical shape. The present study proposed the microbial synthesis of F-shaped gold nanoparticles within 48 h using the Bhargavaea indica DC1 strain. The F-shaped gold nanoparticles were synthesized extracellularly by the reduction of auric acid in the culture supernatant of B. indica DC1. The shape, size, purity, and crystalline nature of F-shaped gold nanoparticles were revealed by various instrumental techniques including UV-Vis, FE-TEM, EDX, elemental mapping, XRD, and DLS. The UV-Vis absorbance showed a maximum peak at 536 nm. FE-TEM revealed the F-shaped structure of nanoparticles. The EDX peak obtained at 2.3 keV indicated the purity. The peaks obtained on XRD analysis corresponded to the crystalline nature of the gold nanoparticles. In addition, the results of elemental mapping indicated the maximum distribution of gold elements in the nanoproduct obtained. Particle size analysis revealed that the average diameter of the F-shaped gold nanoparticles was 106 nm, with a polydispersity index (PDI) of 0.178. Thus, the methodology developed for the synthesis of F-shaped gold nanoparticles is completely green and economical.

Comparative analysis of textile metal threads from liturgical vestments and folk costumes in Croatia

NASA Astrophysics Data System (ADS)

Šimić, Kristina; Zamboni, Ivana; Fazinić, Stjepko; Mudronja, Domagoj; Sović, Lea; Gouasmia, Sabrina; Soljačić, Ivo

2018-02-01

Textile is essential for everyday life in all societies. It is used in clothes for protection and warmth but also to indicate class and position, show wealth and social status. Threads from precious metals have also been used in combination with fibres for decoration in order to create luxury fabrics for secular and religious elites. We performed elemental analysis of 17th to 20th century metal threads from various textile articles of liturgical vestments and festive folk costumes collected in the museums of northern, southern and central Croatian regions. In order to determine elemental concentrations in threads we performed comparative X-ray Spectroscopy measurements using: (i) Scanning Electron Microscopy with Energy Dispersive X-ray Spectroscopy (SEM-EDX) at the Faculty of Textile Technology, (ii) X-ray Fluorescence Spectroscopy (XRF) at the Croatian Conservation Institute and (iii) Particle Induced X-ray Spectroscopy (PIXE) at the Ruđer Bošković Institute Tandem Accelerator Facility using ion micro beam. Rutherford Backscattering Spectroscopy (RBS) was performed as well on selected samples. SEM-EDX investigations of cross-sections along with the surfaces were also performed. In this work we report and discuss the results obtained by the three X-ray methods and RBS for major (gold, silver, copper) and minor elements on different threads like stripes, wires and "srma" (metal thread wrapped around textile yarn).

Ozone Gas Effect on Mineral Content of Dentin exposed to Streptococcus mutans Biofilm: An Energy-dispersive X-ray Evaluation.

PubMed

Chaves, Rafaella M; Estrela, Carlos; Cardoso, Paula C; de Je Barata, Terezinha; de Souza, João B; de Torres, Érica M; Estrela, Cyntia Ra; Magalhães, Ana Pr; Lopes, Lawrence G

2017-04-01

This study aims to assess the effect of ozone gas on dentin exposed to Streptococcus mutans biofilm by evaluation of mineral content [log calcium-to-phosphorus (Ca/P)] using energy-dispersive X-ray (EDX) spectroscopy. Five human third molars were sectioned into four slices of dentin and distributed in four groups: I - control (no treatment); II - ozone therapy; III - biofilm development; IV - ozone therapy followed by biofilm development. Mineral content (log Ca/P) was evaluated by EDX. Data were analyzed by analysis of variance and Tukey's test (p < 0.05). Results showed that the mineral content of control group (I) was similar to ozone group (II), and was statistically higher than biofilm (III) and ozone + biofilm (IV). The lowest log Ca/P was determined in biofilm group (III). It can be concluded that ozone gas did not grant preventive effects of demineralization by S. mutans biofilm on dentin surface. Ozone gas therapy may be an alternative noninvasive treatment aiming to reduce the levels of caries-associated microorganisms. This therapy may, thereby, be an alternative and/or complementary treatment strategy in preventive dentistry.

Palladium nanoparticle deposition via precipitation: a new method to functionalize macroporous silicon

PubMed Central

Scheen, Gilles; Bassu, Margherita; Douchamps, Antoine; Zhang, Chao; Debliquy, Marc; Francis, Laurent A

2014-01-01

We present an original two-step method for the deposition via precipitation of Pd nanoparticles into macroporous silicon. The method consists in immersing a macroporous silicon sample in a PdCl2/DMSO solution and then in annealing the sample at a high temperature. The impact of composition and concentration of the solution and annealing time on the nanoparticle characteristics is investigated. This method is compared to electroless plating, which is a standard method for the deposition of Pd nanoparticles. Scanning electron microscopy and computerized image processing are used to evaluate size, shape, surface density and deposition homogeneity of the Pd nanoparticles on the pore walls. Energy-dispersive x-ray spectroscopy (EDX) and x-ray photoelectron spectroscopy (XPS) analyses are used to evaluate the composition of the deposited nanoparticles. In contrast to electroless plating, the proposed method leads to homogeneously distributed Pd nanoparticles along the macropores depth with a surface density that increases proportionally with the PdCl2 concentration. Moreover EDX and XPS analysis showed that the nanoparticles are composed of Pd in its metallic state, while nanoparticles deposited by electroless plating are composed of both metallic Pd and PdOx. PMID:27877732

Thermal behaviour of chrome shavings and of sludges recovered after digestion of tanned solid wastes with calcium hydroxide

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

Tahiri, S.; Albizane, A.; Messaoudi, A.

2007-07-01

The thermal behaviour of chrome shavings and of sludges recovered after digestion of tanned wastes with Ca(OH){sub 2} was studied. Ashes obtained after incineration of wastes at various temperatures were analysed by X-ray diffraction and EDX method. The main crystallized phases present in the ash obtained at 600 deg. C are Cr{sub 2}O{sub 3} and NaCl. The diffractograms revealed an increase in the intensities of the chromium oxide peaks and a very notable decrease of the amount of sodium chloride at 1100 deg. C. EDX analysis revealed a total disappearance of the chlorine peak at this temperature. Scanning electron micrographsmore » show that the waste lost its fibrous aspect when the temperature increases. Formation of aggregates was noted after 550 deg. C. Combustion of organic matters and decarbonation phenomenon are the main stages observed on GTA and DTA curves of sludges. These phenomena are, respectively, exothermic and endothermic. The diffractogram of sludges recorded at 550 deg. C, in the presence of a constant oxygen surplus, revealed the presence of CaCrO{sub 4} and CaCO{sub 3}.« less

Synthesis and characterization of magnesium aluminate (MgAl2O4) spinel (MAS) thin films

NASA Astrophysics Data System (ADS)

Ahmad, Syed Muhammad; Hussain, Tousif; Ahmad, Riaz; Siddiqui, Jamil; Ali, Dilawar

2018-01-01

In a quest to identify more economic routes for synthesis of magnesium aluminate (MgAl2O4) spinel (MAS) thin films, dense plasma focus device was used with multiple plasma focus shots. Structural, bonding between composite films, surface morphological, compositional and hardness properties of MAS thin films were investigated by using x-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive x-rays (EDX) analysis and Vickers micro hardness test respectively. In XRD graph, the presence of MgAl2O4 diffraction peaks in crystallographic orientations (222), (400) and (622) pointed out the successful formation of polycrystalline thin films of MgAl2O4 with face centered cubic structure. The FTIR spectrums showed a major common transmittance band at 697.95 cm-1 which belongs to MgAl2O4. SEM micrographs illustrated a mesh type, granular and multi layers microstructures with significant melting effects. EDX spectrum confirmed the existence of magnesium, oxygen and aluminum in MAS films. A common increasing behavior in micro-hardness of composite MgAl2O4 films by increasing number of plasma focus shots was found.

Synthesis, characterization and antimicrobial activity of dextran sulphate stabilized silver nanoparticles

NASA Astrophysics Data System (ADS)

Cakić, Milorad; Glišić, Slobodan; Nikolić, Goran; Nikolić, Goran M.; Cakić, Katarina; Cvetinov, Miroslav

2016-04-01

Dextran sulphate stabilized silver nanoparticles (AgNPs - DS) were synthesized from aqueous solution of silver nitrate (AgNO3) and dextran sulphate sodium salt (DS). The characterization of AgNPs - DS was performed by ultraviolet-visible spectroscopy (UV-VIS), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and antimicrobial activity. The formation of AgNPs - DS was monitored by colour changes of the reaction mixture from yellowish to brown and by measuring the surface plasmon resonance absorption peak in UV-VIS spectra at 420 nm. The SEM analysis was used for size and shape determination of AgNPs - DS. The presence of elemental silver and its crystalline structure in AgNPs - DS were confirmed by EDX and XRD analyses. The possible functional groups of DS responsible for the reduction and stabilization of AgNPs were determinated by FTIR spectroscopy. The AgNPs - DS showed strong antibacterial activity against Staphylococcus aureus ATCC 25923, Bacillus cereus ATCC 11778, Bacillus luteus in haus strain, Bacillus subtilis ATTC 6633, Listeria monocytogenes ATCC 15313, Escherichia coli ATTC 25922, Pseudomonas aeruginosa ATTC 27853, Klebsiella pneumoniae ATTC 700603, Proteus vulgaris ATTC 8427, and antifungal activity against Candida albicans ATTC 2091.

Data Fitting to Study Ablated Hard Dental Tissues by Nanosecond Laser Irradiation.

PubMed

Al-Hadeethi, Y; Al-Jedani, S; Razvi, M A N; Saeed, A; Abdel-Daiem, A M; Ansari, M Shahnawaze; Babkair, Saeed S; Salah, Numan A; Al-Mujtaba, A

2016-01-01

Laser ablation of dental hard tissues is one of the most important laser applications in dentistry. Many works have reported the interaction of laser radiations with tooth material to optimize laser parameters such as wavelength, energy density, etc. This work has focused on determining the relationship between energy density and ablation thresholds using pulsed, 5 nanosecond, neodymium-doped yttrium aluminum garnet; Nd:Y3Al5O12 (Nd:YAG) laser at 1064 nanometer. For enamel and dentin tissues, the ablations have been performed using laser-induced breakdown spectroscopy (LIBS) technique. The ablation thresholds and relationship between energy densities and peak areas of calcium lines, which appeared in LIBS, were determined using data fitting. Furthermore, the morphological changes were studied using Scanning Electron Microscope (SEM). Moreover, the chemical stability of the tooth material after ablation has been studied using Energy-Dispersive X-Ray Spectroscopy (EDX). The differences between carbon atomic % of non-irradiated and irradiated samples were tested using statistical t-test. Results revealed that the best fitting between energy densities and peak areas of calcium lines were exponential and linear for enamel and dentin, respectively. In addition, the ablation threshold of Nd:YAG lasers in enamel was higher than that of dentin. The morphology of the surrounded ablated region of enamel showed thermal damages. For enamel, the EDX quantitative analysis showed that the atomic % of carbon increased significantly when laser energy density increased.

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.

Seasonal variability of aerosols and their characteristics in urban and rural locations of Delhi-NCR

NASA Astrophysics Data System (ADS)

Bhardwaj, Purnima; Pandey, Alok Kumar; Kumar, Krishan; Jain, V. K.

2017-10-01

Present study shows the seasonal variation of the Aerosol Optical Depth (AOD) and aerosols characteristics in an urban and rural environment over Delhi-NCR. Aerosol sampling was carried out using a Mini-Volume sampler at an urban and rural location in Delhi-NCR. A relatively higher PM2.5 (particulate matter of size < 2.5 μm) concentrations were observed at the urban sampling site than the rural one in the summer as well as winter season. PM2.5 samples were further analyzed by Scanning Electron Microscopy (SEM) and Energy Dispersive X-Ray Spectroscopy (EDX) in order to understand the morphology and elemental composition of the PM2.5 aerosols. Summer SEM results showed the dominance of fluffy agglomerate (soot) in urban area whereas the rural area was relatively clean. The winter season SEM results showed the presence of aggregates of smaller particles at urban site whereas flaky, round and irregular shaped particles were observed at the rural site. EDX analysis showed the presence of elements such as C, Cu, Zn, Ga and Fe (representative elements) in varying concentrations at both the urban and rural sampling locations. NASA's Aqua satellite MODIS sensor AOD data for summer and winter seasons have been used to study the spatial distributions of aerosols over the study region. AOD was found to be relatively higher in urban area as compared to the rural area in both the summer and winter seasons indicating the contribution of high amount of anthropogenic aerosols in the urban atmosphere.

A novel bifunctional endo-/exo-type cellulase from an anaerobic ruminal bacterium.

PubMed

Ko, Kyong-Cheol; Han, Yunjon; Choi, Jong Hyun; Kim, Geun-Joong; Lee, Seung-Goo; Song, Jae Jun

2011-03-01

An anaerobic microorganism termed AN-C16-KBRB was isolated from the bovine rumen and demonstrated cellulolytic activity on a NB agar plate containing azo-carboxymethyl cellulose. The 16S rRNA gene of the strain was 98% similar to that of Clostridiaceae bacterium SK082 (AB298754) as the highest homology. A novel celEdx16 gene encoding a bifunctional endo-/exocellulase (CelEdx16) was cloned by the shotgun method from AN-C16-KBRB, and the enzyme was characterized. The celEdx16 gene had an open reading frame of 1,104-base pairs, which encoded 367 amino acids to yield a protein of molecular mass 40.4 kDa. The amino acid sequence was 53% identical to that of an endoglucanase from Clostridium thermocellum. CelEdx16 was overexpressed in Escherichia coli and purified using Ni-NTA affinity chromatography. The specific endocellulase and exocellulase activities of CelEdx16 were 15.9 and 3.6 x 10⁻² U mg⁻¹, respectively. The Michaelis-Menten constant (K (m) values) and the maximal reaction velocities (V(max) values) of CelEdx16 were 47.1 μM and 9.6 x 10⁻³ μmole min⁻¹ when endocellulase activity was measured and 106.3 μM and 2.1 x 10⁻⁵ μmol min⁻¹ when exocellulase activity was assessed. CelEdx16 was optimally active at pH 5.0 and 40 °C.

Investigation on a Roman copper alloy artefact from Pompeii (Italy).

PubMed

Baraldi, Pietro; Baraldi, Cecilia; Ferrari, Giorgia; Foca, Giorgia; Marchetti, Andrea; Tassi, Lorenzo

2006-01-01

A selection of samples, obtained from a particular copper-alloy domestic artefact of Roman style from Pompeii, has been analysed by using different techniques (IR, Raman, SEM-EDX, FAAS), in order to investigate the chemical nature and composition of the metals utilised for such manufacturing pieces. The surface analysis of the bright red metallic microfragments conducted by different analytical techniques, emphasises the presence of pure unalloyed copper and confirms the absence of other metallic species on the upper layers. On the contrary, the mapping analysis of the section of the laminar metal of the investigated sample shows a consistent enrichment in tin content. Finally, destructive analysis by FAAS confirms that the artefact looks like a bronze metal alloy, with a medium Sn content of about 6.5%.

A smarter way to search, share and utilize open-spatial online data for energy R&D - Custom machine learning and GIS tools in U.S. DOE's virtual data library & laboratory, EDX

NASA Astrophysics Data System (ADS)

Rose, K.; Bauer, J.; Baker, D.; Barkhurst, A.; Bean, A.; DiGiulio, J.; Jones, K.; Jones, T.; Justman, D.; Miller, R., III; Romeo, L.; Sabbatino, M.; Tong, A.

2017-12-01

As spatial datasets are increasingly accessible through open, online systems, the opportunity to use these resources to address a range of Earth system questions grows. Simultaneously, there is a need for better infrastructure and tools to find and utilize these resources. We will present examples of advanced online computing capabilities, hosted in the U.S. DOE's Energy Data eXchange (EDX), that address these needs for earth-energy research and development. In one study the computing team developed a custom, machine learning, big data computing tool designed to parse the web and return priority datasets to appropriate servers to develop an open-source global oil and gas infrastructure database. The results of this spatial smart search approach were validated against expert-driven, manual search results which required a team of seven spatial scientists three months to produce. The custom machine learning tool parsed online, open systems, including zip files, ftp sites and other web-hosted resources, in a matter of days. The resulting resources were integrated into a geodatabase now hosted for open access via EDX. Beyond identifying and accessing authoritative, open spatial data resources, there is also a need for more efficient tools to ingest, perform, and visualize multi-variate, spatial data analyses. Within the EDX framework, there is a growing suite of processing, analytical and visualization capabilities that allow multi-user teams to work more efficiently in private, virtual workspaces. An example of these capabilities are a set of 5 custom spatio-temporal models and data tools that form NETL's Offshore Risk Modeling suite that can be used to quantify oil spill risks and impacts. Coupling the data and advanced functions from EDX with these advanced spatio-temporal models has culminated with an integrated web-based decision-support tool. This platform has capabilities to identify and combine data across scales and disciplines, evaluate potential environmental, social, and economic impacts, highlight knowledge or technology gaps, and reduce uncertainty for a range of `what if' scenarios relevant to oil spill prevention efforts. These examples illustrate EDX's growing capabilities for advanced spatial data search and analysis to support geo-data science needs.

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.

Instrumentation and Metrology for Nanotechnology

DTIC Science & Technology

2004-01-29

dimension measurements of 3D structures, overlay, defect detection, and analysis . Critical dimension ( CD ) measurement must account for sidewall shape and...critical dimension measurements of 3D structures, overlay, defect detection, and analysis . CD measurement must account for sidewall shape and line...energy dispersive X-ray (EDX) analysis on films containing as-prepared FePt nanoparticles revealed a distribution of particle compositions. Although

Formulation of microemulsion propolis fluoride (PF) as varnish topical agent to stop activity of teeth caries

NASA Astrophysics Data System (ADS)

Sahlan, Muhamad; Prakoso, Chandra Dwi; Darwita, Risqa Rina; Hermansyah, Heri

2017-02-01

Topical fluoride is proven to have higher efficacy in preventing dental caries with low production cost and easy to apply. The objective of this research is to formulate alternative agent topical fluoride NH4F 5% mixed with extract ethanol propolis (EEP) in the micro-emulsion system that has high stability, antimicrobial activity, and remineralization capability to arrest teeth caries activity. By using total plate count (TPC) analysis, formulation 2.7% EEP; 6,3% surfactant; and 90,9% NH4F shows good perform to inhibit cariogenic bacteria development around 78-80%. Scanning Electron Microscopy (SEM) and Energy Dispersive X-Ray (EDX) result also showed that sample successfully remineralized enamel surface. In addition, sample showed good pH, flavonoid, and polyphenol stability for 40 days.

Sustainable conversion of agro-wastes into useful adsorbents

NASA Astrophysics Data System (ADS)

Bello, Olugbenga Solomon; Owojuyigbe, Emmanuel Seun; Babatunde, Monsurat Abiodun; Folaranmi, Folasayo Eunice

2017-11-01

Preparation and characterization of raw and activated carbon derived from three different selected agricultural wastes: kola nut pod raw and activated (KNPR and KNPA), bean husk raw and activated (BHR and BHA) and coconut husk raw and activated (CHR and CHA) were investigated, respectively. Influences of carbonization and acid activation on the activated carbon were investigated using SEM, FTIR, EDX, pHpzc and Boehm titration techniques, respectively. Carbonization was done at 350 °C for 2 h followed by activation with 0.3 M H3PO4 (ortho-phosphoric acid). Results obtained from SEM, FTIR, and EDX revealed that, carbonization followed by acid activation had a significant influence on morphology and elemental composition of the samples. SEM showed well-developed pores on the surface of the precursors after acid treatment, FTIR spectra revealed reduction, broadening, disappearance or appearance of new peaks after acid activation. EDX results showed highest percentage of carbon by atom respectively in the order BHA > KNPA > CHA respectively. The pHpzc was found to be 5.32, 4.57 and 3.69 for KNPA, BHA and CHA, respectively. Boehm titration result compliments that of pHpzc, indicating that the surfaces of the prepared adsorbents are predominantly acidic. This study promotes a sustainable innovative use of agro-wastes in the production of cheap and readily available activated carbons, thereby ensuring more affordable water and effluent treatment adsorbents.

Use of calcium-containing endodontic sealers as apical barrier in fluid-contaminated wide-open apices.

PubMed

Prati, Carlo; Siboni, Francesco; Polimeni, Antonella; Bossu, Maurizio; Gandolfi, Maria Giovanna

2014-12-30

The sealing of wide-open apex roots is still a challenge and requires the use of apical barrier techniques. The aim was to evaluate ex vivo the sealing and the apical morphology of 3 commercial calcium oxide (CaO)-containing sealers - namely, 2 zinc oxide-based (CRCS and Sealapex) and a calcium silicate MTA-based (TechBiosealer Endo) - placed in wet root canals with artificial wide-open apices.
 Thirty human single-rooted teeth were shaped with Protaper and an artificial open apex (diameter size 110) was created. Each root was inserted in a custom-designed support containing simulated body fluid (Hank's balanced salt solution, HBSS) at the bottom simulating the presence of periapical fluid in the canal. Each sealer (TechBiosealer Endo, CRCS, Sealapex) was compacted to the apical 5 mm and the filled roots stored in HBSS at 37°C. The sealing was evaluated as microinfiltrated fluid since 24 hours up to 6 months using a high-precision digital fluid flow meter. The sealers were also studied for setting time in HBSS, calcium releasing (statistical analysis by 2-way ANOVA followed by Student-Newman-Keuls test, P<0.05) and surface morpho-chemistry by ESEM-EDX and OM analysis.
 All sealers showed a stable seal. TechBiosealer Endo maintained a better seal than the other materials (P<0.05) and ESEM-EDX and OM analyses showed the presence of apatite deposits.
 The clinical use of hydraulic hydrophilic MTA-based sealers can be recommended to stop/reduce the fluid flow rate through the apex. The artificial apical barrier in wet wide apices is a suitable technique able to seal wet root canals.

Superconductivity in Bi/Ni bilayer system: Clear role of superconducting phases found at Bi/Ni interface

NASA Astrophysics Data System (ADS)

Liu, L. Y.; Xing, Y. T.; Merino, I. L. C.; Micklitz, H.; Franceschini, D. F.; Baggio-Saitovitch, E.; Bell, D. C.; Solórzano, I. G.

2018-01-01

Bi/Ni bilayers with varying Bi and Ni layer thicknesses have been prepared by (a) pulsed-laser deposition (PLD) at 300 K and (b) thermal evaporation at 4.2 K. A two-step superconducting transition appears on the electrical transport measurements in the samples prepared by PLD. High-resolution transmission and scanning transmission electron microscopy, supported by energy-dispersive x-ray spectroscopy (EDXS) analysis, reveal that two superconducting intermetallic alloys, namely NiBi and NiBi3, are formed by interdiffusion, if the bilayers are prepared at 300 K. The Tc of the two phases behaves very differently in an external magnetic field and the upper critical magnetic fields at zero temperature [Bc 2(0 ) ] were estimated as 1.1 and 7.4 T, respectively. The lower value corresponds to the Bc 2(0) of NiBi3 phase and the higher one is supposed to be of NiBi. These alloys are responsible for the superconductivity and the two-step transition appearing in the Bi/Ni bilayer system. Surprisingly, the Bi-rich phase (NiBi3) is formed near the Ni layer, while the Ni-rich phase (NiBi) is formed far from the Ni layer. The EDXS analysis at nanometer scale clearly shows an unusual increase of Ni concentration near the interface of Bi/substrate. The limited thickness of Bi layer in the interdiffusion process results in an unexpected distribution of Ni concentration. Samples prepared at 4.2 K after annealing at 300 K do not show any superconductivity, which indicates that a nonepitaxial Bi/Ni interface does not induce superconductivity in the case interdiffusion does not occur. These results offer a deeper understanding of the superconductivity in the Bi/Ni bilayer system.

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.

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.

Investigation on the structural characterization of pulsed p-type porous silicon

NASA Astrophysics Data System (ADS)

Wahab, N. H. Abd; Rahim, A. F. Abd; Mahmood, A.; Yusof, Y.

2017-08-01

P-type Porous silicon (PS) was sucessfully formed by using an electrochemical pulse etching (PC) and conventional direct current (DC) etching techniques. The PS was etched in the Hydrofluoric (HF) based solution at a current density of J = 10 mA/cm2 for 30 minutes from a crystalline silicon wafer with (100) orientation. For the PC process, the current was supplied through a pulse generator with 14 ms cycle time (T) with 10 ms on time (Ton) and pause time (Toff) of 4 ms respectively. FESEM, EDX, AFM, and XRD have been used to characterize the morphological properties of the PS. FESEM images showed that pulse PS (PPC) sample produces more uniform circular structures with estimated average pore sizes of 42.14 nm compared to DC porous (PDC) sample with estimated average size of 16.37nm respectively. The EDX spectrum for both samples showed higher Si content with minimal presence of oxide.

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.

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

Modification of PdO/CeZrO2 doped with transition metals (Y and Fe) for reducibility properties

NASA Astrophysics Data System (ADS)

Shah, M. Nazri Abu; Jai, Junaidah; Faeqah, Nor; Ismail, Kamariah Noor; Hadi, Abdul

2017-12-01

This paper describes the synthesis of modified nanocatalysts of PdO/CeZrYO2(PdO/CZY), PdO/CeZrFeO2(PdO/CZF) and PdO/CeZrO2(PdO/CZ) via microemulsion followed by deposition - precipitation method. The structural, textural and redox properties of the synthesized nanocatalysts were investigated. The diffractogram of XRD showed that all the synthesized nanocatalysts indicate a symmetrical pattern of cubic phase crystallinity. The amount of PdO was detected using EDX analysis and PdO/CZF portrayed the highest Pd contents of about 4.63 %. Therefore it shows a good potential to have reducibility properties and can be manifested active at low temperature reduction.

Chemical Imaging of Ambient Aerosol Particles: Observational Constraints on Mixing State Parameterization

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

O'Brien, Rachel; Wang, Bingbing; Laskin, Alexander

2015-09-28

A new parameterization for quantifying the mixing state of aerosol populations has been applied for the first time to samples of ambient particles analyzed using spectro-microscopy techniques. Scanning transmission x-ray microscopy/near edge x-ray absorption fine structure (STXM/NEXAFS) and computer controlled scanning electron microscopy/energy dispersive x-ray spectroscopy (CCSEM/EDX) were used to probe the composition of the organic and inorganic fraction of individual particles collected on June 27th and 28th during the 2010 Carbonaceous Aerosols and Radiative Effects (CARES) study in the Central Valley, California. The first field site, T0, was located in downtown Sacramento, while T1 was located near the Sierramore » Nevada Mountains. Mass estimates of the aerosol particle components were used to calculate mixing state metrics, such as the particle-specific diversity, bulk population diversity, and mixing state index, for each sample. Both microscopy imaging techniques showed more changes over these two days in the mixing state at the T0 site than at the T1 site. The STXM data showed evidence of changes in the mixing state associated with a build-up of organic matter confirmed by collocated measurements and the largest impact on the mixing state was due to an increase in soot dominant particles during this build-up. The CCSEM/EDX analysis showed the presence of two types of particle populations; the first was dominated by aged sea salt particles and had a higher mixing state index (indicating a more homogeneous population), the second was dominated by carbonaceous particles and had a lower mixing state index.« less

SIMS chemical and isotopic analysis of impact features from LDEF experiments AO187-1 and AO187-2

NASA Technical Reports Server (NTRS)

Stadermann, Frank J.; Amari, Sachiko; Foote, John; Swan, Pat; Walker, Robert M.; Zinner, Ernst

1995-01-01

Previous secondary ion mass spectrometry (SIMS) studies of extended impact features from LDEF capture cell experiment AO187-2 showed that it is possible to distinguish natural and man-made particle impacts based on the chemical composition of projectile residues. The same measurement technique has now been applied to specially prepared gold target impacts from experiment AO187-1 in order to identify the origins of projectiles that left deposits too thin to be analyzed by conventional energy-dispersive x-ray (EDX) spectroscopy. The results indicate that SIMS may be the method of choice for the analysis of impact deposits on a variety of sample surfaces. SIMS was also used to determine the isotopic compositions of impact residues from several natural projectiles. Within the precision of the measurements all analyzed residues show isotopically normal compositions.

Discrimination between biologically relevant calcium phosphate phases by surface-analytical techniques

NASA Astrophysics Data System (ADS)

Kleine-Boymann, Matthias; Rohnke, Marcus; Henss, Anja; Peppler, Klaus; Sann, Joachim; Janek, Juergen

2014-08-01

The spatially resolved phase identification of biologically relevant calcium phosphate phases (CPPs) in bone tissue is essential for the elucidation of bone remodeling mechanisms and for the diagnosis of bone diseases. Analytical methods with high spatial resolution for the discrimination between chemically quite close phases are rare. Therefore the applicability of state-of-the-art ToF-SIMS, XPS and EDX as chemically specific techniques was investigated. The eight CPPs hydroxyapatite (HAP), β-tricalcium phosphate (β-TCP), α-tricalcium phosphate (α-TCP), octacalcium phosphate (OCP), dicalcium phosphate dihydrate (DCPD), dicalcium phosphate (DCP), monocalcium phosphate (MCP) and amorphous calcium phosphate (ACP) were either commercial materials in high purity or synthesized by ourselves. The phase purity was proven by XRD analysis. All of the eight CPPs show different mass spectra and the phases can be discriminated by applying the principal component analysis method to the mass spectrometric data. The Ca/P ratios of all phosphates were determined by XPS and EDX. With both methods some CPPs can be distinguished, but the obtained Ca/P ratios deviate systematically from their theoretical values. It is necessary in any case to determine a calibration curve, respectively the ZAF values, from appropriate standards. In XPS also the O(1s)-satellite signals are correlated to the CPPs composition. Angle resolved and long-term XPS measurements of HAP clearly prove that there is no phosphate excess at the surface. Decomposition due to X-ray irradiation has not been observed.

Electrochemical deposition of copper decorated titania nanotubes and its visible light photocatalytic performance

NASA Astrophysics Data System (ADS)

Lim, Y. C.; Siti, A. S.; Nur Amiera, P.; Devagi, K.; Lim, Y. P.

2017-09-01

Coupling of titania with narrow band gap materials has been a promising strategy in preparing visible light responsive photocatalyst. In this work, self-organized copper decorated TiO2 nanotube (Cu/TNT) was prepared via electrodeposition of Cu onto highly ordered titania nanotube arrays (TNT). The catalysts were characterized by X-ray diffraction, diffuse reflectance spectroscopy (DRS), field emission scanning electron microscopy (FESEM) and energy-dispersive X-ray spectroscopy (EDX). The DRS studies clearly show the extended absorption of Cu/TNT into the visible region and present a red shift of band gap to 2.1 eV. FESEM analysis has shown the dispersion of cubic-like Cu particles upon electrodeposition and EDX analysis supports the presence of copper species on the nanotubes surface. The photocatalytic ability of Cu/TNT was evaluated by the degradation of methyl orange from aqueous solution under low power visible light illumination. Compared to TNT, an appreciable improvement in methyl orange removal was observed for Cu/TNT and the highest removal efficiency of 80% was achieved. The effects of catalyst loading and samples repeatability were investigated and under optimum conditions, the removal efficiency of methyl orange over Cu/TNT had further increased to 93.4%. This work has demonstrated a feasible and simple way to introduce narrow band gap transition metal into nanotube arrays, which could create novel properties for functionalized nanotube arrays as well as promise a wide range of applications.

Arsenic scavenging by aluminum-substituted ferrihydrites in a circumneutral pH river impacted by acid mine drainage.

PubMed

Adra, Areej; Morin, Guillaume; Ona-Nguema, Georges; Menguy, Nicolas; Maillot, Fabien; Casiot, Corinne; Bruneel, Odile; Lebrun, Sophie; Juillot, Farid; Brest, Jessica

2013-11-19

Ferrihydrite (Fh) is a nanocrystalline ferric oxyhydroxide involved in the retention of pollutants in natural systems and in water-treatment processes. The status and properties of major chemical impurities in natural Fh is however still scarcely documented. Here we investigated the structure of aluminum-rich Fh, and their role in arsenic scavenging in river-bed sediments from a circumneutral river (pH 6-7) impacted by an arsenic-rich acid mine drainage (AMD). Extended X-ray absorption fine structure (EXAFS) spectroscopy at the Fe K-edge shows that Fh is the predominant mineral phase forming after neutralization of the AMD, in association with minor amount of schwertmannite transported from the AMD. TEM-EDXS elemental mapping and SEM-EDXS analyses combined with EXAFS analysis indicates that Al(3+) substitutes for Fe(3+) ions into the Fh structure in the natural sediment samples, with local aluminum concentration within the 25-30 ± 10 mol %Al range. Synthetic aluminous Fh prepared in the present study are found to be less Al-substituted (14-20 ± 5 mol %Al). Finally, EXAFS analysis at the arsenic K-edge indicates that As(V) form similar inner-sphere surface complexes on the natural and synthetic Al-substituted Fh studied. Our results provide direct evidence for the scavenging of arsenic by natural Al-Fh, which emphasize the possible implication of such material for scavenging pollutants in natural or engineered systems.

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.

Fabrication of solar light induced Fe-TiO{sub 2} immobilized on glass-fiber and application for phenol photocatalytic degradation

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

Lin, Shaohua, E-mail: linsh75@163.com; Zhang, Xiwang; Sun, Qinju

2013-11-15

Graphical abstract: - Highlights: • Fe-doped TiO{sub 2} immobilized on glass-fiber net were prepared by sol–gel method. • Fe inhibited the phase transition of TiO{sub 2} from anatase to rutile. • The optimal Fe doping dose was around 0.005 wt%. • The optimal calcination temperature was around 600 °C. - Abstract: Iron-doped anatase titanium dioxide catalysts coated on glass-fiber were successfully synthesized by a dip-coating sol–gel method. The prepared catalysts were characterized by scanning electron microscopy (SEM) with energy dispersive X-ray (EDX) analysis, X-ray diffraction (XRD), UV-Vis diffuse reflectance spectroscopy to understand the synthesis mechanism, and their photocatalytic activities weremore » evaluated by photodegradation of phenol under simulated solar irradiation. EDX analysis confirmed the existence of iron in the immobilized catalysts. XRD suggested that the phase transition of the catalysts from anatase to rutile were restrained, and almost pure anatase TiO{sub 2} could retain even the calcination temperature reached 800 °C. The UV-Vis diffuse reflectance spectroscopy of the catalysts showed a red shift and increased photoabsorbance in the visible range for all the doped samples. Iron loading and calcination temperature have obvious influences on photocatalytic activity. In this study, the optimal doping dose and calcination temperature were around 0.005 wt% and 600 °C, respectively.« 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.

Quantitative determination of low-Z elements in single atmospheric particles on boron substrates by automated scanning electron microscopy-energy-dispersive X-ray spectrometry.

PubMed

Choël, Marie; Deboudt, Karine; Osán, János; Flament, Pascal; Van Grieken, René

2005-09-01

Atmospheric aerosols consist of a complex heterogeneous mixture of particles. Single-particle analysis techniques are known to provide unique information on the size-resolved chemical composition of aerosols. A scanning electron microscope (SEM) combined with a thin-window energy-dispersive X-ray (EDX) detector enables the morphological and elemental analysis of single particles down to 0.1 microm with a detection limit of 1-10 wt %, low-Z elements included. To obtain data statistically representative of the air masses sampled, a computer-controlled procedure can be implemented in order to run hundreds of single-particle analyses (typically 1000-2000) automatically in a relatively short period of time (generally 4-8 h, depending on the setup and on the particle loading). However, automated particle analysis by SEM-EDX raises two practical challenges: the accuracy of the particle recognition and the reliability of the quantitative analysis, especially for micrometer-sized particles with low atomic number contents. Since low-Z analysis is hampered by the use of traditional polycarbonate membranes, an alternate choice of substrate is a prerequisite. In this work, boron is being studied as a promising material for particle microanalysis. As EDX is generally said to probe a volume of approximately 1 microm3, geometry effects arise from the finite size of microparticles. These particle geometry effects must be corrected by means of a robust concentration calculation procedure. Conventional quantitative methods developed for bulk samples generate elemental concentrations considerably in error when applied to microparticles. A new methodology for particle microanalysis, combining the use of boron as the substrate material and a reverse Monte Carlo quantitative program, was tested on standard particles ranging from 0.25 to 10 microm. We demonstrate that the quantitative determination of low-Z elements in microparticles is achievable and that highly accurate results can be obtained using the automatic data processing described here compared to conventional methods.

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.

Formation of silicon carbide by laser ablation in graphene oxide-N-methyl-2-pyrrolidone suspension on silicon surface

NASA Astrophysics Data System (ADS)

Jaleh, Babak; Ghasemi, Samaneh; Torkamany, Mohammad Javad; Salehzadeh, Sadegh; Maleki, Farahnaz

2018-01-01

Laser ablation of a silicon wafer in graphene oxide-N-methyl-2-pyrrolidone (GO-NMP) suspension was carried out with a pulsed Nd:YAG laser (pulse duration = 250 ns, wavelength = 1064 nm). The surface of silicon wafer before and after laser ablation was studied using optical microscopy, scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX). The results showed that the ablation of silicon surface in liquid by pulsed laser was done by the process of melt expulsion under the influence of the confined plasma-induced pressure or shock wave trapped between the silicon wafer and the liquid. The X-ray diffraction‌ (XRD) pattern of Si wafer after laser ablation showed that 4H-SiC layer is formed on its surface. The formation of the above layer was also confirmed by Raman spectroscopy, and X-ray photoelectron spectroscopy‌ (XPS), as well as EDX was utilized. The reflectance of samples decreased with increasing pulse energy. Therefore, the morphological alteration and the formation of SiC layer at high energy increase absorption intensity in the UV‌-vis regions. Theoretical calculations confirm that the formation of silicon carbide from graphene oxide and silicon wafer is considerably endothermic. Development of new methods for increasing the reflectance without causing harmful effects is still an important issue for crystalline Si solar cells. By using the method described in this paper, the optical properties of solar cells can be improved.

Data Fitting to Study Ablated Hard Dental Tissues by Nanosecond Laser Irradiation

PubMed Central

Abdel-Daiem, A. M.; Ansari, M. Shahnawaze; Babkair, Saeed S.; Salah, Numan A.; Al-Mujtaba, A.

2016-01-01

Laser ablation of dental hard tissues is one of the most important laser applications in dentistry. Many works have reported the interaction of laser radiations with tooth material to optimize laser parameters such as wavelength, energy density, etc. This work has focused on determining the relationship between energy density and ablation thresholds using pulsed, 5 nanosecond, neodymium-doped yttrium aluminum garnet; Nd:Y3Al5O12 (Nd:YAG) laser at 1064 nanometer. For enamel and dentin tissues, the ablations have been performed using laser-induced breakdown spectroscopy (LIBS) technique. The ablation thresholds and relationship between energy densities and peak areas of calcium lines, which appeared in LIBS, were determined using data fitting. Furthermore, the morphological changes were studied using Scanning Electron Microscope (SEM). Moreover, the chemical stability of the tooth material after ablation has been studied using Energy-Dispersive X-Ray Spectroscopy (EDX). The differences between carbon atomic % of non-irradiated and irradiated samples were tested using statistical t-test. Results revealed that the best fitting between energy densities and peak areas of calcium lines were exponential and linear for enamel and dentin, respectively. In addition, the ablation threshold of Nd:YAG lasers in enamel was higher than that of dentin. The morphology of the surrounded ablated region of enamel showed thermal damages. For enamel, the EDX quantitative analysis showed that the atomic % of carbon increased significantly when laser energy density increased. PMID:27228169

Synthesis and characterization of Ag-doped TiO2 nanotubes on Ti-6Al-4V and Ti-6Al-7Nb alloy

NASA Astrophysics Data System (ADS)

Ulfah, Ika Maria; Bachtiar, Boy M.; Murnandityas, Arnita Rut; Slamet

2018-05-01

The present paper is focused on comparative behavior of nanotubes growth on Ti-6Al-4V and Ti-6Al-7Nb alloy using electrochemical anodization method. These alloys were anodized in electrolytes solution containing glycerol, water and 0.5wt.% of NH4F. Silver-doped TiO2 nanotubes were synthesized using photo-assisted deposition (PAD) at various Ag loading concentration in 0.05 M, 0.10 M, and 0.15 M. The phase composition and morphological characteristics were investigated by XRD and FESEM/EDX, respectively. The surface wettability was measured by contact angle meter. The results showed that TiO2 nanotubes can be grown on these surface alloys. XRD profiles revealed crystal formation of anatase, rutile and Ag on these surface alloys. According to FESEM images, the average nanotube diameter of Ti-6Al-4V alloy and Ti-6Al-7Nb alloy are 134 nm and 120 nm, respectively. EDX-Mapping analysis showed that Ag desposited over surface of TiO2 nanotubes. The surface wettability indicated hydrophilicity properties on Ti-4Al-4V alloy and Ti-6Al-7Nb alloy surface. This study may contribute to the development of silver-doped TiO2 nanotubes on Ti-6Al-4V alloy and Ti-6Al-7Nb alloy can be considered in various photocatalytic applications such as biomedical devicesdue to photocatalytic mechanism and antibacterial ability.

Matrix change of bone grafting substitute after implantation into guinea pig bulla.

PubMed

Punke, Ch; Zehlicke, T; Just, T; Holzhüter, G; Gerber, T; Pau, H W

2012-05-01

Many different surgical techniques have been developed to remove open mastoid cavities. In addition to autologous materials, alloplastic substances have been used. A very slow absorption of these materials and extrusion reactions have been reported. We investigated a newly developed, highly porous bone grafting material to eliminate open mastoid cavities, in an animal model. To characterise the transformation process, the early tissue reactions were studied in relation to the matrix transformation of the bone material. NanoBone (NB), a highly porous bone grafting material based on calcium phosphate and silica, was filled into the open bullae from 20 guinea pigs. The bullae were examined histologically. Energy dispersive X-ray spectroscopy (EDX) was used to investigate the change in the elemental composition at different sampling times. The surface topography of the sections was examined by electron microscopy. After 1 week, periodic acid-Schiffs (PAS) staining demonstrated accumulation of glycogen and proteins, particularly in the border area of the NB particles. After 2 weeks, the particles were evenly coloured after PAS staining. EDX analysis showed a rapid absorption of the silica in the bone grafting material. NanoBone showed a rapid matrix change after implantation in the bullae of guinea pigs. The absorption of the silica matrix and replacement by PAS-positive substances like glycoproteins and mucopolysaccharides seems to play a decisive role in the degradation processes of NB. This is associated with the good osteoinductive properties of the material.

A pharmacokinetic/pharmacodynamic investigation: assessment of edivoxetine and atomoxetine on systemic and central 3,4-dihydroxyphenylglycol, a biochemical marker for norepinephrine transporter inhibition.

PubMed

Kielbasa, William; Pan, Alan; Pereira, Alvaro

2015-03-01

Inhibition of norepinephrine (NE) reuptake into noradrenergic nerves is a common therapeutic target in the central nervous system (CNS). In noradrenergic nerves, NE is oxidized by monoamine oxidase to 3,4-dihydroxyphenylglycol (DHPG). In this study, 40 healthy male subjects received the NE transporter (NET) inhibitor edivoxetine (EDX) or atomoxetine (ATX), or placebo. The pharmacokinetic and pharmacodynamic profile of these drugs in plasma and cerebrospinal fluid (CSF) was assessed. In Part A, subjects received EDX once daily (QD) for 14 or 15 days at targeted doses of 6mg or 9mg. In Part B, subjects received 80mg ATX QD for 14 or 15 days. Each subject received a lumbar puncture before receiving drug and after 14 or 15 days of dosing. Plasma and urine were collected at baseline and after 14 days of dosing. Edivoxetine plasma and CSF concentrations increased dose dependently. The time to maximum plasma concentration of EDX was 2h, and the half-life was 9h. At the highest EDX dose of 9mg, DHPG concentrations were reduced from baseline by 51% at 8h postdose in CSF, and steady-state plasma and urine DHPG concentrations decreased by 38% and 26%, respectively. For 80mg ATX, the decrease of plasma, CSF, or urine DHPG was similar to EDX. Herein we provide clinical evidence that EDX and ATX decrease DHPG concentrations in the periphery and CNS, presumably via NET inhibition. EDX and ATX concentrations measured in the CSF confirmed the availability of those drugs in the CNS. Copyright © 2015 Elsevier B.V. and ECNP. All rights reserved.

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.

CMOS compatible electrode materials selection in oxide-based memory devices

NASA Astrophysics Data System (ADS)

Zhuo, V. Y.-Q.; Li, M.; Guo, Y.; Wang, W.; Yang, Y.; Jiang, Y.; Robertson, J.

2016-07-01

Electrode materials selection guidelines for oxide-based memory devices are constructed from the combined knowledge of observed device operation characteristics, ab-initio calculations, and nano-material characterization. It is demonstrated that changing the top electrode material from Ge to Cr to Ta in the Ta2O5-based memory devices resulted in a reduction of the operation voltages and current. Energy Dispersed X-ray (EDX) Spectrometer analysis clearly shows that the different top electrode materials scavenge oxygen ions from the Ta2O5 memory layer at various degrees, leading to different oxygen vacancy concentrations within the Ta2O5, thus the observed trends in the device performance. Replacing the Pt bottom electrode material with CMOS compatible materials (Ru and Ir) further reduces the power consumption and can be attributed to the modification of the Schottky barrier height and oxygen vacancy concentration at the electrode/oxide interface. Both trends in the device performance and EDX results are corroborated by the ab-initio calculations which reveal that the electrode material tunes the oxygen vacancy concentration via the oxygen chemical potential and defect formation energy. This experimental-theoretical approach strongly suggests that the proper selection of CMOS compatible electrode materials will create the critical oxygen vacancy concentration to attain low power memory performance.

Carbide-derived carbon (CDC) linear actuator properties in combination with conducting polymers

NASA Astrophysics Data System (ADS)

Kiefer, Rudolf; Aydemir, Nihan; Torop, Janno; Kilmartin, Paul A.; Tamm, Tarmo; Kaasik, Friedrich; Kesküla, Arko; Travas-Sejdic, Jadranka; Aabloo, Alvo

2014-03-01

Carbide-derived Carbon (CDC) material is applied for super capacitors due to their nanoporous structure and their high charging/discharging capability. In this work we report for the first time CDC linear actuators and CDC combined with polypyrrole (CDC-PPy) in ECMD (Electrochemomechanical deformation) under isotonic (constant force) and isometric (constant length) measurements in aqueous electrolyte. CDC-PPy actuators showing nearly double strain under cyclic voltammetric and square wave potential measurements in comparison to CDC linear actuators. The new material is investigated by SEM (scanning electron microscopy) and EDX (energy dispersive X-ray analysis) to reveal how the conducting polymer layer and the CDC layer interfere together.

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.

Synthesis of MnFe2O4 magnetic nano hollow spheres by a facile solvothermal route and its characterization

NASA Astrophysics Data System (ADS)

Dey, Chaitali; Chaudhuri, Arka; Goswami, Madhuri Mandal

2018-04-01

Herein, we report the synthesis of manganese ferrite (MnFe2O4) magnetic nano hollow sphere (NHS) by a solvothermal route. Crystalline phase was confirmed by X-ray diffraction (XRD), energy dispersive x-ray (EDX). Magnetic measurements were done in vibrating sample magnetometer (VSM) and morphological structure was analyzed by field emission high resolution scanning electron microscope (FESEM) and structural characterization was confirmed by Fourier transform infrared spectroscopy (FTIR), thermal analysis was performed by thermo-gravimetric analysis-differential thermal analysis (TGA-DTA). The size of the NHS was around 470 nm, this large size may show a potential applicability in industrial application, like dye adsorption, catalysis etc. In addition, because of its ferromagnetic character at room temperature, it can be easily separated by external magnetic field after the application is done.

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

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

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.

PROBIT: A Probit Analysis Program for the DRES (Defence Research Establishment Suffield) Computer Facility,

DTIC Science & Technology

1986-07-01

p are are also discussed. When iteration is terminated, we can determine the effective dose at the A percentile level or EDX ; that is the dose at...corresponds to the lower limit, fl.. The fiducial or Fieller limits on x , i.e., the EDX are then f’ = exp If.1 (36) It can be readily shown that g = t2 v-1...4 .4+ 1W (n 0 CL C ~o 0 0 X U) -W CLW W 24W Q X C W C > VW U)w5 z C z 5memo f- G5555t (j) tSS a;C w CO W QZ 1 I- ~ ~ ~ C (. 5r 5W <A * a W Www w V

Tuning effect of polysaccharide Chitosan on structural, morphological, optical and photoluminescence properties of ZnO nanoparticles

NASA Astrophysics Data System (ADS)

Magesh, G.; Bhoopathi, G.; Nithya, N.; Arun, A. P.; Ranjith Kumar, E.

2018-05-01

Chitosan/ZnO nanocomposites was synthesized by in-situ chemical precipitation method. The effect of polysaccharide Chitosan concentration (0.1 g, 0.5 g, 1 g and 3 g) was investigated by X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM) with Energy dispersive spectroscopy (EDX), High Resolution Transmission Electron Microscopy (HRTEM), UV-visible (UV), Fourier Transform Infrared (FTIR) and Photoluminescence Spectroscopy (PL). XRD pattern confirms the hexagonal wurtzite structure of the Chitosan/ZnO nanocomposites. The structural morphology and the elemental composition of the samples were analysed by FESEM and EDX respectively. From TEM analysis, it is observed that the particles in spindle shape morphology with average particle size ranges 10-20 nm. UV-Vis analysis reveals that the Chitosan concentration affect the absorption band edge and shift towards lower wavelength. The oxygen vacancy induced photoluminescence of ZnO nanoparticles was observed and its intensity decreases by tuning the Chitosan concentration.

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

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.

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

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.

Assessment of Bracket Surface Morphology and Dimensional Change

PubMed Central

Radhakrishnan, Pillai Devu; Sapna Varma, N. K.; Ajith, V. V.

2017-01-01

Objective: The objective of this study was to compare the surface morphology and dimensional stability of the bracket slot at the onset of treatment and after 12 months of intraoral exposure. The study also compared the amount of calcium at the bracket base which indicates enamel loss among the three orthodontic brackets following debonding after 12 months of intraoral exposure. Materials and Methods: The sample consisted of 60 (0.022” MBT) canine brackets. They were divided into three groups: self-ligating, ceramic bracket with metal slot, and stainless steel (SS) brackets. The slot dimensions, micromorphologic characteristics of as-received and retrieved brackets were measured with a stereomicroscope and scanning electron microscope (SEM), respectively. The amount of calcium at the bracket base which indicates enamel damage was quantified using energy-dispersive X-ray spectrometry (EDX). Results: The results showed statistically significant alterations (P < 0.05) in the right vertical dimension, internal tie wing width (cervical), right and left depth of the slot (Kruskal–Wallis test). Multiple comparison using Mann–Whitney test showed that ceramic brackets underwent (P < 0.05) minimal alterations in the right vertical dimension, internal tie wing width (cervical), right and left depth of the slot (0.01 mm, −0.003 mm, 0.006 mm, −0.002 mm, respectively) when compared with the changes seen in SS and self-ligating brackets. SEM analysis revealed an increase in the surface roughness of ceramic with metal slot brackets and self-ligating bracket showed the least irregularity. The presence of calcium was noted on all evaluated brackets under EDX, but ceramic with metal slot brackets showed a significantly greater amount of enamel loss (P = 0.001). Conclusion: Ceramic brackets were found to be dimensionally stable when compared to SS and self-ligating. Self-ligating bracket showed minimal surface irregularity. Ceramic with metal slot brackets showed a greater amount of enamel loss following debonding. PMID:28566855

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.

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

Synthesis of CaCu3Ti4O12 by modified Sol-gel method with Hydrothermal process

NASA Astrophysics Data System (ADS)

Masingboon, C.; Rungruang, S.

2017-09-01

CaCu3Ti4O12 powders were synthesized by modified Sol-gel method with Hydrothermal process using Ca(NO3)2· 4H2O, Cu(NO3)2·3H2O, Ti(OC3H7)4 and freshly extracted egg white (ovalbumin) in aqueous medium. The precursor was calcined at 800, 900 and 1000 °C in air for 8 h to obtain nanocrystalline powders of CaCu3Ti4O12. The calcined CaCu3Ti4O12 powders were characterized by XRD, TEM and EDX. The XRD results indicated that all calcined samples have a typical perovskite CaCu3Ti4O12 structure and a small amount of CaTiO3, CuO and TiO2. TEM micrographs showed particle size 100 - 500 nm and EDX results showed elements of CaCu3Ti4O12 powders have calcium, copper, titanium and oxygen.

Effect of copper and nickel doping on the optical and structural properties of ZnO

NASA Astrophysics Data System (ADS)

Muǧlu, G. Merhan; Sarıtaş, S.; ćakıcı, T.; Şakar, B.; Yıldırım, M.

2017-02-01

The present study is focused on the Cu doped ZnO and Ni doped ZnO dilute magnetic semiconductor thin films. ZnO:Cu and ZnO:Ni thin films were grown by Chemically Spray Pyrolysis (CSP) method on glass substrates. Optical analysis of the films was done spectral absorption and transmittance measurements by UV-Vis double beam spectrophotometer technique. The structure, morphology, topology and elemental analysis of ZnO:Cu and ZnO:Ni dilute magnetic thin films were investigated by X-ray diffraction (XRD), Raman Analysis, field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), atomic force microscopy (AFM) techniques, respectively. Also The magnetic properties of the ZnO:Ni thin film was investigated by vibrating sample magnetometer (VSM) method. VSM measurements of ZnO:Ni thin film showed that the ferromagnetic behavior.

Improving Signal-to-Noise Ratio in Scanning Transmission Electron Microscopy Energy-Dispersive X-Ray (STEM-EDX) Spectrum Images Using Single-Atomic-Column Cross-Correlation Averaging.

PubMed

Jeong, Jong Seok; Mkhoyan, K Andre

2016-06-01

Acquiring an atomic-resolution compositional map of crystalline specimens has become routine practice, thus opening possibilities for extracting subatomic information from such maps. A key challenge for achieving subatomic precision is the improvement of signal-to-noise ratio (SNR) of compositional maps. Here, we report a simple and reliable solution for achieving high-SNR energy-dispersive X-ray (EDX) spectroscopy spectrum images for individual atomic columns. The method is based on standard cross-correlation aided by averaging of single-column EDX maps with modifications in the reference image. It produces EDX maps with minimal specimen drift, beam drift, and scan distortions. Step-by-step procedures to determine a self-consistent reference map with a discussion on the reliability, stability, and limitations of the method are presented here.

Green engineered biomolecule-capped silver and copper nanohybrids using Prosopis cineraria leaf extract: Enhanced antibacterial activity against microbial pathogens of public health relevance and cytotoxicity on human breast cancer cells (MCF-7).

PubMed

Jinu, U; Gomathi, M; Saiqa, I; Geetha, N; Benelli, G; Venkatachalam, P

2017-04-01

This research focused on green engineering and characterization of silver (PcAgNPs) and copper nanoparticles (PcCuNPs) using Prosopis cineraria (Pc) leaf extract prepared by using microwave irradiation. We studied their enhanced antimicrobial activity on human pathogens as well as cytotoxicity on breast cancer cells (MCF-7). Biofabricated silver and copper nanoparticles exhibited UV-Visible absorbance peaks at 420 nm and 575 nm, confirming the bioreduction and stabilization of nanoparticles. Nanoparticles were characterized by FTIR, XRD, FESEM, and EDX analysis. FTIR results indicated the presence of alcohols, alkanes, aromatics, phenols, ethers, benzene, amines and amides that were possibly involved in the reduction and capping of silver and copper ions. XRD analysis was performed to confirm the crystalline nature of the silver and copper nanoparticles. FESEM analysis suggested that the nanoparticles were hexagonal or spherical in shape with size ranging from 20 to 44.49 nm and 18.9-32.09 nm for AgNPs and CuNPs, respectively. EDX analysis confirmed the presence of silver and copper elemental signals in the nanoparticles. The bioengineered silver and copper nanohybrids showed enhanced antimicrobial activity against Gram-positive and Gram-negative MDR human pathogens. MTT assay results indicated that CuNPs show potential cytotoxic effect followed by AgNPs against MCF-7 cancer cell line. IC 50 were 65.27 μg/ml, 37.02 μg/ml and 197.3 μg/ml for PcAgNPs, PcCuNPs and P. cineraria leaf extracts, respectively, treated MCF-7 cells. The present investigation highlighted an effective protocol for microwave-assisted synthesis of biomolecule-loaded silver and copper nanoparticles with enhanced antibacterial and anticancer activity. Results strongly suggested that bioengineered AgNPs and CuNPs could be used as potential tools against microbial pathogens and cancer cells. Copyright © 2017 Elsevier Ltd. All rights reserved.

Analysis of particulate contaminations of infusion solutions in a pediatric intensive care unit.

PubMed

Jack, Thomas; Brent, Bernadette E; Boehne, Martin; Müller, Meike; Sewald, Katherina; Braun, Armin; Wessel, Armin; Sasse, Michael

2010-04-01

To examine the physical properties and chemical composition of particles captured by in-line microfilters in critically ill children, and to investigate the inflammatory and cytotoxic effects of particles on endothelial cells (HUVEC) and macrophages in vitro. Prospective, observational study of microfilters following their use in the pediatric intensive care unit. In vitro model utilizing cytokine assays to investigate the effects of particles on human endothelial cells and murine macrophages. Twenty filter membranes from nine patients and five controls were examined by electron microscopy (EM) and energy dispersion spectroscopy (EDX). The average number of particles found on the surface of the used membranes was 550 cm(2). EDX analysis confirmed silicon as a major particle constituent. Half of the filter membranes showed conglomerates containing an unaccountable number of smaller particles. In vitro, glass particles were used to mimic the high silicon content particles. HUVEC and murine macrophages were exposed to different contents of particles, and cytokine levels were assayed to assess their immune response. Levels of interleukin-1beta, interleukin-6, interleukin-8, and tumor necrosis factor alpha were suppressed. Particle contamination of infusion solutions exists despite a stringent infusion regiment. The number and composition of particles depends on the complexity of the applied admixtures. Beyond possible physical effects, the suppression of macrophage and endothelial cell cytokine secretion in vitro suggests that microparticle infusion in vivo may have immune-modulating effects. Further clinical trials are necessary to determine whether particle retention by in-line filtration has an influence on the outcome of intensive care patients.

Fabrication of CdS nanowires with increasing anionic precursor by SILAR method

NASA Astrophysics Data System (ADS)

Dariani, R. S.; Salehi, F.

2016-05-01

CdS nanowires were fabricated on glass substrate at room temperature by SILAR method with cadmium nitrate cationic and sodium sulfide anionic precursors. The deposition were done at different S:Cd concentration ratios of 1:1, 3:1, 5:1, and 7:1. Nanowires growth procedure was studied in the mentioned concentrations. The number of immersion cycles was kept constant at 15 cycles. EDX analysis showed that in all stoichiometric ratios, S/Cd composition ratio remains at about unity. Our results indicated that S:Cd concentration ratio of 7:1 had the longest nanowires with hexagonal structure. The main objective of this paper was to produce CdS nanowires with increasing concentration of sulfur.

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

Jeong, Sang Hoon; Kim, Jae Hwan; Yi, Sang Min

Quantum dots (QDs) are rapidly emerging as an important class of nanoparticles (NPs) with potential applications in medicine. However, little is known about penetration of QDs through human skin. This study investigated skin penetration of QDs in both in vivo and in vitro human skin. Using the tape stripping method, this study demonstrates for the first time that QDs can actually penetrate through the stratum corneum (SC) of human skin. Transmission electron microscope (TEM) and energy diverse X-ray (EDX) analysis showed accumulation of QDs in the SC of a human skin equivalent model (HSEM) after dermal exposure to QDs. Thesemore » findings suggest possible transdermal absorption of QDs after dermal exposure over a relatively long period of time.« less

Structural phase analysis and photoluminescence properties of Mg-doped TiO2 nanoparticles

NASA Astrophysics Data System (ADS)

Ali, T.; Ashraf, M. Anas; Ali, S. Asad; Ahmed, Ateeq; Tripathi, P.

2018-05-01

In this paper, we report the synthesis, characterization and photoluminescence properties of Mg-doped TiO2 nanoparticles (NPs). The samples were synthesized by sol-gel method and characterized using the standard analytical techniques such as X-ray diffraction (XRD), Transmission electron microscope (TEM), Energy dispersive X-ray spectroscopy (EDX), UV-visible and photoluminescence spectroscopy. The powder XRD spectra revealed that the synthesized samples are pure and crystalline in nature and showing tetragonal anatase phase of TiO2 NPs. UV-visible spectrum illustrates that an absorption edge shifts toward the visible region. This study may provide a new insight for making the nanomaterials which can be used in photocatalytic applications.

Pseudomonas aeruginosa KUCD1, a possible candidate for cadmium bioremediation

PubMed Central

Sinha, Sangram; Mukherjee, Samir Kumar

2009-01-01

A cadmium (8 mM) resistant Pseudomonas aeruginosa strain KUCd1 exhibiting high Cd accumulation under in vitro aerobic condition has been reported. The isolate showed a significant ability to remove more than 75% and 89% of the soluble cadmium during the active growth phase from the growth medium and from Cd-amended industrial wastewater under growth supportive condition. Transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDXS) suggest the presence of Cd in the cells from mid stationary phase. The cell fractionation study revealed membrane and periplasm to be the major accumulating site in this strain. The chemical nature of the accumulated Cd was studied by X-ray powder diffraction analysis. PMID:24031411

A potential cause for kidney stone formation during space flights: enhanced growth of nanobacteria in microgravity.

PubMed

Ciftçioglu, Neva; Haddad, Ruwaida S; Golden, D C; Morrison, Dennis R; McKay, David S

2005-02-01

Although some information is available regarding the cellular/molecular changes in immune system exposed to microgravity, little is known about the reasons of the increase in the kidney stone formation in astronauts during and/or after long duration missions at zero gravity (0 g). In our earlier studies, we have assessed a unique agent, nanobacteria (NB), in kidney stones and hypothesized that NB have an active role in calcium phosphate-carbonate deposition in kidney. In this research we studied effect of microgravity on multiplication and calcification of NB in vitro. We examined NB cultures in High Aspect Rotating Vessels (HARVs) designed at the NASA's Johnson Space Center, which are designed to stimulate some aspects of microgravity. Multiplication rate and calcium phosphate composition of those NB were compared with NB cultured on stationary and shaker flasks. Collected aliquots of the cultures from different incubation periods were analyzed using spectrophotometer, SEM, TEM, EDX, and x-ray diffraction techniques. The results showed that NB multiplied 4.6x faster in HARVs compared to stationary cultures, and 3.2x faster than shaker flask conditions. X-ray diffraction and EDX analysis showed that the degree of apatite crystal formation and the properties of the apatite depend on the specific culture conditions used. We now report an increased multiplication rate of NB in microgravity-simulated conditions. Thus, NB infection may have a potential role in kidney stone formation in crew members during space flights. For further proof to this hypothesis, screening of the NB antigen and antibody level in flight crew before and after flight would be necessary.

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.

Structural properties of ultrafine Ba-hexaferrite nanoparticles

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

Makovec, Darko, E-mail: Darko.Makovec@ijs.si; Primc, Darinka; Sturm, Saso

2012-12-15

Crystal structure of ultrafine Ba-hexaferrite (BaFe{sub 12}O{sub 19}) nanoparticles was studied using X-ray diffractometry (XRD), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDXS), X-ray absorption fine structure (XAFS), and Moessbauer spectroscopy (MS), to be compared to the structure of larger nanoparticles and the bulk. The nanoparticles were synthesized with hydrothermal treatment of an appropriate suspension of Ba and Fe hydroxides in the presence of a large excess of OH{sup -}. The ultrafine nanoparticles were formed in a discoid shape, {approx}10 nm wide and only {approx}3 nm thick, comparable to the size of the hexagonal unit cell in the c-direction.more » The HRTEM image analysis confirmed the hexaferrite structure, whereas EDXS showed the composition matching the BaFe{sub 12}O{sub 19} formula. XAFS and MS analyses showed considerable disorder of the structure, most probably responsible for the low magnetization. - Graphical abstract: Left: HREM image of an ultrafine Ba-hexaferrite nanoparticle (inset: TEM image of the nanoparticles); Right: the experimental HRTEM image is compared with calculated image and corresponding atomic model. Highlights: Black-Right-Pointing-Pointer Crystal structure of ultrafine Ba-hexaferrite (BaFe{sub 12}O{sub 19}) nanoparticles was compared to the structure of the bulk. Black-Right-Pointing-Pointer Thickness the discoid nanoparticles was comparable to the size of the hexagonal unit cell in the c-direction. Black-Right-Pointing-Pointer Considerable disorder of the nanoparticles' structure is most probably responsible for their low magnetization.« less

Effects of rare earth doping on multi-core iron oxide nanoparticles properties

NASA Astrophysics Data System (ADS)

Petran, Anca; Radu, Teodora; Borodi, Gheorghe; Nan, Alexandrina; Suciu, Maria; Turcu, Rodica

2018-01-01

New multi-core iron oxide magnetic nanoparticles doped with rare earth metals (Gd, Eu) were obtained by a one step synthesis procedure using a solvothermal method for potential biomedical applications. The obtained clusters were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), energy-dispersive X-ray microanalysis (EDX), X-ray photoelectron spectroscopy (XPS) and magnetization measurements. They possess high colloidal stability, a saturation magnetization of up to 52 emu/g, and nearly spherical shape. The presence of rare earth ions in the obtained samples was confirmed by EDX and XPS. XRD analysis proved the homogeneous distribution of the trivalent rare earth ions in the inverse-spinel structure of magnetite and the increase of crystal strain upon doping the samples. XPS study reveals the valence state and the cation distribution on the octahedral and tetrahedral sites of the analysed samples. The observed shift of the XPS valence band spectra maximum in the direction of higher binding energies after rare earth doping, as well as theoretical valence band calculations prove the presence of Gd and Eu ions in octahedral sites. The blood protein adsorption ability of the obtained samples surface, the most important factor of the interaction between biomaterials and body fluids, was assessed by interaction with bovine serum albumin (BSA). The rare earth doped clusters surface show higher afinity for binding BSA. In vitro cytotoxicity test results for the studied samples showed no cytotoxicity in low and medium doses, establishing a potential perspective for rare earth doped MNC to facilitate multiple therapies in a single formulation for cancer theranostics.

Characterization of Airborne Particles Collected from Car Engine Air Filters Using SEM and EDX Techniques.

PubMed

Heredia Rivera, Birmania; Gerardo Rodriguez, Martín

2016-10-01

Particulate matter accumulated on car engine air-filters (CAFs) was examined in order to investigate the potential use of these devices as efficient samplers for collecting street level air that people are exposed to. The morphology, microstructure, and chemical composition of a variety of particles were studied using scanning electron microscopy (SEM) and energy-dispersive X-ray (EDX). The particulate matter accumulated by the CAFs was studied in two categories; the first was of removed particles by friction, and the second consisted of particles retained on the filters. Larger particles with a diameter of 74-10 µm were observed in the first category. In the second one, the detected particles had a diameter between 16 and 0.7 µm. These particles exhibited different morphologies and composition, indicating mostly a soil origin. The elemental composition revealed the presence of three groups: mineral (clay and asphalt), metallic (mainly Fe), and biological particles (vegetal and animal debris). The palynological analysis showed the presence of pollen grains associated with urban plants. These results suggest that CAFs capture a mixture of atmospheric particles, which can be analyzed in order to monitor urban air. Thus, the continuous availability of large numbers of filters and the retroactivity associated to the car routes suggest that these CAFs are very useful for studying the high traffic zones within a city.

Characterization of Airborne Particles Collected from Car Engine Air Filters Using SEM and EDX Techniques

PubMed Central

Heredia Rivera, Birmania; Gerardo Rodriguez, Martín

2016-01-01

Particulate matter accumulated on car engine air-filters (CAFs) was examined in order to investigate the potential use of these devices as efficient samplers for collecting street level air that people are exposed to. The morphology, microstructure, and chemical composition of a variety of particles were studied using scanning electron microscopy (SEM) and energy-dispersive X-ray (EDX). The particulate matter accumulated by the CAFs was studied in two categories; the first was of removed particles by friction, and the second consisted of particles retained on the filters. Larger particles with a diameter of 74–10 µm were observed in the first category. In the second one, the detected particles had a diameter between 16 and 0.7 µm. These particles exhibited different morphologies and composition, indicating mostly a soil origin. The elemental composition revealed the presence of three groups: mineral (clay and asphalt), metallic (mainly Fe), and biological particles (vegetal and animal debris). The palynological analysis showed the presence of pollen grains associated with urban plants. These results suggest that CAFs capture a mixture of atmospheric particles, which can be analyzed in order to monitor urban air. Thus, the continuous availability of large numbers of filters and the retroactivity associated to the car routes suggest that these CAFs are very useful for studying the high traffic zones within a city. PMID:27706087

Galvanic coupling of steel and gold alloy lingual brackets with orthodontic wires.

PubMed

Polychronis, Georgios; Al Jabbari, Youssef S; Eliades, Theodore; Zinelis, Spiros

2018-03-06

The aim of this research was to assess galvanic behavior of lingual orthodontic brackets coupled with representative types of orthodontic wires. Three types of lingual brackets: Incognito (INC), In-Ovation L (IOV), and STb (STB) were combined with a stainless steel (SS) and a nickel-titanium (NiTi) orthodontic archwire. All materials were initially investigated by scanning electron microscopy / x-ray energy dispersive spectroscopy (SEM/EDX) while wires were also tested by x-ray diffraction spectroscopy (XRD). All bracket-wire combinations were immersed in acidic 0.1M NaCl 0.1M lactic acid and neutral NaF 0.3% (wt) electrolyte, and the potential differences were continuously recorded for 48 hours. The SEM/EDX analysis revealed that INC is a single-unit bracket made of a high gold (Au) alloy while IOV and STB are two-piece appliances in which the base and wing are made of SS alloys. The SS wire demonstrated austenite and martensite iron phase, while NiTi wire illustrated an intense austenite crystallographic structure with limited martensite. All bracket wire combinations showed potential differences below the threshold of galvanic corrosion (200 mV) except for INC and STB coupled with NiTi wire in NaF media. The electrochemical results indicate that all brackets tested demonstrated galvanic compatibility with SS wire, but fluoride treatment should be used cautiously with NiTi wires coupled with Au and SS brackets.

Characterisation of well-adhered ZrO2 layers produced on structured reactors using the sonochemical sol-gel method

NASA Astrophysics Data System (ADS)

Jodłowski, Przemysław J.; Chlebda, Damian K.; Jędrzejczyk, Roman J.; Dziedzicka, Anna; Kuterasiński, Łukasz; Sitarz, Maciej

2018-01-01

The aim of this study was to obtain thin zirconium dioxide coatings on structured reactors using the sonochemical sol-gel method. The preparation method of metal oxide layers on metallic structures was based on the synergistic combination of three approaches: the application of ultrasonic irradiation during the synthesis of Zr sol-gel based on a precursor solution containing zirconium(IV) n-propoxide, the addition of stabilszing agents, and the deposition of ZrO2 on the metallic structures using the dip-coating method. As a result, dense, uniform zirconium dioxide films were obtained on the FeCrAlloy supports. The structured reactors were characterised by various physicochemical methods, such as BET, AFM, EDX, XRF, XRD, XPS and in situ Raman spectroscopy. The results of the structural analysis by Raman and XPS spectroscopy confirmed that the metallic surface was covered by a ZrO2 layer without any impurities. SEM/EDX mapping revealed that the deposited ZrO2 covered the metallic support uniformly. The mechanical and high temperature tests showed that the developed ultrasound assisted sol-gel method is an efficient way to obtain thin, well-adhered zirconium dioxide layers on the structured reactors. The prepared metallic supports covered with thin ZrO2 layers may be a good alternative to layered structured reactors in several dynamics flow processes, for example for gas exhaust abatement.

Electron Microscopy and Image Analysis for Selected Materials

NASA Technical Reports Server (NTRS)

Williams, George

1999-01-01

This particular project was completed in collaboration with the metallurgical diagnostics facility. The objective of this research had four major components. First, we required training in the operation of the environmental scanning electron microscope (ESEM) for imaging of selected materials including biological specimens. The types of materials range from cyanobacteria and diatoms to cloth, metals, sand, composites and other materials. Second, to obtain training in surface elemental analysis technology using energy dispersive x-ray (EDX) analysis, and in the preparation of x-ray maps of these same materials. Third, to provide training for the staff of the metallurgical diagnostics and failure analysis team in the area of image processing and image analysis technology using NIH Image software. Finally, we were to assist in the sample preparation, observing, imaging, and elemental analysis for Mr. Richard Hoover, one of NASA MSFC's solar physicists and Marshall's principal scientist for the agency-wide virtual Astrobiology Institute. These materials have been collected from various places around the world including the Fox Tunnel in Alaska, Siberia, Antarctica, ice core samples from near Lake Vostoc, thermal vents in the ocean floor, hot springs and many others. We were successful in our efforts to obtain high quality, high resolution images of various materials including selected biological ones. Surface analyses (EDX) and x-ray maps were easily prepared with this technology. We also discovered and used some applications for NIH Image software in the metallurgical diagnostics facility.

Effect of Eu3+ doping on the structural, morphological and luminescence properties ZnO nanostructures

NASA Astrophysics Data System (ADS)

Vinoditha, U.; Balakrishna, K. M.; Sarojini, B. K.; Narayana, B.; Kumara, K.

2018-05-01

Pure and Eu3+ ions (1, 3, 5 atomic wt%) doped ZnO nanostructures are synthesized by a surfactant assisted hydrothermal method. The effect of doping concentrations on structural, morphological and optical properties of ZnO nanostructures is studied. The XRD analysis shows good crystallinity and the phase purity of the ZnO nanostructures. A shift in the standard Zn-O stretching mode after Eu3+ doping is observed in the FTIR spectra. The images of FESEM demonstrate the morphological variations from hexagonal nanorods to nanoflowers on varying the dopant concentrations. Substitution of Eu3+ ions into Zn2+ sites is confirmed by EDX analysis. The dominance of particle shape over the UV-Visible absorption properties of the prepared samples is noticed. The photoluminescence (PL) emission of undoped and doped ZnO nanostructures show dominant near band edge emission (NBE) in the UV region and minor defect induced deep level emissions in the visible region.

Use of different rapid mixing devices for controlling the properties of magnetite nanoparticles produced by precipitation

NASA Astrophysics Data System (ADS)

Wei, Li; Hervé, Muhr; Edouard, Plasari

2012-03-01

Magnetite nanoparticles were precipitated by the classic Massart's method in a 2.5 L stirred tank reactor where the injection of reagent solutions was effectuated by different micro-mixers (T-tube and Hartridge-Roughton rapid mixing devices). The specific surface area, the average particle size and the particle size distribution were highly influenced by changing operating parameters. Laser Diffraction, BET adsorption, Energy-Dispersive X-ray Spectroscopy (EDX), Raman spectroscopy and Transmission Electron Microscopy (TEM) were used for characterizing magnetite nanoparticles. Especially, Hartridge-Roughton micromixer appears to be the most efficient mixing device for producing magnetite nanoparticles. The average particle size of magnetite nanoparticles prepared by Hartridge-Roughton rapid mixing device was less than 10 nm and the EDX and Raman spectroscopy shows that the particle purity is quite high.

Morphology of one-time coated palladium-alumina composite membrane prepared by sol-gel process and electroless plating technique

NASA Astrophysics Data System (ADS)

Sari, R.; Dewi, R.; Pardi; Hakim, L.; Diana, S.

2018-03-01

Palladium coated porous alumina ceramic membrane tube was obtained using a combination of sol-gel process and electroless plating technique. The thickness, structure and composition of palladium-alumina composite membrane were analyzed by transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), and atomic force microscopy (AFM). Palladium particle size was 6.18 to 7.64 nm. Palladium membrane with thickness of approximately 301.5 to 815.1 nm was formed at the outer surface of the alumina layer. EDX data confirmed the formation of palladium-alumina membrane containing 45% of palladium. From this research it shows the combination of sol-gel process and electroless plating technique with one-time coating can produce a homogeneous and smoother palladium nano layer film on alumina substrate.

Characterization of carbon silica hybrid fillers obtained by pyrolysis of waste green tires by the STEM–EDX method

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

Al-Hartomy, Omar A.; Department of Physics, Faculty of Science, University of Tabuk, Tabuk 71491; Al-Ghamdi, Ahmed A.

2015-03-15

Dual phase carbon–silica hybrid fillers obtained by pyrolysis-cum-water vapor of waste green tires have been characterized by energy dispersive X-ray spectroscopy in a scanning transmission electron microscope, silicate analysis, weight analysis, atomic absorption spectroscopy and by inductively coupled plasma–optical emission spectroscopy. The results achieved have shown that the location and distribution of the phases in the carbon silica hybrid fillers as well as their most essential characteristics are influenced by the pyrolysis conditions. The carbon phase of the filler thus obtained is located predominantly in the space among silica aggregates which have already been existing while it has been formedmore » by elastomer destruction in the course of pyrolysis. The presence of ZnS also has been found in the hybrid fillers investigated. - Highlights: • Dual phase fillers obtained by pyrolysis of waste green tires have been characterized. • The STEM–EDX method was used for characterization. • The phase distributions in the fillers are influenced by the pyrolysis conditions.« less

Self-assembly of silicon nanowires studied by advanced transmission electron microscopy

PubMed Central

Agati, Marta; Amiard, Guillaume; Borgne, Vincent Le; Castrucci, Paola; Dolbec, Richard; De Crescenzi, Maurizio; El Khakani, My Alì

2017-01-01

Scanning transmission electron microscopy (STEM) was successfully applied to the analysis of silicon nanowires (SiNWs) that were self-assembled during an inductively coupled plasma (ICP) process. The ICP-synthesized SiNWs were found to present a Si–SiO2 core–shell structure and length varying from ≈100 nm to 2–3 μm. The shorter SiNWs (maximum length ≈300 nm) were generally found to possess a nanoparticle at their tip. STEM energy dispersive X-ray (EDX) spectroscopy combined with electron tomography performed on these nanostructures revealed that they contain iron, clearly demonstrating that the short ICP-synthesized SiNWs grew via an iron-catalyzed vapor–liquid–solid (VLS) mechanism within the plasma reactor. Both the STEM tomography and STEM-EDX analysis contributed to gain further insight into the self-assembly process. In the long-term, this approach might be used to optimize the synthesis of VLS-grown SiNWs via ICP as a competitive technique to the well-established bottom-up approaches used for the production of thin SiNWs. PMID:28326234

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.

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.

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.

Mechanism of Action of TiF4 on Dental Enamel Surface: SEM/EDX, KOH-Soluble F, and X-Ray Diffraction Analysis.

PubMed

Comar, Lívia P; Souza, Beatriz M; Al-Ahj, Luana P; Martins, Jessica; Grizzo, Larissa T; Piasentim, Isabelle S; Rios, Daniela; Buzalaf, Marília Afonso Rabelo; Magalhães, Ana Carolina

2017-10-12

This in vitro study aimed to evaluate the action of TiF4 on sound and carious bovine and human enamel. Sound (S) and pre-demineralised (DE) bovine and human (primary and permanent) enamel samples were treated with TiF4 (pH 1.0) or NaF varnishes (pH 5.0), containing 0.95, 1.95, or 2.45% F for 12 h. The enamel surfaces were analysed using SEM-EDX (scanning electron microscopy/energy-dispersive X-ray spectroscopy) (n = 10, 5 S and 5 DE) and KOH-soluble fluoride was quantified (n = 20, 10 S and 10 DE). Hydroxyapatite powder produced by precipitation method was treated with the corresponding fluoride solutions for 1 min (n = 2). The formed compounds were detected using X-ray diffraction (XRD). All TiF4 varnishes produced a coating layer rich in Ti and F on all types of enamel surface, with micro-cracks in its extension. TiF4 (1.95 and 2.45% F) provided higher fluoride deposition than NaF, especially for bovine enamel (p < 0.0001). It also induced a higher fluoride deposition on DE samples compared to S samples (p < 0.0001), except for primary enamel. The Ti content was higher for bovine and human primary enamel than human permanent enamel, with some differences between S and DE. The XRD analysis showed that TiF4 induced the formation of new compounds such as CaF2, TiO2, and Ti(HPO4)2·H2O. In conclusion, TiF4 (>0.95% F) interacts better, when compared to NaF, with bovine and human primary enamel than with human permanent enamel. TiF4 provoked higher F deposition compared to NaF. Carious enamel showed higher F uptake than sound enamel by TiF4 application, while Ti uptake was dependent on the enamel condition and origin. © 2017 S. Karger AG, Basel.

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.

Synthesis and spectral characterization of Zn(II) microsphere series for antimicrobial application

NASA Astrophysics Data System (ADS)

Singh, Ajay K.; Pandey, Sarvesh K.; Pandey, O. P.; Sengupta, S. K.

2014-09-01

Microsphere series have been synthesized by reacting zinc(II) acetate dihydrate with Schiff bases derived from 2-hydrazino-5-[substituted phenyl]-1,3,4-thiadiazole/oxadiazole/triazole with salicylaldehyde. Elemental analysis suggests that the complexes have 1:2 and 1:1 stoichiometry of the type [Zn(L)2(H2O)2] and [Zn(L‧)(H2O)2]; LH = Schiff bases derived from 2-hydrazino-5-[substituted phenyl]-1,3,4-thia/oxadiazole with salicylaldehyde; L‧H2 = Schiff bases derived from 3-(substituted phenyl)-4-amino-5-hydrazino-1,2,4-triazole and salicylaldehyde and were characterized by elemental analyses, IR, 1H NMR and 13C NMR spectral data. Scanning electron microscopy (SEM) showed that synthesized materials have microsphere like structure and there EDX analysis comparably matches with elemental analysis. For the antimicrobial application Schiff bases and their zinc(II) complexes were screened for four bacteria e.g. Bacillus subtilis, Pseudomonas aeruginosa, Salmonella typhi, Streptococcus pyogenes and four fungi e.g. Cyrtomium falcatum, Aspergillus niger, Fusarium oxysporium and Curvularia pallescence by the reported method. Schiff base and Zn(II) compounds showed significant antimicrobial activities. However, activities increase upon chelation. Thermal analysis (TGA) data of compound (10) showed its stability up to 300 °C.

Surface Coating of Gypsum-Based Molds for Maxillofacial Prosthetic Silicone Elastomeric Material: The Surface Topography.

PubMed

Khalaf, Salah; Ariffin, Zaihan; Husein, Adam; Reza, Fazal

2015-07-01

This study aimed to compare the surface roughness of maxillofacial silicone elastomers fabricated in noncoated and coated gypsum materials. This study was also conducted to characterize the silicone elastomer specimens after surfaces were modified. A gypsum mold was coated with clear acrylic spray. The coated mold was then used to produce modified silicone experimental specimens (n = 35). The surface roughness of the modified silicone elastomers was compared with that of the control specimens, which were prepared by conventional flasking methods (n = 35). An atomic force microscope (AFM) was used for surface roughness measurement of silicone elastomer (unmodified and modified), and a scanning electron microscope (SEM) was used to evaluate the topographic conditions of coated and noncoated gypsum and silicone elastomer specimens (unmodified and modified) groups. After the gypsum molds were characterized, the fabricated silicone elastomers molded on noncoated and coated gypsum materials were evaluated further. Energy-dispersive X-ray spectroscopy (EDX) analysis of gypsum materials (noncoated and coated) and silicone elastomer specimens (unmodified and modified) was performed to evaluate the elemental changes after coating was conducted. Independent t test was used to analyze the differences in the surface roughness of unmodified and modified silicone at a significance level of p < 0.05. Roughness was significantly reduced in the silicone elastomers processed against coated gypsum materials (p < 0.001). The AFM and SEM analysis results showed evident differences in surface smoothness. EDX data further revealed the presence of the desired chemical components on the surface layer of unmodified and modified silicone elastomers. Silicone elastomers with lower surface roughness of maxillofacial prostheses can be obtained simply by coating a gypsum mold. © 2014 by the American College of Prosthodontists.

Characterization of a new TiF(4) and β-cyclodextrin inclusion complex and its in vitro evaluation on inhibiting enamel demineralization.

PubMed

Nassur, Camila; Alexandria, Adílis Kalina; Pomarico, Luciana; de Sousa, Valeria Pereira; Cabral, Lúcio Mendes; Maia, Lucianne Cople

2013-03-01

Titanium tetrafluoride (TiF(4)) is an effective but instable caries preventive agent. As the stability problems could be minimized through the use of drug carriers this study aimed to prepare and characterize a new TiF(4) nanoinclusion complex and to evaluate its potential in inhibiting enamel demineralization under pH cycling conditions. The TiF(4) nanosystems were prepared using β-cyclodextrin (βCD) and sodium montmorillonite (MMTNa). Bovine enamel blocks (n=48) with known surface microhardness (SMH), were randomly assigned to 4 groups (n=12) and submitted to one of the following treatments: distilled deionized water (as negative control) and solutions containing 1% βCD, 1% TiF(4) and TiF(4):βCD. The solutions were blinded applied once on the blocks with a microbrush(®) on the surface for 1min before pH-cycling. After that, samples were reavaluated by SMH, %SMH loss, cross-sectional microhardness (CSMH), scanning electron microscope (SEM) and energy dispersive spectrometry (EDX). The inclusion complex of TiF(4):βCD offered better protection against demineralization in the subsurface. The SEM analysis showed that TiF(4) and TiF(4):βCD samples presented the most intact enamel than the control. The EDX analysis identified titanium in TiF(4) and TiF(4):βCD groups. TiF(4):βCD has higher potential on inhibiting demineralization in the inner enamel. TiF(4):βCD is a new alternative to TiF(4) stabilization in order to reduce enamel subsurface demineralization. Copyright © 2012 Elsevier Ltd. 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.

Extreme Pressure Synergistic Mechanism of Bismuth Naphthenate and Sulfurized Isobutene Additives

NASA Astrophysics Data System (ADS)

Xu, Xin; Hu, Jianqiang; Yang, Shizhao; Xie, Feng; Guo, Li

A four-ball tester was used to evaluate the tribological performances of bismuth naphthenate (BiNap), sulfurized isobutene (VSB), and their combinations. The results show that the antiwear properties of BiNap and VSB are not very visible, but they possess good extreme pressure (EP) properties, particularly sulfur containing bismuth additives. Synergistic EP properties of BiNap with various sulfur-containing additives were investigated. The results indicate that BiNap exhibits good EP synergism with sulfur-containing additives. The surface analytical tools, such as X-ray photoelectron spectrometer (XPS) scanning electron microscope (SEM) and energy dispersive X-ray (EDX), were used to investigate the topography, composition contents, and depth profile of some typical elements on the rubbing surface. Smooth topography of wear scar further confirms that the additive showed good EP capacities, and XPS and EDX analyzes indicate that tribochemical mixed protective films composed of bismuth, bismuth oxides, sulfides, and sulfates are formed on the rubbing surface, which improves the tribological properties of lubricants. In particular, a large number of bismuth atoms and bismuth sulfides play an important role in improving the EP properties of oils.

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.

Rapid oxidation of sulfide mine tailings by reaction with potassium ferrate.

PubMed

Murshed, Mohamed; Rockstraw, David A; Hanson, Adrian T; Johnson, Michael

2003-01-01

The chemistry of sulfide mine tailings treated with potassium ferrate (K2FeO4) in aqueous slurry has been investigated. The reaction system is believed to parallel a geochemical oxidation in which ferrate ion replaces oxygen. This chemical system utilized in a pipeline (as a plug flow reactor) may have application eliminating the potential for tailings to leach acid while recovering the metal from the tailings. Elemental analyses were performed using an ICP spectrometer for the aqueous phase extract of the treated tailings; and an SEM-EDX for the tailing solids. Solids were analyzed before and after treatments were applied. ICP shows that as the mass ratio of ferrate ion to tailings increases, the concentration of metals in the extract solution increases; while EDX indicates a corresponding decrease in sulfur content of the tailing solids. The extraction of metal and reduction in sulfide content is significant. The kinetic timeframe is on the order of minutes.

RNi2B2C (R = Ho, Dy, Tb and Pr) single crystals grown by the cold copper crucible method

NASA Astrophysics Data System (ADS)

Durán, A.; Munoz, E.; Bernès, S.; Escudero, R.

2000-08-01

Single crystals of RNi2B2C (R = Ho, Dy, Tb, Pr) have been grown on cold copper crucibles in a high-frequency induction furnace. As a result, shiny metallic and brittle platelike single crystals were obtained. They were examined by x-ray and scanning electron microscopy with WDX/EDX for local composition analysis and show a very good crystallographic structure and compositions. Resistivity and dc magnetic measurements were performed to study superconducting and magnetic properties. Besides known electronic properties of the RNi2B2C family, we report for the first time results for PrNi2B2C single crystals successfully obtained by this technique.

Development of a novel myconanomining approach for the recovery of agriculturally important elements from jarosite waste.

PubMed

Bedi, Ankita; Singh, Braj Raj; Deshmukh, Sunil K; Aggarwal, Nisha; Barrow, Colin J; Adholeya, Alok

2018-05-01

In this study, an ecofriendly and economically viable waste management approach have been attempted towards the biosynthesis of agriculturally important nanoparticles from jarosite waste. Aspergillus terreus strain J4 isolated from jarosite (waste from Debari Zinc Smelter, Udaipur, India), showed good leaching efficiency along with nanoparticles (NPs) formation under ambient conditions. Fourier-transform infrared spectroscopy (FT-IR) and transmission electron microscopy (TEM) confirmed the formation of NPs. Energy dispersive X-ray spectroscopy (EDX analysis) showed strong signals for zinc, iron, calcium and magnesium, with these materials being leached out. TEM analysis and high resolution transmission electron microscopy (HRTEM) showed semi-quasi spherical particles having average size of 10-50nm. Thus, a novel biomethodology was developed using fungal cell-free extract for bioleaching and subsequently nanoconversion of the waste materials into nanostructured form. These biosynthesized nanoparticles were tested for their efficacy on seed emergence activity of wheat (Triticum aestivum) seeds and showed enhanced growth at concentration of 20ppm. These nanomaterials are expected to enhance plant growth properties and being targeted as additives in soil fertility and crop productivity enhancement. Copyright © 2017. Published by Elsevier B.V.

A potential cause for kidney stone formation during space flights: enhanced growth of nanobacteria in microgravity

NASA Technical Reports Server (NTRS)

Ciftcioglu, Neva; Haddad, Ruwaida S.; Golden, D. C.; Morrison, Dennis R.; McKay, David S.

2005-01-01

BACKGROUND: Although some information is available regarding the cellular/molecular changes in immune system exposed to microgravity, little is known about the reasons of the increase in the kidney stone formation in astronauts during and/or after long duration missions at zero gravity (0 g). In our earlier studies, we have assessed a unique agent, nanobacteria (NB), in kidney stones and hypothesized that NB have an active role in calcium phosphate-carbonate deposition in kidney. In this research we studied effect of microgravity on multiplication and calcification of NB in vitro. METHODS: We examined NB cultures in High Aspect Rotating Vessels (HARVs) designed at the NASA's Johnson Space Center, which are designed to stimulate some aspects of microgravity. Multiplication rate and calcium phosphate composition of those NB were compared with NB cultured on stationary and shaker flasks. Collected aliquots of the cultures from different incubation periods were analyzed using spectrophotometer, SEM, TEM, EDX, and x-ray diffraction techniques. RESULTS: The results showed that NB multiplied 4.6x faster in HARVs compared to stationary cultures, and 3.2x faster than shaker flask conditions. X-ray diffraction and EDX analysis showed that the degree of apatite crystal formation and the properties of the apatite depend on the specific culture conditions used. CONCLUSION: We now report an increased multiplication rate of NB in microgravity-simulated conditions. Thus, NB infection may have a potential role in kidney stone formation in crew members during space flights. For further proof to this hypothesis, screening of the NB antigen and antibody level in flight crew before and after flight would be necessary.

Characterization of U/Pu Particles Originating From the Nuclear Weapon Accidents at Palomares, Spain, 1966 And Thule, Greenland, 1968

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

Lind, O.C.; Salbu, B.; Janssens, K.

2007-07-10

Following the USAF B-52 bomber accidents at Palomares, Spain in 1966 and at Thule, Greenland in 1968, radioactive particles containing uranium (U) and plutonium (Pu) were dispersed into the environment. To improve long-term environmental impact assessments for the contaminated ecosystems, particles from the two sites have been isolated and characterized with respect to properties influencing particle weathering rates. Low [239]Pu/[235]U (0.62-0.78) and [240]Pu/[239]Pu (0.055-0.061) atom ratios in individual particles from both sites obtained by Inductively Coupled Plasma Mass Spectrometry (ICP-MS) show that the particles contain highly enriched U and weapon-grade Pu. Furthermore, results from electron microscopy with Energy Dispersive X-raymore » analysis (EDX) and synchrotron radiation (SR) based micrometer-scale X-ray fluorescence ({micro}-XRF) 2D mapping demonstrated that U and Pu coexist throughout the 1-50 {micro}m sized particles, while surface heterogeneities were observed in EDX line scans. SR-based micrometer-scale X-ray Absorption Near Edge Structure Spectroscopy ({micro}-XANES) showed that the particles consisted of an oxide mixture of U (predominately UO[2] with the presence ofU[3][8]) and Pu ((III)/(IV), (V)/(V) or (III), (IV) and (V)). Neither metallic U or Pu nor uranyl or Pu(VI) could be observed. Characteristics such as elemental distributions, morphology and oxidation states are remarkably similar for the Palomares and Thule particles, reflecting that they originate from similar source and release scenarios. Thus, these particle characteristics are more dependent on the original material from which the particles are derived (source) and the formation of particles (release scenario) than the environmental conditions to which the particles have been exposed since the late 1960s.« less

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

Chemical imaging of ambient aerosol particles: Observational constraints on mixing state parameterization

DOE PAGES

O'Brien, Rachel E.; Wang, Bingbing; Laskin, Alexander; ...

2015-08-26

In this study, a new parameterization for quantifying the mixing state of aerosol populations has been applied for the first time to samples of ambient particles analyzed using spectro-microscopy techniques. Scanning transmission X-ray microscopy/near edge X-ray absorption fine structure (STXM/NEXAFS) and computer-controlled scanning electron microscopy/energy dispersive X-ray spectroscopy (CCSEM/EDX) were used to probe the composition of the organic and inorganic fraction of individual particles collected on 27 and 28 June during the 2010 Carbonaceous Aerosols and Radiative Effects study in the Central Valley, California. The first field site, T0, was located in downtown Sacramento, while T1 was located near themore » Sierra Nevada Mountains. Mass estimates of the aerosol particle components were used to calculate mixing state metrics, such as the particle-specific diversity, bulk population diversity, and mixing state index, for each sample. The STXM data showed evidence of changes in the mixing state associated with a buildup of organic matter confirmed by collocated measurements, and the largest impact on the mixing state was due to an increase in soot dominant particles during this buildup. The mixing state from STXM was similar between T0 and T1, indicating that the increased organic fraction at T1 had a small effect on the mixing state of the population. The CCSEM/EDX analysis showed the presence of two types of particle populations: the first was dominated by aged sea-salt particles and had a higher mixing state index (indicating a more homogeneous population); the second was dominated by carbonaceous particles and had a lower mixing state index.« less

The role of extracellular DNA in uranium precipitation and biomineralisation.

PubMed

Hufton, Joseph; Harding, John H; Romero-González, Maria E

2016-10-26

Bacterial extra polymeric substances (EPS) have been associated with the extracellular precipitation of uranium. Here we report findings on the biomineralisation of uranium, with extracellular DNA (eDNA) used as a model biomolecule representative of EPS. The complexation and precipitation of eDNA with uranium were investigated as a function of pH, ionic strength and varying concentrations of reactants. The role of phosphate moieties in the biomineralisation mechanism was studied by enzymatically releasing phosphate (ePO 4 ) from eDNA compared to abiotic phosphate (aPO 4 ). The eDNA-uranium precipitates and uranium minerals obtained were characterised by Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FT-IR) spectroscopy, Scanning Electron Microscopy-Energy Dispersive X-Ray analysis (SEM-EDX), X-Ray Powder Diffraction (XRD) and X-Ray Photoelectron Spectroscopy (XPS). ATR-FT-IR showed that at pH 5, the eDNA-uranium precipitation mechanism was predominantly mediated by interactions with phosphate moieties from eDNA. At pH 2, the uranium interactions with eDNA occur mainly through phosphate. The solubility equilibrium was dependent on pH with the formation of precipitate reduced as the pH increased. The XRD data confirmed the formation of a uranium phosphate precipitate when synthesised using ePO 4 . XPS and SEM-EDX studies showed the incorporation of carbon and nitrogen groups from the enzymatic orthophosphate hydrolysis on the obtained precipitated. These results suggested that the removal of uranium from solution occurs via two mechanisms: complexation by eDNA molecules and precipitation of a uranium phosphate mineral of the type (UO 2 HPO 4 )·xH 2 O by enzymatic orthophosphate hydrolysis. This demonstrated that eDNA from bacterial EPS is a key contributor to uranium biomineralisation.

Biocompatibility of MgF2-coated MgNd2 specimens in contact with mucosa of the nasal sinus - a long term study.

PubMed

Weber, Constantin M; Eifler, Rainer; Seitz, Jan-Marten; Maier, Hans J; Reifenrath, Janin; Lenarz, Thomas; Durisin, Martin

2015-05-01

Up to now, different surgical techniques and stent systems have already been developed and tested for the continuous and adequate ventilation of the frontal sinuses. However, the results achieved still remain poor. Magnesium-based implants have been successfully used in numerous clinical applications. Offering excellent biocompatibility and biodegradability it may be the ideal material for the development of novel implants of the nasal sinus. Here, we present for the first time results on the behaviour of magnesium alloy in a unique environment, i.e. in contact to the nasal mucosa, air and nasal secretion. In a prospective longitudinal study, magnesium fluoride-coated MgNd2 specimens were implanted in the frontal sinuses of 12 minipigs for the investigation of biocompatibility and of the interface between the implant and the mucosa. Endoscopic examinations, histopathological evaluation and EDX measurements were performed regularly up to 180days. Endoscopic evaluation showed focal mucosal reaction, however, without affecting the patency of the sinus. In addition, no signs of bacterial infections were observed. The EDX analyses showed a marginal but steady increase in the Mg concentration in the mucosa over 180days. Histological analysis revealed a locally confined moderate mucosal hyperplasia and unspecific inflammatory reaction. Furthermore, we did not find any osteoinductive effects of the magnesium alloy. The results indicate the excellent biocompatibility of the MgNd2 alloy in contact with nasal mucosa and provide a novel material compound and solid proof-of-principle for the development of magnesium-based nasal stents. Copyright © 2015 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Oxidation behavior of a ferritic stainless steel Crofer22 APU with thermal cycling

NASA Astrophysics Data System (ADS)

Song, MyoungYoup; Duong, Anh T.; Mumm, Daniel R.

2013-01-01

Crofer22 APU specimens were prepared by grinding with grit 80 and 120 SiC grinding papers and were thermally cycled. The variation in oxidation behavior with thermal cycling was then investigated. Observation of microstructure, measurement of area specific resistance (ASR), analysis of the atomic percentages of the elements by EDX, and XRD analysis were performed. XRD patterns showed that the (Cr, Mn)3O4 spinel phase grew on the surface of the Crofer22 APU samples ground with grit 120. For the samples ground with grit 80, the ASR increased as the number of thermal cycles increased. Plots of ln (ASR/T) vs. 1/T for the samples ground with grit 80 after n = 4, 20 and 40 exhibited good linearity, and the apparent activation energies were between 63.7 kJ/mole and 76.3 kJ/mole.

Variation with thermal cycling in microstructure and area specific resistance of a ferritic stainless steel having rough surfaces

NASA Astrophysics Data System (ADS)

Song, Myoung Youp; Mumm, Daniel R.; Song, Jiunn

2013-03-01

Crofer22 APU specimens were prepared by grinding with grit 120 and 400 SiC grinding papers, and were then thermally cycled. The variation in oxidation behavior with thermal cycling was then investigated. Observation of microstructures, measurement of area-specific resistance (ASR), analysis of the atomic percentages of the elements by EDX, and XRD analysis were performed. XRD patterns showed that the (Cr, Mn)3O4 spinel phase grew on the surface of the Crofer22 APU samples ground using grit 120. For the samples ground with grit 400, ASR increased as the number of thermal cycles ( n) increased. Plots of ln (ASR/T) vs. 1/ T for the samples ground with grit 400 after n = 4, 20, and 40 exhibited good linearity, and the apparent activation energies were between 73.4 kJ/mole and 82.5 kJ/mole.

Experimental analysis of energy absorption behaviour of Al-tube filled with pumice lightweight concrete under axial loading condition

NASA Astrophysics Data System (ADS)

Rajak, D. K.; Deshpande, P. G.; Kumaraswamidhas, L. A.

2017-08-01

This Paper aimed at experimental investigation of compressive behaviour of square tube filled with pumice lightweight concrete (PLC). Square section of 20×20×30 mm is investigated, which is the backbone structure. The compression deformation result shows the better folding mechanism, displacement value, and energy absorption. PLC concrete filled with aluminium thin-wall tubes has been revealed superior energy absorption capacity (EAC) under low strain rate at room temperature. Superior EAC resulted as a result of mutual deformation benefit between aluminium section and PLC is also analysed. PLC was characterised by Fourier Transform Infrared (FTIR) and Field Emission Scanning Electron Microscopy (FESEM), and Energy Dispersive X-ray Spectrometry (EDX) analysis for better understanding of material behaviour. Individual and comparative load bearing graphs is logged for better prospective of analysing. Novel approach aimed at validation of porous lightweight concrete for better lightweight EA filler material.

Functionalization of SBA-15 mesoporous silica by Cu-phosphonate units: Probing of synthesis route

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

Laskowski, Lukasz, E-mail: lukasz.laskowski@kik.pcz.pl; Czestochowa University of Technology, Institute of Physics, Al. Armii Krajowej 19, 42-201 Czestochowa; Laskowska, Magdalena, E-mail: magdalena.laskowska@onet.pl

2014-12-15

Mesoporous silica SBA-15 containing propyl-copper phosphonate units was investigated. The structure of mesoporous samples was tested by N{sub 2} isothermal sorption (BET and BHJ analysis), TEM microscopy and X-Ray scattering. Quantitative analysis EDX has given information about proportions between component atoms in the sample. Quantitative elemental analysis has been carried out to support EDX. To examine bounding between copper atoms and phosphonic units the Raman spectroscopy was carried out. As a support of Raman scattering, the theoretical calculations were made based on density functional theory, with the B3LYP method. By comparison of the calculated vibrational spectra of the molecule withmore » experimental results, distribution of the active units inside silica matrix has been determined. - Graphical abstract: The present study is devoted to mesoporous silica SBA-15 containing propyl-copper phosphonate units. The species were investigated to confirm of synthesis procedure correctness by the micro-Raman technique combined with DFT numerical simulations. Complementary research was carried out to test the structure of mesoporous samples. - Highlights: • SBA-15 silica functionalized with propyl-copper phosphonate units was synthesized. • Synthesis efficiency probed by Raman study supported with DFT simulations. • Homogenous distribution of active units was proved. • Synthesis route enables precise control of distance between copper ions.« less

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.

Recycling of pneumatic scrap tyre into nano-crumb rubber by pulsed laser ablation in different pH media

NASA Astrophysics Data System (ADS)

Ezaan Khamsan, Nur; Bidin, Noriah; Islam, Shumaila; Daud, Suzairi; Krishnan, Ganesan; Bakar, Mohamad Aizat A.; Naqiuddin Razali, Muhamad; Khamis, Jamil

2018-05-01

Nano crumb rubber from scrap tyre is synthesized via 1064 nm pulsed Nd:YAG laser ablation in three different pH media i.e. DI-water (pH∼6.45), D-limonene (pH∼3.47) and NaOH solution (pH∼13.41). Field Emission Scanning Electron Microscope (FESEM) results show spherical morphology of crumb rubber with high degree of aggregation in DI-water and in D-limonene. However, dispersion of crumb rubbers is observed in NaOH solution. The smallest particles size is obtained in NaOH solution within the range of 10.9 nm – 74.3 nm. Energy-dispersive X-ray spectroscopy (EDX) and FTIR analysis confirmed the elements distribution and chemical bonding of rubber with DI-water, D-limonene and NaOH solution. The experimental findings shows that pulsed Nd:YAG laser ablation has potential for fabricating nano-crumb rubber in liquid media.

Comparison of 2-limb versus 3-limb electrodiagnostic studies in the evaluation of chronic inflammatory demyelinating polyneuropathy.

PubMed

Vo, Mary L; Hanineva, Aneliya; Chin, Russell L; Carey, Bridget T; Latov, Norman; Langsdorf, Jennifer A

2015-04-01

European Federation of Neurological Societies/Peripheral Nerve Society electrodiagnostic (EDx) criteria for the definite diagnosis of chronic inflammatory demyelinating polyneuropathy (CIDP) require the presence of demyelinating findings (DF) in at least 2 nerves. Data are lacking, however, regarding the optimal number of nerves to test. We retrospectively reviewed EDx data from 53 patients with CIDP and compared the number of DF found on 2- and 3-limb testing. A median of 3 (range 2-5) DF were found on 2-limb testing compared with 5 (range 4-7) DF when 3 limbs were evaluated. Two-limb EDx studies were sufficient to diagnose definite CIDP in 92.3% of typical, 84.2% of asymmetric, and 66.7% of distal phenotypes. Testing a third limb increased diagnostic certainty in 11 patients (20.8%) to definite CIDP. Three-limb testing may increase diagnostic sensitivity of definite CIDP, especially in patients with atypical phenotypes. Larger prospective studies are needed to better assess the benefit of performing 3-limb EDx studies. © 2014 Wiley Periodicals, Inc.

Characterisation of gunshot residue from three ammunition types using suppressed anion exchange chromatography.

PubMed

Gilchrist, Elizabeth; Jongekrijg, Fleur; Harvey, Laura; Smith, Norman; Barron, Leon

2012-09-10

Gunshot residue (GSR) is commonly analysed in forensic casework using either scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX) or gas chromatography-mass spectrometry (GC-MS). Relatively little work has been reported on the post-discharge GSR content of non-metallic inorganic or low molecular weight organic anions to distinguish between different ammunition types. The development of an analytical method using suppressed micro-bore anion exchange chromatography (IC) is presented for the analysis of GSR. A hydroxide gradient was optimised for the separation of 19 forensically relevant organic and inorganic anions in <23min and sensitivities of the order of 0.12-3.52ng of anion detected for all species were achieved. Along with an optimised extraction procedure, this method was applied to the analysis of post-ignition residues from three selected ammunition types. By profiling and comparing the anionic content in each ammunition residue, the possibility to distinguish between each type using their anionic profiles and absolute weight is presented. The potential for interference is also discussed with respect to sample types which are typically problematic in the analysis of GSR using SEM-EDX and GC-MS. To the best of our knowledge this represents the first study on the analysis of inorganic anions in GSR using suppressed ion chromatography. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

Working Smarter Not Harder - Developing a Virtual Subsurface Data Framework for U.S. Energy R&D

NASA Astrophysics Data System (ADS)

Rose, K.; Baker, D.; Bauer, J.; Dehlin, M.; Jones, T. J.; Rowan, C.

2017-12-01

The data revolution has resulted in a proliferation of resources that span beyond commercial and social networking domains. Research, scientific, and engineering data resources, including subsurface characterization, modeling, and analytical datasets, are increasingly available through online portals, warehouses, and systems. Data for subsurface systems is still challenging to access, discontinuous, and varies in resolution. However, with the proliferation of online data there are significant opportunities to advance access and knowledge of subsurface systems. The Energy Data eXchange (EDX) is an online platform designed to address research data needs by improving access to energy R&D products through advanced search capabilities. In addition, EDX hosts private, virtualized computational workspaces in support of multi-organizational R&D. These collaborative workspaces allow teams to share working data resources and connect to a growing number of analytical tools to support research efforts. One recent application, a team digital data notebook tool, called DataBook, was introduced within EDX workspaces to allow teams to capture contextual and structured data resources. Starting with DOE's subsurface R&D community, the EDX team has been developing DataBook to support scientists and engineers working on subsurface energy research, allowing them to contribute and curate both structured and unstructured data and knowledge about subsurface systems. These resources span petrophysical, geologic, engineering, geophysical, interpretations, models, and analyses associated with carbon storage, water, oil, gas, geothermal, induced seismicity and other subsurface systems to support the development of a virtual subsurface data framework. The integration of EDX and DataBook allows for these systems to leverage each other's best features, such as the ability to interact with other systems (Earthcube, OpenEI.net, NGDS, etc.) and leverage custom machine learning algorithms and capabilities to enhance user experience, make access and connection to relevant subsurface data resources more efficient for research teams to use, analyze and draw insights. Ultimately, the public and private resources in EDX seek to make subsurface energy research more efficient, reduce redundancy, and drive innovation.

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.

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.

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

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.

Assessment of annual air pollution levels with PM1, PM2.5, PM10 and associated heavy metals in Algiers, Algeria.

PubMed

Talbi, Abdelhamid; Kerchich, Yacine; Kerbachi, Rabah; Boughedaoui, Ménouèr

2018-01-01

Concentrations of particulate matter less than 1  μm, 2.5  μm, 10 μm and their contents of heavy metals were investigated in two different stations, urban and roadside at Algiers (Algeria). Sampling was conducted during two years by a high volume samplers (HVS) equipped with a cascade impactor at four levels stage, for one year sampling. The characterization of the heavy metals associated to the particulate matter (PM) was carried out by X-Ray Fluorescence analysis (XRF). The annual average concentration of PM 1 , PM 2.5 and PM 10 in both stations were 18.24, 32.23 and 60.01 μg m -3 respectively. The PM 1 , PM 2.5 and PM 10 concentrations in roadside varied from 13.46 to 25.59 μg m -3 , 20.82-49.85 μg m -3 and 45.90-77.23 μg m -3 respectively. However in the urban station, the PM 1 , PM 2.5 and PM 10 concentrations varied from 10.45 to 26.24 μg m -3 , 18.53-47.58 μg m -3 and 43.8-91.62 μg m -3 . The heavy metals associated to the PM were confirmed by Scanning Electron Microscopy-Energy Dispersive X-Ray analyses (SEM-EDX). The different spots of PM 2.5 analysis by SEM-EDX shows the presence of nineteen elements with anthropogenic and natural origins, within the heavy metal detected, the lead was found with maximum of 5% (weight percent). In order to determine the source contributions of PM levels at the two sampling sites sampling, principal compound analysis (PCA) was applied to the collected data. Statistical analysis confirmed anthropogenic source with traffic being a significant source and high contribution of natural emissions. At both sites, the PM 2.5 /PM 10 ratio is lower than that usually recorded in developed countries. The study of the back-trajectories of the air masses starting from Sahara shows that desert dust influences the concentration and the composition of the PM measured in Algiers. Copyright © 2017 Elsevier Ltd. All rights reserved.

5 Ways That edX Could Change Education

ERIC Educational Resources Information Center

Parry, Marc

2012-01-01

Since MIT and Harvard started edX, their joint experiment with free online courses, the venture has attracted enormous attention for opening the ivory tower to the world. But in the process, the world will become part of an expensive and ambitious experiment testing some of the most interesting--and difficult--questions in digital education. Can…

Hereditary motor and sensory neuropathy with proximal predominance (HMSN-P).

PubMed

Campellone, Joseph V

2013-06-01

Hereditary motor and sensory neuropathy with proximal predominance (HMSN-P) is a rare disorder inherited in an autosomal dominant fashion. Patients present with slowly progressive proximal-predominant weakness, painful muscle cramps, fasciculations, large-fiber sensory loss, and areflexia. Electrodiagnostic (EDX) studies typically reveal abnormalities consistent with a sensorimotor neuronopathy. A patient with HMSN-P underwent EDX studies, revealing ongoing and chronic neurogenic denervation, motor unit instability, and neuromyotonic discharges, further defining the spectrum of EDX findings in HMSN-P. The clinical, pathological, and genetic features are also reviewed. The appearance of HMSN-P in the United States and elsewhere calls for clinicians in nonendemic regions to be familiar with this rare disorder, which has typically been geographically confined.

A simple and low temperature process for super-hydrophilic rutile TiO 2 thin films growth

NASA Astrophysics Data System (ADS)

Mane, R. S.; Joo, Oh-Shim; Min, Sun-Ki; Lokhande, C. D.; Han, Sung-Hwan

2006-11-01

We investigate an environmentally friendly aqueous solution system for rutile TiO2 violet color nanocrystalline thin films growth on ITO substrate at room temperature. Film shows considerable absorption in visible region with excitonic maxima at 434 nm. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), selected area electron diffraction (SAED), UV-vis, water surface contact angle and energy dispersive X-ray analysis (EDX) techniques in addition to actual photo-image that shows purely rutile phase of TiO2 with violet color, super-hydrophilic and densely packed nanometer-sized spherical grains of approximate diameter 3.15 ± 0.4 nm, characterize the films. Band gap energy of 4.61 eV for direct transition was obtained for the rutile TiO2 films. Film surface shows super-hydrophilic behavior, as exhibited water contact angle was 7°. Strong visible absorption (not due to chlorine) leaves future challenge to use these films in extremely thin absorber (ETA) solar cells.

Valorization of titanium metal wastes as tanning agent used in leather industry.

PubMed

Crudu, Marian; Deselnicu, Viorica; Deselnicu, Dana Corina; Albu, Luminita

2014-10-01

The development of new tanning agents and new technologies in the leather sector is required to cope with the increasingly higher environmental pressure on the current tanning materials and processes such as tanning with chromium salts. In this paper, the use of titanium wastes (cuttings) resulting from the process of obtaining highly pure titanium (ingots), for the synthesis of new tanning agent and tanning bovine hides with new tanning agent, as alternative to tanning with chromium salts are investigated. For this purpose, Ti waste and Ti-based tanning agent were characterized for metal content by inductively coupled plasma mass spectrometry (ICP-MS) and chemical analysis; the tanned leather (wet white leather) was characterized by Scanning Electron Microscope/Energy Dispersive Using X-ray (Analysis). SEM/EDX analysis for metal content; Differential scanning calorimetric (DSC), Micro-Hot-Table and standard shrinkage temperature showing a hydrothermal stability (ranged from 75.3 to 77°C) and chemical analysis showing the leather is tanned and can be processed through the subsequent mechanical operations (splitting, shaving). On the other hand, an analysis of major minor trace substances from Ti-end waste (especially vanadium content) in new tanning agent and wet white leather (not detected) and residue stream was performed and showed that leachability of vanadium is acceptable. The results obtained show that new tanning agent obtained from Ti end waste can be used for tanning bovine hides, as eco-friendly alternative for chrome tanning. Copyright © 2014 Elsevier Ltd. All rights reserved.

Physicochemical and optical properties of combustion-generated particles from Ship Diesel Engines

NASA Astrophysics Data System (ADS)

Kim, H.; Jeong, S.; Jin, H. C.; Kim, J. Y.

2015-12-01

Shipping contributes significantly to the anthropogenic burden of particulate matter (PM), and is among the world's highest polluting combustion sources per fuel consumed. Moreover, ships are a highly concentrated source of pollutants which are emitted into clean marine environments (e.g., Artic region). Shipping utilizes heavy fuel oil (HFO) which is less distilled compared to fuels used on land and few investigations on shipping related PM properties are available. BC is one of the dominant combustion products of ship diesel engines and its chemical and microphysical properties have a significant impact on climate by influencing the amount of albedo reduction on bright surfaces such as in polar regions. We have carried out a campaign to characterize the PM emissions from medium-sized marine engines in Gunsan, Jeonbuk Institute of Automotive Technology. The properties of ship-diesel PM have characterized depending on (1) fuel sulfur content (HFO vs. ULSD) and (2) engine conditions (Running state vs. Idling state). Scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), energy-dispersive X-ray spectroscopy (EDX) equipped with HRTEM and Raman spectroscopy were used for physicochemical analysis. Optical properties, which are ultimately linked to the snow/ice albedo decrease impacting climate, were assessed as well. PM generated under high engine temperature conditions had typical features of soot, e.g., concentric circles comprised of closely packed graphene layers, however PM generated by the idling state at low combustion temperature was characterized by amorphous and droplet-like carbonaceous particles with no crystalline structure. Significant differences in optical properties depending on the combustion conditions were also observed. Particles from running conditions showed wavelength-independent absorbing properties, whereas the particles from idling conditions showed enhanced absorption at shorter wavelengths, which is characteristic of brown carbon. Regarding different fuel types, distinctive structure differences were not observed, but EDX results showed that PM generated by HFO combustion has sulfur content in PM whereas ULSD generated 100% carbon composed PM.

The activation of the G protein-coupled estrogen receptor (GPER) inhibits the proliferation of mouse melanoma K1735-M2 cells.

PubMed

Ribeiro, Mariana P C; Santos, Armanda E; Custódio, José B A

2017-11-01

The activation of the G protein-coupled estrogen receptor (GPER) by its specific agonist G-1 inhibits prostate cancer and 17β-estradiol-stimulated breast cancer cell proliferation. Tamoxifen (TAM), which also activates the GPER, decreases melanoma cell proliferation, but its action mechanism remains controversial. Here we investigated the expression and the effects of GPER activation by G-1, TAM and its key metabolite endoxifen (EDX) on melanoma cells. Mouse melanoma K1735-M2 cells expressed GPER and G-1 reduced cell biomass, and the number of viable cells, without increasing cell death. Rather, G-1 decreased cell division by blocking cell cycle progression in G2. Likewise, TAM and EDX exhibited an antiproliferative activity in melanoma cells due to decreased cell division. Both G-1 and the antiestrogens showed a trend to decrease the levels of phosphorylated ERK 1/2 after 1 h treatment, although only EDX, the most potent antiproliferative antiestrogen, induced significant effects. Importantly, the targeting of GPER with siRNA abolished the cytostatic activity of both G-1 and antiestrogens, suggesting that the antitumor actions of antiestrogens in melanoma cells involve GPER activation. Our results unveil a new target for melanoma therapy and identify GPER as a key mediator of antiestrogen antiproliferative effects, which may contribute to select the patients that benefit from an antiestrogen-containing regimen. Copyright © 2017 Elsevier B.V. All rights reserved.

Exciting transition metal doped dilute magnetic thin films: MgO:Er and ZnO:Er

NASA Astrophysics Data System (ADS)

Ćakıcı, T.; Sarıtaş, S.; Muǧlu, G. Merhan; Yıldırım, M.

2017-02-01

Erbium doped MgO and doped ZnO thin films have reasonably important properties applications in spintronic devices. These films were synthesized on glass substrates by Chemical Spray Pyrolysis (CSP) method. In the literature there has been almost no report on preparation of MgO:Er dilute magnetic thin films by means of CSP. Because doped thin films show different magnetic behaviors, depending upon the type of magnetic material ions, concentration of them, synthesis route and experimental conditions, synthesized MgO:Er and ZnO:Er films were compared to thin film properties. Optical analyses of the synthesized thin films were examined spectral absorption and transmittance measurements by UV-Vis double beam spectrophotometer technique. Structural analysis of the thin films was examined by using XRD, Raman Analysis, FE-SEM, EDX and AFM techniques. Also, magnetic properties of the MgO:Er and ZnO:Er films were investigated by vibrating sample magnetometer (VSM) which show that diamagnetic behavior of the MgO:Er thin film and ferromagnetic (FM) behavior of the ZnO:Er film were is formed.

Microstructural and optical properties of CdS nanoparticles synthesized by sol gel method

NASA Astrophysics Data System (ADS)

Mahdi, Hadeel Salih; Parveen, Azra; Agrawal, Shraddha; Azam, Ameer

2018-05-01

Semiconductor nanoparticles of CdS are of great interest for both fundamental research and industrial development due to their unique size-dependent optical and electronic properties and their exciting utilization in the fields of light-emitting diode, electro-chemical cells, laser, hydrogen producing catalyst, biological label. We present a scheme to measure the optical properties of CdS nanoparticles The peaks were indexed by powder-x software. The XRD pattern analysis showed that CdS composition was found to have hexagonal structure with well crystalline nature. the surface morphology and the composition of the samples were investigated by SEM (JEOL, japan). The image shows the presence of large spherical aggregates of smaller individual nanoparticles of various sizes for pure cds. to check the chemical composition of the material, energy dispersive X-ray (EDX) spectroscopic analysis was also performed which further confirmed the presence of cd and s ions in the matrix. The optical absorption spectra of CdS sample was recorded by uv-vis spectrophotometer in the range of 200 to 800 nm.

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.

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.

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.

Effect of Electron Beam Irradiation on Structural and Optical Properties of Cu-Doped In2O3 Films Prepared by RF Magnetron Sputtering

NASA Astrophysics Data System (ADS)

Krishnan, R. Reshmi; Sanjeev, Ganesh; Prabhu, Radhakrishna; Pillai, V. P. Mahadevan

2018-02-01

Undoped and Cu-doped In2O3 films were prepared by radiofrequency magnetron sputtering technique. The effects of Cu doping and high-energy electron beam irradiation on the structural and optical properties of as-prepared films were investigated using techniques such as x-ray diffraction, x-ray photoelectron spectroscopy (XPS), lateral scanning electron microscopic image analysis, energy-dispersive x-ray (EDX) spectroscopy, micro-Raman, and ultraviolet-visible (UV-vis) spectroscopy. Moderate doping of Cu in In2O3 enhanced the intensity of (222) peak, indicating alignment of crystalline grains along <111>. Electron beam irradiation promoted orientation of crystalline grains along <111> in undoped and moderately Cu-doped films. EDX spectroscopic and XPS analyses revealed incorporation of Cu2+ ions in the lattice. The transmittance of Cu-doped films decreased with e-beam irradiation. Systematic reduction of the bandgap energy with increase in Cu doping concentration was seen in unirradiated and electron-beam-irradiated films.

Czochralski growth of LaPd2Al2 single crystals

NASA Astrophysics Data System (ADS)

Doležal, P.; Rudajevová, A.; Vlášková, K.; Kriegner, D.; Václavová, K.; Prchal, J.; Javorský, P.

2017-10-01

The present study is focused on the preparation of single crystalline LaPd2Al2 by the Czochralski method. Differential scanning calorimetry (DSC) and energy dispersive X-ray spectroscopy (EDX) analyses reveal that LaPd2Al2 is an incongruently melting phase which causes difficulties for the preparation of single crystalline LaPd2Al2 by the Czochralski method. Therefore several non-stoichiometric polycrystalline samples were studied for its preparation. Finally the successful growth of LaPd2Al2 without foreign phases has been achieved by using a non-stoichiometric precursor with atomic composition 22:39:39 (La:Pd:Al). X-ray powder diffraction, EDX analysis and DSC were used for the characterisation. A single crystalline sample was separated from the ingot prepared by the Czochralski method using the non-stoichiometric precursor. The presented procedure for the preparation of pure single phase LaPd2Al2 could be modified for other incongruently melting phases.

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.

Characterization of Arsenic Contamination on Rust from Ton Containers

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

Gary S. Groenewold; Recep Avci; Robert V. Fox

The speciation and spatial distribution of arsenic on rusted steel surfaces affects both measurement and removal approaches. The chemistry of arsenic residing in the rust of ton containers that held the chemical warfare agents bis(2-chloroethyl)sulfide (sulfur mustard) and 2-chlorovinyldichloroarsine (Lewisite) is of particular interest, because while the agents have been decontaminated, residual arsenic could pose a health or environmental risk. The chemistry and distribution of arsenic in rust samples was probed using imaging secondary ion mass spectrometry (SIMS), X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy, and scanning electron microscopy/energy dispersive X-ray spectroscopy (SEM/EDX). Arsenic in the +3 and or +5more » oxidation state is homogeneously distributed at the very top-most layer of the rust samples, and is intimately associated with iron. Sputter depth profiling followed by SIMS and XPS shows As at a depth of several nm, in some cases in a reduced form. The SEM/EDX experiments show that As is present at a depth of several microns, but is inhomogeneously distributed; most locations contained oxidized As at concentrations of a few percent, however several locations showed very high As in a metallic form. These results indicate that the rust material must be removed if the steel containers are to be cleared of arsenic.« less

Study on Sumbawa gold recovery using centrifuge

NASA Astrophysics Data System (ADS)

Ferdana, A. D.; Petrus, H. T. B. M.; Bendiyasa, I. M.; Prijambada, I. D.; Hamada, F.; Sachiko, T.

2018-01-01

The Artisanal Small Gold Mining in Sumbawa has been processing gold with mercury (Hg), which poses a serious threat to the mining and global environment. One method of gold processing that does not use mercury is by gravity method. Before processing the ore first performed an analysis of Mineragraphy and analysis of compound with XRD. Mineragraphy results show that gold is associated with chalcopyrite and covelite and is a single particle (native) on size 58.8 μm, 117 μm up to 294 μm. characterization with XRD shows that the Sumbawa Gold Ore is composed of quartz, pyrite, pyroxene, and sericite compounds. Sentrifugation is one of separation equipment of gravity method to increase concentrate based on difference of specific gravity. The optimum concentration result is influenced by several variables, such as water flow rate and particle size. In this present research, the range of flow rate is 5 lpm and 10 lpm, the particle size - 100 + 200 mesh and -200 +300 mesh. Gold concentration in concentrate is measured by EDX. The result shows that the optimum condition is obtained at a separation with flow rate 5 lpm and a particle size of -100 + 200 mesh.

Corrosion Behavior of Ti60 Alloy under a Solid NaCl Deposit in Wet Oxygen Flow at 600 °C

PubMed Central

Fan, Lei; Liu, Li; Yu, Zhongfen; Cao, Min; Li, Ying; Wang, Fuhui

2016-01-01

The corrosion behavior of Ti60 alloy covered with a solid NaCl deposit in wet oxygen flow at 600 °C has been studied further by SEM, EDX, XPS, XRD, TEM and EPMA analysis. The results show that solid NaCl and H2O react with Ti oxides, which destroyed the Ti oxide scale to yield the non-protective Na4Ti5O12 and other volatile species. The resulting corrosion product scale was multilayered and contained abundant rapid diffusion channels leading to the fast diffusion which improved the corrosion rate. A possible mechanism has been proposed for the NaCl-covered Ti60 alloy, based on the experimental results. PMID:27357732

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.

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.

Preparation of Ag-loaded octahedral Bi2WO6 photocatalyst and its photocatalytic activity

NASA Astrophysics Data System (ADS)

An, Liang; Wang, Guanghui; Zhou, Xuan; Wang, Yi; Gao, Fang; Cheng, Yang

2014-12-01

In this work, an Ag-loaded octahedral Bi2WO6 photocatalyst has been successfully prepared by the hydrothermal method and photo deposition method. X-ray diffraction (XRD), energy dispersive analysis of X-ray (EDX), field-emission scanning electron microscopy (FE-SEM) and ultra-violet adsorption spectrum (UV-Vis) were employed for characterization of the composite photocatalyst. Furthermore, two different photocatalysts including the obtained Ag-loaded octahedral Bi2WO6 were employed here for photodegradation of model contaminated water of Orange II (OII). Results show that Ag-loaded Bi2WO6 photocatalyst exhibits superior photocatalytic properties compared to the undoped Bi2WO6. The reasons for improvement in photocatalytic activity of the Ag-loaded octahedral Bi2WO6 were also discussed.

Studying Learning in the Worldwide Classroom Research into edX's First MOOC

ERIC Educational Resources Information Center

Breslow, Lori; Pritchard, David E.; DeBoer, Jennifer; Stump, Glenda S.; Ho, Andrew D.; Seaton, Daniel T.

2013-01-01

"Circuits and Electronics" (6.002x), which began in March 2012, was the first MOOC developed by edX, the consortium led by MIT and Harvard. Over 155,000 students initially registered for 6.002x, which was composed of video lectures, interactive problems, online laboratories, and a discussion forum. As the course ended in June 2012,…

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

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.

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.

Correlative Instrumental Neutron Activation Analysis, Light Microscopy, Transmission Electron Microscopy, and X-ray Microanalysis for Qualitative and Quantitative Detection of Colloidal Gold Spheres in Biological Specimens

NASA Astrophysics Data System (ADS)

Hillyer, Julián F.; Albrecht, Ralph M.

1998-10-01

: Colloidal gold, conjugated to ligands or antibodies, is routinely used as a label for the detection of cell structures by light (LM) and electron microscopy (EM). To date, several methods to count the number of colloidal gold labels have been employed with limited success. Instrumental neutron activation analysis (INAA), a physical method for the analysis of the elemental composition of materials, can be used to provide a quantitative index of gold accumulation in bulk specimens. Given that gold is not naturally found in biological specimens in any substantial amount and that colloidal gold and ligand conjugates can be prepared to yield uniform bead sizes, the amount of label can be calculated in bulk biological samples by INAA. Here we describe the use of INAA, LM, transmission EM, and X-ray microanalysis (EDX) in a model to determine both distribution (localization) and amount of colloidal gold at the organ, tissue, cellular, and ultrastructural levels in whole animal systems following administration. In addition, the sensitivity for gold in biological specimens by INAA is compared with that of inductively coupled plasma mass spectrometry (ICP-MS). The correlative use of INAA, LM, TEM, and EDX can be useful, for example, in the quantitative and qualitative tracking of various labeled molecular species following administration in vivo.

Investigation of electrochemical migration on Sn-0.7Cu-0.3Ag-0.03P-0.005Ni solder alloy in HNO3 solution

NASA Astrophysics Data System (ADS)

Sarveswaran, C.; Othman, N. K.; Ali, M. Yusuf Tura; Ani, F. Che; Samsudin, Z.

2015-09-01

Current issue in lead-free solder in term of its reliability is still under investigation. This high impact research attempts to investigate the electrochemical migration (ECM) on Sn-0.7Cu-0.3Ag-0.03P-0.005Ni solder alloy by Water Drop Test (WDT) in different concentration of HNO3 solution. The concentration of HNO3 solution used in this research was 0.05, 0.10, 0.50 and 1M. Optical Microscope (OM), Field Emission Scanning Electron Microscope (FESEM) and Energy Dispersive X-Ray Analysis (EDX) were carried out in order to analysis the ECM behavior based on the growth of dendrite formation after WDT. In general, the results demonstrated that dendrite growth is faster in higher concentration compared with low concentration of HNO3. The concentration of HNO3 solution used has a strong correlation with Mean-Time-To-Failure (MTTF). As the concentration of HNO3 increases, the MTTF value decreases. Based on the MTTF results the solder alloy in 1M HNO3 solution is most susceptible to ECM. SnO2 forms as a corrosion by-product in the samples proved by EDX analysis. The solder alloy poses a high reliability risk in microelectronic devices during operation in 1M HNO3 solution.

Influence of lateral and in-depth metal segregation on the patterning of ohmic contacts for GaN-based devices

NASA Astrophysics Data System (ADS)

Redondo-Cubero, A.; Vázquez, L.; Alves, L. C.; Corregidor, V.; Romero, M. F.; Pantellini, A.; Lanzieri, C.; Muñoz, E.

2014-05-01

The lateral and in-depth metal segregation of Au/Ni/Al/Ti ohmic contacts for GaN-based high electron mobility transistors were analysed as a function of the Al barrier's thickness (d). The surface of the contacts, characterized by atomic force and scanning electron microscopy, shows a transition from a fractal network of rough and complex island-like structures towards smoother and cauliflower-like fronts with increasing d. Rutherford backscattering spectrometry and energy dispersive x-ray spectroscopy (EDXS) at different energies were used to confirm the in-depth intermixing of the metals relevant for the final contact resistance. EDXS mapping reveals a significant lateral segregation too, where the resulting patterns depend on two competing NiAlx and AuAlx phases, the intermixing being controlled by the available amount of Al. The optimum ohmic resistance is not affected by the patterning process, but is mainly dependent on the partial interdiffusion of the metals.

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.

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.

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.

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.

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.

Enhanced larvicidal, antibacterial, and photocatalytic efficacy of TiO2 nanohybrids green synthesized using the aqueous leaf extract of Parthenium hysterophorus.

PubMed

Thandapani, Keerthika; Kathiravan, Manikandan; Namasivayam, Elangovan; Padiksan, Indira Arulselvi; Natesan, Geetha; Tiwari, Manish; Giovanni, Benelli; Perumal, Venkatachalam

2018-04-01

Titanium dioxide nanoparticles are emerging as a biocompatible nanomaterial with multipurpose bioactivities. In this study, titanium dioxide (TiO 2 ) nanoparticles were effectively synthesized using the aqueous leaf extracts of Parthenium hysterophorus prepared by microwave irradiation. TiO 2 nanoparticles were fabricated by treating the P. hysterophorus leaf extracts with the TiO 4 solution. Biologically active compounds such as alcohols, phenols, alkanes, and fluoroalkanes were involved in bioreduction of TiO 4 into TiO 2 . The formation of green-engineered TiO 2 nanoparticles was confirmed by UV-vis spectroscopy, Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM), and energy-dispersive X-ray (EDX) spectroscopy and further characterized by X-ray diffraction (XRD) studies. UV-vis spectroscopy analysis showed maximum absorbance at 420 nm due to surface plasmon resonance of synthesized TiO 2 NPs. FTIR spectrum of the engineered TiO 2 NPs showed the presence of bioactive compounds in the leaf extract, which acted as capping and reducing agents. FESEM exhibited an average size of 20-50 nm and a spherical shape of TiO 2 NPs. EDX analysis indicated the presence of TiO 2 NPs by observing the peaks of titanium ions. XRD results pointed out the crystalline nature of engineered TiO 2 NPs. The larvicidal activity of TiO 2 NPs was studied on fourth instar larvae of dengue, Zika virus, and filariasis mosquito vectors Aedes aegypti and Culex quinquefasciatus. Antimicrobial efficacy of TiO 2 NPs was assessed on clinically isolated pathogens Escherichia coli, Staphylococcus aureus, Pseudomonas aeruginosa, Klebsiella pneumoniae, Proteus vulgaris, and Staphylococcus epidermidis. Besides, we found that TiO 2 NPs are able to quickly degrade the industrially harmful pigments methylene blue, methyl orange, crystal violet, and alizarin red dyes under sunlight illumination. Overall, this novel, simple, and eco-friendly approach can be of interest for the control of vector-borne diseases, as well as to formulate new bactericidal agents and to efficiently degrade dye solutions in the polluted areas.

Investigations of direct methanol fuel cell (DMFC) fading mechanisms

NASA Astrophysics Data System (ADS)

Sarma, Loka Subramanyam; Chen, Ching-Hsiang; Wang, Guo-Rung; Hsueh, Kan-Lin; Huang, Chiou-Ping; Sheu, Hwo-Shuenn; Liu, Ding-Goa; Lee, Jyh-Fu; Hwang, Bing-Joe

In this report, we present the microscopic investigations on various fading mechanisms of a direct methanol fuel cell (DMFC). High energy X-ray diffraction (XRD), X-ray absorption spectroscopy (XAS), energy dispersive X-ray spectroscopy (EDX), and Raman spectroscopic analysis were applied to a membrane-electrode-assembly (MEA) before and after fuel cell operation to figure out the various factors causing its fading. High energy XRD analysis of the fresh and faded MEA revealed that the agglomeration of the catalyst particles in the cathode layer of the faded MEA was more significant than in the anode layer of the faded MEA. The XAS analysis demonstrated that the alloying extent of Pt (J Pt) and Ru (J Ru) in the anode catalyst was increased and decreased, respectively, from the fresh to the faded MEA, indicating that the Ru environment in the anode catalyst was significantly changed after the fuel cell operation. Based on the X-ray absorption edge jump measurements at the Ru K-edge on the anode catalyst of the fresh and the faded MEA it was found that Ru was dissolved from the Pt-Ru catalyst after the fuel cell operation. Both the Ru K-edge XAS and EDX analysis on the cathode catalyst layer of the faded MEA confirms the presence of Ru environment in the cathode catalyst due to the Ru crossover from the anode to the cathode side. The changes in the membrane and the gas diffusion layer (GDL) after the fuel cell operation were observed from the Raman spectroscopy analysis.

Treated and untreated rock dust: Quartz content and physical characterization.

PubMed

Soo, Jhy-Charm; Lee, Taekhee; Chisholm, William P; Farcas, Daniel; Schwegler-Berry, Diane; Harper, Martin

2016-11-01

Rock dusting is used to prevent secondary explosions in coal mines, but inhalation of rock dusts can be hazardous if the crystalline silica (e.g., quartz) content in the respirable fraction is high. The objective of this study is to assess the quartz content and physical characteristics of four selected rock dusts, consisting of limestone or marble in both treated (such as treatment with stearic acid or stearates) and untreated forms. Four selected rock dusts (an untreated and treated limestone and an untreated and treated marble) were aerosolized in an aerosol chamber. Respirable size-selective sampling was conducted along with particle size-segregated sampling using a Micro-Orifice Uniform Deposit Impactor. Fourier Transform Infrared spectroscopy and scanning electron microscopy with energy-dispersive X-ray (SEM-EDX) analyses were used to determine quartz mass and particle morphology, respectively. Quartz percentage in the respirable dust fraction of untreated and treated forms of the limestone dust was significantly higher than in bulk samples, but since the bulk percentage was low the enrichment factor would not have resulted in any major change to conclusions regarding the contribution of respirable rock dust to the overall airborne quartz concentration. The quartz percentage in the marble dust (untreated and treated) was very low and the respirable fractions showed no enrichment. The spectra from SEM-EDX analysis for all materials were predominantly from calcium carbonate, clay, and gypsum particles. No free quartz particles were observed. The four rock dusts used in this study are representative of those presented for use in rock dusting, but the conclusions may not be applicable to all available materials.

Phytosynthesized gold nanoparticles from C. roxburghii DC. leaf and their toxic effects on normal and cancer cell lines.

PubMed

Balashanmugam, Pannerselvam; Durai, Prabhu; Balakumaran, Manickam Dakshinamoorthi; Kalaichelvan, Pudupalayam Thangavelu

2016-12-01

Gold nanoparticles are considered of great importance compared to other noble metal nanoparticles and its wide range of applications like pharmaceutics, therapeutics and diagnostics etc. During the past decade, phytosynthesized gold nanoparticles (AuNPs) are more focused in in vitro and in vivo study. The present study was focused on the gold chloride and phytosynthesized gold nanoparticles from aqueous leaf extract of Cassia roxburghii and their toxic effects on African green monkey normal kidney Vero cell line and three different cancer cell lines such as HepG2, MCF7 and HeLa. Phytosynthesized AuNPs were characterized by HRTEM, EDX, XRD and FTIR analysis. The particles size range of 25-35nm was confirmed by HRTEM. The elemental gold and the crystalline nature of AuNPs were confirmed by EDX and XRD, respectively. The reduction of functional groups was confirmed by FTIR. In in vitro study, the IC 50 of HepG2 cells was found to be 30μg/ml compared to other cell lines, HeLa and MCF7 cell line showing IC 50 of 50μg/ml and normal Vero cell line also nontoxic up to 75μg/ml confirmed by MTT assay. Further, apoptosis in HepG2 was analyzed by fluorescence microscope and DNA fragmentation was observed in HepG2 treated cells. These results suggested that phytosynthesized AuNPs of C. roxburghii extract clearly limited toxic on normal cells but toxic in cancer cells. Copyright © 2016 Elsevier B.V. All rights reserved.

Astaxanthin modulates osteopontin and transforming growth factor β1 expression levels in a rat model of nephrolithiasis: a comparison with citrate administration.

PubMed

Alex, Manju; Sauganth Paul, M V; Abhilash, M; Mathews, Varghese V; Anilkumar, T V; Nair, R Harikumaran

2014-09-01

To evaluate the effect of astaxanthin on renal angiotensin-I converting enzyme (ACE) levels, osteopontin (OPN) and transforming growth factor β1 (TGF-β1) expressions and the extent of crystal deposition in experimentally induced calcium oxalate kidney stone disease in a male Wistar rat model. To compare the efficacy of astaxanthin treatment with a currently used treatment strategy (citrate administration) for kidney stones. The expression of OPN was assessed by immunohistochemistry. One step reverse transcriptase polymerase chain reaction followed by densitometry was used to assess renal OPN and TGF-β1 levels. Renal ACE levels were quantified by an enzyme-linked immunosorbent assay method. Crystal deposition in kidney was analysed by scanning electron microscopic (SEM)-energy-dispersive X-ray (EDX). The renal ACE levels and the expression of OPN and TGF-β1 were upregulated in the nephrolithiasis-induced rats. Astaxanthin treatment reduced renal ACE levels and the expression OPN and TGF-β1. SEM-EDX analysis showed that crystal deposition was reduced in the astaxanthin-treated nephrolithiatic group. Astaxanthin treatment was more effective than citrate administration in the regulation of renal ACE levels, OPN and TGF-β1 expressions. Astaxanthin administration reduced renal calcium oxalate crystal deposition possibly by modulating the renal renin-angiotensin system (RAS), which reduced the expression of OPN and TGF-β1 levels. Astaxanthin administration was more effective than citrate treatment in reducing crystal deposition and down-regulating the expression of OPN and TGF-β1. © 2013 The Authors. BJU International © 2013 BJU International.

Characterizing the residual glass in a MgO/Al2O3/SiO2/ZrO2/Y2O3 glass-ceramic

PubMed Central

Seidel, Sabrina; Patzig, Christian; Wisniewski, Wolfgang; Gawronski, Antje; Hu, Yongfeng; Höche, Thomas; Rüssel, Christian

2016-01-01

The non-isochemical crystallization of glasses leads to glass-ceramics in which the chemical composition of the amorphous matrix differs from that of the parent glass. It is challenging to solely analyse the properties of these residual glassy phases because they frequently contain finely dispersed crystals. In this study, the composition of the residual glass matrix after the crystallization of a glass with the mol% composition 50.6 SiO2 · 20.7 MgO · 20.7 Al2O3 · 5.6 ZrO2 · 2.4 Y2O3 is analysed by scanning transmission electron microscopy (STEM) including energy dispersive X-ray analysis (EDXS). A batch of the residual glass with the determined composition is subsequently melted and selected properties are analysed. Furthermore, the crystallization behaviour of this residual glass is studied by X-ray diffraction, scanning electron microscopy including electron backscatter diffraction and STEM-EDXS analyses. The residual glass shows sole surface crystallization of indialite and multiple yttrium silicates while bulk nucleation does not occur. This is in contrast to the crystallization behaviour of the parent glass, in which a predominant bulk nucleation of spinel and ZrO2 is observed. The crystallization of the residual glass probably leads to different crystalline phases when it is in contact to air, rather than when it is enclosed within the microstructure of the parent glass-ceramics. PMID:27734918

Green synthesis and characterization of silver nanoparticles using Artemisia absinthium aqueous extract--A comprehensive study.

PubMed

Ali, Mohammad; Kim, Bosung; Belfield, Kevin D; Norman, David; Brennan, Mary; Ali, Gul Shad

2016-01-01

Unlike chemical synthesis, biological synthesis of nanoparticles is gaining tremendous interest, and plant extracts are preferred over other biological sources due to their ample availability and wide array of reducing metabolites. In this project, we investigated the reducing potential of aqueous extract of Artemisia absinthium L. for synthesizing silver nanoparticles (AgNPs). Optimal synthesis of AgNPs with desirable physical and biological properties was investigated using ultra violet-visible spectroscopy (UV-vis), dynamic light scattering (DLS), transmission electron microscopy (TEM) and energy-dispersive X-ray analysis (EDX). To determine their appropriate concentrations for AgNP synthesis, two-fold dilutions of silver nitrate (20 to 0.62 mM) and aqueous plant extract (100 to 0.79 mg ml(-1)) were reacted. The results showed that silver nitrate (2mM) and plant extract (10 mg ml(-1)) mixed in different ratios significantly affected size, stability and yield of AgNPs. Extract to AgNO3 ratio of 6:4v/v resulted in the highest conversion efficiency of AgNO3 to AgNPs, with the particles in average size range of less than 100 nm. Furthermore, the direct imaging of synthesized AgNPs by TEM revealed polydispersed particles in the size range of 5 to 20 nm. Similarly, nanoparticles with the characteristic peak of silver were observed with EDX. This study presents a comprehensive investigation of the differential behavior of plant extract and AgNO3 to synthesize biologically stable AgNPs. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

Hepatoprotective effect of engineered silver nanoparticles coated bioactive compounds against diethylnitrosamine induced hepatocarcinogenesis in experimental mice.

PubMed

Prasannaraj, Govindaraj; Venkatachalam, Perumal

2017-02-01

Nanoparticle based drug delivery can rapidly improves the therapeutic potential of anti-cancer agents. The present study focused to evaluate the hepatoprotective activity of silver nanoparticles (AgNPs) synthesized using aqueous extracts of Andrographis paniculata leaves (ApAgNPs) and Semecarpus anacardium nuts (SaAgNPs) against diethylnitrosamine (DEN) induced liver cancer in mice model. The physico-chemical properties of synthesized AgNPs were characterized by Fourier transform infrared (FTIR) spectroscopy, Transmission Electron Microscopy (TEM), Selected Area Electron Diffraction (SAED), X-ray Diffraction (XRD), Energy Dispersive X-ray (EDX) spectrum, Zeta potential and Dynamic Light Scattering (DLS) analysis. The surface plasmon resonance (SPR) absorption spectrum revealed a strong peak at 420nm for both SaAgNPs and ApAgNPs. FTIR results exhibited the presence of possible functional groups in the synthesized AgNPs. TEM analysis determined the hexagonal, and spherical shape of the synthesized silver nanoparticles. The XRD and SAED pattern confirmed the crystalline nature and crystalline size of the AgNPs. EDX result clearly showed strong silver signals in the range between 2 and 4keV. Zeta potential measurements indicated a sharp peak at -3.93 and -13.8mV for ApAgNPs and SaAgNPs, respectively. DLS measurement expressed the particle size distribution was 70 and 60nm for ApAgNPs and SaAgNPs, respectively. DEN (20mg/kg b.wt.) was subjected to induce liver cancer in mice for 8weeks and treated with biosynthesized silver nanoparticles. Interestingly, ApAgNPs and SaAgNPs treated DEN induced animal groups show a decreased level of aspartate amino transferase (AST), alanine amino transferase (ALT), serum glutamate oxaloacetate transaminase (SGOT), serum glutamate pyruvate transaminase (SGPT) activity and elevated level of catalase (CAT), glutathione peroxidase (GPx), glutathione S-transferase (GST) and superoxide dismutase (SOD) activity over untreated DEN control animals group. Histopathological investigation reveals decreased fat accumulation, appearance of binucleated cells in nanoparticle treated animals and showed mere normal cells induced by DEN. Argyrophilic nucleolar organiser region (AgNORs) had a significant decrease in number of acidic proteins and mast cells assay showed decrease of metachromatic cells in nanoparticles treated animal groups over control. Present results strongly suggest that biomolecule coated silver nanoparticles exposure showed potential hepatoprotective effect against DEN induced liver cancer and could be used as an effective anticancer nanodrug. Copyright © 2017. Published by Elsevier B.V.

Purification of simulated waste water using green synthesized silver nanoparticles of Piliostigma thonningii aqueous leave extract

NASA Astrophysics Data System (ADS)

Shittu, K. O.; Ihebunna, O.

2017-12-01

Synthesis of nanoparticles from various biological systems has been reported, but among all such systems, biosynthesis of nanoparticles from plants is considered the most suitable method. The use of plant material not only makes the process eco-friendly, but also the abundance makes it more economical. The aim of this study was to biologically synthesize silver nanoparticle using Piliostigma thonningii aqueous leaf extract and applied in the purification of laboratory stimulated waste with optimization using the different conditions of silver nanoparticle production such as time, temperature, pH, concentration of silver nitrate and volume of the aqueous extract. The biosynthesized silver nanoparticles were characterized by UV-visible spectrophotometry, nanosizer, energy dispersive x-ray analysis (EDX), transmission electron microscopy (TEM) and Fourier transform infrared (FTIR) spectroscopy. The time intervals for the reaction with aqueous silver nitrate solution shows an increase in the absorbance with time and became constant giving a maximum absorbance at 415 nm at 60 min of incubation. The pH of 6.5, temperature 65 °C, 1.25 mM of silver nitrate and 5 ml of plant extract was the best condition with maximum absorbance. The results from nanosizer, UV-vis and TEM suggested the biosynthesis silver nanoparticle to be spherical ranging from 50 nm to 114 nm. The EDX confirmed the elemental synthesis of silver at 2.60 keV and FTIR suggested the capping agent to be hydroxyl (OH) group with -C=C stretching vibrations. The synthesized silver nanoparticle also shows heavy metal removal activity in laboratory simulated waste water. The safety toxicity studies show no significant difference between the orally administered silver nanoparticles treated water group and control group, while the histopathological studies show well preserved hepatic architecture for the orally administered silver nanoparticle treated waste water group when compared with the control group. Therefore, it can be concluded that the biosynthesized silver nanoparticles have efficient ability in heavy metal removal without sub chronic adverse effects in experimental rats.

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.

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,...

Adsorption of Cd2+ ions on plant mediated SnO2 nanoparticles

NASA Astrophysics Data System (ADS)

Haq, Sirajul; Rehman, Wajid; Waseem, Muhammad; Shahid, Muhammad; Mahfooz-ur-Rehman; Hussain Shah, Khizar; Nawaz, Mohsan

2016-10-01

Plant mediated SnO2 nanoparticles were synthesized by using SnCl4.5H2O as a precursor material. The nanoparticles were then characterized for BET surface area measurements, energy dispersive x-rays (EDX), scanning electron microscopy (SEM), UV-vis diffuse reflectance (DRS) spectra and x-rays diffraction (XRD) analysis. The successful synthesis of SnO2 nanoparticles was confirmed by EDX analysis. The particle sizes were in the range 19-27 nm whereas the crystallite size computed from XRD measurement was found to be 19.9 nm. Batch adsorption technique was employed for the removal of Cd2+ ions from aqueous solution. The sorption studies of Cd2+ ions were performed at pHs 4 and 6. The equilibrium concentration of Cd2+ ions was determined by atomic absorption spectrometer (flame mode). The uptake of Cd2+ ions was affected by initial concentration, pH and temperature of the electrolytic solution. It was observed that the adsorption of Cd2+ ions enhanced with increase in the initial concentration of Cd2+ ions whereas a decrease in the percent adsorption was detected. From the thermodynamic parameters, the adsorption process was found spontaneous and endothermic in nature. The n values confirmed 2:1 exchange mechanism between surface protons and Cd2+ ions.

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.

Characteristics of uranium biosorption from aqueous solutions on fungus Pleurotus ostreatus.

PubMed

Zhao, Changsong; Liu, Jun; Tu, Hong; Li, Feize; Li, Xiyang; Yang, Jijun; Liao, Jiali; Yang, Yuanyou; Liu, Ning; Sun, Qun

2016-12-01

Uranium(VI) biosorption from aqueous solutions was investigated in batch studies by using fungus Pleurotus ostreatus biomass. The optimal biosorption conditions were examined by investigating the reaction time, biomass dosage, pH, temperature, and uranium initial concentration. The interaction between fungus biomass and uranium was confirmed using Fourier transformed infrared (FT-IR), scanning electronic microscopy energy dispersive X-ray (SEM-EDX), and X-ray photoelectron spectroscopy (XPS) analysis. Results exhibited that the maximum biosorption capacity of uranium on P. ostreatus was 19.95 ± 1.17 mg/g at pH 4.0. Carboxylic, amine, as well as hydroxyl groups were involved in uranium biosorption according to FT-IR analysis. The pseudo-second-order model properly evaluated the U(VI) biosorption on fungus P. ostreatus biomass. The Langmuir equation provided better fitting in comparison with Freundlich isotherm models. The obtained thermodynamic parameters suggested that biosorption is feasible, endothermic, and spontaneous. SEM-EDX and XPS were additionally conducted to comprehend the biosorption process that could be described as a complex process involving several mechanisms of physical adsorption, chemisorptions, and ion exchange. Results obtained from this work indicated that fungus P. ostreatus biomass can be used as potential biosorbent to eliminate uranium or other radionuclides from aqueous solutions.

Measuring mass-based hygroscopicity of atmospheric particles through in situ imaging

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

Piens, Dominique S.; Kelly, Stephen T.; Harder, Tristan H.

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 of 158 other particles from the sample broadly agreed with those of the humidified particles, indicating the potential to infer atmospheric hygroscopic behavior from a selected subset of particles. As a result, these methods offer unique quantitative capabilities to characterize and correlate the hygroscopicity and chemistry of individual submicrometer atmospheric particles.« less

Measuring mass-based hygroscopicity of atmospheric particles through in situ imaging

DOE PAGES

Piens, Dominique S.; Kelly, Stephen T.; Harder, Tristan H.; ...

2016-04-18

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 of 158 other particles from the sample broadly agreed with those of the humidified particles, indicating the potential to infer atmospheric hygroscopic behavior from a selected subset of particles. As a result, these methods offer unique quantitative capabilities to characterize and correlate the hygroscopicity and chemistry of individual submicrometer atmospheric particles.« less

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.

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

Nieroda, Pawel; Zybala, Rafal; Wojciechowski, Krzysztof T.

The aim of the study was to develop a fast and simple method for preparation of polycrystalline Mg{sub 2}Si. For this purpose a Spark Plasma Sintering (SPS) method was used and synthesis conditions were adjusted in such a manner that no excess Mg was required. Materials were synthesized by the direct reaction of Mg and Si raw powders. To determine the phase and chemical composition, the fabricated samples were studied by X-ray diffraction and SEM microscopy coupled with EDX chemical analysis. Thermoelectric properties of samples (thermal conductivity, electrical conductivity and Seebeck coefficient) were measured all over temperature range of 300-650more » K. The analysis by the scanning thermoelectric microprobe (STM) shows that samples have uniform distribution of Seebeck coefficient with mean value of about -405 {mu}VK{sup -1} and standard deviation of 94 {mu}VK{sup -1}. Prepared materials have intrinsic band gap of 0.45 eV and thermal conductivity {lambda}= 7.5 Wm{sup -1}K{sup -1} at room temperature.« less

Praseodymium - A Competent Dopant for Luminescent Downshifting and Photocatalysis in ZnO Thin Films

NASA Astrophysics Data System (ADS)

Narayanan, Nripasree; Deepak, N. K.

2018-05-01

Highly transparent and conducting Zinc oxide (ZnO) thin films doped with Praseodymium (Pr) were deposited on glass substrates by using the spray pyrolysis method. The X-ray diffraction (XRD) analysis revealed the polycrystallinity of the deposited films with a hexagonal wurtzite structure, whereas the energy-dispersive X-ray spectroscopy (EDX) analysis confirmed the incorporation of Pr in the films. The optical energy gap decreased by Pr doping due to the merging of the conduction band with the impurity bands formed within the forbidden gap. The room temperature photoluminescence spectra of the Pr-doped film showed enhancement of visible emission, suggesting efficient luminescent downshifting. The photocatalytic activity of the Pr-doped films is higher than that of undoped films due to the effective suppression of the rapid recombination of the photo-generated electron-hole pairs. The impurity levels formed within the forbidden gap act as efficient luminescent centers and electron traps, which lead to luminescent downshifting and enhanced photocatalytic activity.

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

Biosynthesis of cobalt oxide nanoparticles using endophytic fungus Aspergillus nidulans.

PubMed

Vijayanandan, Ajuy Sundar; Balakrishnan, Raj Mohan

2018-07-15

Metallic oxide nanoparticles have profound applications in electrochemical devices, supercapacitors, biosensors and batteries. Though four fungi were isolated from Nothapodytes foetida, Aspergillus nidulans was found to be suitable for synthesis of cobalt oxide nanoparticles, as it has proficient tolerance towards metal under study. The broth containing precursor solution and organism Aspergillus nidulans had changed from pink to orange indicating the formation of nanoparticles. Characterization by x-ray diffraction analysis (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR) and energy dispersive x-ray analysis (EDX) confirmed the formation of spinel cobalt oxide nanoparticles at an average size of 20.29 nm in spherical shape with sulfur-bearing proteins acting as a capping agent for the synthesized nanoparticles. The nanoparticles could be applied in energy storage, as a specific capacitance of 389 F/g showed competence. The study was a greener attempt to synthesize cobalt oxide nanoparticles using endophytic fungus. Copyright © 2018 Elsevier Ltd. All rights reserved.

Detection of mercury in the 411-year-old beard hairs of the astronomer Tycho Brahe by elemental analysis in electron microscopy.

PubMed

Jonas, Ludwig; Jaksch, Heiner; Zellmann, Erhard; Klemm, Kerstin I; Andersen, Peter Hvilshøj

2012-10-01

Hairs more than 400 years old of the famous astronomer Tycho Brahe were studied by electron microscopy to evaluate the hypothesis that Johannes Kepler murdered his teacher Brahe by mercury intoxication. The beard hairs showed a well-preserved ultrastructure with typical hair scales and melanosomes. The authors detected an accumulation of electron-dense granules of about 10 nm inside the outer hair scales, but not in the hair shaft and roots. At the places of these heavy-metal-containing granules they detected mercury besides other elements by energy dispersive X-ray analysis (EDX, Oxford, UK) in a field cathode scanning electron microscope (SEM, Gemini, Zeiss). The mercury-containing granules were found over the whole length of hairs, but only in the outer hair scales. Nevertheless, surface coatings of hairs were free of mercury. This distribution of mercury does not support the murder hypothesis, but could be related to precipitation of mercury dust from the air during long-term alchemistic activities.

Preparation of granular activated carbons from yellow mombin fruit stones for CO2 adsorption.

PubMed

Fiuza, Raildo Alves; Medeiros de Jesus Neto, Raimundo; Correia, Laise Bacelar; Carvalho Andrade, Heloysa Martins

2015-09-15

Stones of yellow mombin, a native fruit of the tropical America and West Indies, were used as starting materials to produce activated carbons, subsequently used as adsorbent for CO2 capture. The carbonaceous materials were either chemically activated with HNO3, H3PO4 and KOH or physically activated with CO2. The carbon samples were characterized by SEM, EDX, TG/DTA, Raman spectroscopy, physical adsorption for textural analysis and by acid-base titrations. The CO2 adsorption capacity and adsorption cycles were investigated by TG. The results indicate that the capacity of CO2 adsorption may be maximized on highly basic surfaces of micropores smaller than 1 nm. The KOH activated carbon showed high and stable capacity of CO2 adsorption after 10 cycles. Copyright © 2015 Elsevier Ltd. All rights reserved.

Tribochemistry of contact interfaces of nanocrystalline molybdenum carbide films

NASA Astrophysics Data System (ADS)

Kumar, D. Dinesh; Kumar, N.; Panda, Kalpataru; Kamalan Kirubaharan, A. M.; Kuppusami, P.

2018-07-01

Transition metal carbides (TMC) are known for their improved tribological properties and are sensitive to the tribo-atmospheric environment. Nanocrystalline molybdenum carbide (MoC) thin films were deposited by DC magnetron sputtering technique using reactive CH4 gas. The friction and wear resistance properties of MoC thin films were significantly improved in humid-atmospheric condition as compared to high-vacuum tribo-condition. A comprehensive chemical analysis of deformed contact interfaces was carried out by X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray spectroscopy (EDX) and Raman spectroscopy. XPS and Raman spectroscopy showed the formation of stable molybdenum-oxide (MoO), molybdenum carbide (MoC) and amorphous carbon (a-C) tribo-phases. Moreover, during the sliding in humid-atmospheric condition, these phases were extensively deposited on the sliding steel ball counter body which significantly protected against undesirable friction and wear.

Nanostructured ZnO Films for Room Temperature Ammonia Sensing

NASA Astrophysics Data System (ADS)

Dhivya Ponnusamy; Sridharan Madanagurusamy

2014-09-01

Zinc oxide (ZnO) thin films have been deposited by a reactive dc magnetron sputtering technique onto a thoroughly cleaned glass substrate at room temperature. X-ray diffraction revealed that the deposited film was polycrystalline in nature. The field emission scanning electron micrograph (FE-SEM) showed the uniform formation of a rugby ball-shaped ZnO nanostructure. Energy dispersive x-ray analysis (EDX) confirmed that the film was stoichiometric and the direct band gap of the film, determined using UV-Vis spectroscopy, was 3.29 eV. The ZnO nanostructured film exhibited better sensing towards ammonia (NH3) at room temperature (˜30°C). The fabricated ZnO film based sensor was capable of detecting NH3 at as low as 5 ppm, and its parameters, such as response, selectivity, stability, and response/recovery time, were also investigated.

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.

Surface morphological properties of Ag-Al2O3 nanocermet layers using dip-coating technique

NASA Astrophysics Data System (ADS)

Muhammad, Nor Adhila; Suhaimi, Siti Fatimah; Zubir, Zuhana Ahmad; Daud, Sahhidan

2017-12-01

Ag-Al2O3 nanocermet layer was deposited on Cu coated glass substrate using dip-coating technique. The aim of this study was to observe the surface morphology properties of Ag-Al2O3 nanocermet layers after annealing process at 350°C in H2. The surface morphology of Ag-Al2O3 nanocermet will be characterized by Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM) and X-Ray Diffractometer (XRD), respectively. The results show that nearly isolated Ag particles having a large and small size were present in the Al2O3 dielectric matrix after annealing process. The face centered cubic crystalline structure of Ag nanoparticles inclusion in the amorphous alumina dielectric matrix was confirmed using XRD pattern and supported by EDX spectra analysis.

Clinical findings and electrodiagnostic testing in 108 consecutive cases of lumbosacral radiculopathy due to herniated disc.

PubMed

Mondelli, M; Aretini, A; Arrigucci, U; Ginanneschi, F; Greco, G; Sicurelli, F

2013-10-01

This prospective study aim to examine whether clinical findings and electrodiagnostic testing (EDX) in patients with lumbosacral monoradiculopathy due to herniated disc (HD) differ as a function of root involvement level (L5 vs. S1) and HD zone (paramedian vs. intraforaminal). All patients with L4, L5 or S1 monoradiculopathy were prospectively enrolled at four electromyography (EMG) labs over a 2-year period. The diagnosis was based on a congruence between patient history and MRI evidence of HD. We compared the sensitivities of clinical findings and EDX with respect to both root involvement level and HD zone. Multivariate logistic regression was performed in order to verify the association between abnormal EMG, clinical, and neuroradiological findings. One hundred and eight patients (mean age 47.7 years, 55% men) were consecutively enrolled. Sensory loss in the painful dermatome was the most frequent finding at physical examination (56% of cases). EMG was abnormal in at least one muscle supplied by femoral and sciatic nerves in 45 cases (42%). Inclusion of paraspinal muscles increased sensitivity to only 49% and that of proximal muscles was useless. Motor and sensory neurography was seldom abnormal. The most frequent motor neurographic abnormalities were a delay of F-wave minimum latency and decrease in the compound muscle action potential amplitude from extensor digitorum brevis and abductor hallucis in L5 and S1 radiculopathies, respectively. Sensory neurography was usually normal, the amplitude of sensory nerve action potential was seldom reduced when HD injured dorsal root ganglion or postganglionic root fibres. Multivariate logistic regression analysis showed that EMG abnormalities could be predicted by myotomal muscular weakness, abnormal deep reflexes, and paraesthesiae. The only clinical and electrophysiological differences with respect to root involvement level concerned deep reflexes and motor neurography of deep peroneal and tibial nerves. Only some EDX parameters are helpful for the diagnosis of lumbosacral radiculopathy. EMG was abnormal in less than 50% of cases and its abnormalities could be predicted by some clinical findings. However, neurography is useful as a tool for differential diagnosis between radiculopathy and more diffuse disorders of the peripheral nervous system (polyneuropathy, plexopathy). Copyright © 2013 Elsevier Masson SAS. All rights reserved.

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.

Influences of Co doping on the structural and optical properties of ZnO nanostructured

NASA Astrophysics Data System (ADS)

Majeed Khan, M. A.; Wasi Khan, M.; Alhoshan, Mansour; Alsalhi, M. S.; Aldwayyan, A. S.

2010-07-01

Pure and Co-doped ZnO nanostructured samples have been synthesized by a chemical route. We have studied the structural and optical properties of the samples by using X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), field-emission transmission electron microscope (FETEM), energy-dispersive X-ray (EDX) analysis and UV-VIS spectroscopy. The XRD patterns show that all the samples are hexagonal wurtzite structures. Changes in crystallite size due to mechanical activation were also determined from X-ray measurements. These results were correlated with changes in particle size followed by SEM and TEM. The average crystallite sizes obtained from XRD were between 20 to 25 nm. The TEM images showed the average particle size of undoped ZnO nanostructure was about 20 nm whereas the smallest average grain size at 3% Co was about 15 nm. Optical parameters such as absorption coefficient ( α), energy band gap ( E g ), the refractive index ( n), and dielectric constants ( σ) have been determined using different methods.

Characterization of SnO2 Film with Al-Zn Doping Using Sol-Gel Dip Coating Techniques

NASA Astrophysics Data System (ADS)

Doyan, A.; Susilawati; Ikraman, N.; Taufik, M.

2018-04-01

Sn1-2x AlxZnxO2 film has been developed using sol-gel dip coating technique. The materials SnCl2.2H2O, AlCl3 and ZnCl2 dissolved in water and ethanol with 5:95 volume ratio. Variations dopant concentration x = 0.000, 0.005, 0.0025, and 0.050. The film was grown with sol concentration 0.4 M, the withdrawal speed of 12 cm/min and sintering at 600 °C for 30 minutes. The characteristics Sn1-2x AlxZnxO2 films with various doping concentration phase were characterized by XRD. The morphological characteristics and the composition of the constituent elements of the film were characterized by SEM-EDX. The characteristics of the shape, structure, and size of the particles were characterized by TEM. The XRD results show that all films have a tetragonal SnO2 rutile phase without any secondary phase with an average particle size in the range 5.14 – 2.09 nm. The SEM results show that the film grown has a smooth morphology with a striped texture (x = 0.00), and there is a crack (x = 0.050). The EDX results show that the composition and distribution of the constituent elements of the film are uniformly distributed. TEM results show that the particle films has tetragonal rutile structure, orthorhombic and amorphous with a spherical shape.

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.

Green synthesis of silver nanoparticles using Achillea biebersteinii flower extract and its anti-angiogenic properties in the rat aortic ring model.

PubMed

Baharara, Javad; Namvar, Farideh; Ramezani, Tayebe; Hosseini, Nasrin; Mohamad, Rosfarizan

2014-04-15

Silver nanoparticles display unique physical and biological properties which have attracted intensive research interest because of their important medical applications. In this study silver nanoparticles (Ab.Ag-NPs) were synthesized for biomedical applications using a completely green biosynthetic method using Achillea biebersteinii flowers extract. The structure and properties of Ab.Ag-NPs were investigated using UV-visible spectroscopic techniques, transmission electron microscopy (TEM), zeta potential and energy dispersive X-ray spectrometers (EDS). The UV-visible spectroscopic analysis showed the absorbance peak at 460 nm, which indicates the synthesis of silver nanoparticles. The average particle diameter as determined by TEM was found to be 12±2 nm. The zeta potential analysis indicated that Ab.Ag-NPs have good stability EDX analysis also exhibits presentation of silver element. As angiogenesis is an important phenomenon and as growth factors imbalance in this process causes the acceleration of several diseases including cancer, the anti-angiogenic properties of Ab.Ag-NPs were evaluated using the rat aortic ring model. The results showed that Ab.Ag-NPs (200 μg/mL) lead to a 50% reduction in the length and number of vessel-like structures. The synthesized silver nanoparticles from the Achillea biebersteinii flowers extract, which do not involve any harmful chemicals were well-dispersed and stabilized through this green method and showed potential therapeutic benefits against angiogenesis.

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.

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.

STEM-EDX tomography of bimetallic nanoparticles: A methodological investigation

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

Slater, Thomas J. A.; Janssen, Arne; Camargo, Pedro H. C.

This paper presents an investigation of the limitations and optimization of energy dispersive X-ray (EDX) tomography within the scanning transmission electron microscope, focussing on application of the technique to characterising the 3D elemental distribution of bimetallic AgAu nanoparticles. The detector collection efficiency when using a standard tomography holder is characterised using a tomographic data set from a single nanoparticle and compared to a standard low background double tilt holder. Optical depth profiling is used to investigate the angles and origin of detector shadowing as a function of specimen field of view. A novel time-varied acquisition scheme is described to compensatemore » for variations in the intensity of spectrum images at each sample tilt. Lastly, the ability of EDX spectrum images to satisfy the projection requirement for nanoparticle samples is discussed, with consideration of the effect of absorption and shadowing variations« less

STEM-EDX tomography of bimetallic nanoparticles: A methodological investigation

DOE PAGES

Slater, Thomas J. A.; Janssen, Arne; Camargo, Pedro H. C.; ...

2015-10-22

This paper presents an investigation of the limitations and optimization of energy dispersive X-ray (EDX) tomography within the scanning transmission electron microscope, focussing on application of the technique to characterising the 3D elemental distribution of bimetallic AgAu nanoparticles. The detector collection efficiency when using a standard tomography holder is characterised using a tomographic data set from a single nanoparticle and compared to a standard low background double tilt holder. Optical depth profiling is used to investigate the angles and origin of detector shadowing as a function of specimen field of view. A novel time-varied acquisition scheme is described to compensatemore » for variations in the intensity of spectrum images at each sample tilt. Lastly, the ability of EDX spectrum images to satisfy the projection requirement for nanoparticle samples is discussed, with consideration of the effect of absorption and shadowing variations« less

Corrosion and Microstructure Correlation in Molten LiCl-KCl Medium

NASA Astrophysics Data System (ADS)

Ravi Shankar, A.; Mathiya, S.; Thyagarajan, K.; Kamachi Mudali, U.

2010-07-01

Pyrochemical reprocessing in molten chloride salt medium has been considered as one of the best options for the reprocessing of spent metallic fuels of future fast breeder reactors. The unit operations such as salt preparation, electrorefining, and cathode processing involve the presence of molten LiCl-KCl eutectic salt from 673 to 1373 K (400 to 1100 °C). The present work discusses the corrosion behavior of electroformed nickel (EF Ni) without and with nickel-tungsten (Ni-W) coating, 316L SS, and INCONEL 625 alloy in molten LiCl-KCl eutectic salt at 673 K, 773 K, and 873 K (400 °C, 500 °C, and 600 °C) in the presence of air. The weight percent loss of the exposed samples was determined by the weight loss method and surface morphology of the salt exposed, and product layers were examined by scanning electron microscopy (SEM). X-ray diffraction (XRD) and energy-dispersive X-ray (EDX) analysis were also carried out on the exposed and corrosion product layers to understand the phases present and the corrosion mechanism involved. The results of the present study indicated that INCONEL 625 alloy showed superior corrosion resistance compared to electroformed nickel (EF Ni), EF Ni with nickel-tungsten (Ni-W) coating (EF Ni-W), and 316L SS. The EF Ni with Ni-W coating exhibits better corrosion resistance than EF Ni without tungsten coating. Based on the surface morphology, XRD, and EDX analysis of corrosion product layers, the mechanism of corrosion of INCONEL 625 and 316L involves formation of chromium-rich compound at the surface and subsequent spallation. For the EF Ni, the porous thick NiO corrosion product allows the penetration of salt, thus accelerating the corrosion. Improved corrosion resistance of EF Ni-W was attributed to the W-rich NiO layer, while for INCONEL 625, the adherent and protective NiO layer improved the corrosion resistance. The article highlights the results of the present investigation.

Down-top nanofabrication of binary (CdO)x (ZnO)1-x nanoparticles and their antibacterial activity.

PubMed

Al-Hada, Naif Mohammed; Mohamed Kamari, Halimah; Abdullah, Che Azurahanim Che; Saion, Elias; Shaari, Abdul H; Talib, Zainal Abidin; Matori, Khamirul Amin

2017-01-01

In the present study, binary oxide (cadmium oxide [CdO]) x (zinc oxide [ZnO]) 1-x nanoparticles (NPs) at different concentrations of precursor in calcination temperature were prepared using thermal treatment technique. Cadmium and zinc nitrates (source of cadmium and zinc) with polyvinylpyrrolidone (capping agent) have been used to prepare (CdO) x (ZnO) 1-x NPs samples. The sample was characterized by X-ray diffraction (XRD), scanning electron microscopy, energy-dispersive X-ray (EDX), transmission electron microscopy (TEM), and Fourier transform infrared (FTIR) spectroscopy. XRD patterns analysis revealed that NPs were formed after calcination, which showed a cubic and hexagonal crystalline structure of (CdO) x (ZnO) 1-x NPs. The phase analysis using EDX spectroscopy and FTIR spectroscopy confirmed the presence of Cd and Zn as the original compounds of prepared (CdO) x (ZnO) 1-x NP samples. The average particle size of the samples increased from 14 to 33 nm as the concentration of precursor increased from x=0.20 to x=0.80, as observed by TEM results. The surface composition and valance state of the prepared product NPs were determined by X-ray photoelectron spectroscopy (XPS) analyses. Diffuse UV-visible reflectance spectra were used to determine the optical band gap through the Kubelka-Munk equation; the energy band gap was found to decrease for CdO from 2.92 to 2.82 eV and for ZnO from 3.22 to 3.11 eV with increasing x value. Additionally, photoluminescence (PL) spectra revealed that the intensity in PL increased with an increase in particle size. In addition, the antibacterial activity of binary oxide NP was carried out in vitro against Escherichia coli ATCC 25922 Gram (-ve), Salmonella choleraesuis ATCC 10708, and Bacillus subtilis UPMC 1175 Gram (+ve). This study indicated that the zone of inhibition of 21 mm has good antibacterial activity toward the Gram-positive B. subtilis UPMC 1175.

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.

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

Zinc oxide nanorods functionalized paper for protein preconcentration in biodiagnostics

NASA Astrophysics Data System (ADS)

Tiwari, Sadhana; Vinchurkar, Madhuri; Rao, V. Ramgopal; Garnier, Gil

2017-03-01

Distinguishing a specific biomarker from a biofluid sample containing a large variety of proteins often requires the selective preconcentration of that particular biomarker to a detectable level for analysis. Low-cost, paper-based device is an emerging opportunity in diagnostics. In the present study, we report a novel Zinc oxide nanorods functionalized paper platform for the preconcentration of Myoglobin, a cardiac biomarker. Zinc oxide nanorods were grown on a Whatman filter paper no. 1 via the standard hydrothermal route. The growth of Zinc oxide nanorods on paper was confirmed by a combination of techniques consisting of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS,) scanning electron microscopy (SEM), and energy dispersive spectroscopy (EDX) analysis. The Zinc oxide nanorods modified Whatman filter paper (ZnO-NRs/WFP) was further tested for use as a protein preconcentrator. Paper-based ELISA was performed for determination of pre-concentration of cardiac marker protein Myoglobin using the new ZnO-NRs/WFP platform. The ZnO-NRs/WFP could efficiently capture the biomarker even from a very dilute solution (Myoglobin < 50 nM). Our ELISA results show a threefold enhancement in protein capture with ZnO-NRs/WFP compared to unmodified Whatman filter paper, allowing accurate protein analysis and showing the diagnostic concept.

Engineered carbon (biochar) prepared by direct pyrolysis of Mg-accumulated tomato tissues: characterization and phosphate removal potential.

PubMed

Yao, Ying; Gao, Bin; Chen, Jianjun; Zhang, Ming; Inyang, Mandu; Li, Yuncong; Alva, Ashok; Yang, Liuyan

2013-06-01

An innovative method was developed to produce engineered biochar from magnesium (Mg) enriched tomato tissues through slow pyrolysis in a N2 environment. Tomato plants treated with 25mM Mg accumulated much higher level of Mg in tissue, indicating Mg can be substantially enriched in tomato plants, and pyrolysis process further concentrated Mg in the engineered biochar (8.8% Mg). The resulting Mg-biochar composites (MgEC) showed better sorption ability to phosphate (P) in aqueous solutions compared to the other four tomato leaves biochars. Statistical analysis showed a strong and significant correlation between P removal rate and biochar Mg content (R(2)=0.78, and p<0.001), indicating the enriched Mg in the engineered biochar is the main factor controlling its P removal ability. SEM-EDX, XRD and XPS analyses showed that nanoscale Mg(OH)2 and MgO particles were presented on the surface of MgEC, which serve as the main adsorption sites for aqueous P. Copyright © 2013 Elsevier Ltd. All rights reserved.

In2O3-ZnO heterostructure development in electrical and photoluminescence properties of In2O3 1-D nanostructures

NASA Astrophysics Data System (ADS)

Shariati, M.; Ghafouri, V.

2014-05-01

Indium Oxide quasi one-dimensional (1D) nanostructures known as nanowires and nanorods synthesis using the thermal evaporation method, has been articulated. To nucleate growth sites, substrate seeding promoted 1D nanostructures growth. The catalyst-mediated growth mechanism showed more favorable morphologies and physical properties in under vacuum conditions associated with bottom-up technique. Scanning electron microscopy (SEM) results showed that the Zn-doped 1D nanostructures had spherical caps. The X-ray diffraction (XRD) pattern and energy-dispersive X-ray (EDX) spectrum indicated that these caps intensively associated with ZnO. Therefore, it was reasonable that the vapor-liquid-solid mechanism (VLS) was responsible for the growth of the In2O3-ZnO heterostructure nanowires. This technique enhances optical and electrical properties in nanostructures. The photoluminescence (PL) analysis in Zn-doped In2O3 nanowires and nanorods shows that the intensity of the visible and UV-region emissions overwhelmingly increases and resistance measurement professes the improvement of linear conductance in VLS growth mechanism.

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.

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.

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.

Effect of solvents on sol-gel spin-coated nanostructured Al-doped ZnO thin films: a film for key optoelectronic applications

NASA Astrophysics Data System (ADS)

Kumar, K. Deva Arun; Valanarasu, S.; Kathalingam, A.; Ganesh, V.; Shkir, Mohd.; AlFaify, S.

2017-12-01

Aluminum-doped zinc oxide (AZO) thin films were deposited by sol-gel spin coating technique onto the glass substrates using different solvents such as 2-methoxyethanol, methanol, ethanol and isopropanol. Prepared films were characterized by XRD, Raman spectrum, SEM, UV-visible spectrophotometer, photoluminescence (PL) and electrical studies. XRD studies showed that all the prepared films are hexagonal wurtzite structure with polycrystalline nature oriented along (002) direction. SEM images showed uniform particles of size around 60 nm distributed regularly on to the entire glass substrate. EDX analysis confirmed the composition of grown AZO film consisting of Al, Zn and O elements. The prepared films showed highest optical transmittance 94% in the visible range and band gap 3.30 eV. PL spectra for all AZO films showed a strong UV emission peak at 387 nm. The AZO films prepared using isopropanol solvent showed high carrier concentration and low resistivity values as 1.72 × 1020 cm-3 and 2.90 × 10-3 Ω cm, respectively, with high figure of merit ( ϕ) value 8.42 × 10-3 (Ω/sq)-1.

Green synthesis and characterization of Carica papaya leaf extract coated silver nanoparticles through X-ray diffraction, electron microscopy and evaluation of bactericidal properties

PubMed Central

Banala, Rajkiran Reddy; Nagati, Veera Babu; Karnati, Pratap Reddy

2015-01-01

The evolution of nanotechnology and the production of nanomedicine from various sources had proven to be of intense value in the field of biomedicine. The smaller size of nanoparticles is gaining importance in research for the treatment of various diseases. Moreover the production of nanoparticles is eco-friendly and cost effective. In the present study silver nanoparticles were synthesized from Carica papaya leaf extract (CPL) and characterized for their size and shape using scanning electron microscopy and transmission electron microscopy, respectively. Fourier transform infrared spectroscopy (FTIR), Energy dispersive X-ray spectroscopy (EDS/EDX) and X-ray diffraction spectroscopy (XRD) were conducted to determine the concentration of metal ions, the shape of molecules. The bactericidal activity was evaluated using Luria Bertani broth cultures and the minimum inhibition concentration (MIC) and minimum bactericidal concentration (MBC) were estimated using turbidimetry. The data analysis showed size of 50–250 nm spherical shaped nanoparticles. The turbidimetry analysis showed MIC and MBC was >25 μg/mL against both Gram positive and Gram negative bacteria in Luria Bertani broth cultures. In summary the synthesized silver nanoparticles from CPL showed acceptable size and shape of nanoparticles and effective bactericidal activity. PMID:26288570

Green synthesis and characterization of Carica papaya leaf extract coated silver nanoparticles through X-ray diffraction, electron microscopy and evaluation of bactericidal properties.

PubMed

Banala, Rajkiran Reddy; Nagati, Veera Babu; Karnati, Pratap Reddy

2015-09-01

The evolution of nanotechnology and the production of nanomedicine from various sources had proven to be of intense value in the field of biomedicine. The smaller size of nanoparticles is gaining importance in research for the treatment of various diseases. Moreover the production of nanoparticles is eco-friendly and cost effective. In the present study silver nanoparticles were synthesized from Carica papaya leaf extract (CPL) and characterized for their size and shape using scanning electron microscopy and transmission electron microscopy, respectively. Fourier transform infrared spectroscopy (FTIR), Energy dispersive X-ray spectroscopy (EDS/EDX) and X-ray diffraction spectroscopy (XRD) were conducted to determine the concentration of metal ions, the shape of molecules. The bactericidal activity was evaluated using Luria Bertani broth cultures and the minimum inhibition concentration (MIC) and minimum bactericidal concentration (MBC) were estimated using turbidimetry. The data analysis showed size of 50-250 nm spherical shaped nanoparticles. The turbidimetry analysis showed MIC and MBC was >25 μg/mL against both Gram positive and Gram negative bacteria in Luria Bertani broth cultures. In summary the synthesized silver nanoparticles from CPL showed acceptable size and shape of nanoparticles and effective bactericidal activity.

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.

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.

Investigation of electrochemical migration on Sn-0.7Cu-0.3Ag-0.03P-0.005Ni solder alloy in HNO{sub 3} solution

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

Sarveswaran, C.; Othman, N. K.; Ali, M. Yusuf Tura

2015-09-25

Current issue in lead-free solder in term of its reliability is still under investigation. This high impact research attempts to investigate the electrochemical migration (ECM) on Sn-0.7Cu-0.3Ag-0.03P-0.005Ni solder alloy by Water Drop Test (WDT) in different concentration of HNO{sub 3} solution. The concentration of HNO{sub 3} solution used in this research was 0.05, 0.10, 0.50 and 1M. Optical Microscope (OM), Field Emission Scanning Electron Microscope (FESEM) and Energy Dispersive X-Ray Analysis (EDX) were carried out in order to analysis the ECM behavior based on the growth of dendrite formation after WDT. In general, the results demonstrated that dendrite growth ismore » faster in higher concentration compared with low concentration of HNO{sub 3}. The concentration of HNO{sub 3} solution used has a strong correlation with Mean-Time-To-Failure (MTTF). As the concentration of HNO{sub 3} increases, the MTTF value decreases. Based on the MTTF results the solder alloy in 1M HNO{sub 3} solution is most susceptible to ECM. SnO{sub 2} forms as a corrosion by-product in the samples proved by EDX analysis. The solder alloy poses a high reliability risk in microelectronic devices during operation in 1M HNO{sub 3} solution.« less

Characterization of ball-milled carbon nanotube dispersed aluminum mixed powders

NASA Astrophysics Data System (ADS)

Maleque, M. A.; Abdullah, U.; Yaacob, I.; Ali, Y.

2016-04-01

Currently, carbon nanotube (CNT) is attracting much interest as fibrous materials for reinforcing aluminum matrix composites due to unique properties, such as high strength, elastic modulus, flexibility and high aspect ratios. However, the quality of the dispersion is the major concerning factor which determines the homogeneity of the enhanced mechanical and tribological properties of the composite. This work study and characterized carbon nanotube dispersion in ballmilled CNT-aluminum mixed powders with four different formulations such as 1, 1.5, 2 and 2.5 wt% CNT under high energy planetary ball milling operations. The ball milling was performed for two hours at constant milling speed of 250 rpm under controlled atmosphere. The characterization is performed using FESEM and EDX analyzer for mapping, elemental and line analysis. The experimental results showed homogeneous dispersion of CNTs in aluminum matrix. The composite mixture showed similar pattern from mapping, elemental and line analysis. Identification of only two peaks proved that controlled atmosphere during milling prevented the formation of inter metallic compounds such as aluminum carbide in the composite mixture. Therefore, this CNT-A1 composite powder mixture can be used for new nano-composite development without any agglomeration problem.

Hexavalent chromium reduction potential of Cellulosimicrobium sp. isolated from common effluent treatment plant of tannery industries.

PubMed

Bharagava, Ram Naresh; Mishra, Sandhya

2018-01-01

Present study deals with the isolation and characterization of a bacterium capable for the effective reduction of Cr(VI) from tannery wastewater. Based on the 16S rRNA gene sequence analysis, this bacterium was identified as Cellulosimicrobium sp. (KX710177). During the Cr(VI) reduction experiment performed at 50, 100, 200,and 300mg/L of Cr(VI) concentrations, the bacterium showed 99.33% and 96.98% reduction at 50 and 100mg/L at 24 and 96h, respectively. However, at 200 and 300mg/L concentration of Cr(VI), only 84.62% and 62.28% reduction was achieved after 96h, respectively. The SEM analysis revealed that bacterial cells exposed to Cr(VI) showed increased cell size in comparison to unexposed cells, which might be due to either the precipitation or adsorption of reduced Cr(III) on bacterial cells. Further, the Energy Dispersive X-ray (EDX) analysis showed some chromium peaks for cells exposed to Cr(VI), which might be either due to the presence of precipitated reduced Cr(III) on cells or complexation of Cr(III) with cell surface molecules. The bacterium also showed resistance and sensitivity against the tested antibiotics with a wide range of MIC values ranging from 250 to 800mg/L for different heavy metals. Thus, this multi-drug and multi-metal resistant bacterium can be used as a potential agent for the effective bioremediation of metal contaminated sites. Copyright © 2017 Elsevier Inc. All rights reserved.

Preparation and characterization of mechanically alloyed AB3-type based material LaMg2Ni5Al4 and its solid-gaz hydrogen storage reaction

NASA Astrophysics Data System (ADS)

Jaafar, Hassen; Aymard, Luc; Dachraoui, Walid; Demortière, Arnaud; Abdellaoui, Mohieddine

2018-04-01

We developed in the present paper the synthesis of a new AB3-type compound LaMg2Ni5Al4 by mechanical alloying (MA) process. ​​X-ray diffraction analysis (XRD) was used to determine the structural properties and the phase evolution of the powder mixtures. Two different synthesis pathways have been investigated. The first starting from elemental metals and the second from a mixture of two binary compounds LaNi5 (CaCu5-type structure, P6/mmm space group) and Al(Mg) solid solution (cubic Fm-3 m space group). The results show multiphase alloys which contain LaMg2Ni5Al4 main phase with hexagonal PuNi3-type structure (R-3 m space group). Rietveld analysis shows that using a planetary ball mill, we obtain a good yield of LaMg2Ni5Al4 compound after 5 h of mechanical alloying for both synthesis pathways. TEM analysis confirmed XRD results. SEM-EDX analysis of the final product was in agreement with the nominal chemical formula. A setup of possible solid-gaz hydrogenation reaction will be described so far at the end of this work. Electrochemical results demonstrate evidence on hydrogen absorption in the AB3 material and the discharge capacity was equal to 5.9 H/f.u.

Potassium-doped n-type bilayer graphene

NASA Astrophysics Data System (ADS)

Yamada, Takatoshi; Okigawa, Yuki; Hasegawa, Masataka

2018-01-01

Potassium-doped n-type bilayer graphene was obtained. Chemical vapor deposited bilayer and single layer graphene on copper (Cu) foils were used. After etching of Cu foils, graphene was dipped in potassium hydroxide aqueous solutions to dope potassium. Graphene on silicon oxide was characterized by X-ray photoelectron spectroscopy (XPS), energy dispersive X-ray spectroscopy (EDX), and Raman spectroscopy. Both XPS and EDX spectra indicated potassium incorporation into the bilayer graphene via intercalation between the graphene sheets. The downward shift of the 2D peak position of bilayer graphene after the potassium hydroxide (KOH) treatment was confirmed in Raman spectra, indicating that the KOH-treated bilayer graphene was doped with electrons. Electrical properties were measured using Hall bar structures. The Dirac points of bilayer graphene were shifted from positive to negative by the KOH treatment, indicating that the KOH-treated bilayer graphene was n-type conduction. For single layer graphene after the KOH treatment, although electron doping was confirmed from Raman spectra, the peak of potassium in the X-ray photoelectron spectroscopy (XPS) spectrum was not detected. The Dirac points of single layer graphene with and without the KOH treatment showed positive.

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.

Neurite outgrowth stimulatory effects of myco synthesized AuNPs from Hericium erinaceus (Bull.: Fr.) Pers. on pheochromocytoma (PC-12) cells

PubMed Central

Raman, Jegadeesh; Lakshmanan, Hariprasath; John, Priscilla A; Zhijian, Chan; Periasamy, Vengadesh; David, Pamela; Naidu, Murali; Sabaratnam, Vikineswary

2015-01-01

Background Hericium erinaceus has been reported to have a wide range of medicinal properties such as stimulation of neurite outgrowth, promotion of functional recovery of axonotmetic peroneal nerve injury, antioxidant, antihypertensive, and antidiabetic properties. In recent years, the green synthesis of gold nanoparticles (AuNPs) has attracted intense interest due to the potential use in biomedical applications. The aim of this study was to investigate the effects of AuNPs from aqueous extract of H. erinaceus on neurite outgrowth of rat pheochromocytoma (PC-12) cells. Methods The formation of AuNPs was characterized by UV–visible spectrum, energy dispersive X-ray (EDX), field-emission scanning electron microscope (FESEM), transmission electron microscopy (TEM), particle size distribution, and Fourier transform-infrared spectroscopy (FTIR). Furthermore, the neurite extension study of synthesized AuNPs was evaluated by in vitro assay. Results The AuNPs exhibited maximum absorbance between 510 and 600 nm in UV–visible spectrum. FESEM and TEM images showed the existence of nanoparticles with sizes of 20–40 nm. FTIR measurements were carried out to identify the possible biomolecules responsible for capping and efficient stabilization of the nanoparticles. The purity and the crystalline properties were confirmed by EDX diffraction analysis, which showed strong signals with energy peaks in the range of 2–2.4 keV, indicating the existence of gold atoms. The synthesized AuNPs showed significant neurite extension on PC-12 cells. Nerve growth factor 50 ng/mL was used as a positive control. Treatment with different concentrations (nanograms) of AuNPs resulted in neuronal differentiation and neuronal elongation. AuNPs induced maximum neurite outgrowth of 13% at 600 ng/mL concentration. Conclusion In this study, the AuNPs synthesis was achieved by a simple, low-cost, and rapid bioreduction approach. AuNPs were shown to have potential neuronal differentiation and stimulated neurite outgrowth. The water-soluble bioconstituents could be responsible for the neuroactivity. This is the first report for the biosynthesis of AuNPs using the hot aqueous extract of H. erinaceus. PMID:26425086

Neurite outgrowth stimulatory effects of myco synthesized AuNPs from Hericium erinaceus (Bull.: Fr.) Pers. on pheochromocytoma (PC-12) cells.

PubMed

Raman, Jegadeesh; Lakshmanan, Hariprasath; John, Priscilla A; Zhijian, Chan; Periasamy, Vengadesh; David, Pamela; Naidu, Murali; Sabaratnam, Vikineswary

2015-01-01

Hericium erinaceus has been reported to have a wide range of medicinal properties such as stimulation of neurite outgrowth, promotion of functional recovery of axonotmetic peroneal nerve injury, antioxidant, antihypertensive, and antidiabetic properties. In recent years, the green synthesis of gold nanoparticles (AuNPs) has attracted intense interest due to the potential use in biomedical applications. The aim of this study was to investigate the effects of AuNPs from aqueous extract of H. erinaceus on neurite outgrowth of rat pheochromocytoma (PC-12) cells. The formation of AuNPs was characterized by UV-visible spectrum, energy dispersive X-ray (EDX), field-emission scanning electron microscope (FESEM), transmission electron microscopy (TEM), particle size distribution, and Fourier transform-infrared spectroscopy (FTIR). Furthermore, the neurite extension study of synthesized AuNPs was evaluated by in vitro assay. The AuNPs exhibited maximum absorbance between 510 and 600 nm in UV-visible spectrum. FESEM and TEM images showed the existence of nanoparticles with sizes of 20-40 nm. FTIR measurements were carried out to identify the possible biomolecules responsible for capping and efficient stabilization of the nanoparticles. The purity and the crystalline properties were confirmed by EDX diffraction analysis, which showed strong signals with energy peaks in the range of 2-2.4 keV, indicating the existence of gold atoms. The synthesized AuNPs showed significant neurite extension on PC-12 cells. Nerve growth factor 50 ng/mL was used as a positive control. Treatment with different concentrations (nanograms) of AuNPs resulted in neuronal differentiation and neuronal elongation. AuNPs induced maximum neurite outgrowth of 13% at 600 ng/mL concentration. In this study, the AuNPs synthesis was achieved by a simple, low-cost, and rapid bioreduction approach. AuNPs were shown to have potential neuronal differentiation and stimulated neurite outgrowth. The water-soluble bioconstituents could be responsible for the neuroactivity. This is the first report for the biosynthesis of AuNPs using the hot aqueous extract of H. erinaceus.

Modifying glass fiber surface with grafting acrylamide by UV-grafting copolymerization for preparation of glass fiber reinforced PVDF composite membrane.

PubMed

Luo, Nan; Zhong, Hui; Yang, Min; Yuan, Xing; Fan, Yaobo

2016-01-01

Experimental design and response surface methodology (RSM) were used to optimize the modification of conditions for glass surface grafting with acrylamide (AM) monomer for preparation of a glass fiber reinforced poly(vinylidene fluoride) (PVDF) composite membrane (GFRP-CM). The factors considered for experimental design were the UV (ultraviolet)-irradiation time, the concentrations of the initiator and solvent, and the kinds and concentrations of the silane coupling agent. The optimum operating conditions determined were UV-irradiation time of 25 min, an initiator concentration of 0-0.25 wt.%, solvent of N-Dimethylacetamide (DMAC), and silane coupling agent KH570 with a concentration of 7 wt.%. The obtained optimal parameters were located in the valid region and the experimental confirmation tests conducted showed good accordance between predicted and experimental values. Under these optimal conditions, the water absorption of the grafted modified glass fiber was improved from 13.6% to 23%; the tensile strength was enhanced and the peeling strength of the glass fiber reinforced PVDF composite membrane was improved by 23.7% and 32.6% with an AM concentration at 1 wt.% and 2 wt.%. The surface composition and microstructure of AM grafted glass fiber were studied via several techniques including Field Emission Scanning Electron Microscopy (FESEM), Fourier transform infrared spectroscopy-attenuated total reflectance (FTIR-ATR) and energy dispersive X-ray spectroscopy (EDX). The analysis of the EDX and FTIR-ATR results confirmed that the AM was grafted to the glass fiber successfully by detecting and proving the existence of nitrogen atoms in the GFRP-CM. Copyright © 2015. Published by Elsevier B.V.

Surface-pattern geometry, topography, and chemical modifications during KrF excimer laser micro-drilling of p-type Si (111) wafers in ambient environment of HCl fumes in air

NASA Astrophysics Data System (ADS)

Zakria Butt, Muhammad; Saher, Sobia; Waqas Khaliq, Muhammad; Siraj, Khurram

2016-11-01

Eight mirror-like polished p-type Si (111) wafers were irradiated with 100, 200, 300, 400, 800, 1200, 1600, and 2000 KrF excimer laser pulses in ambient environment of HCl fumes in air. The laser parameters were: wavelength = 248 nm, pulse width = 20 ns, pulse energy = 20 mJ, and repetition rate = 20 Hz. For each set of laser pulses, characterization of the rectangular etched patterns formed on target surface was done by optical/scanning electron microscopy, XRD, and EDX techniques. The average etched depth increased with the increase in number of laser pulses from 100 to 2000 in accord with Sigmoidal (Boltzmann) function, whereas the average etch rate followed an exponential decay with the increase in number of laser pulses. However, the etched area, maximum etched depth, and maximum etch rate were found to increase linearly with the number of laser pulses, but the rate of increase was faster for 100-400 laser pulses (region I) than that for 800-2000 laser pulses (region II). The elemental composition for each etched-pattern determined by EDX shows that both O and Cl contents increase progressively with the increase in the number of laser shots in region I. However, in region II both O and Cl contents attain saturation values of about 39.33 wt.% and 0.14 wt.%, respectively. Perforation of Si wafers was achieved on irradiation with 1200-2000 laser pulses. XRD analysis confirmed the formation of SiO2, SiCl2 and SiCl4 phases in Si (111) wafers due to chemical reaction of silicon with both HCl fumes and oxygen in air.

Observation and Analysis of In Situ Carbonaceous Matter in Naklha. Part 2

NASA Technical Reports Server (NTRS)

Gibson, E. K., Jr.; Clemett, S. J.; Thomas-Kerpta, K. L.; McKay, D. S.; Wentworth, S. J.; Robert, F.; Verchovsky, A. B.; Wright, I. P.; Pillinger, C. T.; Rice, T.;

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.

Develop Techniques for Ion Implantation of PLZT for Adaptive Optics

DTIC Science & Technology

1989-11-01

WL-TR-89-26 FIGURES (Continued) Fizure Page 20 EDX elemental spectrum from perovskite region of the sample shown in Fig. 15. 65 21 EDX elemental...pyroelectric response. 126 84 Result of doping PZT with La and Mn (Ref. 7). 127 85 APW results along the lin for several perovskite - type compounds and ReO 2...structure of the calcined powder was analyzed and shown to be mainly the hexagonal/rhombohedral phase within 17 WL-TR-89-26 the perovskite structure of

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.

Investigation of the effectiveness of nutrient release from sludge foam after hybrid pretreatment processes by IR analysis and EDX Quantification.

PubMed

Machnicka, Alicja; Grübel, Klaudiusz

2016-12-01

One of the problems in wastewater treatment technologies is the formation of foam/scum. It is thought that filamentous microorganisms are responsible for foam formation and foam elimination/destruction can be carried out by various methods, among which disintegration is included. Hybrid disintegration (chemical decomposition and hydrodynamic cavitation) of foam microorganisms results in the transfer of phosphates, ammonium nitrogen, magnesium and potassium from the foam solids into the liquid phase. Application of both methods as a hybrid pretreatment process caused an increase in the concentration of phosphates of about 650 mg [Formula: see text] L(-1) and ammonium nitrogen of about 30 mg [Formula: see text] L(-1). The concentration of Mg(2+) and K(+) in the solution increased from 6.8 and 26.1 mg Mg(2+) L(-1) to 32.2 and 82.2 mg K(+) L(-1), respectively. The presence of nutrients and metal cations in the solid phase of foam was acknowledged by EDX Quantification. The confirmation of physico-chemical changes and release of cellular matter as a result of cellular lysis (hybrid disintegration) was done by infrared analysis. It was demonstrated that the disintegration of foam permits the removal of a part of nutrients in the form of struvite.

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.

Synthesis of zinc sulfide nanoparticles and their incorporation into poly(hydroxybutyrate) matrix in the formation of a novel nanocomposite

NASA Astrophysics Data System (ADS)

Riaz, Shahina; Raza, Zulfiqar Ali; Majeed, Muhammad Irfan; Jan, Tariq

2018-05-01

In the present study, zinc sulfide (ZnS) nanoparticles (NPs) were successfully synthesized through a modified chemical precipitation protocol and then mediated into poly(hydroxybutyrate) (PHB) matrix to get ZnS/PHB nanocomposite. Mean diameter and zeta potential of ZnS NPs, as determined using dynamic light scattering technique (DLS), were observed to be 53 nm and ‑89 mV, respectively. The structural investigations performed using x-ray diffraction (XRD) technique depicted the phase purity of ZnS NPs exhibiting cubic crystal structure. Fourier transform infrared (FTIR) spectroscopic analysis was conducted to identify the presence or absence of bonding vibrational modes on the surface of synthesized single phase ZnS NPs. The FTIR analysis confirmed the metal to sulphur bond formation by showing the characteristic band at 1123 cm‑1. The UV–vis absorption spectra of ZnS NPs confirmed the synthesis of particles in nanoscale regime showing a λ max of 302 nm. These NPs were then successfully incorporated into PHB matrix to synthesize ZnS/PHB nanocomposite. The synthesis of nanocomposite was confirmed by EDX analysis. The chemical bonding and structural properties of ZnS/PHB nanocomposite were determined by FTIR and XRD analysis, respectively. The FTIR analysis confirmed the synthesis of ZnS/PHB nanocomposite. Moreover, XRD analysis showed that structure of nanocomposite was completely controlled by ZnS NPs as pure PHB exhibited orthorhombic crystal structure while the nanocomposite demonstrated cubic crystal structure of ZnS. Thermal properties of nanocomposite were studied through thermogravimetric analysis revealing that the incorporation of ZnS NPs into PHB matrix lead to enhance heat resistance properties of PHB.

Analysis of the co-deposition of Al2O3 particles with nickel by an electrolytic route: The influence of organic additives presence and Al2O3 concentration

NASA Astrophysics Data System (ADS)

Temam, H. B.; Temam, E. G.

2016-04-01

Alloy coatings were prepared by co-deposition of Al2O3 particles in Ni matrix on carbon steel substrate from nickel chloride bath in which metallic powders were held in suspension. The influence of metal powder amount in the bath on chemical composition, morphology, thickness, microhardness and corrosion behavior of obtained coatings, has been investigated. It was shown that the presence of Al2O3 particles in deposit greatly improves the hardness and the wear resistance of alloy coatings. Characterization by microanalysis (EDX) of the various deposits elaborated confirms that the rate of particles incorporated increases as the concentration of solid particles increasing. The results showed that the presence of organic additives in Ni-Al2O3 electrolyte deposition led to an increase in the hardness and corrosion resistance of the deposits.

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.

Transport of silver nanoparticles in single fractured sandstone

NASA Astrophysics Data System (ADS)

Neukum, Christoph

2018-02-01

Silver nanoparticles (Ag-NP) are used in various consumer products and are one of the most prevalent metallic nanoparticle in commodities and are released into the environment. Transport behavior of Ag-NP in groundwater is one important aspect for the assessment of environmental impact and protection of drinking water resources in particular. Ag-NP transport processes in saturated single-fractured sandstones using triaxial flow cell experiments with different kind of sandstones is investigated. Ag-NP concentration and size are analyzed using flow field-flow fractionation and coupled SEM-EDX analysis. Results indicate that Ag-NP are more mobile and show generally lower attachment on rock surface compared to experiments in undisturbed sandstone matrix and partially fractured sandstones. Ag-NP transport is controlled by the characteristics of matrix porosity, time depending blocking of attachment sites and solute chemistry. Where Ag-NP attachment occur, it is heterogeneously distributed on the fracture surface.

High T(sub c) superconductor/ferroelectric heterostructures

NASA Astrophysics Data System (ADS)

Ryder, Daniel F., Jr.

1994-12-01

Thin films of the ferroelectric perovskite, Ba(x) Sr(1-x) TiO3 (BST), were deposited on superconducting (100)YBa2Cu3O(x)(YBCO)/ (100)Yttria-stabilized zirconia(YSZ) substrates and (100)Si by ion-beam sputtering. Microstructural and compositional features of the ceramic bilayer were assessed by a combination of x-ray diffraction (XRD) and scanning electron microscopy. The films were smooth and featureless, and energy dispersive x-ray spectroscopy (EDX) data indicated that film composition closely matched target composition. XRD analysis showed that films deposited on YBCO substrates were highly c-axis textured, while the films deposited on (100)Si did not exhibit any preferred growth morphology. The superconducting properties of the YBCO substrate layer were maintained throughout the processing stages and, as such, it was demonstrated that ion beam sputtering is a viable method for the deposition of Ferroelectric/YBCO heterostructures.

Effect of nitric acid treatment on activated carbon derived from oil palm shell

NASA Astrophysics Data System (ADS)

Allwar, Allwar; Hartati, Retno; Fatimah, Is

2017-03-01

The primary object of this work is to study the effect of nitric acid on the porous and morphology structure of activated carbon. Production of activated carbon from oil palm shell was prepared with pyrolysis process at temperature 900°C and by introduction of 10 M nitric acid. Determination of surface area, pore volume and pore size distribution of activated carbon was conducted by the N2 adsorption-desorption isotherm at 77 K. Morphology structure and elemental micro-analysis of activated carbon were estimated by Scanning Electron Microscopy (SEM) and energy dispersive X-ray (EDX), respectively. The result shows that activated carbon after treating with nitric acid proved an increasing porous characteristics involving surface area, pore volume and pore size distribution. It also could remove the contaminants including metals and exhibit an increasing of pores and crevices all over the surface.

Thermoluminescence properties of CaO powder obtained from chicken eggshells

NASA Astrophysics Data System (ADS)

Nagabhushana, K. R.; Lokesha, H. S.; Satyanarayana Reddy, S.; Prakash, D.; Veerabhadraswamy, M.; Bhagyalakshmi, H.; Jayaramaiah, J. R.

2017-09-01

Eggshell wastage has created serious problem in disposal of the food processing industry which has been triggered the thoughts of researchers to use wasted eggshells as good source of calcium. In the present work, calcium oxide (CaO) has been synthesized by combustion process in furnace (F-CaO) and microwave oven (M-CaO) using the source of chicken eggshells. The obtained F-CaO and M-CaO are characterized by XRD, SEM with EDX and thermoluminescence (TL) technique. XRD pattern of both the samples show cubic phase with crystallite size 45-52 nm. TL glow curves are recorded for various gamma radiation dose (300-4000 Gy). Two TL glows, a small peak at 424 K and stronger peak at 597 K are observed. TL response of M-CaO is 2.67 times higher than F-CaO sample. TL kinetic parameters are calculated by computerized curve deconvolution analysis (CCDA) and discussed.

A New Green Ionic Liquid-Based Corrosion Inhibitor for Steel in Acidic Environments.

PubMed

Atta, Ayman M; El-Mahdy, Gamal A; Al-Lohedan, Hamad A; Ezzat, Abdel Rahman O

2015-06-17

This work examines the use of new hydrophobic ionic liquid derivatives, namely octadecylammonium tosylate (ODA-TS) and oleylammonium tosylate (OA-TS) for corrosion protection of steel in 1 M hydrochloric acid solution. Their chemical structures were determined from NMR analyses. The surface activity characteristics of the prepared ODA-TS and OA-TS were evaluated from conductance, surface tension and contact angle measurements. The data indicate the presence of a double bond in the chemical structure of OA-TS modified its surface activity parameters. Potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) measurements, scanning electron microscope (SEM), Energy dispersive X-rays (EDX) analysis and contact angle measurements were utilized to investigate the corrosion protection performance of ODA-TS and OA-TS on steel in acidic solution. The OA-TS and ODA-TS compounds showed good protection performance in acidic chloride solution due to formation of an inhibitive film on the steel surface.

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.

Effect of Carbon Nanotubes on Corrosion and Tribological Properties of Pulse-Electrodeposited Co-W Composite Coatings

NASA Astrophysics Data System (ADS)

Edward Anand, E.; Natarajan, S.

2015-01-01

Cobalt-Tungsten (Co-W) alloy coatings possessing high hardness and wear/corrosion resistance, due to their ecofriendly processing, have been of interest to the researchers owing to its various industrial applications in automobile, aerospace, and machine parts. This technical paper reports Co-W alloy coatings dispersed with multiwalled carbon nanotubes (MWCNTs) produced by pulse electrodeposition from aqueous bath involving cobalt sulfate, sodium tungstate, and citric acid on stainless steel substrate (SS316). Studies on surface morphology through SEM, microhardness by Vickers method, microwear by pin-on-disk method, and corrosion behavior through potentiodynamic polarization method for the Co-W-CNT coatings were reported. Characterization studies were done by SEM and EDX analysis. The results showed that the corrosion and tribological properties of the pulse-electrodeposited Co-W-CNT alloy coatings were greatly influenced by its morphology, microhardness, %W, and MWCNT content in the coatings.

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.

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.

Composition and distribution of elements and ultrastructural topography of a human cardiac calculus.

PubMed

Cheng, Ching-Li; Chang, Hsiao-Huang; Huang, Pei-Jung; Chu, Yu-Ting; Lin, Shan-Yang

2013-04-01

Trace elements (TEs) may contribute to the formation of calculi or stones or be involved in the aetiopathogenesis of stone diseases. The compositions and spatial distribution of elements from the inner nucleus to outer crust of the cardiac calculus were investigated by energy-dispersive X-ray fluorescence (EDXRF) spectrometer. The surface topograph, distribution map of elements, elemental and chemical compositions were also determined by environmental scanning electron microscope (ESEM)-energy-dispersive X-ray (EDX) analysis. Twenty-five elements were identifiable from 18 positions on the cardiac calculus by EDXRF spectrometer, in which the highest concentrations of toxic TEs (Ni, Pt, Hg, Sn, Pb, W, Au, Al, Si) and higher levels of essential TEs (Ca, Sr, Cr, P) were detected. A moderate positive Pearson's correlation between TEs concentrations of Mg, Ca or P and location differences from centre to periphery in the cardiac calculus was observed. A positive correlation was also found for Ca/Zn and Ca/Cu, indicating the gradual increase of calcium concentration from inner nucleus to outer crust of cardiac calculus. The drop-like nodules/crystals on the surface of petrous part of cardiac calculus were observed from ESEM analysis. ESEM-EDX analysis determined the calculus to be predominantly composed of calcium hydroxyapatite and cholesterol, as indicated by the petrous surface and drop-like nodules/crystals, respectively. This composition was confirmed using a portable Raman analyser. The spatial distribution analysis indicated a gradual increase in Mg, P and Ca concentrations from the inner nucleus to the outer crust of the cardiac calculus. The major chemical compositions of calcium hydroxyapatite and cholesterol were detected on this cardiac calculus.

Effect of bismuth oxide on white mineral trioxide aggregate: chemical characterization and physical properties.

PubMed

Grazziotin-Soares, R; Nekoofar, M H; Davies, T E; Bafail, A; Alhaddar, E; Hübler, R; Busato, A L S; Dummer, P M H

2014-06-01

To assess the effect of bismuth oxide (Bi2 O3 ) on the chemical characterization and physical properties of White mineral trioxide aggregate (MTA) Angelus. Commercially available White MTA Angelus and White MTA Angelus without Bi2 O3 provided by the manufacturer especially for this study were subjected to the following tests: Rietveld X-ray diffraction analysis (XRD), energy-dispersive X-ray analysis (EDX), scanning electron microscopy (SEM), compressive strength, Vickers microhardness test and setting time. Chemical analysis data were reported descriptively, and physical properties were expressed as means and standard deviations. Data were analysed using Student's t-test and Mann-Whitney U test (P = 0.05). Calcium silicate peaks were reduced in the diffractograms of both hydrated materials. Bismuth particles were found on the surface of White MTA Angelus, and a greater amount of particles characterized as calcium hydroxide was observed by visual examination on White MTA without Bi2 O3 . The material without Bi2 O3 had the shortest final setting time (38.33 min, P = 0.002), the highest Vickers microhardness mean value (72.35 MPa, P = 0.000) and similar compressive strength results (P = 0.329) when compared with the commercially available White MTA Angelus containing Bi2 O3 . The lack of Bi2 O3 was associated with an increase in Vickers microhardness, a reduction in final setting time, absence of Bi2 O3 peaks in diffractograms, as well as a large amount of calcium and a morphology characteristic of calcium hydroxide in EDX/SEM analysis. © 2013 International Endodontic Journal. Published by John Wiley & Sons Ltd.

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.

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.

Isolation and characterization of Bacillus cereus IST105 from electroplating effluent for detoxification of hexavalent chromium.

PubMed

Naik, Umesh Chandra; Srivastava, Shaili; Thakur, Indu Shekhar

2011-08-01

Electroplating industries are the main sources of heavy metals, chromium, nickel, lead, zinc, cadmium and copper. The highest concentrations of chromium (VI) in the effluent cause a direct hazards to human and animals. Therefore, there is a need of an effective and affordable biotechnological solution for removal of chromium from electroplating effluent. Bacterial strains were isolated from electroplating effluent to find out higher tolerant isolate against chromate. The isolate was identified by 16S rDNA sequence analysis. Absorbed chromium level of bacterium was determined by inductively coupled plasma-atomic emission spectrometer (ICP-AES), atomic absorption spectrophotometer (AAS), scanning electron microscope (SEM), transmission electron microscope (TEM) and energy dispersive X-ray analysis (EDX). Removal of metals by bacterium from the electroplating effluent eventually led to the detoxification of effluent confirmed by MTT assay. Conformational changes of functional groups of bacterial cell surface were studied through Fourier transform infrared spectroscopy. The chromate tolerant isolate was identified as Bacillus cereus. Bacterium has potency to remove more than 75% of chromium as measured by ICP-AES and AAS. The study indicated the accumulation of chromium (VI) on bacterial cell surface which was confirmed by the SEM-EDX and TEM analysis. The biosorption of metals from the electroplating effluent eventually led to the detoxification of effluent. The increased survivability of Huh7 cells cultured with treated effluent also confirmed the detoxification as examined by MTT assay. Isolated strain B. cereus was able to remove and detoxify chromium (VI). It would be an efficient tool of the biotechnological approach in mitigating the heavy metal pollutants.

Compositional analysis of projectile residues on LDEF instrument AO187-1

NASA Technical Reports Server (NTRS)

Bernhard, Ronald P.; Horz, F.

1992-01-01

Impact craters greater than 30 microns and associated projectile residues were analyzed by Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Analysis (EDXA). Objectives were to analyze a statistically significant number of projectiles to evaluate their chemical variability and possible clustering into discrete particle types. Bay A11 exposed six collector surfaces of anodized 1100-T4 (greater than 99 percent pure) aluminum sheets, 0.32 cm thick, yielding an exposed surface area of 1.1 sq. m. Four of the six panels have been retained at JSC, and were optically scanned, one (A11E00E) was prepared for SEM/EDX analysis. Bay A03 was occupied by high purity (99.99 percent) gold sheets, 0.5 mm thick, yielding an exposed surface area of 0.85 sq. m. Sample processing included the optical scanning (6X), labeling, and dislodging (by a punch-die device) of each individual impact greater than 75 microns for the aluminum and 30 microns for the gold. The 209 craters were dislodged form A11E00E, having crater diameters up to 3500 microns. Optical examination of the gold surfaces detected 238 craters, 198 of which were retained at JSC and analyzed via SEM/EDX. The analytical procedures included maximizing the geometric efficiency (take-off angles), using relatively long count times (500-1000 sec) and sufficiently high accelerating currents (25-30Kev). Despite diligent examination, a large number of craters did not exhibit measurable signals above background. Detectable resides were classified as either micrometeoritic or as man-made debris.

Nakhla: a Martian Meteorite with Indigenous Organic Carbonaceous Features

NASA Technical Reports Server (NTRS)

McKay, D. S.; Gibson, E. K.; Thomas-Keprta, K. L.; Clemett, S. J.; Le, L.; Rahman, Z.; Wentworth, S. J.

2011-01-01

The Nakhla meteorite possesses discrete, well defined, structurally coherent morphologies of carbonaceous phases present within iddingsite alteration zones. Based upon both isotopic measurements and analysis of organic phases the presence of pre-terrestrial organics is now recognized. Within the microcrystalline layers of Nakhla s iddingsite, discrete clusters of salt crystals are present. These salts are predominantly halite (NaCl) with minor MgCl2 crystals. Some CaSO4, likely gypsum, appears to be partially intergrown with some of the halite. EDX mapping shows discrete C-rich features are interspersed among these crystals. A hollow semi-spherical bowl structure ( 3 m ) has been identified and analyzed after using a focused ion beam (FIB) to cut a transverse TEM thin section of the feature and the underlying iddingsite. TEM/EDX analysis reveals that the feature is primarily carbonaceous containing C with lesser amounts of Si, S, Ca, Cl, F, Na, and minor Mn and Fe; additionally a small peak consistent with N, which has been previously seen in Nakhla carbonaceous matter, is also present. Selected area electron diffraction (SAED) shows that this C-rich material is amorphous (lacking any long-range crystallographic order) and is not graphite or carbonate. Micro-Raman spectra acquired from the same surface from which the FIB section was extracted demonstrate a typical kerogen-like D and G band structure with a weak absorption peak at 1350 and a stronger peak at 1600/cm. The C-rich feature is intimately associated with both the surrounding halite and underlying iddingsite matrix. Both iddingsite and salts are interpreted as having formed as evaporate assemblages from progressive evaporation of water bodies on Mars. This assemblage, sans the carbonaceous moieties, closely resembles iddingsite alteration features previously described which were interpreted as indigenous Martian assemblages. These distinctive macromolecular carbonaceous structures in Nakhla may represent one of the sources of the high molecular weight organic material previously identified in Nakhla. While we do not speculate on the origin of these unique carbonaceous structures, we note that the significance of such observations is that it may allow us to construct a C-cycle for Mars based on the C chemistry of the Martian meteorites with obvious implications for astrobiology and the prebiotic evolution of Mars. In any case, our observations strongly suggest that organic C exists as micrometersize, discrete structures on Mars.

Synthesis and Characterization of Polyethylene/Starch Nanocomposites: A Spherical Starch-Supported Catalyst and In Situ Ethylene Polymerization.

PubMed

Zhanga, Hao; Xi, Shixia; Wang, Shuwei; Liu, Jingsheng; Yoon, Keun-Byoung; Lee, Dong-Ho; Zhang, Hexin; Zhang, Xuequan

2017-01-01

In the present article, a novel spherical starch-supported vanadium (V)-based Ziegler-Natta catalyst was synthesized. The active centers of the obtained catalyst well dispersed in the starch through the SEM-EDX analysis. The effects of reaction conditions on ethylene polymerization were studied. The synthesized catalyst exhibited high activity toward ethylene polymerization in the presence of ethylaluminium sesquichloride (EASC) cocatalyst. Interestingly, the fiber shape PE was obtained directly during the polymerization process.

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.

The effect of milling time on the synthesis of Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy

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

Kursun, C., E-mail: celalkursun@ksu.edu.tr; Gogebakan, M., E-mail: gogebakan@ksu.edu.tr

In the present work, nanocrystalline Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy was produced by mechanical alloying from mixtures of pure crystalline Cu, Mg, Ti and Ni powders using a Fritsch planetary ball mill with a ball to powder ratio of 10:1. Morphological changes, microstructural evolution and thermal behaviour of the Cu-Mg-Ti-Ni powders at different stages of milling were characterised by X-ray diffraction (XRD), scanning electron microscopy with energy-dispersive X-ray detection (SEM/EDX) and differential thermal analysis (DTA). This alloy resulted in formation of single phase solid solution with FCC structure α-Cu (Mg, Ti, Ni) after 80 h of milling. In the initialmore » stage of milling different sized and shaped elemental powders became uniform during mechanical alloying. The homogeneity of the Cu{sub 54}Mg{sub 22}Ti{sub 18}Ni{sub 6} alloy increased with increasing milling time. The EDX result also confirmed the compositional homogeneity of the powder alloy. The crystallite size of alloy was calculated below 10 nm from XRD data.« less

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.

A Natural Experiment on the Condition-Dependence of Achromatic Plumage Reflectance in Black-Capped Chickadees

PubMed Central

D'Alba, Liliana; Van Hemert, Caroline; Handel, Colleen M.; Shawkey, Matthew D.

2011-01-01

Honest advertisement models posit that only individuals in good health can produce and/or maintain ornamental traits. Even though disease has profound effects on condition, few studies have experimentally tested its effects on trait expression and even fewer have identified a mechanistic basis for these effects. Recent evidence suggests that black and white, but not grey, plumage colors of black-capped chickadees (Poecile atricapillus) are sexually selected. We therefore hypothesized that birds afflicted with avian keratin disorder, a condition that affects the beak and other keratinized tissues, would show reduced expression of black and white, but not grey, color. UV-vis spectrometry of black-capped chickadees affected and unaffected by avian keratin disorder revealed spectral differences between them consistent with this hypothesis. To elucidate the mechanistic bases of these differences, we used scanning electron microscopy (SEM), electron-dispersive x-ray spectroscopy (EDX) and a feather cleaning experiment. SEM showed extreme feather soiling in affected birds, and EDX revealed that this was most likely from external sources. Experimentally cleaning the feathers increased color expression of ornamental feathers of affected, but not unaffected, birds. These data provide strong evidence that black and white color is an honest indicator in chickadees, and that variation in feather dirtiness, likely due to differences in preening behavior is a mechanism for this association. PMID:21991378

A natural experiment on the condition-dependence of achromatic plumage reflectance in black-capped chickadees.

PubMed

D'Alba, Liliana; Van Hemert, Caroline; Handel, Colleen M; Shawkey, Matthew D

2011-01-01

Honest advertisement models posit that only individuals in good health can produce and/or maintain ornamental traits. Even though disease has profound effects on condition, few studies have experimentally tested its effects on trait expression and even fewer have identified a mechanistic basis for these effects. Recent evidence suggests that black and white, but not grey, plumage colors of black-capped chickadees (Poecile atricapillus) are sexually selected. We therefore hypothesized that birds afflicted with avian keratin disorder, a condition that affects the beak and other keratinized tissues, would show reduced expression of black and white, but not grey, color. UV-vis spectrometry of black-capped chickadees affected and unaffected by avian keratin disorder revealed spectral differences between them consistent with this hypothesis. To elucidate the mechanistic bases of these differences, we used scanning electron microscopy (SEM), electron-dispersive x-ray spectroscopy (EDX) and a feather cleaning experiment. SEM showed extreme feather soiling in affected birds, and EDX revealed that this was most likely from external sources. Experimentally cleaning the feathers increased color expression of ornamental feathers of affected, but not unaffected, birds. These data provide strong evidence that black and white color is an honest indicator in chickadees, and that variation in feather dirtiness, likely due to differences in preening behavior is a mechanism for this association.

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.

A natural experiment on the condition-dependence of achromatic plumage reflectance in black-capped chickadees

USGS Publications Warehouse

D'Alba, L.; Van Hemert, C.; Handel, Colleen M.; Shawkey, M.D.

2011-01-01

Honest advertisement models posit that only individuals in good health can produce and/or maintain ornamental traits. Even though disease has profound effects on condition, few studies have experimentally tested its effects on trait expression and even fewer have identified a mechanistic basis for these effects. Recent evidence suggests that black and white, but not grey, plumage colors of black-capped chickadees (Poecile atricapillus) are sexually selected. We therefore hypothesized that birds afflicted with avian keratin disorder, a condition that affects the beak and other keratinized tissues, would show reduced expression of black and white, but not grey, color. UV-vis spectrometry of black-capped chickadees affected and unaffected by avian keratin disorder revealed spectral differences between them consistent with this hypothesis. To elucidate the mechanistic bases of these differences, we used scanning electron microscopy (SEM), electron-dispersive x-ray spectroscopy (EDX) and a feather cleaning experiment. SEM showed extreme feather soiling in affected birds, and EDX revealed that this was most likely from external sources. Experimentally cleaning the feathers increased color expression of ornamental feathers of affected, but not unaffected, birds. These data provide strong evidence that black and white color is an honest indicator in chickadees, and that variation in feather dirtiness, likely due to differences in preening behavior is a mechanism for this association.

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.

ZnO/TiO2 nanocomposite rods synthesized by microwave-assisted method for humidity sensor application

NASA Astrophysics Data System (ADS)

Ashok, CH.; Venkateswara Rao, K.

2014-12-01

The nanocomposite rods shows well known properties compared with nano structured materials for various applications like light-emitting diodes, electron field emitters, solar cells, optoelectronics, sensors, transparent conductors and fabrication of nano devices. Present paper investigates the properties of ZnO/TiO2 nanocomposite rods. The bi component of ZnO/TiO2 nanocomposite rods was synthesized by microwave-assisted method which is very simple, rapid and uniform in heating. The frequency of microwaves 2.45 GHz was used and temperature maintained 180 °C. Zinc acetate and titanium isopropoxide precursors were used in the preparation. The obtained ZnO/TiO2 nanocomposite rods were annealed at 500 °C and 600 °C. ZnO/TiO2 nanocomposite rods have been characterized by X-ray Diffraction (XRD) for average crystallite size and phase of the composite material, Particle Size Analyser (PSA) for average particle size, Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM) for morphology study, Energy Dispersive X-ray Spectrometry (EDX) for elemental analysis, and Thermal Gravimetric and Differential Thermal Analysis (TG-DTA) for thermal property.

Thermodynamic modeling of solid solutions between monosulfate and monochromate 3CaO Bullet Al{sub 2}O{sub 3} Bullet Ca[(CrO{sub 4}){sub x}(SO{sub 4}){sub 1-x}] Bullet nH{sub 2}O

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

Leisinger, Sabine M., E-mail: sabine.leisinger@eawag.ch; Institute of Biogeochemistry and Pollutant Dynamics, ETH, CH-8092 Zurich; Lothenbach, Barbara

2012-01-15

In hydrated cement paste AFm-phases are regarded to play an important role in the binding of the toxic contaminant chromate through isomorphic substitution with sulfate. Solid solutions formation can lower the solubility of the solids, thus reducing chromate leaching concentrations. Solid solutions between monosulfate and monochromate were synthesized and characterized by X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDX) and inductive coupled plasma optical emission spectroscopy (ICP-OES). Based on the measured ion concentrations in solution total solubility products of the solid solution series were determined. For pure monochromate a logK = - 28.4more » {+-} 0.7 was determined. Results from solid and solution analysis showed that limited solid solutions exist. Based on XRD diffractograms a solid solution with a miscibility gap 0.15 < Crx < 0.85 with a dimensionless Guggenheim parameter of 2.43 was proposed.« less

Analytical electron microscopy as a powerful tool in plant cell biology: examples using electron energy loss spectroscopy and X-ray microanalysis.

PubMed

Lichtenberger, O; Neumann, D

1997-08-01

Energy filtering transmission electron microscopy in combination with energy dispersive X-ray analysis (EDX) and quantumchemical calculations opens new possibilities for elemental and bone analysis at the ultrastructural level. The possibilities and limitations of these methods, applied to botanical samples, are discussed and some examples are given. Ca-oxalate crystals in plant cell vacuoles show a specific C K-edge in the electron energy loss spectrum (EELS), which allows a more reliable identification than light microscopical or cytochemical methods. In some dicots crystalline inclusions can be observed in different cell compartments, which are identified as silicon dioxide or calcium silicate by the fine structure of the Si L2,3-edge. Their formation is discussed on the basis of EEL-spectra and quantumchemical calculations. Examples concerning heavy metal detoxification are given for some tolerant plants. In Minuartia Zn is bound as Zn-silicate in cell walls; Armeria accumulates Cu in leaf idioblasts by chelation with phenolic compounds and Cd is precipitated as CdS/phytochelatin-complexes in tomato.

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.

Winter urban air particles from Rome (Italy): Effects on the monocytic-macrophagic RAW 264.7 cell line

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

Pozzi, Roberta; De Berardis, Barbara; Paoletti, Luigi

2005-11-15

Epidemiological data show an association between exposure to elevated levels of particulate matter (PM), in particular the fine fraction (<2.5{mu}m in diameter), and an increase in cardiovascular mortality and respiratory symptoms. The aim of this study was to compare the in vitro toxicity of coarse and fine particulate matter collected with a cascade impactor during winter in an urban area of Rome in relation to their physicochemical characterization (size distribution and chemical composition) as assessed by analytical electron microscopy (SEM/EDX). The X-ray microanalysis data of single particles of coarse and fine matter were analyzed by hierarchical cluster analysis to determinemore » the principal component of the two granulometric fractions. The main chemical difference between the two fractions was the greater abundance of carbonaceous particles in the fine fraction. We compared the ability of coarse and fine fractions, carbon black (CB), and residual oil fly ash (ROFA) to induce arachidonic acid release and tumor necrosis factor-{alpha} (TNF-{alpha}) production in the monocytic-macrophagic RAW 264.7 cell line at concentrations of 30 and 120{mu}g/mL. Our results showed that CB and ROFA were consistently less effective than both fractions of urban particles at inducing an inflammatory reaction in RAW 264.7 cells. Both PM fractions dose-dependently increased TNF-{alpha} production in RAW 264.7 cells after 5 and 24h of incubation, and only the TNF-{alpha} production induced by coarse particles at 30{mu}g/mL decreased significantly (P<0.01) after 24h of treatment. In our in vitro model the winter fine fraction was more reactive than the winter coarse fraction, in contrast to a previously examined summer sample. In the summer sample, coarse particles produced higher levels of inflammatory mediators than fine particles and the CB was consistently less effective than the urban particles. The different behaviors between summer and winter urban fractions may be due to their different physicochemical characteristics; in fact, the comparison of the two samples' characterization by SEM/EDX and X-ray photoelectron spectroscopy (XPS) analysis showed that in winter the carbonaceous particles are more abundant than in summer and that winter particles carry a greater quantity of organic compounds. We suggest that the higher concentration of organic compounds on fine carbonaceous particles may partially explain the higher activation of RAW 264.7 cells by fine particles.« less

Effect of rare earth doping on optical and spectroscopic characteristics of BaZrO3:Eu3+,Tb3+ perovskites.

PubMed

Katyayan, Shambhavi; Agrawal, Sadhana

2018-04-04

This paper reports structural investigations of rare earth doped BaZrO 3 phosphors synthesized by Solid state reaction technique with varying concentrations of Eu 3+ and Tb 3+ from 0 mol% to 2 mol%. The synthesized phosphors show enhanced variable emissions in the visible region corresponding to different hypersensitive electronic transitions of Eu 3+ and Tb 3+ ions. With cubic structure confirmed in XRD analysis, the FESEM images show uniform grain connectivity and homogeneity of prepared samples. The TEM micrographs of the synthesized phosphors show agglomerated irregular structures. The synthesized phosphors were also subjected to FTIR, Raman, EDXS analysis along with studies of thermoluminescent and photoluminescent characteristics. On subjecting to 229 nm (UV) excitation, the phosphors show enhanced PL emissions corresponding to 571 nm ( 5 D 0 - 7 F 0 ), 591 nm ( 5 D 0 - 7 F 1 ), 615 nm ( 5 D 0 - 7 F 2 ) and 678 nm ( 5 D 0 - 7 F 4 ) hypersensitive transitions of Eu 3+ ions and emission peaks at 489 nm ( 5 D 4 - 7 F 6 ), 539 nm ( 5 D 4 - 7 F 5 ), 589 nm ( 5 D 4 - 7 F 4 ) and 632 nm ( 5 D 4 - 7 F 3 ) accounting for electronic transitions of Tb 3+ ions respectively. The computed average PL lifetime is 14.014 s. In the TL analysis, the second order of kinetics with the activation energy varying from 5.0 × 10 -1 eV to 6.6 × 10 -1 eV is reported. The maximum TL lifetime is estimated as 19.4985 min in the TL lifetime analysis.

Effect of rare earth doping on optical and spectroscopic characteristics of BaZrO3:Eu3+,Tb3+ perovskites

NASA Astrophysics Data System (ADS)

Katyayan, Shambhavi; Agrawal, Sadhana

2018-06-01

This paper reports structural investigations of rare earth doped BaZrO3 phosphors synthesized by Solid state reaction technique with varying concentrations of Eu3+ and Tb3+ from 0 mol% to 2 mol%. The synthesized phosphors show enhanced variable emissions in the visible region corresponding to different hypersensitive electronic transitions of Eu3+ and Tb3+ ions. With cubic structure confirmed in XRD analysis, the FESEM images show uniform grain connectivity and homogeneity of prepared samples. The TEM micrographs of the synthesized phosphors show agglomerated irregular structures. The synthesized phosphors were also subjected to FTIR, Raman, EDXS analysis along with studies of thermoluminescent and photoluminescent characteristics. On subjecting to 229 nm (UV) excitation, the phosphors show enhanced PL emissions corresponding to 571 nm (5D0-7F0), 591 nm (5D0-7F1), 615 nm (5D0-7F2) and 678 nm (5D0-7F4) hypersensitive transitions of Eu3+ ions and emission peaks at 489 nm (5D4-7F6), 539 nm (5D4-7F5), 589 nm (5D4-7F4) and 632 nm (5D4-7F3) accounting for electronic transitions of Tb3+ ions respectively. The computed average PL lifetime is 14.014 s. In the TL analysis, the second order of kinetics with the activation energy varying from 5.0 × 10‑1 eV to 6.6 × 10‑1 eV is reported. The maximum TL lifetime is estimated as 19.4985 min in the TL lifetime analysis.

Transport Properties and Magnetoresistance of La0.8Ca0.13Ag0.07MnO3 Perovskite Manganite Synthesized by Sol-Gel Method

NASA Astrophysics Data System (ADS)

Kurniawan, B.; Ruli, F.; Imaduddin, A.; Kamila, R.

2018-05-01

In this paper, we investigate the transport properties and magnetoresistance effect of La0.8Ca0.13Ag0.07MnO3 perovskite manganite synthesized by sol-gel method. The XRD pattern of the sample shows a rhombohedral perovskite structure with space group R3¯c. The EDX analysis confirms that the sample contains all expected chemical elements without any additional impurity. The temperature dependence of electrical resistivity was measured using a cryogenic magnetometer. The results show a metal-insulator transition temperature (TM-I ) at 280 K. The resistivity of the sample increases with an increase of temperature below TM-I . Theoretical analyses of the temperature dependence of resistivity suggest that the resistivity due to electron-electron scattering is predominant below TI-M. The resistivity of the sample decreases when applied magnetic field 1 T at a temperature range of 10 K to 300 K. The magnetoresistance of La0.8Ca0.13Ag0.07MnO3 emanates from spin-polarized tunneling process at the grain boundary.

Degradation of magnesium and its alloys: dependence on the composition of the synthetic biological media.

PubMed

Mueller, Wolf-Dieter; de Mele, Monica Fernández Lorenzo; Nascimento, Maria Lucia; Zeddies, Miriam

2009-08-01

Magnesium and its alloys are highly degradable metals that are potentially useful as biomaterials, especially in orthopaedic and cardiovascular applications. However, the in vivo corrosion has proved to be too high. Because of the complexity of in vivo conditions, a careful study of the corrosion of magnesium in synthetic solutions that simulate the in vivo environment is necessary as a first approach to predict the actual in vivo situation. The aim of this work was to evaluate the influence of the electrolyte composition on the corrosion behavior of magnesium and two Mg-alloys in synthetic biological media. Pure magnesium and its alloys (AZ31 and LAE442) were employed in the experiments. Electrochemical potentiodynamic polarization curves were recorded in sodium chloride and PBS electrolytes with different chloride ion and albumin concentration. Optical and SEM observations complemented by EDX analysis were made. The results showed that magnesium corrosion is localized in chloride- and albumin-containing buffer solutions. They also showed that the chloride concentration and the presence of buffer and protein strongly affect the electrochemical behavior of magnesium and magnesium alloys.

Electrical conductivity of graphite oxide nanoplatelets obtained from bamboo: Effect of the deoxidation degree

NASA Astrophysics Data System (ADS)

Gross, K.; Prias-Barragan, J. J.; Sangiao, S.; de Teresa, J. M.; Lajaunie, L.; Arenal, R.; Ariza-Calderón, H.; Prieto, P.

Given the high interest in the fabrication and application of carbon-based materials, we present a new and cost-effective method for the synthesis of graphite oxide nanoplatelets (GONP) using bamboo pyroligneous acid (BPA) as source. GONP-BPA present lateral dimensions of 5-100 micro-meter and thickness less than 80 nm, as confirmed by TEM. EEL spectra show that locally the carbon is mainly in sp2 bonding configuration and confirm a short/medium range crystalline order. Elemental analysis by EDX confirms the presence of oxygen in an atomic percentage ranging from 17 to 5%. For electrical characterization, single platelets were contacted by focused-ion-beam-induced deposition of Pt nanowires. The four-point probe electrical conductivity shows a direct correlation with the oxygen percentage. Three orders of magnitude conductivity rise is observed by the oxygen reduction, reaching a value of 2.3x103 S/m at the final deoxidation degree. The results suggest that GONP-BPA could be used in the development of advanced devices and sensors.

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.

Mesoporous Nickel Oxide (NiO) Nanopetals for Ultrasensitive Glucose Sensing

NASA Astrophysics Data System (ADS)

Mishra, Suryakant; Yogi, Priyanka; Sagdeo, P. R.; Kumar, Rajesh

2018-01-01

Glucose sensing properties of mesoporous well-aligned, dense nickel oxide (NiO) nanostructures (NSs) in nanopetals (NPs) shape grown hydrothermally on the FTO-coated glass substrate has been demonstrated. The structural study based investigations of NiO-NPs has been carried out by X-ray diffraction (XRD), electron and atomic force microscopies, energy dispersive X-ray (EDX), and X-ray photospectroscopy (XPS). Brunauer-Emmett-Teller (BET) measurements, employed for surface analysis, suggest NiO's suitability for surface activity based glucose sensing applications. The glucose sensor, which immobilized glucose on NiO-NPs@FTO electrode, shows detection of wide range of glucose concentrations with good linearity and high sensitivity of 3.9 μA/μM/cm2 at 0.5 V operating potential. Detection limit of as low as 1 μΜ and a fast response time of less than 1 s was observed. The glucose sensor electrode possesses good anti-interference ability, stability, repeatability & reproducibility and shows inert behavior toward ascorbic acid (AA), uric acid (UA) and dopamine acid (DA) making it a perfect non-enzymatic glucose sensor.

TEM analysis of irradiation-induced interaction layers in coated UMo/X/Al trilayer systems (X= Ti, Nb, Zr, and Mo)

NASA Astrophysics Data System (ADS)

Chiang, H.-Y.; Wiss, T.; Park, S.-H.; Dieste-Blanco, O.; Petry, W.

2018-02-01

Uranium-molybdenum (UMo) alloy powder embedded in an Al matrix is considered as a promising candidate for fuel conversion of research reactors. A modified system with a diffusion barrier X as coating, UMo/X/Al trilayer (X = Ti, Zr, Nb, and Mo), has been investigated to suppress interdiffusion between UMo and the Al matrix. The trilayer systems were tested by swift heavy ion irradiation, the thereby created interaction zone has been analyzed by scanning transmission electron microscopy (STEM) and energy-dispersive X-ray spectroscopy (EDX). Detailed structural characterization are presented and compared to earlier μ-XRD analysis.

Iridium Oxide pH Sensor Based on Stainless Steel Wire for pH Mapping on Metal Surface

NASA Astrophysics Data System (ADS)

Shahrestani, S.; Ismail, M. C.; Kakooei, S.; Beheshti, M.; Zabihiazadboni, M.; Zavareh, M. A.

2018-03-01

A simple technique to fabricate the iridium oxide pH sensor is useful in several applications such as medical, food processing and engineering material where it is able to detect the changes of pH. Generally, the fabrication technique can be classified into three types: electro-deposition iridium oxide film (EIrOF), activated iridium oxide film (AIROF) and sputtering iridium oxide film (SIROF). This study focuses on fabricating electrode, calibration and test. Electro-deposition iridium oxide film is a simple and effective method of fabricating this kind of sensor via cyclic voltammetry process. The iridium oxide thick film was successfully electrodeposited on the surface of stainless steel wire with 500 cycles of sweep potential. A further analysis under FESEM shows detailed image of iridium oxide film which has cauliflower-liked microstructure. EDX analysis shows the highest element present are iridium and oxygen which concluded that the process is successful. The iridium oxide based pH sensor has shown a good performance in comparison to conventional glass pH sensor when it is being calibrated in buffer solutions with 2, 4, 7 and 9 pH values. The iridium oxide pH sensor is specifically designed to measure the pH on the surface of metal plate.

Cellulase assisted synthesis of nano-silver and gold: Application as immobilization matrix for biocatalysis.

PubMed

Mishra, Abhijeet; Sardar, Meryam

2015-01-01

In the present study, we report in vitro synthesis of silver and gold nanoparticles (NPs) using cellulase enzyme in a single step reaction. Synthesized nanoparticles were characterized by UV-VIS spectroscopy, Dynamic Light Spectroscopy (DLS), Transmission Electron Microscopy (TEM), Energy-dispersive X-ray Spectroscopy (EDX), X-ray Diffraction (XRD), Circular Dichroism (CD) and Fourier Transform Infrared Spectroscopy (FTIR). UV-visible studies shows absorption band at 415nm and 520nm for silver and gold NPs respectively due to surface plasmon resonance. Sizes of NPs as shown by TEM are 5-25nm for silver and 5-20nm for gold. XRD peaks confirmed about phase purity and crystallinity of silver and gold NPs. FTIR data shows presence of amide I peak on both the NPs. The cellulase assisted synthesized NPs were further exploited as immobilization matrix for cellulase enzyme. Thermal stability analysis reveals that the immobilized cellulase on synthesized NPs retained 77-80% activity as compared to free enzyme. While reusability data suggests immobilized cellulase can be efficiently used up to sixth cycles with minimum loss of enzyme activity. The secondary structural analysis of cellulase enzyme during the synthesis of NPs and also after immobilization of cellulase on these NPs was carried out by CD spectroscopy. Copyright © 2015 Elsevier B.V. All rights reserved.

Direct synthesis of nitrogen-containing carbon nanotubes on carbon paper for fuel cell electrode

NASA Astrophysics Data System (ADS)

Yin, Wong Wai; Daud, Wan Ramli Wan; Mohamad, Abu Bakar; Kadhum, Abdul Amir Hassan; Majlan, Edy Herianto; Shyuan, Loh Kee

2012-06-01

Organic catalyst has recently been identified as the potential substitution for expensive platinum electrocatalyst for fuel cell application. Numerous studies have shown that the nitrogen-containing carbon nanotubes (N-CNT) can be synthesized through spray pyrolysis or floating chemical vapor deposition (CVD) technique using various type of organometallic as precursors. This paper presents the method of synthesis and the initial findings of the growth of N-CNT directly on carbon paper using a modified CVD technique. In this research, nickel (II) phthalocyanines (Ni-Pc) as precursor was dissolved in ethanol solvent, stirred and sonicated to become homogenized. The solution was poured into a bubbler and heated up to allow the mixture to vaporize. Subsequently, the solution vapor was flowed into the tubical reactor maintained at 900°C. Carbon paper sputtered with nickel nanoparticles was used as the substrate. The synthesized sample was examined through Field Emission Scanning Electron Microscopy (FESEM), Atomic Force Microscopy (AFM) and Fourier Transform Infra-Red (FTIR). Long, entangled and compartmentalized nanotubes with tube diameter ranging 23-27 nm were found covered the carbon paper surface with approximate of 5.5-6.0 μm in thickness. EDX analysis has successfully showed the presence of nitrogen in the carbon nanotube. FTIR analysis showed the presence of the C-N bond on CNT.

Properties of transparent conducting tin monoxide(SnO) thin films prepared by chemical spray pyrolysis method

NASA Astrophysics Data System (ADS)

Eqbal, Ebitha; Anila, E. I.

2018-01-01

Transparent conducting Stannous Oxide (SnO) thin films were obtained by chemical spray pyrolysis method on glass substrates for 0.1 M and 0.25 M concentration of precursor solutions. Their structural, morphological, optical and electrical properties were investigated. X-ray diffraction (XRD) study shows polycrystalline nature of the films with orthorhombic crystal structure. The morphological analysis was carried out by Scanning electron microscopy (SEM) and elemental analysis was done by Energy dispersive X-ray spectroscopy (EDX). The band gap of 0.1 M and 0.25 M thin film samples were found to be 3.58eV with 82% transmission and 3 eV with 30% transmission respectively. The film thickness, refractive index (n) and extinction coefficient (k) of the films were obtained by ellipsometric technique. Hall effect measurements reveal p-type conduction with mobility 7.8 cm2V-1s-1 and 15 cm2V-1s-1 and conductivity of 8.5 S/cm and 17.1 S/cm respectively for the 0.1 M and 0.25 M samples. Photoluminescence (PL) spectrum of the samples show a broad emission which covers near band edge (NBE) as well as deep level emission (DLE) in the region 380 nm-620 nm.

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.

Advanced surface chemical analysis of continuously manufactured drug loaded composite pellets.

PubMed

Hossain, Akter; Nandi, Uttom; Fule, Ritesh; Nokhodchi, Ali; Maniruzzaman, Mohammed

2017-04-15

The aim of the present study was to develop and characterise polymeric composite pellets by means of continuous melt extrusion techniques. Powder blends of a steroid hormone (SH) as a model drug and either ethyl cellulose (EC N10 and EC P7 grades) or hydroxypropyl methylcellulose (HPMC AS grade) as polymeric carrier were extruded using a Pharma 11mm twin screw extruder in a continuous mode of operation to manufacture extruded composite pellets of 1mm length. Molecular modelling study using commercial Gaussian 09 software outlined a possible drug-polymer interaction in the molecular level to develop solid dispersions of the drug in the pellets. Solid-state analysis conducted via a differential scanning calorimetry (DSC), hot stage microscopy (HSM) and X-ray powder diffraction (XRPD) analyses revealed the amorphous state of the drug in the polymer matrices. Surface analysis using SEM/energy dispersive X-ray (EDX) of the produced pellets arguably showed a homogenous distribution of the C and O atoms in the pellet matrices. Moreover, advanced chemical surface analysis conducted via atomic force microscopy (AFM) showed a homogenous phase system having the drug molecule dispersed onto the amorphous matrices while Raman mapping confirmed the homogenous single-phase drug distribution in the manufactured composite pellets. Such composite pellets are expected to deliver multidisciplinary applications in drug delivery and medical sciences by e.g. modifying drug solubility/dissolutions or stabilizing the unstable drug (e.g. hormone, protein) in the composite network. Copyright © 2016. Published by Elsevier Inc.

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.

Spatially resolved quantification of agrochemicals on plant surfaces using energy dispersive X-ray microanalysis.

PubMed

Hunsche, Mauricio; Noga, Georg

2009-12-01

In the present study the principle of energy dispersive X-ray microanalysis (EDX), i.e. the detection of elements based on their characteristic X-rays, was used to localise and quantify organic and inorganic pesticides on enzymatically isolated fruit cuticles. Pesticides could be discriminated from the plant surface because of their distinctive elemental composition. Findings confirm the close relation between net intensity (NI) and area covered by the active ingredient (AI area). Using wide and narrow concentration ranges of glyphosate and glufosinate, respectively, results showed that quantification of AI requires the selection of appropriate regression equations while considering NI, peak-to-background (P/B) ratio, and AI area. The use of selected internal standards (ISs) such as Ca(NO(3))(2) improved the accuracy of the quantification slightly but led to the formation of particular, non-typical microstructured deposits. The suitability of SEM-EDX as a general technique to quantify pesticides was evaluated additionally on 14 agrochemicals applied at diluted or regular concentration. Among the pesticides tested, spatial localisation and quantification of AI amount could be done for inorganic copper and sulfur as well for the organic agrochemicals glyphosate, glufosinate, bromoxynil and mancozeb. (c) 2009 Society of Chemical Industry.

Copper diffusion in Ti Si N layers formed by inductively coupled plasma implantation

NASA Astrophysics Data System (ADS)

Ee, Y. C.; Chen, Z.; Law, S. B.; Xu, S.; Yakovlev, N. L.; Lai, M. Y.

2006-11-01

Ternary Ti-Si-N refractory barrier films of 15 nm thick was prepared by low frequency, high density, inductively coupled plasma implantation of N into TixSiy substrate. This leads to the formation of Ti-N and Si-N compounds in the ternary film. Diffusion of copper in the barrier layer after annealing treatment at various temperatures was investigated using time-of-flight secondary ion mass spectrometer (ToF-SIMS) depth profiling, X-ray diffractometer (XRD), field emission scanning electron microscopy (FESEM), energy dispersive X-ray (EDX) and sheet resistance measurement. The current study found that barrier failure did not occur until 650 °C annealing for 30 min. The failure occurs by the diffusion of copper into the Ti-Si-N film to form Cu-Ti and Cu-N compounds. FESEM surface morphology and EDX show that copper compounds were formed on the ridge areas of the Ti-Si-N film. The sheet resistance verifies the diffusion of Cu into the Ti-Si-N film; there is a sudden drop in the resistance with Cu compound formation. This finding provides a simple and effective method of monitoring Cu diffusion in TiN-based diffusion barriers.

Glycolysis of carbon fiber-epoxy unidirectional mat catalysed by sodium hydroxide

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

Zaini, Mariana Binti Mohd; Badri, Khairiah Haji

2014-09-03

This study was conducted to recycle carbon fibre-epoxy (CFRP) composite in woven sheet/ mat form. The CFRP was recycled through glycolysis with polyethlyene glycol (PEG 200) as the solvent. The CFRP was loaded into the solvent at a ratio of 4:1 (w/w). PEG200 was diluted with water to a ratio of 80:20 (v/v). This reaction was catalysed by sodium hydroxide (NaOH) solution with varying concentrations at 1.5, 1.7 and 1.9% (w/v). The glycolysis was conducted at 180-190 °C. The recovered CF (rCF) was analysed using Fourier Transform Infrared (FTIR), Scanning Electron Microscopy (SEM) and Energy Dispersive X-Ray (EDX) while themore » degraded solution was analysed using FTIR and the epoxy content was determined. The FTIR spectrum of the rCF exhibited the disappearance of the COC peak belonged to epoxy and supported by the SEM micrographs that showed clear rCF. On the other hand, the analysed filtrate detected the disappearance of oxygen peak element in the EDX spectrum for all rCF samples. This gave an indication that the epoxy resin has been removed from the surface of the carbon fiber.« less

Glycolysis of carbon fiber-epoxy unidirectional mat catalysed by sodium hydroxide

NASA Astrophysics Data System (ADS)

Zaini, Mariana Binti Mohd; Badri, Khairiah Haji

2014-09-01

This study was conducted to recycle carbon fibre-epoxy (CFRP) composite in woven sheet/ mat form. The CFRP was recycled through glycolysis with polyethlyene glycol (PEG 200) as the solvent. The CFRP was loaded into the solvent at a ratio of 4:1 (w/w). PEG200 was diluted with water to a ratio of 80:20 (v/v). This reaction was catalysed by sodium hydroxide (NaOH) solution with varying concentrations at 1.5, 1.7 and 1.9% (w/v). The glycolysis was conducted at 180-190 °C. The recovered CF (rCF) was analysed using Fourier Transform Infrared (FTIR), Scanning Electron Microscopy (SEM) and Energy Dispersive X-Ray (EDX) while the degraded solution was analysed using FTIR and the epoxy content was determined. The FTIR spectrum of the rCF exhibited the disappearance of the COC peak belonged to epoxy and supported by the SEM micrographs that showed clear rCF. On the other hand, the analysed filtrate detected the disappearance of oxygen peak element in the EDX spectrum for all rCF samples. This gave an indication that the epoxy resin has been removed from the surface of the carbon fiber.

Fate of Lu(III) sorbed on 2-line ferrihydrite at pH 5.7 and aged for 12 years at room temperature. II: insights from STEM-EDXS and DFT calculations.

PubMed

Yokosawa, Tadahiro; Prestat, Eric; Polly, Robert; Bouby, Muriel; Dardenne, Kathy; Finck, Nicolas; Haigh, Sarah J; Denecke, Melissa A; Geckeis, Horst

2018-04-18

Transformation products of two-line ferrihydrite associated with Lu(III) were studied after 12 years of aging using aberration-corrected high-angle annular dark field scanning transmission electron microscopy (HAADF-STEM), high-efficiency energy-dispersive X-ray spectroscopy (EDXS), and density functional theory (DFT). The transformation products consisted of hematite nanoparticles with overgrown goethite needles. High-efficiency STEM-EDXS revealed that Lu is only associated with goethite needles, and atomic-resolution HAADF-STEM reveals structural incorporation of Lu within goethite, partially replacing structural Fe sites. This finding corroborates those recently obtained by AsFlFFF and EXAFS spectroscopy on the same sample (Finck et al. 2018). DFT calculations indicate that Lu incorporation within goethite or hematite are almost equally likely, suggesting that experimental parameters such as temperature and reaction time which affect reaction kinetics, play important roles in determining the Lu uptake. It seems likely that these results may be transferable to predict the behavior of chemically homologous trivalent actinides.

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.

Surface Studies of Ultra Strength Drilling Steel after Corrosion Fatigue in Simulated Sour Environment

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

M. Ziomek-Moroz; J.A. Hawk; R. Thodla

2012-05-06

The Unites States predicted 60% growth in energy demand by 2030 makes oil and natural gas primary target fuels for energy generation. The fact that the peak of oil production from shallow wells (< 5000 m) is about to be reached, thereby pushing the oil and natural gas industry into deeper wells. However, drilling to depths greater than 5000 m requires increasing the strength-to weight ratio of the drill pipe materials. Grade UD-165 is one of the ultra- high yield strength carbon steels developed for ultra deep drilling (UDD) activities. Drilling UDD wells exposes the drill pipes to Cl{sup -},more » HCO{sub 3}{sup -}/CO{sub 3}{sup 2-}, and H{sub 2}S-containig corrosive environments (i.e., sour environments) at higher pressures and temperatures compared to those found in conventional wells. Because of the lack of synergism within the service environment, operational stresses can result in catastrophic brittle failures characteristic for environmentally assisted cracking (EAC). Approximately 75% of all drill string failures are caused by fatigue or corrosion fatigue. Since there is no literature data on the corrosion fatigue performance of UD-165 in sour environments, research was initiated to better clarify the fatigue crack growth (FCGR) behavior of this alloy in UDD environments. The FCGR behavior of ultra-strength carbon steel, grade UD-165, was investigated by monitoring crack growth rate in deaerated 5%NaCl solution buffered with NaHCO{sub 3}/Na{sub 2}CO{sub 3} and in contact with H{sub 2}S. The partial pressure of H{sub 2}S (p{sub H2S}) was 0.83 kPa and pH of the solution was adjusted by NaOH to 12. The fatigue experiments were performed at 20 and 85 C in an autoclave with surface investigations augmented by scanning electron microscopy (SEM) and energy dispersive x-ray (EDX) spectroscopy. In this study, research focused on surface analyses supported by the fatigue crack growth rate measurements. Fig. 1 shows an SEM micrograph of the crack that propagated from the notch in the solution at 20 C. Accumulation of the corrosion products is visible along the crack. The EDX chemical analysis near the crack tip found iron, sulfur and oxygen in the passive layer. The surface of the sample after the fatigue test in the sour environment at 85{sup o}, Fig. 2, C looks different from that fatigued surface at 20 C. The crack propagates across the passive film that covers the surface fairly uniformly. Some spallation of the passive film is observed near the notch. The EDX chemical analysis of the passive film near the crack tip identified mainly iron, carbon and oxygen. It appears that temperature plays a very important role in formation of the passive film. This may be associated with different solubility of H{sub 2}S in the solution, which will be further studied.« less

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.

Quantitative description of yttrium aluminate ceramic composition by means of Er+3 microluminescence spectrum

NASA Astrophysics Data System (ADS)

Videla, F. A.; Tejerina, M. R.; Moreira-Osorio, L.; Conconi, M. S.; Orzi, D. J. O.; Flores, T.; Ponce, L. V.; Bilmes, G. M.; Torchia, G. A.

2018-05-01

The composition of erbium-doped yttrium aluminate ceramics was analyzed by means of confocal luminescence spectroscopy, EDX, and X-ray diffraction. A well-defined linear correlation was found between a proposed estimator computed from the luminescence spectrum and the proportion of ceramic phases coexisting in different samples. This result shows the feasibility of using erbium luminescence spectroscopy to perform a quantitative determination of different phases of yttrium aluminates within a micrometric region in nanograined ceramics.

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.

Elucidating the Wavelength Dependence of Phonon Scattering in Nanoparticle-Matrix Composites using Phonon Spectroscopy

DTIC Science & Technology

2016-07-11

composites with x - ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Rutherford backscattering spectroscopy...RBS), particle-induced x - ray emission (PIXE), and energy dispersive x - ray spectroscopy (EDX). This work complements earlier works on CdSe...sample shows only In2Se3 and CdIn2Se4 XRD peaks (Figure 1.4e), it is stoichiometrically   Figure 1.4. X - ray diffraction patterns of (a) γ-In2Se3

Biomimetic novel nanoporous niobium oxide coating for orthopaedic applications

NASA Astrophysics Data System (ADS)

Pauline, S. Anne; Rajendran, N.

2014-01-01

Niobium oxide was synthesized by sol-gel methodology and a crystalline, nanoporous and adherent coating of Nb2O5 was deposited on 316L SS using the spin coating technique and heat treatment. The synthesis conditions were optimized to obtain a nanoporous morphology. The coating was characterized using attenuated total reflectance-Infrared spectroscopy (ATR-IR), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray analysis (EDX), atomic force microscopy (AFM) and transmission electron microscopy (TEM) and the formation of crystalline Nb2O5 coating with nanoporous morphology was confirmed. Mechanical studies confirmed that the coating has excellent adherence to the substrate and the hardness value of the coating was excellent. Contact angle analysis showed increased hydrophilicity for the coated substrate. In vitro bioactivity test confirmed that the Nb2O5 coating with nanoporous morphology facilitated the growth of hydroxyapatite (HAp). This was further confirmed by the solution analysis test where increased uptake of calcium and phosphorous ions from simulated body fluid (SBF) was observed. Electrochemical evaluation of the coating confirmed that the crystalline coating is insulative and protective in nature and offered excellent corrosion protection to 316L SS. Thus, this study confirmed that the nanoporous crystalline Nb2O5 coating conferred bioactivity and enhanced corrosion resistance on 316L SS.

Biosorption and biotransformation of chromium by Serratia sp. isolated from tannery effluent.

PubMed

Srivastava, Shaili; Thakur, Indu Shekhar

2012-01-01

A bacterium isolated from soil and sediment ofa leather tanning mill's effluent was identified as Serratia sp. by the analysis of 16S rDNA. Scanning electron microscopy-energy dispersive X-ray analysis (SEM-EDX) and transmission electron microscopy (TEM) were used to assess morphological changes and confirm chromium biosorption in Serratia sp. both in a shake-flask culture containing chromium and in a tannery wastewater. The SEMEDX and the elemental analysis of the chromate-containing samples confirmed the binding of chromium with the bacterial biomass. The TEM exhibited chromium accumulation throughout the bacterial cell, with some granular deposits in the cell periphery and in the cytoplasm. X-ray diffraction analysis (XRD) was used to quantify the chromium and to determine the chemical nature of the metal-microbe interaction. The XRD data showed the crystalline character of the precipitates, which consisted of mainly calcium chromium oxide, chromium fluoride phosphate and related organo-Cr(III) complex crystals. The XRD data also revealed a strong involvement of cellular carboxyl and phosphate groups in chromium binding by the bacterial biomass. The results of the study indicated that a combined mechanism of ion-exchange, complexation, croprecipitation and immobilization was involved in the biosorption of chromium by bacterial cells in contaminated environments.

Gunshot residue (GSR) analysis by single particle inductively coupled plasma mass spectrometry (spICP-MS).

PubMed

Heringer, Rodrigo D; Ranville, James F

2018-05-25

Single particle inductively coupled plasma mass spectrometry (spICP-MS) was investigated as a screening-level technique for the analysis and characterization of inorganic gunshot residue (IGSR) nanoparticles. spICP-MS works with undigested samples whereby nanoparticles (NPs) in a suspension are individually atomized and ionized as they reach the plasma, each resulting in a pulse of analyte ions that can be quantified. The method is rapid, and signals from hundreds of NPs can be collected in 1-2min per sample. The technique is quantitative for NP mass and number concentration when only one element (single element mode) is measured using a quadrupole MS. Likewise, a qualitative elemental fingerprint can be obtained for individual NPs when peak-hopping between two elements (dual element mode). For this proof of concept study, each shooter's hand was sampled with ultrapure water or swab to obtain NPs suspensions. Measurements of antimony, barium, and lead were performed using both analysis modes. With no sample preparation and fully automated sample introduction, it is possible to analyze more than 100 samples in a day. Results show that this technique opens a new perspective for future research on GSR sample identification and characterization and can complement SEM/EDX analysis. Copyright © 2018 Elsevier B.V. All rights reserved.

Decomposition of Ag-based soldering alloys used in space maintainers after intra-oral exposure. A retrieval analysis study.

PubMed

Soteriou, Despo; Ntasi, Argyro; Papagiannoulis, Lisa; Eliades, Theodore; Zinelis, Spiros

2014-02-01

The aim of this study was to evaluate the elemental alterations of Ag soldering alloys used in space maintainers after intra-oral exposure. Twenty devices were fabricated by using two different soldering alloys; US (Dentaurum Universal Silver Solder, n = 10) and OS (Leone Orthodontic Solder, n = 10). All devices were manufactured by the same technician. Surface morphology and elemental quantitative analysis of the soldering alloys before and after intra-oral placement in patients was determined by scanning electron microscopy and energy-dispersive X-ray microanalysis (SEM/EDX). Statistical analysis was performed by t-test, Mann Whitney tests and Pearson's correlation. For all tests a 95% confidence level was used (α = 0.05). Both soldering alloys demonstrated substantially increase in surface roughness after intra-oral aging. Statistical analysis illustrated a significant decrease in the Cu and Zn content after treatment. OS demonstrated higher Cu release than US (p < 0.05). The remaining relative concentrations of Cu and Zn after the treatment did not show any correlation (p > 0.05) with intra-oral exposure time, apart from Zn in OS (r = 0.840, p = 0.04). Both soldering alloys demonstrated a significant Cu and Zn reduction after intra-oral exposure that may raise biocompatibility concerns.

Synthesis and characterization of nanosilver-silicone hydrogel composites for inhibition of bacteria growth.

PubMed

Helaly, F M; El-Sawy, S M; Hashem, A I; Khattab, A A; Mourad, R M

2017-02-01

Nanosilver-silicone hydrogel (NAgSiH) composites for contact lenses were synthesized to asses the antimicrobial effects. Silicone hydrogel (SiH) films were synthesized followed by impregnation in silver nitrate solutions (10, 20, 30, 40, 60, 80ppm) and in-situ chemical reduction of silver ions using sodium borohydride (NaBH 4 ). The silver nano particles (AgNPS) were identified by UV-vis absorption spectroscopy, Energy-dispersive X-ray spectroscopy (EDX) mapping and EDX spectrum. Physico-mechanical and chemical properties of NAgSIH films were studied. The antimicrobial effect of the hydrogels against Escherichia coli, Pseudomonas aeruginosa, Bacillus subtilis and Staphylococcus aureus was evaluated. The numbers of viable bacterial cells on NAgSiH surface or in solution compared to control SiH were examined. The NAgSiH films were successfully synthesized. FTIR results indicated that AgNPS had no effect on the bulk structure of the prepared SiH films. From TGA analysis, NAgSiH(R80) and SiH(R0) films had the same maximum decomposition temperature (404°C). UV-vis absorption spectroscopy and EDX mapping and spectrum emphasized that AgNPS were in spherical shape. The maximum absorption wavelength of NAgSiH films were around 400nm. The light transmittance decreased as the concentration of AgNPS increased, but still greater than 90% at wavelength around 555nm. The Young's modulus increased gradually from 1.06MPa of SiH(R0) to highest value 1.38MPa of NAgSiH(R80). AgNPS incorporated into SiH films reduced the bacterial cell growth and prevented colonization. Groups NAgSiH(R60,R80) demonstrated an excellent reduction in bacterial viability in solution and on the SiH surface. NAgSiH composites were successfully synthesized and possessed an excellent antimicrobial effects. Copyright © 2016 British Contact Lens Association. Published by Elsevier Ltd. All rights reserved.

Down-top nanofabrication of binary (CdO)x (ZnO)1–x nanoparticles and their antibacterial activity

PubMed Central

Al-Hada, Naif Mohammed; Mohamed Kamari, Halimah; Abdullah, Che Azurahanim Che; Saion, Elias; Shaari, Abdul H; Talib, Zainal Abidin; Matori, Khamirul Amin

2017-01-01

In the present study, binary oxide (cadmium oxide [CdO])x (zinc oxide [ZnO])1–x nanoparticles (NPs) at different concentrations of precursor in calcination temperature were prepared using thermal treatment technique. Cadmium and zinc nitrates (source of cadmium and zinc) with polyvinylpyrrolidone (capping agent) have been used to prepare (CdO)x (ZnO)1–x NPs samples. The sample was characterized by X-ray diffraction (XRD), scanning electron microscopy, energy-dispersive X-ray (EDX), transmission electron microscopy (TEM), and Fourier transform infrared (FTIR) spectroscopy. XRD patterns analysis revealed that NPs were formed after calcination, which showed a cubic and hexagonal crystalline structure of (CdO)x (ZnO)1–x NPs. The phase analysis using EDX spectroscopy and FTIR spectroscopy confirmed the presence of Cd and Zn as the original compounds of prepared (CdO)x (ZnO)1–x NP samples. The average particle size of the samples increased from 14 to 33 nm as the concentration of precursor increased from x=0.20 to x=0.80, as observed by TEM results. The surface composition and valance state of the prepared product NPs were determined by X-ray photoelectron spectroscopy (XPS) analyses. Diffuse UV–visible reflectance spectra were used to determine the optical band gap through the Kubelka–Munk equation; the energy band gap was found to decrease for CdO from 2.92 to 2.82 eV and for ZnO from 3.22 to 3.11 eV with increasing x value. Additionally, photoluminescence (PL) spectra revealed that the intensity in PL increased with an increase in particle size. In addition, the antibacterial activity of binary oxide NP was carried out in vitro against Escherichia coli ATCC 25922 Gram (−ve), Salmonella choleraesuis ATCC 10708, and Bacillus subtilis UPMC 1175 Gram (+ve). This study indicated that the zone of inhibition of 21 mm has good antibacterial activity toward the Gram-positive B. subtilis UPMC 1175. PMID:29200844

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.

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.

Valorization of titanium metal wastes as tanning agent used in leather industry

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

Crudu, Marian, E-mail: mariancrudu@yahoo.com; Deselnicu, Viorica, E-mail: viorica.deselnicu@icpi.ro; Deselnicu, Dana Corina, E-mail: d_deselnicu@yahoo.com

2014-10-15

Highlights: • Valorization of titanium wastes which cannot be recycled in metallurgical industry. • Transferring Ti waste into raw materials for obtaining Ti based tanning agent. • Characterization of new Ti based tanning agents and leather tanned with them. • Characterization of sewage waste water and sludge resulted from leather manufacture. • Analysis of the impact of main metal component of Ti waste. - Abstract: The development of new tanning agents and new technologies in the leather sector is required to cope with the increasingly higher environmental pressure on the current tanning materials and processes such as tanning with chromiummore » salts. In this paper, the use of titanium wastes (cuttings) resulting from the process of obtaining highly pure titanium (ingots), for the synthesis of new tanning agent and tanning bovine hides with new tanning agent, as alternative to tanning with chromium salts are investigated. For this purpose, Ti waste and Ti-based tanning agent were characterized for metal content by inductively coupled plasma mass spectrometry (ICP-MS) and chemical analysis; the tanned leather (wet white leather) was characterized by Scanning Electron Microscope/Energy Dispersive Using X-ray (Analysis). SEM/EDX analysis for metal content; Differential scanning calorimetric (DSC), Micro-Hot-Table and standard shrinkage temperature showing a hydrothermal stability (ranged from 75.3 to 77 °C) and chemical analysis showing the leather is tanned and can be processed through the subsequent mechanical operations (splitting, shaving). On the other hand, an analysis of major minor trace substances from Ti-end waste (especially vanadium content) in new tanning agent and wet white leather (not detected) and residue stream was performed and showed that leachability of vanadium is acceptable. The results obtained show that new tanning agent obtained from Ti end waste can be used for tanning bovine hides, as eco-friendly alternative for chrome tanning.« less

Spectral and raw quasi in-situ energy dispersive X-ray data captured via a TEM analysis of an ODS austenitic stainless steel sample under 1 MeV Kr2+ high temperature irradiation.

PubMed

Brooks, Adam J; Yao, Zhongwen

2017-10-01

The data presented in this article is related to the research experiment, titled: ' Quasi in-situ energy dispersive X-ray spectroscopy observation of matrix and solute interactions on Y-Ti-O oxide particles in an austenitic stainless steel under 1 MeV Kr 2+ high temperature irradiation' (Brooks et al., 2017) [1]. Quasi in-situ analysis during 1 MeV Kr 2+ 520 °C irradiation allowed the same microstructural area to be observed using a transmission electron microscope (TEM), on an oxide dispersion strengthened (ODS) austenitic stainless steel sample. The data presented contains two sets of energy dispersive X-ray spectroscopy (EDX) data collected before and after irradiation to 1.5 displacements-per-atom (~1.25×10 -3  dpa/s with 7.5×10 14  ions cm -2 ). The vendor software used to process and output the data is the Bruker Esprit v1.9 suite. The data includes the spectral (counts vs. keV energy) of the quasi in-situ scanned region (512×512 pixels at 56k magnification), along with the EDX scanning parameters. The.raw files from the Bruker Esprit v1.9 output are additionally included along with the.rpl data information files. Furthermore included are the two quasi in-situ HAADF images for visual comparison of the regions before and after irradiation. This in-situ experiment is deemed ' quasi' due to the thin foil irradiation taking place at an external TEM facility. We present this data for critical and/or extended analysis from the scientific community, with applications applying to: experimental data correlation, confirmation of results, and as computer based modeling inputs.

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.

Elemental fractionation and magnetic properties of melt-based Y1Ba2Cu3Oz containing excess Tb or Pt

NASA Technical Reports Server (NTRS)

Hojaji, Hamid; Barkatt, Aaron; Hu, Shouxiang; Michael, Karen A.; Thorpe, Arthur N.; Talmy, Inna G.; Haught, Debbie A.; Alterescu, Sidney

1990-01-01

Scanning electron microscopy of certain partially melted Y-Ba-Cu-O materials containing minority metal oxide species (Y:Tb:Ba:Cu = 1:0.1:2:3 or Y:Ba:Cu with Pt impurities), accompanied by both EDX and EMP analysis, indicates that the minority species (Tb or Pt) is quantitatively concentrated in a relatively small number of 123-type grains. High magnetic susceptibility and magnetization observed for these materials indicate that such elemental distribution is not detrimental to superconducting behavior.

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

Green and rapid synthesis of silver nanoparticles using Borago officinalis leaf extract: anticancer and antibacterial activities.

PubMed

Singh, Hina; Du, Juan; Yi, Tae-Hoo

2017-11-01

This study highlights the facile, reliable, cost effective, and ecofriendly synthesis of silver nanoparticles (AgNPs) using Borago officinalis leaves extract efficiently. The biosynthesis of AgNPs was verified by UV-Vis spectrum which showed the surface plasmon resonance (SPR) band at 422 nm. Transmission electron microscope (TEM) analysis revealed that the particles were spherical, hexagonal, and irregular in shape and had size ranging from 30 to 80 nm. The energy dispersive X-ray spectroscopy (EDX) and elemental mapping have displayed the purity and maximum distribution of silver in the AgNPs. The crystalline nature of AgNPs had been identified using X-ray diffraction (XRD) and selected area diffraction pattern (SAED). The particle size analysis revealed that the Z-average diameter of the AgNPs was 50.86 nm with polydispersity index (PDI) 0.136. Zeta potential analysis displayed the colloidal stability of AgNPs. This work also showed the efficacy of AgNPs against lung cancer cell lines (A549) and cervical cancer cell line (HeLa), in vitro. The AgNPs showed cytotoxicity to the A549 and HeLa cancer cell line at the concentrations 5 and 2 μg/ml. The AgNPs were also explored for the antibacterial activity including biofilm inhibition against pathogenic bacteria. The B. officinalis leaves extract can be used efficiently for green synthesis AgNPs. The biosynthesized AgNPs demonstrated potentials as anticancer and antibacterial agents. This work provides helpful insight into the development of new anticancer and antimicrobial agents.

Mechanical properties, microstructural and thermal evolution of Mg65Ni20Y15-xSix (X = 1, 2, 3) alloys by mechanical alloying

NASA Astrophysics Data System (ADS)

Kursun, Celal; Gogebakan, Musa; Eskalen, Hasan

2018-03-01

We report on a work of the influence of the mechanical alloying on the microstructure, thermal and mechanical features of Mg65Ni20Y15-xSix (X = 1, 2, 3) alloys. The Mg-based alloys were produced by mechanical alloying technique from mixtures of pure crystalline Mg, Ni, Y and Si powders. These alloys were investigated using a variety of analytical techniques including x-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDX) and differential scanning calorimetry (DSC). The mechanical properties of the alloys were investigated by Vickers microhardness (HV) tester. After 75 h of milling time, three different intermetallic phases were obtained. These phases were defined as Mg24Y5, Mg2Ni3Si and Mg2Ni by XRD data. The particle and crystallite sizes of the Mg-based alloys were decreased by increasing milling time and they were calculated 2 μm and ˜9 nm, respectively. From the EDX analysis, it was determined that compositional homogeneity of the Mg-based alloys was fairly high. The microhardness values of the Mg65Ni20Y15-xSix (X = 1, 2, 3) alloys increased by increasing Si into the alloys and were determined 101, 131 and 158 HV, respectively.

Calcium transport mechanism in molting crayfish revealed by microanalysis

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

Mizuhira, V.; Ueno, M.

1983-01-01

Crayfish provide a good model in which to study the transport mechanism of Ca ions. During the molting stage, decalcified Ca ions are transferred into the blood and accumulate in the gastrolith epithelium, after which a gastrolith is formed on the surface of the epithelium. The gastrolith is dissolved in the stomach after molting, and the Ca is reabsorbed and redistributed throughout the newly formed exoskeleton. We studied the mechanism of Ca transport by cytochemical precipitation of Ca ions and by electron microanalysis, including X-ray microanalysis (EDX) and electron energy-loss spectroscopy (EELS), with a computer. In EDX analysis, the finemore » precipitates of K-antimonate in the gastrolith mitochondria clearly defined Ca with antimony; we also observed a large amount of Ca-oxalate in the mitochondria, and Ca-K X-ray pulses were clearly defined. Ca-K X-rays were also detected from fresh freeze-substituted mitochondria. Finally, we succeeded in taking a Ca-L EELS image from the mitochondria of fresh freeze-substituted thin sections. Only a very small amount of Ca was detected from the cell membrane and other organelles. Ca-adenosine triphosphatase (ATPase) and Mg-ATPase activity was also very clearly demonstrated in the mitochondria. These enzymes may play an important role in Ca metabolism.« less

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.

SEM, EDX and Raman and infrared spectroscopic study of brianyoungite Zn3(CO3,SO4)(OH)4 from Esperanza Mine, Laurion District, Greece

NASA Astrophysics Data System (ADS)

Frost, Ray L.; López, Andrés; Wang, Lina; Scholz, Ricardo; Sampaio, Ney Pinheiro

2015-10-01

The mineral brianyoungite, a carbonate-sulphate of zinc, has been studied by scanning electron microscopy (SEM) with chemical analysis using energy dispersive spectroscopy (EDX) and Raman and infrared spectroscopy. Multiple carbonate stretching modes are observed and support the concept of non-equivalent carbonate units in the brianyoungite structure. Intense Raman band at 1056 cm-1 with shoulder band at 1038 cm-1 is assigned to the CO32- ν1 symmetric stretching mode. Two intense Raman bands at 973 and 984 cm-1 are assigned to the symmetric stretching modes of the SO42- anion. The observation of two bands supports the concept of the non-equivalence of sulphate units in the brianyoungite structure. Raman bands at 704 and 736 cm-1 are assigned to the CO32- ν4 bending modes and Raman bands at 507, 528, 609 and 638 cm-1 are assigned to the CO32- ν2 bending modes. Multiple Raman and infrared bands in the OH stretching region are observed, proving the existence of water and hydroxyl units in different molecular environments in the structure of brianyoungite. Vibrational spectroscopy enhances our knowledge of the molecular structure of brianyoungite.

Characterization of bacteria isolated from palaeoproterozoic metasediments for sequestration of carbon dioxide and formation of calcium carbonate.

PubMed

Srivastava, Shaili; Bharti, Randhir K; Thakur, Indu Shekhar

2015-01-01

Bacterial community of palaeoproterozoic metasediments was enriched in the chemostat in the presence of different concentrations of NaHCO3. Six bacterial isolates were isolated from the chemostat on nutrient agar plates on the basis of distinct morphology. Denaturing gradient gel electrophoresis (DGGE) proved the presence of six operational taxonomic units (OTUs) at 50 and 100 mM NaHCO3. The OTU was reduced to three and one at enrichment concentration of 150 and 200 mM NaHCO3 respectively. These six isolates were tested for sequestration of carbon dioxide by (14)C metabolic labeling of NaH(14)CO3. Among the six isolates, one of the bacterium showed better potency to fix radiolabeled NaH(14)CO3. The isolate (ISTD04) was identified as Serratia sp. by 16S ribosomal RNA (16S rRNA) sequence analysis and was found to be same as the DGGE OTU sequence at 200-mM NaHCO3 concentration. The bacterium was tested for product formation in form of calcite crystals in presence of 5 % CO2. Scanning electron microscopy (SEM) of product formed by the bacterium revealed defined faceted rhombohedral structure which resembled calcite and vaterite phases of the crystal. Formation of calcium carbonate crystals was further confirmed by Fourier transform infrared (FTIR) spectroscopy as carbonate group showing strong vibration at 1,456 cm(-1). Major calcite phase diffraction peaks were determined by X-ray diffraction (XRD) analysis, and energy-dispersive X-ray (EDX) analysis showed the presence of CaO (72 %) and carbon (18 %). Bacterium use bicarbonate as carbon source for their growth as well as by-product formation in form of calcite shows carbon circulation and storage.

Determining the Effect of Centrifugal Force on the Desired Growth and Properties of PCPDTBT as p-Type Nanowires

NASA Astrophysics Data System (ADS)

Doris, Muhamad; Aziz, Fakhra; Alhummiany, Haya; Bawazeer, Tahani; Alsenany, Nourah; Mahmoud, Alaa; Zakaria, Rozalina; Sulaiman, Khaulah; Supangat, Azzuliani

2017-01-01

In this study, low-bandgap polymer poly{[4,4-bis(2-ethylhexyl)-cyclopenta-(2,1- b;3,4- b')dithiophen]-2,6-diyl- alt-(2,1,3-benzothiadiazole)-4,7-diyl} (PCPDTBT) nanostructures have been synthesized via a hard nanoporous alumina template of centrifugal process. Centrifuge has been used to infiltrate the PCPDTBT solution into the nanoporous alumina by varying the rotational speeds. The rotational speed of centrifuge is directly proportional to the infiltration force that penetrates into the nanochannels of the template. By varying the rotational speed of centrifuge, different types of PCPDTBT nanostructures are procured. Infiltration force created during the centrifugal process has been found a dominant factor in tuning the morphological, optical, and structural properties of PCPDTBT nanostructures. The field emission scanning electron microscopy (FESEM) images proved the formation of nanotubes and nanowires. The energy-dispersive X-ray spectroscope (EDX) analysis showed that the nanostructures were composed of PCPDTBT with complete dissolution of the template.

The structural and electrical properties of polycrystalline La0.8Ca0.17Ag0.03MnO3 manganites

NASA Astrophysics Data System (ADS)

Ruli, F.; Kurniawan, B.; Imaduddin, A.

2018-04-01

In this paper, the authors report the electrical properties of polycrystalline La0.8Ca0.17Ag0.03MnO3 manganites synthesized using sol-gel method. The X-ray diffraction (XRD) patterns of polycrystalline La0.8Ca0.17Ag0.03MnO3 samples reveal an orthorhombic perovskite structure with Pnma space group. Analysis using energy dispersive X-ray (EDX) confirms that the sample contains all expected chemical elements without any additional impurity. The measurement of resistivity versus temperature using cryogenic magnetometer was performed to investigate the electrical properties. The results show that the electrical resistivity of polycrystalline La0.8Ca0.17Ag0.03MnO3 exhibits metalic behavior below 244 K. The temperature dependence of electrical resistivity dominantly emanates from electron-electron scattering and the grain/domain boundary play a important role in conduction mechanism in polycrystalline La0.8Ca0.17Ag0.03MnO3.

Characterization of iron-phosphate-silicate chemical garden structures.

PubMed

Barge, Laura M; Doloboff, Ivria J; White, Lauren M; Stucky, Galen D; Russell, Michael J; Kanik, Isik

2012-02-28

Chemical gardens form when ferrous chloride hydrate seed crystals are added or concentrated solutions are injected into solutions of sodium silicate and potassium phosphate. Various precipitation morphologies are observed depending on silicate and phosphate concentrations, including hollow plumes, bulbs, and tubes. The growth of precipitates is controlled by the internal osmotic pressure, fluid buoyancy, and membrane strength. Additionally, rapid bubble-led growth is observed when silicate concentrations are high. ESEM/EDX analysis confirms compositional gradients within the membranes, and voltage measurements across the membranes during growth show a final potential of around 150-200 mV, indicating that electrochemical gradients are maintained across the membranes as growth proceeds. The characterization of chemical gardens formed with iron, silicate, and phosphate, three important components of an early earth prebiotic hydrothermal system, can help us understand the properties of analogous structures that likely formed at submarine alkaline hydrothermal vents in the Hadean-structures offering themselves as the hatchery of life. © 2011 American Chemical Society

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.

Jingle-bell-shaped ferrite hollow sphere with a noble metal core: Simple synthesis and their magnetic and antibacterial properties

NASA Astrophysics Data System (ADS)

Li, Siheng; Wang, Enbo; Tian, Chungui; Mao, Baodong; Kang, Zhenhui; Li, Qiuyu; Sun, Guoying

2008-07-01

In this paper, a simple strategy is developed for rational fabrication of a class of jingle-bell-shaped hollow structured nanomaterials marked as Ag@ MFe 2O 4 ( M=Ni, Co, Mg, Zn), consisting of ferrite hollow shells and metal nanoparticle cores, using highly uniform colloidal Ag@C microspheres as template. The final composites were obtained by direct adsorption of metal cations Fe 3+ and M 2+ on the surface of the Ag@C spheres followed by calcination process to remove the middle carbon shell and transform the metal ions into pure phase ferrites. The as-prepared composites were characterized by X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray analysis (EDX), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), UV-vis spectroscopy and SQUID magnetometer. The results showed that the composites possess the magnetic property of the ferrite shell and the optical together with antibacterial property of the Ag core.

Scanning electron microscopy (SEM) and X-ray dispersive spectrometry evaluation of direct laser metal sintering surface and human bone interface: a case series.

PubMed

Mangano, Carlo; Piattelli, Adriano; Raspanti, Mario; Mangano, Francesco; Cassoni, Alessandra; Iezzi, Giovanna; Shibli, Jamil Awad

2011-01-01

Recent studies have shown that direct laser metal sintering (DLMS) produces structures with complex geometry and consequently that allow better osteoconductive properties. The aim of this patient report was to evaluate the early bone response to DLMS implant surface retrieved from human jaws. Four experimental DLMS implants were inserted in the posterior mandible of four patients during conventional dental implant surgery. After 8 weeks, the micro-implants and the surrounding tissue were removed and prepared for scanning electron microscopy (SEM) and histomorphometric analysis to evaluate the bone-implant interface. The SEM and EDX evaluations showed a newly formed tissue composed of calcium and phosphorus. The bone-to-implant contact presented a mean of 60.5 ± 11.6%. Within the limits of this patient report, data suggest that the DLMS surfaces presented a close contact with the human bone after a healing period of 8 weeks.

Optical and magnetic properties of zinc oxide quantum dots doped with cobalt and lanthanum.

PubMed

Yu, Shiyong; Zhao, Jing; Su, Hai-Quan

2013-06-01

Cobalt and Lanthanum-doped ZnO QDs are synthesized by a modified sol-gel method under atmospheric conditions. The as-prepared quantum dots are characterized by X-ray powder diffraction (XRD), energy dispersive X-ray (EDX) analysis and high resolution transmission electron microscopy (HRTEM). The optical properties of the products are studied by fluorescent spectroscopy. With a proper Co and La doping, these nanoparticles possess exceptionally small size and enhanced fluorescence. Hysteresis loops of un-doped ZnO QDs and Co and La-doped ZnO QDs indicate that both the samples show ferromagnetic behavior at room temperature. Finally, these nanoparticles can label the BGC 803 cells successfully in short time and present no evidence of toxicity or adverse affect on cell growth even at the concentration up to 1 mM. We expect that the as-prepared Co and La-doped ZnO QDs can provide a better reliability of the collected data and find promising applications in biological, medical and other fields.

Investigation of white pigments used as make-up during the Greco-Roman period

NASA Astrophysics Data System (ADS)

Welcomme, E.; Walter, P.; van Elslande, E.; Tsoucaris, G.

2006-06-01

Different white pigments were used during antiquity to prepare white make-up for women faces. Combining observations and elemental analysis with structural information, we were able to determine the mineralogical composition of cosmetics, the trace element content and the microstructure of the crystals. SEM/EDX analyses enabled us to describe the choice of materials and their preparation by grinding or chemical synthesis to obtain white pigments. For the Hellenistic period, we have mainly found lead white, which required an elaborated synthesis process. Quantitative X-ray diffraction allowed us to establish different ratios of hydrocerussite 2PbCO3·Pb(OH)2 and cerussite PbCO3. These data can be linked to the chemical conditions of preparation described by ancient authors. On the other hand, analyses of Roman cosmetics from Pompeii, Gaul and Germany show the use of materials commonly found in nature like gypsum or calcite. We will discuss the material properties in relation with the make-up uses.

Fretting Fatigue Experiment and Analysis of AlSi9Cu2Mg Alloy

PubMed Central

Wang, Jun; Xu, Hong; Su, Tiexiong; Zhang, Yi; Guo, Zhen; Mao, Huping; Zhang, Yangang

2016-01-01

An investigation was carried out in order to study the fretting fatigue behavior of an AlSi9Cu2Mg aluminum alloy. The fretting fatigue tests of AlSi9Cu2Mg were performed using a specially designed testing machine. The failure mechanism of fretting fatigue was explored by studying the fracture surfaces, fretting scars, fretting debris, and micro-hardness of fretting fatigue specimens using scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and micro Vickers hardness test techniques. The experimental results show that the fretting fatigue limit (42 MPa) is significantly reduced to approximately 47% of the plain fatigue limit (89 MPa) under 62.5 MPa contact pressure. Furthermore, the fretting fatigue life decreases with increasing alternating stress and increasing contact pressure. The examination results suggest that the stress concentrates induced by oxidation-assisted wear on the contact interface led to the earlier initiation and propagation of crack under the fretting condition. PMID:28774103

Fabrication of cellulose-based aerogels from waste newspaper without any pretreatment and their use for absorbents.

PubMed

Jin, Chunde; Han, Shenjie; Li, Jingpeng; Sun, Qingfeng

2015-06-05

Cellulose-based aerogel (CBA) was prepared from waste newspaper (WNP) without any pretreatment using 1-allyl-3-methyimidazolium chloride (AmImCl) as a solvent via regeneration and an environmentally friendly freeze-drying method. After being treated with trimethylchlorosilane (TMCS) via a simple thermal chemical vapor deposition process, the resulting CBAs were rendered both hydrophobic and oleophilic. Successful silanization on the surface of the porous CBA was verified by a variety of techniques including scanning electron microscopy (SEM), energy-dispersive X-ray analysis (EDX), and water contact angle (WCA) measurements. As a result, the silane-coated, interconnected CBAs not only exhibited good absorption performance for oils (e.g., waste engine oil), but also showed absorption capacity for organic solvents such as chloroform (with a representative weight gain ranging from 11 to 22 times of their own dry weight), making them diversified absorbents for potential applications including sewage purification. Copyright © 2015 Elsevier Ltd. All rights reserved.

Fretting Fatigue Experiment and Analysis of AlSi9Cu2Mg Alloy.

PubMed

Wang, Jun; Xu, Hong; Su, Tiexiong; Zhang, Yi; Guo, Zhen; Mao, Huping; Zhang, Yangang

2016-12-05

An investigation was carried out in order to study the fretting fatigue behavior of an AlSi9Cu2Mg aluminum alloy. The fretting fatigue tests of AlSi9Cu2Mg were performed using a specially designed testing machine. The failure mechanism of fretting fatigue was explored by studying the fracture surfaces, fretting scars, fretting debris, and micro-hardness of fretting fatigue specimens using scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and micro Vickers hardness test techniques. The experimental results show that the fretting fatigue limit (42 MPa) is significantly reduced to approximately 47% of the plain fatigue limit (89 MPa) under 62.5 MPa contact pressure. Furthermore, the fretting fatigue life decreases with increasing alternating stress and increasing contact pressure. The examination results suggest that the stress concentrates induced by oxidation-assisted wear on the contact interface led to the earlier initiation and propagation of crack under the fretting condition.

Fabrication of Cu-Ag core-shell bimetallic superfine powders by eco-friendly reagents and structures characterization

NASA Astrophysics Data System (ADS)

Zhao, Jun; Zhang, Dongming; Zhao, Jie

2011-09-01

Superfine bimetallic Cu-Ag core-shell powders were synthesized by reduction of copper sulfate pentahydrate and silver nitrate with eco-friendly ascorbic acid as a reducing agent and cyclodextrins as a protective agent in an aqueous system. The influence of Ag/Cu ratio on coatings was investigated. Ag was homogeneously distributed on the surface of Cu particles at a mole ratio of Ag/Cu=1. FE-SEM showed an uniformity of Ag coatings on Cu particles. Antioxidation of Cu particles was improved by increasing Ag/Cu ratio. TEM-EDX and UV-vis spectra also revealed that Cu cores were covered by Ag nanoshells on the whole. The surface composition analysis by XPS indicated that only small parts of Cu atoms in the surface were oxidized. It was noted that the hindrance of cyclodextrins chemisorbed on particles plays an important role in forming high quality and good dispersity Cu-Ag (Cu@Ag) core-shell powders.

Study on crystallization kinetics and phase evolution in Li2O-Al2O3-GeO2-P2O5 glass-ceramics system

NASA Astrophysics Data System (ADS)

Das, Anurup; Dixit, Anupam; Goswami, Madhumita; Mythili, R.; Hajra, R. N.

2018-04-01

To address the safety issues related to liquid electrolyte and improve the battery performance, Solid State Electrolytes (SSEs) are now in frontier area of research interest. We report here synthesis of Li-SSE based on Li2O-Al2O3-GeO2-P2O5 (LAGP) system with NASICON structure. Glass sample with nominal composition Li1.5Al0.5Ge1.5P2.5Si0.5O12 was prepared by melt-quenching technique. Non-isothermal crystallization kinetics was studied using DSC and activation energy of crystallisation was calculated to be ˜ 246 kJ/mol using Kissinger's equation. XRD of heat treated samples show the formation of required LiGe2(PO4)3 phase along with other minor phases. Compositional analysis using SEM-EDX confirms enrichment of Ge and Si along the grain boundaries.

Synthesis, Characterization, and Mechanism of Formation of Janus-Like Nanoparticles of Tantalum Silicide-Silicon (TaSi2/Si)

PubMed Central

Nomoev, Andrey V.; Bardakhanov, Sergey P.; Schreiber, Makoto; Bazarova, Dashima Zh.; Baldanov, Boris B.; Romanov, Nikolai A.

2014-01-01

Metal-semiconductor Janus-like nanoparticles with the composition tantalum silicide-silicon (TaSi2/Si) were synthesized for the first time by means of an evaporation method utilizing a high-power electron beam. The composition of the synthesized particles were characterized using high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), selective area electron diffraction (SAED), and energy dispersive X-ray fluorescence (EDX) analysis. The system is compared to previously synthesized core-shell type particles in order to show possible differences responsible for the Janus-like structure forming instead of a core-shell architecture. It is proposed that the production of Janus-like as opposed to core-shell or monophase particles occurs due to the ability of Ta and Si to form compounds and the relative content of Ta and Si atoms in the produced vapour. Based on the results, a potential mechanism of formation for the TaSi2/Si nanoparticles is discussed. PMID:28346996

Synthesis, Characterization, and Mechanism of Formation of Janus-Like Nanoparticles of Tantalum Silicide-Silicon (TaSi₂/Si).

PubMed

Nomoev, Andrey V; Bardakhanov, Sergey P; Schreiber, Makoto; Bazarova, Dashima Zh; Baldanov, Boris B; Romanov, Nikolai A

2014-12-25

Metal-semiconductor Janus-like nanoparticles with the composition tantalum silicide-silicon (TaSi₂/Si) were synthesized for the first time by means of an evaporation method utilizing a high-power electron beam. The composition of the synthesized particles were characterized using high-resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD), selective area electron diffraction (SAED), and energy dispersive X-ray fluorescence (EDX) analysis. The system is compared to previously synthesized core-shell type particles in order to show possible differences responsible for the Janus-like structure forming instead of a core-shell architecture. It is proposed that the production of Janus-like as opposed to core-shell or monophase particles occurs due to the ability of Ta and Si to form compounds and the relative content of Ta and Si atoms in the produced vapour. Based on the results, a potential mechanism of formation for the TaSi₂/Si nanoparticles is discussed.

A vibrational spectroscopic study of the phosphate mineral vantasselite Al4(PO4)3(OH)3·9H2O

NASA Astrophysics Data System (ADS)

Frost, Ray L.; Scholz, Ricardo; Belotti, Fernanda Maria; López, Andrés; Theiss, Frederick L.

2015-08-01

We have studied the phosphate mineral vantasselite Al4(PO4)3(OH)3·9H2O using a combination of SEM with EDX and Raman and infrared spectroscopy. Qualitative chemical analysis shows Al, Fe and P. Raman bands at 1013 and 1027 cm-1 are assigned to the PO43- ν1 symmetric stretching mode. The observation of two bands suggests the non-equivalence of the phosphate units in the vantasselite structure. Raman bands at 1051, 1076 and 1090 cm-1 are attributed to the PO43- ν3 antisymmetric stretching vibration. A comparison is made with the spectroscopy of wardite. Strong infrared bands at 1044, 1078, 1092, 1112, 1133, 1180 and 1210 cm-1 are attributed to the PO43- ν3 antisymmetric stretching mode. Some of these bands may be due to δAl2OH deformation modes. Vibrational spectroscopy offers a mechanism for the study of the molecular structure of vantasselite.

Non-Metallic Ti Oxides and MnS/FeS2 Complex Precipitation in Ti-Killed Steel

NASA Astrophysics Data System (ADS)

Chen, Jieyun; Zhao, Dan; Li, Huigai; Zheng, Shaobo

Titanium deoxidized experiments can be carried in vacuum induction furnace by adding Ti-Fe alloy in molten steel to simulate strip casting. Sub-rapid solidification samples were obtained in the method of suing copper mold. The morphology, the chemical composition and the structures of nanometer precipitations were carried out to investigate by transmission electron microscope (TEM) with Energy Dispersive X ray Spectrum (EDX) and by collecting diffraction patterns with carbon extraction specimens. It has been found that titanium oxides were TiO monoclinic, Ti4O7 anorthic and TiO2 orthogonal structure in one nanometer inclusion, as the composite oxide was precipitated MnS/FeS2 cubic structure during sub-rapid solidification. Thermodynamic calculation analysis showed that it was possible to precipitate different kinds of nonstoichiometric TiOx. The solid solution between MnS/FeS2 will precipitate on the surface of titanium oxides because of good coherency relationship.

First Description of Sulphur-Oxidizing Bacterial Symbiosis in a Cnidarian (Medusozoa) Living in Sulphidic Shallow-Water Environments.

PubMed

Abouna, Sylvie; Gonzalez-Rizzo, Silvina; Grimonprez, Adrien; Gros, Olivier

2015-01-01

Since the discovery of thioautotrophic bacterial symbiosis in the giant tubeworm Riftia pachyptila, there has been great impetus to investigate such partnerships in other invertebrates. In this study, we present the occurrence of a sulphur-oxidizing symbiosis in a metazoan belonging to the phylum Cnidaria in which this event has never been described previously. Scanning Electron Microscope (SEM), Transmission Electron Microscope (TEM) observations and Energy-dispersive X-ray spectroscopy (EDXs) analysis, were employed to unveil the presence of prokaryotes population bearing elemental sulphur granules, growing on the body surface of the metazoan. Phylogenetic assessments were also undertaken to identify this invertebrate and microorganisms in thiotrophic symbiosis. Our results showed the occurrence of a thiotrophic symbiosis in a cnidarian identified as Cladonema sp. This is the first report describing the occurrence of a sulphur-oxidizing symbiosis in a cnidarian. Furthermore, of the two adult morphologies, the polyp and medusa, this mutualistic association was found restricted to the polyp form of Cladonema sp.

Polypyrrole Coated Cellulosic Substrate Modified by Copper Oxide as Electrode for Nitrate Electroreduction

NASA Astrophysics Data System (ADS)

Hamam, A.; Oukil, D.; Dib, A.; Hammache, H.; Makhloufi, L.; Saidani, B.

2015-08-01

The aim of this work is to synthesize polypyrrole (PPy) films on nonconducting cellulosic substrate and modified by copper oxide particles for use in the nitrate electroreduction process. Firstly, the chemical polymerization of polypyrrole onto cellulosic substrate is conducted by using FeCl3 as an oxidant and pyrrole as monomer. The thickness and topography of the different PPy films obtained were estimated using a profilometer apparatus. The electrochemical reactivity of the obtained electrodes was tested by voltamperometry technique and electrochemical impedance spectroscopy. Secondly, the modification of the PPy film surface by incorporation of copper oxide particles is conducted by applying a galvanostatic procedure from a CuCl2 solution. The SEM, EDX and XRD analysis showed the presence of CuO particles in the polymer films with dimensions less than 50 nm. From cyclic voltamperometry experiments, the composite activity for the nitrate electroreduction reaction was evaluated and the peak of nitrate reduction is found to vary linearly with initial nitrate concentration.

FE-SEM, FIB and TEM Study of Surface Deposits of Apollo 15 Green Glass Volcanic Spherules

NASA Technical Reports Server (NTRS)

Ross, Daniel K.; Thomas-Keprta, K. L.; Rahman, Z.; Wentworth, S. J.; McKay, D. S.

2011-01-01

Surface deposits on lunar pyroclastic green (Apollo 15) and orange (Apollo 17) glass spherules have been attributed to condensation from the gas clouds that accompanied fire-fountain eruptions. The fire fountains cast molten lava high above the lunar surface and the silicate melt droplets quenched before landing producing the glass beads. Early investigations showed that these deposits are rich in sulfur and zinc. The deposits are extremely fine-grained and thin, so that it was never possible to determine their chemical compositions cleanly by SEM/EDX or electron probe x-ray analysis because most of the excited volume was in the under-lying silicate glass. We are investigating the surface deposits by TEM, using focused ion beam (FIB) microscopy to extract and thin the surface deposits. Here we report on chemical mapping of a FIB section of surface deposits of an Apollo green glass bead 15401using the ultra-high resolution JEOL 2500 STEM located at NASA Johnson Space Center.

Palladium and palladium-tin supported on multi wall carbon nanotubes or carbon for alkaline direct ethanol fuel cell

NASA Astrophysics Data System (ADS)

Geraldes, Adriana Napoleão; Furtunato da Silva, Dionisio; Martins da Silva, Júlio César; Antonio de Sá, Osvaldo; Spinacé, Estevam Vitório; Neto, Almir Oliveira; Coelho dos Santos, Mauro

2015-02-01

Pd and PdSn (Pd:Sn atomic ratios of 90:10), supported on Multi Wall Carbon Nanotubes (MWCNT) or Carbon (C), are prepared by an electron beam irradiation reduction method. The obtained materials are characterized by X-Ray diffraction (XRD), Energy dispersive X-ray analysis (EDX), Transmission electron Microscopy (TEM) and Cyclic Voltammetry (CV). The activity for ethanol electro-oxidation is tested in alkaline medium, at room temperature, using Cyclic Voltammetry and Chronoamperometry (CA) and in a single alkaline direct ethanol fuel cell (ADEFC), in the temperature range of 60-90 °C. CV analysis finds that Pd/MWCNT and PdSn/MWCNT presents onset potentials changing to negative values and high current values, compared to Pd/C and PdSn/C electrocatalysts. ATR-FTIR analysis, performed during the CV, identifies acetate and acetaldehyde as principal products formed during the ethanol electro-oxidation, with low conversion to CO2. In single fuel cell tests, at 85 °C, using 2.0 mol L-1 ethanol in 2.0 mol L-1 KOH solutions, the electrocatalysts supported on MWCNT, also, show higher power densities, compared to the materials supported on carbon: PdSn/MWCNT, presents the best result (36 mW cm-2). The results show that the use of MWCNT, instead of carbon, as support, plus the addition of small amounts of Sn to Pd, improves the electrocatalytic activity for Ethanol Oxidation Reaction (EOR).

High performance of SDC and GDC core shell type composite electrolytes using methane as a fuel for low temperature SOFC

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

Irshad, Muneeb; Siraj, Khurram, E-mail: razahussaini786@gmail.com, E-mail: khurram.uet@gmail.com; Javed, Fayyaz

Nanocomposites Samarium doped Ceria (SDC), Gadolinium doped Ceria (GDC), core shell SDC amorphous Na{sub 2}CO{sub 3} (SDCC) and GDC amorphous Na{sub 2}CO{sub 3} (GDCC) were synthesized using co-precipitation method and then compared to obtain better solid oxide electrolytes materials for low temperature Solid Oxide Fuel Cell (SOFCs). The comparison is done in terms of structure, crystallanity, thermal stability, conductivity and cell performance. In present work, XRD analysis confirmed proper doping of Sm and Gd in both single phase (SDC, GDC) and dual phase core shell (SDCC, GDCC) electrolyte materials. EDX analysis validated the presence of Sm and Gd in bothmore » single and dual phase electrolyte materials; also confirming the presence of amorphous Na{sub 2}CO{sub 3} in SDCC and GDCC. From TGA analysis a steep weight loss is observed in case of SDCC and GDCC when temperature rises above 725 °C while SDC and GDC do not show any loss. The ionic conductivity and cell performance of single phase SDC and GDC nanocomposite were compared with core shell GDC/amorphous Na{sub 2}CO{sub 3} and SDC/ amorphous Na{sub 2}CO{sub 3} nanocomposites using methane fuel. It is observed that dual phase core shell electrolytes materials (SDCC, GDCC) show better performance in low temperature range than their corresponding single phase electrolyte materials (SDC, GDC) with methane fuel.« less

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.

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.

Application of EIS and SECM Studies for Investigation of Anticorrosion Properties of Epoxy Coatings Containing Zinc Oxide Nanoparticles on Mild Steel in 3.5% NaCl Solution

NASA Astrophysics Data System (ADS)

Raj, X. Joseph

2017-07-01

The effect of corrosion protection performance of epoxy coatings containing ZnO nanoparticle on mild steel in 3.5% NaCl solution was analyzed using scanning electrochemical microscopy and electrochemical impedance spectroscopy (EIS). Line profile and topographic image analysis were measured by applying -0.70 and +0.60 V as the tip potential for the cathodic and anodic reactions, respectively. The tip current at -0.70 V for the epoxy-coated sample with ZnO nanoparticles decreased rapidly, which is due to cathodic reduction in dissolved oxygen. The EIS measurements were taken in 3.5% NaCl after wet and dry cyclic corrosion test. The increase in the film resistance ( R f) and charge transfer resistance ( R ct) values was confirmed by the addition of ZnO nanoparticles in the epoxy coating. SEM/EDX analysis showed that complex oxide layer of zinc was enriched in corrosion products at a scratched area of the coated steel after corrosion testing. FIB-TEM analysis confirmed the presence of the nanoscale complex oxide layer of Zn in the rust of the steel that had a beneficial effect on the corrosion resistance of coated steel by forming protective corrosion products in the wet/dry cyclic test.

The hoard of Beçin—non-destructive analysis of the silver coins

NASA Astrophysics Data System (ADS)

Rodrigues, M.; Schreiner, M.; Mäder, M.; Melcher, M.; Guerra, M.; Salomon, J.; Radtke, M.; Alram, M.; Schindel, N.

2010-05-01

We report the results of an analytical investigation on 416 silver-copper coins stemming from the Ottoman Empire (end of 16th and beginning of 17th centuries), using synchrotron micro X-ray fluorescence analysis (SRXRF). In the past, analyses had already been conducted with energy dispersive X-ray fluorescence analysis (EDXRF), scanning electron microscopy with energy dispersive X-ray spectrometry (SEM/EDX) and proton induced X-ray emission spectroscopy (PIXE). With this combination of techniques it was possible to confirm the fineness of the coinage as well as to study the provenance of the alloy used for the coins. For the interpretation of the data statistical analysis (principal component analysis—PCA) has been performed. A definite local assignment was explored and significant clustering was obtained regarding the minor and trace elements composing the coin alloys.

Electron Microscopy Studies of Comet Wild-2 Particulate Residue Preserved in the Stardust Metallic Foil Craters

NASA Astrophysics Data System (ADS)

Graham, G. A.; Kearsley, A. T.; Dai, Z.; Leroux, H.; Teslich, N. E.; Stroud, R.; Borg, J.; Bradley, J. P.; Horz, F. P.; Zolensky, M.

2006-12-01

The study of comets is fundamental to the understanding of early solar system processes. Much of the current knowledge of cometary compositions comes from `fly-by' missions or remote sensing studies but not, until now, from the laboratory analyses of samples. The Stardust spacecraft (NASA's 4th Discovery mission) was launched in 1999 and in January 2004 had a successful fly-by close to the nucleus of comet Wild 2. During the encounter, the collector tray assembly containing the principle particle capture technology of low- density silica aerogel was deployed. In addition, the metallic foils (1100 series Aluminum) wrapped around the collector frame also picked up material from the 6.1 km/s cometary particle collisions. Since the retrieval of the sample return capsule in January 2006, and as part of the preliminary examination, a selected number of foils have been scanned using SEM-EDX to locate cometary dust derived impact craters. Craters ranging from 100 nanometers to several hundreds of micrometers in diameter, containing both monomineralic and polymineralic projectile melts, have been identified, measured and analyzed. Focused ion beam microscopy techniques have been used to take cross-section slices of either individual craters or specific residue fragments, and thin them to electron transparency. TEM-EDX analysis of these slices shows that crystalline grains are occasionally preserved, despite the high shock pressures and temperatures that caused most of the particle to melt. Observations from the crater residues make a useful addition to studies of the composition and mineralogy of the cometary particulates preserved within the impact tracks in the silica aerogel. This work was in part performed under the auspices of the U.S. Department of Energy, National Nuclear Security Administration by the University of California, Lawrence Livermore National Laboratory under contract No. W-7405-Eng-48.

Mn-Cr isotopic systematics of individual Chainpur chondrules. [Abstract only

NASA Technical Reports Server (NTRS)

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

1994-01-01

Twenty-eight chondrules separated from Chainpur (LL3.4) were surveyed for abundances of Mn, Cr, Na, Fe, Sc, Hf, Ir, and Zn by Instrumental Neutron Activation Analysis (INAA). Six, weighting 0.6-1.5 mg each, were chosen for Scanning Electron Microscopy (SEM)/Energy Dispersive X-ray (EDX) and high-precision Ce-isotopic studies. LL-chondrite-normalized (Mn/Fe)(sub LL) and (Sc/Fe)(sub LL) were found to be useful in categorizing them. Five chondrules (CH-16, -17, -18, -23, and -28) were in the range 0.5 less than (Mn/Fe)(sub LL) less than 1. 4 and 0.5 less than (Sc/Fe)(sub LL) less than 1.4. The sixth (CH-25) had (Mn/Fe)(sub LL) and (Sc/Fe)(sub LL) ratios of 0.40 and 8.1, respectively, and was enriched in the refractory lithophile elements Sc and Hf and the refractory siderophile element Ir by 2.7 and 4.4x LL abundances respectively. SEM/EDX of exterior surfaces of the chondrules showed they consisted of varying proportions of low- and high-Ca pyroxenes, olivine, glass, kamacite/taenite, and Fe-sulfides. Chromium-53/chromium-52 for the six chondrules and bulk Chainpur (WR) are presented. Chromium-54/chromium-52 is close to terrestrial and does not correlate with Mn/Cr. We provisionally ignore the possibility of initial Cr isotopic heterogeneities among the chondrules. Omitting both the CH-25 and WR data, a linear regression gives initial (Mn-53/Mn-55)(sub I) = 8 +/- 4 x 10(exp -6), corresponding to chondrule formation at Delta(t)(sub LEW) = -9 +/- 4 Ma prior to igneous crystallization of the LEW 86010 angrite. If initial (Mn-53/Mn-55)(sub 0) in the solar system were as high as approximately 4.4 x 10(exp -5) when Allende CAI formed, our data suggest Chainpur chondrules formed approximately 9 Ma later, in qualitative agreement with 'late' I-Xe formation ages for most Chainpur chondrules.

Recovery of zinc and cadmium from spent batteries using Cyphos IL 102 via solvent extraction route and synthesis of Zn and Cd oxide nanoparticles.

PubMed

Singh, Rashmi; Mahandra, Harshit; Gupta, Bina

2017-09-01

The overall aim of this study is to separate and recover zinc and cadmium from spent batteries. For this purpose Cyphos IL 102 diluted in toluene was employed for the extraction and recovery of Zn and Cd from Zn-C and Ni-Cd batteries leach liquor. The influence of extractant concentration for the leach liquors of Zn-C (0.01-0.05mol/L) and Ni-Cd (0.04-0.20mol/L) batteries has been investigated. Composition of the leach liquor obtained from Zn-C/Ni-Cd spent batteries is Zn - 2.18g/L, Mn - 4.59g/L, Fe - 4.0×10 -3 g/L, Ni - 0.2×10 -3 g/L/Cd - 4.28g/L, Ni - 0.896×10 -1 g/L, Fe - 0.148g/L, Co - 3.77×10 -3 g/L, respectively. Two stage counter current extraction at A/O 1:1 and 3:2 with 0.04mol/L and 0.2mol/L Cyphos IL 102 for Zn and Cd, respectively provide more than 99.0% extraction of both the metal ions with almost negligible extraction of associated metal ions. A stripping efficiency of around 99.0% for Zn and Cd was obtained at O/A 1:1 using 1.0mol/L HNO 3 in two and three counter current stages, respectively. ZnO and CdO were also synthesized using the loaded organic phase and characterized using XRD, FE-SEM and EDX techniques. XRD peaks of ZnO and CdO correspond to zincite and monteponite, respectively. The average particle size was ∼27.0nm and ∼37.0nm for ZnO and CdO, respectively. The EDX analysis of ZnO and CdO shows almost 1:1 atomic percentage. Copyright © 2017. Published by Elsevier Ltd.

Chemical speciation of size-segregated floor dusts and airborne magnetic particles collected at underground subway stations in Seoul, Korea.

PubMed

Jung, Hae-Jin; Kim, BoWha; Malek, Md Abdul; Koo, Yong Sung; Jung, Jong Hoon; Son, Youn-Suk; Kim, Jo-Chun; Kim, HyeKyoung; Ro, Chul-Un

2012-04-30

Previous studies have reported the major chemical species of underground subway particles to be Fe-containing species that are generated from wear and friction processes at rail-wheel-brake and catenaries-pantographs interfaces. To examine chemical composition of Fe-containing particles in more details, floor dusts were collected at five sampling locations of an underground subway station. Size-segregated floor dusts were separated into magnetic and non-magnetic fractions using a permanent magnet. Using X-ray diffraction (XRD) and scanning electron microscopy/energy dispersive X-ray spectrometry (SEM/EDX), iron metal, which is relatively harmless, was found to be the dominating chemical species in the floor dusts of the <25 μm size fractions with minor fractions of Mg, Al, Si, Ca, S, and C. From SEM analysis, the floor dusts of the <25 μm size fractions collected on railroad ties appeared to be smaller than 10 μm, indicating that their characteristics should somewhat reflect the characteristics of airborne particles in the tunnel and the platform. As most floor dusts are magnetic, PM levels at underground subway stations can be controlled by removing magnetic indoor particles using magnets. In addition, airborne subway particles, most of which were smaller than 10 μm, were collected using permanent magnets at two underground subway stations, namely Jegi and Yangjae stations, in Seoul, Korea. XRD and SEM/EDX analyses showed that most of the magnetic aerosol particles collected at Jegi station was iron metal, whereas those at Yangjae station contained a small amount of Fe mixed with Na, Mg, Al, Si, S, Ca, and C. The difference in composition of the Fe-containing particles between the two subway stations was attributed to the different ballast tracks used. Copyright © 2012 Elsevier B.V. All rights reserved.

Structural, Magnetic and Microwave Properties of Nanocrystalline Ni-Co-Gd Ferrites

NASA Astrophysics Data System (ADS)

Nikzad, Alireza; Parvizi, Roghaieh; Rezaei, Ghasem; Vaseghi, Behrooz; Khordad, Reza

2018-02-01

A series of Co- and Gd-substituted NiFe2O4 ferrite nanoparticles with the formula Ni1- x Co x Fe2- y Gd y O4 (where x = 0.0-1.0 and y = 0.0-0.1) have been successfully synthesized using a hydrothermal method. X-ray diffraction and field emission scanning electron microscopy results indicated that a highly crystallized spherical ferrite nanoparticle structure was obtained along with an increase in the lattice parameters. Compositional analysis of the prepared nanoferrite powders has been carried out using energy-dispersive x-ray (EDX) spectra. The EDX analysis reveals the presence of Ni, Co, Gd and Fe elements in the specimens. Magnetization and the coercive field improved dramatically with an increase in the amount of cobalt and gadolinium added, attributed to the redistribution of cations in the spinel nanoferrite structure. Saturation magnetization and coercivity values up to 99 emu/g and 918 Oe, respectively, were measured using a vibration sample magnetometer at room temperature. Comparative microwave absorption experiments demonstrated that the reflection loss (RL) properties enhanced with increasing substitution of cations in the Ni-ferrite spinel structure for an absorber thickness of 1.8 mm. A maximum RL of - 26.7 dB was obtained for substituted Ni-Co-Gd nanoferrite with x = 1.0 and y = 0.1 at a frequency of 9.4 GHz with a bandwidth of 3.6 GHz (RL ≤ - 10 dB). Experimental results revealed that the synthesized nanoparticles possessed great potential in microwave absorption applications.

Ultrastructure and elemental analysis of Hypoxis hemerocallidea: a multipurpose medicinal plant.

PubMed

Afolayan, Anthony J; Otunola, Gloria A

2014-01-01

Herbal medicine is a popular means of medical management in some parts of the world especially in Africa. Hypoxis hemerocallidea Fisch.C.A.Mey. & Avé-Lall, also known as African potato of the Hypoxidaecae family, is one of the medicinal plants that have enjoyed long usage as an herbal medicine in South Africa. In this study, the morphology and elemental constituents of H. hemerocallidea leaf was investigated to correlate the functional role of the ultrastructure in the production of therapeutic compounds. Fresh leaves of H. hemerocallidea were prepared for analysis using standard methods. The ultrastructure and crystal deposits of the plant were assessed using scanning electron microscopy (SEM), and energy dispersive x-ray (EDX). It was observed that the leaves were characterised by multicelullar glandular and non glandular trichomes which are sparsely distributed over the entire surfaces. The glandular trichomes (GTs) in H. hemerocallidea leaf have boulbous heads which are probably filled with secretions, while the non glandular trichomes were long, fibrous and sparse. EDX-SEM of Hypoxis hemerocallidea leaf revealed that carbon, oxygen, nitrogen and silicon are the major components of the deposits, while other elements such as iron, sulphur, sodium, calcium, magnesium, potassium, manganese, iodine, chromium and iodine were present in small but variable amounts. The presence of these elements which are crucial to maintaining good health, in addition to other bioactive constituents might be accountable for the multipurpose therapeutic uses of Hypoxis hemerocallidea in the treatment of cancers, HIV/AIDS related diseases, urinary tract infections, cardiovascular disorders, diabetes and other chronic ailments of humans.

Total reflection X-ray fluorescence analysis of airborne silver nanoparticles from fabrics.

PubMed

Menzel, Magnus; Fittschen, Ursula Elisabeth Adriane

2014-03-18

Ag nanoparticles (NPs) are usually applied to consumer products because of their antimicrobial properties, which are desired in fabrics for sportswear as well as cloth used for cleaning. Hazards to human health from airborne Ag NPs may occur when the NPs are inhaled. NPs are comparable in size to macromolecules and viruses and able to penetrate deep into the lungs, e.g., the alveoli, where they may cause damage to cells and tissue due to their large surface area. In this study, aerosols released form fabrics treated with Ag NPs were collected using a low pressure Berner impactor and analyzed with total reflection X-ray fluorescence (TXRF). We found that the Ag NPs are released primarily in the form of larger particles, mainly 0.13-2 μm, probably attached to fiber material. Using an electron micro probe, single particles could be identified. The detection of backscattered electrons suggests small spots on the particle consist of a heavier element, which most likely is Ag, although the signal in energy-dispersive X-ray spectroscopy (EDX) was below the lower limit of detection (LOD). To achieve LODs necessary for Ag determination, Ar peaks were eliminated by a nitrogen atmosphere provided by the "Picofox-box". This enables linear calibration and quantification of Ag. The LOD was calculated at 0.2 ng (2.0 ppb). Following the TXRF and scanning electron microscopy (SEM)/EDX analysis, the aerosol samples were dissolved in nitric acid and analyzed with ICPMS to successfully confirm the results obtained by the TXRF measurements.

Microbial Immobilization of Si, Mn, Fe, and Sr Ions in the Nacreous Layer of Sinohyliopsis schlegeli and Environmental Factors

NASA Astrophysics Data System (ADS)

Tazaki, Kazue; Morii, Issei

Environmental changes recorded in the shell nacre of Sinohyliopsis schlegeli were observed with elemental factors of characteristic water and nutrition for eight months in a cultivated drainage pond at Kanazawa University, Ishikawa Prefecture, Japan. Tetracycline as an indicator was injected into the shell nacre once every month from May to November in 2007. Water qualities such as the pH, redox potential, electrical conductivity, dissolved oxygen concentration, and water temperature were measured periodically, and the suspended solids in the water were removed by filtration for optical microscopy, X-ray fluorescence analysis, and scanning electron microscopy-energy dispersive X-ray (SEM-EDX) observations. X-ray fluorescence chemical analysis of shell nacre indicated layers with strong tetracycline accumulation corresponding to high concentrations of Si, Mn, Fe, and Sr ions. The redox potential and dissolved oxygen concentration measurements supported the existence of layers in the nacre. The suspended materials in the drainage pond water comprised mainly of Si, Mn, and Fe elements, which were the same elements involved in microbial immobilization in the shell nacre during the summer of 2007. SEM-EDX analyses confirmed that the ions originated from diatoms, Siderocapsa sp. and Gallionella ferruginea in the stomach. There was little microbial immobilization of the ions in winter. The results suggested elemental immobilization in the layered shell nacre and indicated that Sinohyliopsis schlegeli fed on the ions, to grow the nacre during summer. Sinohyliopsis schlegeli with these biogenic oxides might contribute to the scavenging of heavy metals in natural water.

An eco-benign synthesis of AgNPs using aqueous extract of Longan fruit peel: Antiproliferative response against human breast cancer cell line MCF-7, antioxidant and photocatalytic deprivation of methylene blue.

PubMed

Khan, Arif Ullah; Yuan, Qipeng; Khan, Zia Ul Haq; Ahmad, Aftab; Khan, Faheem Ullah; Tahir, Kamran; Shakeel, Muhammad; Ullah, Sadeeq

2018-05-07

Plants mediated synthesis of noble metal nanoparticles is encountered as a clean, environment friendly, lucrative and benign loom. The current study consists of clean and green synthesis of Silver nanoparticles (AgNPs). Phytoconstituents from Longan (Euphorbia longana Lam.) fruit peel were used to reduce Ag + into AgNPs. Different analytical techniques i.e. UV-vis Spectroscopy, X-ray diffraction spectroscopy (XRD), electron dispersive X-ray (EDX), High-resolution transmission electron microscopy (HRTEM) and Fourier transform infrared spectroscopy (FTIR) were used to analyze the synthesized AgNPs. AgNPs have localized surface plasmon resonance (LSPR) peak at 445 nm which is confirmed by UV-vis spectroscopy. HRTEM showed that the prepared AgNPs are spheroid in shape and well dispersed while XRD results showed that the AgNPs are face centered cubic crystalline. EDX confirmed the elemental composition of AgNPs. The antiproliferative response of AgNPs was assayed by an exhaustive MTT assay. AgNPs showed potent anticancer activity (88%) against breast cancer cells MCF-7. Moreover, the green produced AgNPs effectively scavenged 91% of the stable and harmful 2, 2-diphenyl-1-picrylhydrazyl (DPPH) free radical which confirms its' efficient antioxidant nature. AgNPs have profound photocatalytic degradation (99%) of methylene blue in a short period of time (7 min). The noteworthy biological and photocatalytic responses of the green and cleanly produced AgNPs are encountered to their well dispersion, petite volume and round shaped structure. Copyright © 2018 Elsevier B.V. All rights reserved.

A comparison study of Co and Cu doped MgO diluted magnetic thin films

NASA Astrophysics Data System (ADS)

Sarıtaş, S.; ćakıcı, T.; Muǧlu, G. Merhan; Kundakcı, M.; Yıldırım, M.

2017-02-01

Transition metal-doped MgO diluted magnetic thin films are appropriate candidates for spintronic applications and designing magnetic devices and sensors. Therefore, MgO:Co and MgO:Cu films were deposited on glass substrates by Chemical Spray Pyrolysis (CSP) method different thin film deposition parameters. Deposited different transition metal doped MgO thin films were compared in terms of optic and structural properties. Comparison optic analysis of the films was investigated spectral absorption and transmittance measurements by UV-Vis double beam spectrophotometer technique. Comparison structural analysis of the thin films was examined by using XRD, Raman Analysis, SEM, EDX and AFM techniques. The transition metal-doped; MgO:Co and MgO:Cu thin films maybe have potential applications in spintronics and magnetic data storage.

Galvanic displacement reaction and rapid thermal annealing in size/shape controlling silver nanoparticles on silicon substrate

NASA Astrophysics Data System (ADS)

Ghosh, Tapas; Satpati, Biswarup

2017-05-01

The effect of the thermal annealing on silver nanoparticles deposited on silicon surface has been studied. The silver nanoparticles have been deposited by the galvanic displacement reaction. Rapid thermal annealing (RTA) has been performed on the Si substrate, containing the silver nanoparticles. The scanning transmission electron microscopy (STEM), energy dispersive X-ray (EDX) spectroscopy and scanning electron microscopy (SEM) study show that the galvanic displacement reaction and subsequent rapid thermal annealing could lead to well separated and spherical shaped larger silver nanoparticles on silicon substrate.

One-pot ultrasonic-assisted method for preparation of Ag/AgCl sensitized ZnO nanostructures as visible-light-driven photocatalysts

NASA Astrophysics Data System (ADS)

Naghizadeh-Alamdari, Sara; Habibi-Yangjeh, Aziz; Pirhashemi, Mahsa

2015-02-01

Ultrasonic-assisted method was applied for preparation of Ag/AgCl sensitized ZnO nanostructures by one-pot procedure in water without using any post preparation treatments. The resultant nanocomposites were characterized by XRD, EDX, SEM, DRS, XPS, BET, and PL techniques. In the nanocomposites, ZnO and AgCl have wurtzite hexagonal and cubic crystalline phases, respectively and their surface morphologies remarkably change with increasing mole fraction of silver chloride. The EDX and XPS techniques show that the prepared samples are extremely pure. Ability of the nanocomposites for absorption of visible-light irradiation enhanced with increasing AgCl content. Photocatalytic examination of the nanocomposites was carried out using aqueous solution of methylene blue under visible-light irradiation. The degradation rate constant on the nancomposite rapidly increases with mole fraction of silver chloride up to 0.237. Enhancing activity of the nanocomposite was attributed to its ability for absorbing visible light and separation of electron-hole pairs. Furthermore, influence of ultrasonic irradiation time, calcination temperature, catalyst weight, pH of solution, and scavengers of reactive species on the degradation activity was investigated and the results were discussed. Finally, the photocatalyst has good activity after five successive cycles.

Processing, characterization, and in vitro/in vivo evaluations of powder metallurgy processed Ti-13Nb-13Zr alloys.

PubMed

Bottino, Marco C; Coelho, Paulo G; Henriques, Vinicius A R; Higa, Olga Z; Bressiani, Ana H A; Bressiani, José C

2009-03-01

This article presents details of processing, characterization and in vitro as well as in vivo evaluations of powder metallurgy processed Ti-13Nb-13Zr samples with different levels of porosity. Sintered samples were characterized for density, crystalline phases (XRD), and microstructure (SEM and EDX). Samples sintered at 1000 degrees C showed the highest porosity level ( approximately 30%), featuring open and interconnected pores ranging from 50 to 100 mum in diameter but incomplete densification. In contrast, samples sintered at 1300 and 1500 degrees C demonstrated high densification with 10% porosity level distributed in a homogeneous microstructure. The different sintering conditions used in this study demonstrated a coherent trend that is increase in temperature lead to higher sample densification, even though densification represents a drawback for bone ingrowth. Cytotoxicity tests did not reveal any toxic effects of the starting and processed materials on surviving cell percentage. After an 8-week healing period in rabbit tibias, the implants were retrieved, processed for nondecalcified histological evaluation, and then assessed by backscattered electron images (BSEI-SEM) and EDX. Bone growth into the microstructure was observed only in samples sintered at 1000 degrees C. Overall, a close relation between newly formed bone and all processed samples was observed. (c) 2008 Wiley Periodicals, Inc.

Superplastic Forming of Duplex Stainless Steel for Aerospace Part

NASA Astrophysics Data System (ADS)

Lee, Ho-Sung; Yoon, Jong-Hoon; Yoo, Joon-Tae; Yi, Young-Moo

2011-08-01

In this study, the high temperature forming behavior of duplex stainless steel has been characterized and the outer shell of a combustion chamber was fabricated with pressure difference of hot gas. It consists of two parts which are the outer skin made of stainless steel to sustain the internal pressure and the inner shell made of copper alloy for regenerative cooling channels. Two outer skins partitioned to half with respect to the symmetric axis was prepared by hot gas forming process with a maximum pressure of 7 MPa following to FEM analysis. For inner layer, copper alloy was machined for cooling channels and then placed in the gas pressure welding fixture. It is shown that the optimum condition of gas pressure welding is 7 MPa at 890 °C, for one hour. EDX analysis and scanning electron microscope micrograph confirm the atomic diffusion process is observed at the interface and copper atoms diffuse into steel, while iron and chrome atoms diffuse into copper. The result shows that the manufacturing method with superplastic forming and gas pressure welding of steel and copper alloy has been successful for near net shape manufacturing of scaled combustion chamber of launch vehicle.

Rare earth substitution on structural and optical behaviour of CdSe thin films

NASA Astrophysics Data System (ADS)

Singh, Sarika; Shrivastava, A. K.; Tapdiya, Swati

2018-05-01

A series of Sm2+,Gd2+ doped with Cadmium selenide CdSe (x =0.01) has been prepared by using Chemical bath deposition technique. Structural, Optical and Morphological studies were performed using X-ray diffraction (XRD), UV-Visible spectrometer, Raman Studies and Scanning Electron Microscopy (SEM). XRD patterns confirm the samples with Sm,Gd ions, some diffraction peaks appeared which belongs to the cubic phase structure. The values of lattice parameter (a) decreased and particle size decrease on doping. Morphology of the grown films reveals that surface are homogeneous and uniformly spread on the substrates. The elemental analysis of CdSe doped Sm and Gd (1%) different composition was analyzed by Energy Dispersive X-Rays (EDX). The optical values of some important parameters of the studied films were calculated by UVstudy are determined from transmission spectra at wavelength 200 to 900nm. Optical band gap Eg was calculated by tauc relation. Energy band gap of CdSe doped with Sm and Gd varies at 1.8eV and 1.9eV respectively. Bandgap In Raman analysis, a prominent peak shows that confirmation of nano crystalline phase. And intensity of peaks was decreasing after doping.

The Influence of Porosity on Corrosion Attack of Austenitic Stainless Steel

NASA Astrophysics Data System (ADS)

Abdullah, Z.; Ismail, A.; Ahmad, S.

2017-10-01

Porous metals also known as metal foams is a metallic body having spaces orpores through which liquid or air may pass. Porous metals get an attention from researchers nowadays due to their unique combination of properties includes excellent mechanical and electrical, high energy absorption, good thermal and sound insulation and water and gas permeability. Porous metals have been applied in numerous applications such as in automotive, aerospace and also in biomedical applications. This research reveals the influence of corrosion attack in porous austenitic stainless steel 316L. The cyclic polarization potential analysis was performed on the porous austenitic stainless steel 316L in 3.5% NaCl solution. The morphology and the element presence on the samples before and after corrosion attack was examined using scanning electron microscopy (SEM) and energy dispersive x-ray (EDX) respectively to determine the corrosion mechanism structure. The cyclic polarization potential analysis showed the result of (E corr ) for porous austenitic stainless steel type 316L in the range of -0.40v to -0.60v and breakdown potential (E b ) is -0.3v to -0.4v in NaCl solution.

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.

Transformation of Silver Nanoparticles in Sewage Sludge during Incineration.

PubMed

Meier, Christoph; Voegelin, Andreas; Pradas del Real, Ana; Sarret, Geraldine; Mueller, Christoph R; Kaegi, Ralf

2016-04-05

Silver nanoparticles (Ag-NP) discharged into the municipal sewer system largely accumulate in the sewage sludge. Incineration and agricultural use are currently the most important strategies for sewage sludge management. Thus, the behavior of Ag-NP during sewage sludge incineration is essential for a comprehensive life cycle analysis and a more complete understanding of the fate of Ag-NP in the (urban) environment. To address the transformation of Ag-NP during sewage sludge incineration, we spiked metallic Ag(0)-NP to a pilot wastewater treatment plant and digested the sludge anaerobically. The sludge was then incinerated on a bench-scale fluidized bed reactor in a series of experiments under variable conditions. Complementary results from X-ray absorption spectroscopy (XAS) and electron microscopy-energy dispersive X-ray (EM-EDX) analysis revealed that Ag(0)-NP transformed into Ag2S-NP during the wastewater treatment, in agreement with previous studies. On the basis of a principal component analysis and subsequent target testing of the XAS spectra, Ag(0) was identified as a major Ag component in the ashes, and Ag2S was clearly absent. The reformation of Ag(0)-NP was confirmed by EM-EDX. The fraction of Ag(0) of the total Ag in the ashes was quantified by linear combination fitting (LCF) of XAS spectra, and values as high as 0.8 were found for sewage sludge incinerated at 800 °C in a synthetic flue gas atmosphere. Low LCF totals (72% to 94%) indicated that at least one relevant reference spectrum was missing in the LCF analysis. The presence of spherical Ag-NP with a diameter of <50 nm extending into the sub-nm range was revealed by electron microscopy analyses. The rapid formation of Ag(0)-NP from Ag2S during sewage sludge incineration, as demonstrated in this study, needs to be considered in the life cycle assessment of engineered Ag-NP.

Eco-friendly synthesis of TiO2, Au and Pt doped TiO2 nanoparticles for dye sensitized solar cell applications and evaluation of toxicity

NASA Astrophysics Data System (ADS)

Gopinath, K.; Kumaraguru, S.; Bhakyaraj, K.; Thirumal, S.; Arumugam, A.

2016-04-01

Driven by the demand of pure TiO2, Au and Pt doped TiO2 NPs were successfully synthesized using Terminalia arjuna bark extract. The eco-friendly synthesized NPs were characterized by UV-Vis-DRS, ATR-FT-IR, PL, XRD, Raman, SEM with EDX and TEM analysis. The synthesized NPs were investigation for dye sensitized solar cell applications. UV-Vis-Diffused Reflectance Spectra clearly showed that the expected TiO2 inter band absorption below 306 nm, incorporation of gold shows surface plasma resonant (SPR) near 555 nm and platinum incorporated TiO2 NPs shows absorbance at 460 nm. The energy conversion efficiency for Au doped TiO2 NPs when compared to pure and Pt doped TiO2 NPs. In addition to that, Au noble metal present TiO2 matrix and an improve open-circuit voltage (Voc) of DSSC. Synthesized NPs was evaluated into antibacterial and antifungal activities by disk diffusion method. It is observed that NPs have not shown any activities in all tested bacterial and fungal strains. In this eco-friendly synthesis method to provide non toxic and environmental friendly nanomaterials can be used for solar energy device application.

Effect of reactor temperature on direct growth of carbon nanomaterials on stainless steel

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

Edzatty, A. N., E-mail: nuredzatty@gmail.com; Syazwan, S. M., E-mail: mdsyazwan.sanusi@gmail.com; Norzilah, A. H., E-mail: norzilah@unimap.edu.my

Currently, carbon nanomaterials (CNMs) are widely used for various applications due to their extraordinary electrical, thermal and mechanical properties. In this work, CNMs were directly grown on the stainless steel (SS316) via chemical vapor deposition (CVD). Acetone was used as a carbon source and argon was used as carrier gas, to transport the acetone vapor into the reactor when the reaction occurred. Different reactor temperature such as 700, 750, 800, 850 and 900 °C were used to study their effect on CNMs growth. The growth time and argon flow rate were fixed at 30 minutes and 200 ml/min, respectively. Characterizationmore » of the morphology of the SS316 surface after CNMs growth using Scanning Electron Microscopy (SEM) showed that the diameter of grown-CNMs increased with the reactor temperature. Energy Dispersive X-ray (EDX) was used to analyze the chemical composition of the SS316 before and after CNMs growth, where the results showed that reduction of catalyst elements such as iron (Fe) and nickel (Ni) at high temperature (700 – 900 °C). Atomic Force Microscopy (AFM) analysis showed that the nano-sized hills were in the range from 21 to 80 nm. The best reactor temperature to produce CNMs was at 800 °C.« less

TiO2 Nanotube-Carbon (TNT-C) as Support for Pt-based Catalyst for High Methanol Oxidation Reaction in Direct Methanol Fuel Cell.

PubMed

Abdullah, M; Kamarudin, S K; Shyuan, L K

2016-12-01

In this study, TiO 2 nanotubes (TNTs) were synthesized via a hydrothermal method using highly concentrated NaOH solutions varying from 6 to 12 M at 180 °C for 48 h. The effects of the NaOH concentration and the TNT crystal structure on the performance for methanol oxidation were investigated to determine the best catalyst support for Pt-based catalysts. The results showed that TNTs produced with 10 M NaOH exhibited a length and a diameter of 550 and 70 nm, respectively; these TNTs showed the best nanotube structure and were further used as catalyst supports for a Pt-based catalyst in a direct methanol fuel cell. The synthesized TNT and Pt-based catalysts were analysed by FESEM, TEM, BET, EDX, XRD and FTIR. The electrochemical performance of the catalysts was investigated using cyclic voltammetry (CV) and chronoamperometric (CA) analysis to further understand the methanol oxidation in the direct methanol fuel cell (DMFC). Finally, the result proves that Pt-Ru/TNT-C catalyst shows high performance in methanol oxidation as the highest current density achieved at 3.3 mA/cm 2 (normalised by electrochemically active surface area) and high catalyst tolerance towards poisoning species was established.

Green synthesis of Copper nanoparticle using ionic liquid-based extraction from Polygonum minus and their applications.

PubMed

Ullah, Habib; Wilfred, Cecilia Devi; Shaharun, Maizatul Shima

2018-06-06

The present work reports the extraction of phenolic compounds from Polygonum minus using ionic liquid as extracting solvent. In this work, 1-Butyl-3-methylimidazolium hydrogen sulfate [BMIM][HSO 4 ] was used for the extraction of bioactive compounds. Accordingly, ionic liquids based microwave-assisted extraction treatment for separating of bioactive compounds from polygonum minus was first performed in the present study. The results obtained in this work have high extraction yield in comparison with conventional solvent. UV/Vis results showed that microwave synthesis was fast, well dispersed and nanosized copper nanoparticle (CuNPs) in comparison with conventional synthesis. CuNPs was characterized by X-Rays diffractometer (XRD), Fourier transform infrared (FTIR), dynamic light scattering (DLS), field emission scanning electron microscopy combined with energy dispersive x-rays (FESEM-EDX), and thermogravimetric analysis (TGA). All the instrumental analyses confirmed the particles were nanosized. Furthermore, the antibacterial activity of as-synthesized CuNPs showed effective inhibitory zone against three different bacteria. The photocatalytic degradation of copper nanoparticles was studied using methylene blue (MB) and methyl orange (MO) dyes under UV light and degraded 99.9% within short time 8 and 7 minutes.

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.

Synthesis and characterization of molybdenum catalysts supported on {gamma}-Al{sub 2}O{sub 3}-CeO{sub 2} composite oxides

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

Farooq, Muhammad; Ramli, Anita; Subbarao, Duvvuri

2012-09-26

The physical and chemical properties of a catalyst play a vital role in various industrial applications. Molybdenum catalysts supported on {gamma}-Al{sub 2}O{sub 3} and {gamma}-Al{sub 2}O{sub 3}-CeO{sub 2} mixed oxides with varying loading of CeO{sub 2} (5, 10, 15, 20 wt% with respect to {gamma}-Al{sub 2}O{sub 3}) were prepared by wet impregnation method. The physiochemical properties of these synthesized Mo catalysts were studied with various characterization techniques such as X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), temperature-programmed reduction (TPR), field emission scanning electron microscopy-energy dispersive analysis (FESEM-EDX) and X-ray fluorescence spectrometer (XRF). The results showed that the addition of CeO{submore » 2} into the support affected the binding energies of the elements and reducibility of the metal oxides formed after calcination of catalyst samples due to the change in metal-support interaction. Further, the characterization techniques showed that the active metal was well dispersed on the surface of support material.« less

Temperature and pH effect on reduction of graphene oxides in aqueous solution

NASA Astrophysics Data System (ADS)

Tai, Guoan; Zeng, Tian; Li, Hongxiang; Liu, Jinsong; Kong, Jizhou; Lv, Fuyong

2014-09-01

Reduced graphene oxides (RGOs) have usually been obtained by hydrazine reduction, but hydrazine-related compounds are corrosive, highly flammable and very hazardous, and the obtained RGOs heavily aggregated. Here we investigated extensively the effect of temperature and pH value on the structure of RGOs in hydrothermal environments without any reducing agents. The attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectra showed that reduction rate of GOs remarkably increased with the temperature from 100 to 180 °C and with pH value from 3 to 10. Field emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) exhibited the structural transition of the RGOs. Energy-dispersive x-ray analysis (EDX) showed the reduction degree of the RGO samples quantitatively. The results demonstrate that the GOs can be reduced controllably by a hydrothermal reduction process at pH value of 10 at 140 °C, and the large-scale RGOs are cut into small nanosheets with size from several to a few tens of nanometers with increasing temperature and duration. This study provides a feasible approach to controllably reduce GO with different nanostructures such as porous structures and quantum dots for applications in optoelectronics and biomedicals.

Rice husk ash (RHA) as a partial cement replacement in modifying peat soil properties

NASA Astrophysics Data System (ADS)

Daud, Nik Norsyahariati Nik; Daud, Mohd Nazrin Mohd; Muhammed, Abubakar Sadiq

2018-02-01

This paper describes the effect of rice husk ash (RHA) and ordinary Portland cement (OPC) as a potential binder for modifying the properties of peat soil. The amounts RHA and OPC added to the peat soil sample, as percentage of the dry soil mass were in the range of 10-15% and 15%, respectively. Observations were made for the changes in the properties of the soil such as maximum dry density (MDD), optimum moisture content (OMC) and shear strength. Scanning Electron Micrograph-Energy Dispersive X-Ray (SEM-EDX) test were also conducted to observe the microstructure of treated and untreated peat soil. The results show that the modified soil of MDD and OMC values are increased due to the increment amount of binder material. Shear strength values of modified peat showing a good result by assuming that it is relative to the formation of major reaction products such as calcium silicate hydrate (C-S-H). The presence of C-S-H formation is indicated by the results produced from microstructural analysis of peat before and after modification process. This depicts the potential usage of RHA as a partial cement replacement in peat soil which is also improving its engineering properties.

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.

Evidence for exocellular Arsenic in Fronds of Pteris vittata

DOE PAGES

Datta, Rupali; Das, Padmini; Tappero, Ryan; ...

2017-06-06

The arsenic (As) hyperaccumulating fern species Pteris vittata (PV) is capable of accumulating large quantities of As in its aboveground tissues. Transformation to AsIII and vacuolar sequestration is believed to be the As detoxification mechanism in PV. Here we present evidence for a preponderance of exocellular As in fronds of Pteris vittata despite numerous reports of a tolerance mechanism involving intracellular compartmentalization. Results of an extraction experiment show that 43–71% of the As extruded out of the fronds of PV grown in 0.67, 3.3 and 6.7 mM AsV. SEM-EDX analysis showed that As was localized largely on the lower pinnamore » surface, with smaller amounts on the upper surface, as crystalline deposits. X-ray fluorescence imaging of pinna cross-sections revealed preferential localization of As on the pinna surface in the proximity of veins, with the majority localized near the midrib. Majority of the As in the pinnae is contained in the apoplast rather than vacuoles. Our results provide evidence that exocellular sequestration is potentially a mechanism of As detoxification in PV, particularly at higher As concentrations, raising concern about its use for phytoremediation.« less

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.

Evidence for exocellular Arsenic in Fronds of Pteris vittata

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

Datta, Rupali; Das, Padmini; Tappero, Ryan

The arsenic (As) hyperaccumulating fern species Pteris vittata (PV) is capable of accumulating large quantities of As in its aboveground tissues. Transformation to AsIII and vacuolar sequestration is believed to be the As detoxification mechanism in PV. Here we present evidence for a preponderance of exocellular As in fronds of Pteris vittata despite numerous reports of a tolerance mechanism involving intracellular compartmentalization. Results of an extraction experiment show that 43–71% of the As extruded out of the fronds of PV grown in 0.67, 3.3 and 6.7 mM AsV. SEM-EDX analysis showed that As was localized largely on the lower pinnamore » surface, with smaller amounts on the upper surface, as crystalline deposits. X-ray fluorescence imaging of pinna cross-sections revealed preferential localization of As on the pinna surface in the proximity of veins, with the majority localized near the midrib. Majority of the As in the pinnae is contained in the apoplast rather than vacuoles. Our results provide evidence that exocellular sequestration is potentially a mechanism of As detoxification in PV, particularly at higher As concentrations, raising concern about its use for phytoremediation.« less

Formation of secondary minerals in a lysimeter approach - A mineral-microbe interaction

NASA Astrophysics Data System (ADS)

Schäffner, F.; Merten, D.; De Giudici, G.; Beyer, A.; Akob, D. M.; Ricci, P. C.; Küsel, K.; Büchel, G.

2012-04-01

Heavy metal contamination of large areas due to uranium mining operations poses a serious long-term environmental problem. In the Ronneburg district (eastern Thuringia, Germany), leaching of low grade uranium bearing ores (uranium content < 300 g/t) occurred from 1972 to 1990 using acid mine drainage (AMD; pH 2.7-2.8) and diluted sulphuric acid (10 g/l). Secondary mineral phases like birnessite, todorokite and goethite occur within a natural attenuation process associated with enrichment of heavy metals, especially Cd, Ni, Co, Cu and Zn due to a residual contamination even after remediation efforts. To reveal the processes of secondary mineral precipitation in the field a laboratory lysimeter approach was set up under in situ-like conditions. Homogenized soil from the field site and pure quartz sand were used as substrates. In general, in situ measurements of redox potentials in the substrates showed highly oxidizing conditions (200-750 mV). Water was supplied to the lysimeter from below via a mariottés bottle containing contaminated groundwater from the field. Evaporation processes were allowed, providing a continuous flow of water. This led to precipitation of epsomite and probably aplowite on the top layer of substrate, similar to what is observed in field investigations. After 4 weeks, the first iron and manganese bearing secondary minerals became visible. Soil water samples were used to monitor the behaviour of metals within the lysimeter. Saturation indices (SI) for different secondary minerals were calculated with PHREEQC. The SI of goethite showed oversaturation with respect to the soil solution. SEM-EDX analyses and IR spectroscopy confirmed the formation of goethite. Geochemical data revealed that goethite formation was mainly dominated by Eh/pH processes and that heavy metals, e.g. Zn and U, could be enriched in this phase. Although Eh/pH data does not support formation of manganese minerals, Mn(II)-oxidizing bacteria (MOB) could be isolated from field soil samples, supporting the fact that microorganisms may influence this natural attenuation process. Laser ablation ICP-MS data reveal accumulation of manganese in MOB biomass on Mn(II)-containing agar plates. Furthermore, it was possible to show the importance of iron on this process, as some MOB isolates were able to oxidize manganese independently from the iron content, whereas some are not. The latter isolates are only able to oxidize manganese if iron is present in the media. In the lysimeter, SEM-EDX data showed microorganisms in organic rich phases together with the occurrence of manganese, oxygen, and nickel, indicating manganese oxides enriched in nickel. Although this new mineral phases could not yet be identified microprobe EDX results from polished thin sections showed needle-like mineral structures that are similar to the birnessite and todorokite samples observed from field samples. Hence, the lysimeter experiment revealed that the formation of iron and manganese minerals that are involved in heavy metal natural attenuation is result of both abiotic and biotic processes.

Data of chemical analysis and electrical properties of SnO2-TiO2 composite nanofibers.

PubMed

Bakr, Zinab H; Wali, Qamar; Ismail, Jamil; Elumalai, Naveen Kumar; Uddin, Ashraf; Jose, Rajan

2018-06-01

In this data article, we provide energy dispersive X-ray spectroscopy (EDX) spectra of the electrospun composite (SnO 2 -TiO 2 ) nanowires with the elemental values measured in atomic and weight%. The linear sweep voltammetry data of composite and its component nanofibers are provided. The data collected in this article is directly related to our research article "Synergistic combination of electronic and electrical properties of SnO 2 and TiO 2 in a single SnO 2 -TiO 2 composite nanowire for dye-sensitized solar cells" [1].

In-situ laser-induced synthesis of associated YVO4:Eu3+@SiO2@Au-Ag/C nanohybrids with enhanced luminescence

NASA Astrophysics Data System (ADS)

Kolesnikov, I. E.; lvanova, T. Yu.; Ivanov, D. A.; Kireev, A. A.; Mamonova, D. V.; Golyeva, E. V.; Mikhailov, M. D.; Manshina, A. A.

2018-02-01

Associated luminescence/plasmonic nanoparticles were prepared in a single step process as a result of laser illumination (low intensity CW He-Cd laser) of colloidal solution of YVO4:Eu3+@SiO2 mixed with heterometallic supramolecular complex. The results of SEM-EDX analysis, absorption, steady-state luminescence and luminescence decay measurements revealed formation of associated nanohybrids with core/shell morphology. The obtained nanostructures demonstrated metal enhanced luminescence with enhancement factor of 1.6. The theoretical calculations revealed strong correlation of enhancement factor and plasmonic nanoparticles number.

Superconductivity at different T{sub c} in CdBa{sub 2}Ca{sub 2}Cu{sub 3}O{sub y}

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

Balchev, N.; Lovchinov, V.; Gattef, E.

1995-06-01

A Cd analogue of the Tl and Hg n=3 series with nominal composition CdBa{sub 2}Ca{sub 2}Cu{sub 3}O{sub y} has been synthesized. The samples were superconducting according to magnetic susceptibility measurements. The critical temperature was 103 or 107 K depending on the preparation conditions. The EDX analysis revealed the presence of Cd-1111, Cd-1121, and Cd-2333 as minor phases. The observed diamagnetic effects were attributed to the different T{sub c} of these phases.

Chlorination Kinetics of Titanium Nitride for Production of Titanium Tetrachloride from Nitrided Ilmenite

NASA Astrophysics Data System (ADS)

Ahmadi, Eltefat; Rezan, Sheikh Abdul; Baharun, Norlia; Ramakrishnan, Sivakumar; Fauzi, Ahmad; Zhang, Guangqing

2017-10-01

The kinetics of chlorination of titanium nitride (TiN) was investigated in the temperature range of 523 K to 673 K (250 °C to 400 °C). The results showed that the extent of chlorination slightly increased with increasing temperature and decreasing particle size of titanium nitride at constant flow rate of N2-Cl2 gas mixture. At 523 K (250 °C), the extent of chlorination was 85.6 pct in 60 minutes whereas at 673 K (400 °C), it was 97.7 pct investigated by weight loss measurement and confirmed by ICP analyses. The experimental results indicated that a shrinking unreacted core model with mixed-control mechanism governed the chlorination rate. It was observed that the surface chemical reaction of chlorine gas on the surface of TiN particles was rate controlling in the initial stage and, during later stage, internal (pore) diffusion through the intermediate product layer was rate controlling step. Overall the process follows the mixed-control model incorporating both chemical reaction and internal diffusion control. The activation energy for the chlorination of TiN was found to be about 10.97 kJ mol-1. In processing TiCl4 from TiN and TiO0.02C0.13N0.85, the solids involved in the chlorination process were characterized by X-ray diffraction (XRD), Scanning electron microscopy (SEM) and Energy-dispersive X-ray spectrometer (EDX). The SEM/EDX results demonstrated the consumption of TiN particles with extent of chlorination that showed shrinking core behavior.

Direct Metal Deposition of Functional Graded Structures in Ti- Al System

NASA Astrophysics Data System (ADS)

Shishkovsky, I.; Missemer, F.; Smurov, I.

A direct laser metal deposition (DLMD) technology with co-axial powder injection is used to fabricate a complex functional graded structure (FGS) fabrication. The aim of the study is to demonstrate the possibility to produce intermetallic phases in the Ti-Al powder systems in the course of a single-step DMD process. Besides, relationships between the main laser cladding parameters and the intermetallic phase structures of the built-up objects have been studied. In our research we applied the optical microscopy, X-ray analysis, microhardness measurement and SEM with EDX analysis of the laser-fabricated intermetallics. The discussion of the mechanisms of Ti x Al y (x,y = 1.3) intermetallic transformations in exothermal reactions is also offered in the report.

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.

Effect of heterogeneity and shape on optical properties of urban dust based on three-dimensional modeling of individual particles

NASA Astrophysics Data System (ADS)

Conny, Joseph M.; Ortiz-Montalvo, Diana L.

2017-09-01

We show the effect of composition heterogeneity and shape on the optical properties of urban dust particles based on the three-dimensional spatial and optical modeling of individual particles. Using scanning electron microscopy/energy-dispersive X-ray spectroscopy (SEM/EDX) and focused ion beam (FIB) tomography, spatial models of particles collected in Los Angeles and Seattle accounted for surface features, inclusions, and voids, as well as overall composition and shape. Using voxel data from the spatial models and the discrete dipole approximation method, we report extinction efficiency, asymmetry parameter, and single-scattering albedo (SSA). Test models of the particles involved (1) the particle's actual morphology as a single homogeneous phase and (2) simple geometric shapes (spheres, cubes, and tetrahedra) depicting composition homogeneity or heterogeneity (with multiple spheres). Test models were compared with a reference model, which included the particle's actual morphology and heterogeneity based on SEM/EDX and FIB tomography. Results show particle shape to be a more important factor for determining extinction efficiency than accounting for individual phases in a particle, regardless of whether absorption or scattering dominated. In addition to homogeneous models with the particles' actual morphology, tetrahedral geometric models provided better extinction accuracy than spherical or cubic models. For iron-containing heterogeneous particles, the asymmetry parameter and SSA varied with the composition of the iron-containing phase, even if the phase was <10% of the particle volume. For particles containing loosely held phases with widely varying refractive indexes (i.e., exhibiting "severe" heterogeneity), only models that account for heterogeneity may sufficiently determine SSA.

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.

Facile Preparation of Ultrafine Aluminum Hydroxide Particles with or without Mesoporous MCM-41 in Ambient Environments.

PubMed

Dubovoy, Viktor; Subramanyam, Ravi; Stranick, Michael; Du-Thumm, Laurence; Pan, Long

2017-05-11

An aqueous suspension of nanogibbsite was synthesized via the titration of aluminum aqua acid [Al(H2O)6] 3+ with L-arginine to pH 4.6. Since the hydrolysis of aqueous aluminum salts is known to produce a wide array of products with a wide range of size distributions, a variety of state-of-the-art instruments (i.e., 27 Al/ 1 H NMR, FTIR, ICP-OES, TEM-EDX, XPS, XRD, and BET) were used to characterize the synthesis products and identification of byproducts. The product, which was comprised of nanoparticles (10-30 nm), was isolated using gel permeation chromatography (GPC) column technique. Fourier transform infrared (FTIR) spectroscopy and powder X-ray diffraction (PXRD) identified the purified material as the gibbsite polymorph of aluminum hydroxide. The addition of inorganic salts (e.g., NaCl) induced electrostatic destabilization of the suspension, thereby agglomerating the nanoparticles to yield Al(OH)3 precipitate with large particle sizes. By utilizing the novel synthetic method described here, Al(OH)3 was partially loaded inside the highly ordered mesoporous framework of MCM-41, with average pore dimensions of 2.7 nm, producing an aluminosilicate material with both octahedral and tetrahedral Al (Oh/Td = 1.4). The total Al content, measured using energy-dispersive X-ray spectrometry (EDX), was 11% w/w with a Si/Al molar ratio of 2.9. A comparison of bulk EDX with surface X-ray photoelectron spectroscopy (XPS) elemental analysis provided insight into the distribution of Al within the aluminosilicate material. Furthermore, a higher ratio of Si/Al was observed on the external surface (3.6) as compared to the bulk (2.9). Approximations of O/Al ratios suggest a higher concentration of Al(O)3 and Al(O)4 groups near the core and external surface, respectively. The newly developed synthesis of Al-MCM-41 yields a relatively high Al content while maintaining the integrity of the ordered silica framework and can be used for applications where hydrated or anhydrous Al2O3 nanoparticles are advantageous.