Search results for: fluorescence microscopy

Authors: J. Ramos, V. Gil, A. F. Torres

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The nodular iron is a material that has shown great advantages respect to other materials (steel and gray iron) in the production of machine elements. The engineering industry, especially automobile, are potential users of this material. As it is known, the alloying elements modify the properties of steels and castings. Copper has been investigated as a structural modifier of nodular iron, but studies of its mechanical and tribological implications still need to be addressed for industrial use. With the aim of improving the mechanical properties of nodular iron, alloying elements (Mn, Si, and Cu) are added in order to increase their pearlite (or ferrite) structure according to the percentage of the alloying element. In this research (using induction furnace process) nodular iron with three different percentages of copper (residual, 0,5% and 1,2%) was obtained. Chemical analysis was performed by optical emission spectrometry and microstructures were characterized by Optical Microscopy (ASTM E3) and Scanning Electron Microscopy (SEM). The study of mechanical behavior was carried out in a mechanical test machine (ASTM E8) and a Pin on disk tribometer (ASTM G99) was used to assess wear resistance. It is observed that copper increases the pearlite structure improving the wear behavior; tension behavior. This improvement is observed in higher proportion with 0,5% due to the fact that too much increase of pearlite leads to ductility loss.

Keywords: copper, mechanical properties, nodular iron, pearlite structure, wear

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Authors: A. Srion, W. Thepsuwan, N. Monmaturapoj

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Two Lithium disilicate (LD) glass ceramics based on SiO2-Li2O-K2O-Al2O3 system were prepared through glass melting method and then fabricated into dental crowns via hot pressing at 850˚C and 900˚C in order to study the effect of the pressing temperatures on theirs phase formation and microstructure. The factor such as heat treatment temperature (as-cast glass, 600˚C and 700˚C) of the glass ceramics used to press was also investigated the effect of an initial microstructure before pressing. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used to determine phase formation and microstructure of the samples, respectively. X-ray diffraction result shows that the main crystalline structure was Li2Si2O5 by having Li3PO4, Li0.6Al0.6Si2O6, Li2SiO3, Ca5 (PO4)3F, SiO2 as minor phases. Glass compositions with different heat treatment temperatures exhibited a difference phase formation but have less effect during pressing. Scanning electron microscopy analysis showed microstructure of lath-like of Li2Si2O5 in all glasses. With increasing the initial heat treatment temperature, the longer the lath-like crystals of lithium disilicate were increased especially when using glass heat treatment at 700˚C followed by pressing at 900˚C. This could be suggested that LD1 heat treatment at 700˚C which pressing at 900˚C presented the best formation by hot pressing and compiled microstructure.

Keywords: lithium disilicate, hot pressing, dental crown, microstructure

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Authors: Chandrasekaran, Ravisankar N. Harikrishnan, Rajalakshmi, K. K. Satapathy M. V. R. Prasad, K. V. Kanagasabapathy

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Heavy metals were considered as highly toxic environmental pollutants to soil ecosystem and human health. In present study the 12 heavy metals (Mg, Al, K, Ca, Ti, Fe, V, Cr, Mn, Co,Ni and Zn.) are determined in soils of Yelagiri hills, Tamilnadu by energy dispersive X-ray fluorescence technique. Metal concentrations were used to quantify pollution contamination factors such as enrichment factor (EF), geo-accumulation index (Igeo) and contamination factor (CF) are calculated and reported.

Keywords: soil, heavy metals, EDXRF, pollution contamination factors

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Authors: M.F. Elkady, Sahar Zaki, Desouky Abd-El-Haleem

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Silver nanoparticles (AgNPs) are already widely prepared using different technologies. However, there are limited data on the effects of hydrogen ion concentration on nano-silver production. In this investigation, the impact of the pH reaction medium toward the particle size, agglomeration and the yield of the produced bio-synthesized silver were established. Quasi-spherical silver nanoparticles were synthesized through the biosynthesis green production process using the Egyptian E. coli bacterial strain 23N at different pH values. The formation of AgNPs has been confirmed with ultraviolet–visible spectra through identification of their characteristic peak at 410 nm. The quantitative production yield and the orientation planes of the produced nano-silver were examined using X-ray spectroscopy (EDS) and X-ray diffraction (XRD). Quantitative analyses indicated that the silver production yield was promoted at elevated pH regarded to increase the reduction rate of silver precursor through both chemical and biological processes. As a result, number of the nucleus and thus the size of the silver nanoparticles were tunable through changing pH of the reaction system. Accordingly, the morphological structure and size of the produced silver and its aggregates were determined using scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images. It was considered that the increment in pH value of the reaction media progress the aggregation of silver clusters. However, the presence of stain 23N biomass decreases the possibility of silver aggregation at the pH 7.

Keywords: silver nanoparticles, biosynthesis, reaction media pH, nano-silver characterization

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Authors: Astrid Tannert, Anuradha Ramoji, Christina Ebert, Frederike Gladigau, Lorena Tuchscherr, Jürgen Popp, Ute Neugebauer

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Staphylococcus aureus is a facultative intracellular pathogen, which by entering host cells may evade immunologic host response as well as antimicrobial treatment. In that way, S. aureus can cause persistent intracellular infections which are difficult to treat. Depending on the strain, S. aureus may persist at different intracellular locations like the phagolysosome. The first barrier invading pathogens from the blood stream that they have to cross are the endothelial cells lining the inner surface of blood and lymphatic vessels. Upon proceeding from an acute to a chronic infection, intracellular pathogens undergo certain biochemical and structural changes including a deceleration of metabolic processes to adopt for long-term intracellular survival and the development of a special phenotype designated as small colony variant. In this study, the endothelial cell line Ea.hy 926 was used as a model for acute and chronic S. aureus infection. To this end, Ea.hy 926 cells were cultured on QIAscout™ Microraft Arrays, a special graded cell culture substrate that contains around 12,000 microrafts of 200 µm edge length. After attachment to the substrate, the endothelial cells were infected with GFP-expressing S. aureus for 3 weeks. The acute infection and the development of persistent bacteria was followed by confocal laser scanning microscopy, scanning the whole Microraft Array for the presence and for detailed determination of the intracellular location of fluorescent intracellular bacteria every second day. After three weeks of infection representative microrafts containing infected cells, cells with protruded infections and cells that did never show any infection were isolated and fixed for Raman micro-spectroscopic investigation. For comparison, also microrafts with acute infection were isolated. The acquired Raman spectra are correlated with the fluorescence microscopic images to give hints about a) the molecular alterations in endothelial cells during acute and chronic infection compared to non-infected cells, and b) metabolic and structural changes within the pathogen when entering a mode of persistence within host cells. We thank Dr. Ruth Kläver from QIAGEN GmbH for her support regarding QIAscout technology. Financial support by the BMBF via the CSCC (FKZ 01EO1502) and from the DFG via the Jena Biophotonic and Imaging Laboratory (JBIL, FKZ PO 633/29-1, BA 1601/10-1) is highly acknowledged.

Keywords: correlative image analysis, intracellular infection, pathogen-host adaption, Raman micro-spectroscopy

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Authors: Eman Alzahrani

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Magnetic nanoparticles (MNPs) were fabricated using the chemical co-precipitation method followed by coating the surface of magnetic Fe3O4 nanoparticles with gum arabic (GA). The fabricated magnetic nanoparticles were characterised using transmission electron microscopy (TEM) which showed that the Fe3O4 nanoparticles and GA-MNPs nanoparticles had a mean diameter of 33 nm, and 38 nm, respectively. Scanning electron microscopy (SEM) images showed that the MNPs modified with GA had homogeneous structure and agglomerated. The energy dispersive X-ray spectroscopy (EDAX) spectrum showed strong peaks of Fe and O. X-ray diffraction patterns (XRD) indicated that the naked magnetic nanoparticles were pure Fe3O4 with a spinel structure and the covering of GA did not result in a phase change. The covering of GA on the magnetic nanoparticles was also studied by BET analysis, and Fourier transform infrared spectroscopy. Moreover, the present study reports a fast and simple method for removal and recovery of methylene blue dye (MB) from aqueous solutions by using the synthesised magnetic nanoparticles modified with gum arabic as adsorbent. The experimental results show that the adsorption process attains equilibrium within five minutes. The data fit the Langmuir isotherm equation and the maximum adsorption capacities were 8.77 mg mg-1 and 14.3 mg mg-1 for MNPs and GA-MNPs, respectively. The results indicated that the homemade magnetic nanoparticles were quite efficient for removing MB and will be a promising adsorbent for the removal of harmful dyes from waste-water.

Keywords: Fe3O4 magnetic nanoparticles, gum arabic, co-precipitation, adsorption dye, methylene blue, adsorption isotherm

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Authors: Nishanth Venugopal Menon, Chuah Yon Jin, Samantha Phey, Wu Yingnan, Zhang Ying, Vincent Chan, Kang Yuejun

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Cell Migration is a vital phenomenon that the cells undergo in various physiological processes like wound healing, disease progression, embryogenesis, etc. Cell migration depends primarily on the chemical and physical cues available in the cellular environment. The chemical cue involves the chemokines secreted and gradients generated in the environment while physical cues indicate the impact of matrix properties like nanotopography and stiffness on the cells. Mesenchymal Stem Cells (MSCs) have been shown to have a role wound healing in vivo and its migration to the site of the wound has been shown to have a therapeutic effect. In the field of stem cell based tissue regeneration of bones and cartilage, one approach has been to introduce scaffold laden with MSCs into the site of injury to enable tissue regeneration. In this work, we have studied the combinatorial impact of the substrate physical properties on MSC migration. A microfluidic in vitro model was created to perform the migration studies. The microfluidic model used is a three compartment device consisting of two cell seeding compartments and one migration compartment. Four different PDMS substrates with varying substrate roughness, stiffness and hydrophobicity were created. Its surface roughness and stiffness was measured using Atomic Force Microscopy (AFM) while its hydrphobicity was measured from the water contact angle using an optical tensiometer. These PDMS substrates are sealed to the microfluidic chip following which the MSCs are seeded and the cell migration is studied over the period of a week. Cell migration was quantified using fluorescence imaging of the cytoskeleton (F-actin) to find out the area covered by the cells inside the migration compartment. The impact of adhesion proteins on cell migration was also quantified using a real-time polymerase chain reaction (qRT PCR). These results suggested that the optimal substrate for cell migration would be one with an intermediate level of roughness, stiffness and hydrophobicity. A higher or lower value of these properties affected cell migration negatively. These observations have helped us in understanding that different substrate properties need to be considered in tandem, especially while designing scaffolds for tissue regeneration as cell migration is normally impacted by the combinatorial impact of the matrix. These observations may lead us to scaffold optimization in future tissue regeneration applications.

Keywords: cell migration, microfluidics, in vitro model, stem cell migration, scaffold, substrate properties

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Authors: Iván Castelló, Georgiana Stoica, Emilio Palomares, Fernando Bravo

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We present herein two colour encoded silica nanospheres (2nanoSi) for the fluorescence quantitative ratiometric determination of trypsin in humans. The system proved to be a faster (minutes) method, with two times higher sensitivity than the state-of-the-art biomarkers based sensors for cystic fibrosis (CF), allowing the quantification of trypsin concentrations in a wide range (0-350 mg/L). Furthermore, as trypsin is directly related to the development of cystic fibrosis, different human genotypes, i.e. healthy homozygotic (> 80 mg/L), CF homozygotic (< 50 mg/L), and heterozygotic (> 50 mg/L), respectively, can be determined using our 2nanoSi nanospheres.

Keywords: cystic fibrosis, trypsin, quantum dots, biomarker, homozygote, heterozygote

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Authors: S. Alrekabi, A. Cundy, A. Lampropoulos, I. Savina

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Due to their remarkable mechanical properties, multi-wall carbon nanotubes (MWCNTs) are considered by many researchers to be a highly promising filler and reinforcement agent for enhanced performance cementitious materials. Currently, however, achieving an effective dispersion of MWCNTs remains a major challenge in developing high performance nano-cementitious composites, since carbon nanotubes tend to form large agglomerates and bundles as a consequence of Van der Waals forces. In this study, effective dispersion of low concentrations of MWCNTs at 0.01%, 0.025%, and 0.05% by weight of cement in the composite was achieved by applying different sonication conditions in combination with the use of polycarboxylate ether as a surfactant. UV-Visible spectroscopy and Transmission electron microscopy (TEM) were used to assess the dispersion of MWCNTs in water, while the dispersion states of MWCNTs within the cement composites and their surface interactions were examined by scanning electron microscopy (SEM). A high sonication intensity applied over a short time period significantly enhanced the dispersion of MWCNTs at initial mixing stages, and 0.025% of MWCNTs wt. of cement, caused 86% and 27% improvement in tensile strength and compressive strength respectively, compared with a plain cement mortar.

Keywords: dispersion, mechanical performance, multi wall carbon nanotubes, sonication conditions

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Authors: Gulshan Mammadova

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This paper presents the results of studying the surface microrelief in 2D and 3D models and analyzing the spectroscopy of a three-junction TlInSe₂ crystal. Analysis of the results obtained showed that with a change in the composition of the TlInSe₂ crystal, sharp changes occur in the microrelief of its surface. An X-ray optical diffraction analysis of the TlInSe₂ crystal was experimentally carried out. Based on ellipsometric data, optical functions were determined - the real and imaginary parts of the dielectric permittivity of crystals, the coefficients of optical absorption and reflection, the dependence of energy losses and electric field power on the effective density, the spectral dependences of the real (σᵣ) and imaginary (σᵢ) parts, optical electrical conductivity were experimentally studied. The fluorescence spectra of the ternary compound TlInSe₂ were isolated and analyzed when excited by light with a wavelength of 532 nm. X-ray studies of TlInSe₂ showed that this phase crystallizes into tetragonal systems. Ellipsometric measurements showed that the real (ε₁) and imaginary (ε₂) parts of the dielectric constant are components of the dielectric constant tensor of the uniaxial joints under consideration and do not depend on the angle. Analysis of the dependence of the real and imaginary parts of the refractive index of the TlInSe₂ crystal on photon energy showed that the nature of the change in the real and imaginary parts of the dielectric constant does not differ significantly. When analyzing the spectral dependences of the real (σr) and imaginary (σi) parts of the optical electrical conductivity, it was noticed that the real part of the optical electrical conductivity increases exponentially in the energy range 0.894-3.505 eV. In the energy range of 0.654-2.91 eV, the imaginary part of the optical electrical conductivity increases linearly, reaches a maximum value, and decreases at an energy of 2.91 eV. At 3.6 eV, an inversion of the imaginary part of the optical electrical conductivity of the TlInSe₂ compound is observed. From the graphs of the effective power density versus electric field energy losses, it is known that the effective power density increases significantly in the energy range of 0.805–3.52 eV. The fluorescence spectrum of the ternary compound TlInSe₂ upon excitation with light with a wavelength of 532 nm has been studied and it has been established that this phase has luminescent properties.

Keywords: optical properties, dielectric permittivity, real and imaginary dielectric permittivity, optical electrical conductivity

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Authors: Elenice Maria Schons Silva, Andre Carlos Silva

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The crescent demand for raw material has increased mining activities. Mineral industry faces the challenge of process more complexes ores, with very small particles and low grade, together with constant pressure to reduce production costs and environment impacts. Froth flotation deserves special attention among the concentration methods for mineral processing. Besides its great selectivity for different minerals, flotation is a high efficient method to process fine particles. The process is based on the minerals surficial physicochemical properties and the separation is only possible with the aid of chemicals such as collectors, frothers, modifiers, and depressants. In order to use sustainable and eco-friendly reagents, oils extracted from three different vegetable species (pequi’s pulp, macauba’s nut and pulp, and Jatropha curcas) were studied and tested as apatite collectors. Since the oils are not soluble in water, an alkaline hydrolysis (or saponification), was necessary before their contact with the minerals. The saponification was performed at room temperature. The tests with the new collectors were carried out at pH 9 and Flotigam 5806, a synthetic mix of fatty acids industrially adopted as apatite collector manufactured by Clariant, was used as benchmark. In order to find a feasible replacement for cornstarch the flour and starch of a graniferous variety of sorghum was tested as depressant. Apatite samples were used in the flotation tests. XRF (X-ray fluorescence), XRD (X-ray diffraction), and SEM/EDS (Scanning Electron Microscopy with Energy Dispersive Spectroscopy) were used to characterize the apatite samples. Zeta potential measurements were performed in the pH range from 3.5 to 12.5. A commercial cornstarch was used as depressant benchmark. Four depressants dosages and pH values were tested. A statistical test was used to verify the pH, dosage, and starch type influence on the minerals recoveries. For dosages equal or higher than 7.5 mg/L, pequi oil recovered almost all apatite particles. In one hand, macauba’s pulp oil showed excellent results for all dosages, with more than 90% of apatite recovery, but in the other hand, with the nut oil, the higher recovery found was around 84%. Jatropha curcas oil was the second best oil tested and more than 90% of the apatite particles were recovered for the dosage of 7.5 mg/L. Regarding the depressant, the lower apatite recovery with sorghum starch were found for a dosage of 1,200 g/t and pH 11, resulting in a recovery of 1.99%. The apatite recovery for the same conditions as 1.40% for sorghum flour (approximately 30% lower). When comparing with cornstarch at the same conditions sorghum flour produced an apatite recovery 91% lower.

Keywords: collectors, depressants, flotation, mineral processing

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Authors: Daniel R. McDougall, Martin D. de Jonge, Gordon M. Miskelly, Duncan J. McGillivray, Andrew G. Jeffs

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The chelating agent ethylenediaminetetraacetic acid (EDTA) is commonly added as a cure-all to seawater in aquaculture hatcheries around the world to reduce heavy metal toxicity, significantly improve the survival of larval shellfish, and to therefore improve the overall production efficiency of the aquaculture industry. However, EDTA is not a biodegradable chemical and is considered to be a persistent organic pollutant, which will accumulate in the environment over time. This makes the use of EDTA unsustainable environmentally, and therefore alternatives should be considered. Ethylenediaminedisuccinic acid (EDDS) is a biodegradable alternative to EDTA with very similar metal chelation properties. This study investigates the effect of EDTA and EDDS at two different concentrations, on metal concentrations found within developing New Zealand green-lipped mussel (Perna canaliculus) larvae. P. canaliculus is New Zealand’s main shellfish aquaculture species, providing a major export for New Zealand’s economy, with excellent potential for increased production in the near future. It is well known that the early stages of bivalve development are the most vulnerable to metal toxicity and P. canaliculus is no exception. The commercially used concentration (12 µmol L⁻¹) of EDTA added to P. canaliculus larval rearing tanks often increases the yield of D-larvae by over 80%. This concentration of EDTA and EDDS will be tested in this study, along with a lower concentration (3 µmol L⁻¹). After 48 hours of larval development, the D-larvae will be analyzed for heavy metal content with Inductively Coupled Plasma Mass Spectrometry (ICP-MS) and heavy metal distribution with synchrotron X-ray Fluorescence Microscopy (XFM). In this study, we found that EDDS also improves the yield of P. canaliculus larvae and could be a viable alternative to EDTA in aquaculture. Furthermore, results suggest a higher concentration of chelating agent is more effective for improving the yield of developing P. canaliculus larvae. Metals with significant differences in concentration with the addition of EDTA were Cr, Cu, Zn, Cd and Pb (P < 0.05). We observed for the first time to the author’s best knowledge, metal distribution within 100 µm P. canaliculus D-larvae using synchrotron XFM and found changes in the distribution of metals with the addition of EDTA. XFM also has the potential to provide information about the chemical state of the metals within mussel larvae. This research provides greater insight into the reasons for the effectiveness of adding the chelating agent to aquaculture culture water, and a more environmentally conscious alternative to the currently used EDTA, which could be extremely valuable for the aquaculture industry.

Keywords: EDDS, EDTA, heavy metals, P. canaliculus, toxicity, water treatment

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Authors: Peter W. Woodruff, Georgios Ponirakis, Reem Ibrahim, Amani Ahmed, Hoda Gad, Ioannis N. Petropoulos, Adnan Khan, Ahmed Elsotouhy, Surjith Vattoth, Mahmoud K. M. Alshawwaf, Mohamed Adil Shah Khoodoruth, Marwan Ramadan, Anjushri Bhagat, James Currie, Ziyad Mahfoud, Hanadi Al Hamad, Ahmed Own, Peter Haddad, Majid Alabdulla, Rayaz A. Malik

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Introduction:- We aimed to test the hypothesis that, using corneal confocal microscopy (a non-invasive method for assessing corneal nerve fibre integrity), patients with schizophrenia would show neuronal abnormalities compared with healthy participants. Schizophrenia is a neurodevelopmental and progressive neurodegenerative disease, for which there are no validated biomarkers. Corneal confocal microscopy (CCM) is a non-invasive ophthalmic imaging biomarker that can be used to detect neuronal abnormalities in neuropsychiatric syndromes. Methods:- Patients with schizophrenia (DSM-V criteria) without other causes of peripheral neuropathy and healthy controls underwent CCM, vibration perception threshold (VPT) and sudomotor function testing. The diagnostic accuracy of CCM in distinguishing patients from controls was assessed using the area under the curve (AUC) of the Receiver Operating Characterstics (ROC) curve. Findings:- Participants with schizophrenia (n=17) and controls (n=38) with comparable age (35.7±8.5 vs 35.6±12.2, P=0.96) were recruited. Patients with schizophrenia had significantly higher body weight (93.9±25.5 vs 77.1±10.1, P=0.02), lower Low Density Lipoproteins (2.6±1.0 vs 3.4±0.7, P=0.02), but comparable systolic and diastolic blood pressure, HbA1c, total cholesterol, triglycerides and High Density Lipoproteins were comparable with control participants. Patients with schizophrenia had significantly lower corneal nerve fiber density (CNFD, fibers/mm2) (23.5±7.8 vs 35.6±6.5, p<0.0001), branch density (CNBD, branches/mm2) (34.4±26.9 vs 98.1±30.6, p<0.0001), and fiber length (CNFL, mm/mm2) (14.3±4.7 vs 24.2±3.9, p<0.0001) but no difference in VPT (6.1±3.1 vs 4.5±2.8, p=0.12) and electrochemical skin conductance (61.0±24.0 vs 68.9±12.3, p=0.23) compared with controls. The diagnostic accuracy of CNFD, CNBD and CNFL to distinguish patients with schizophrenia from healthy controls were, according to the AUC, (95% CI): 87.0% (76.8-98.2), 93.2% (84.2-102.3), 93.2% (84.4-102.1), respectively. Conclusion:- In conclusion, CCM can be used to help identify neuronal changes and has a high diagnostic accuracy to distinguish subjects with schizophrenia from healthy controls.

Keywords:

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Authors: Huixia Shi, Can Hu, Jun Zhu, Hongling Guo, Haiyan Li, Hongyan Du

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The identification of human body fluids during forensic investigations is a critical step to determine key details, and present strong evidence to testify criminal in a case. With the popularity of DNA and improved detection technology, the potential question must be revolved that whether the suspect’s DNA derived from saliva or semen, menstrual or peripheral blood, how to identify the red substance or aged blood traces on the spot is blood; How to determine who contribute the right one in mixed stains. In recent years, molecular approaches have been developing increasingly on mRNA, miRNA, DNA methylation and microbial markers, but appear expensive, time-consuming, and destructive disadvantages. Physicochemical methods are utilized frequently such us scanning electron microscopy/energy spectroscopy and X-ray fluorescence and so on, but results only showing one or two characteristics of body fluid itself and that out of working in unknown or mixed body fluid stains. This paper focuses on using chemistry methods Raman spectroscopy and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry to discriminate species of peripheral blood, menstrual blood, semen, saliva, vaginal secretions, urine or sweat. Firstly, non-destructive, confirmatory, convenient and fast Raman spectroscopy method combined with more accurate matrix-assisted laser desorption/ionization time-of-flight mass spectrometry method can totally distinguish one from other body fluids. Secondly, 11 spectral signatures and specific metabolic molecules have been obtained by analysis results after 70 samples detected. Thirdly, Raman results showed peripheral and menstrual blood, saliva and vaginal have highly similar spectroscopic features. Advanced statistical analysis of the multiple Raman spectra must be requested to classify one to another. On the other hand, it seems that the lactic acid can differentiate peripheral and menstrual blood detected by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry, but that is not a specific metabolic molecule, more sensitivity ones will be analyzed in a forward study. These results demonstrate the great potential of the developed chemistry methods for forensic applications, although more work is needed for method validation.

Keywords: body fluids, identification, Raman spectroscopy, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

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Authors: Abdel Ghany F. Shoair, Mai M. A. H. Shanab

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The basic aqueous systems NiSO4.6H₂O / K₂S₂O₈ (PH= 14) or NiSO₄.6H₂O / KBrO₃ (PH = 11.5) were ‎investigated ‎for the ‎catalytic conversion benzyl alcohol and ‎some para-substituted benzyl ‎alcohols to their ‎corresponding ‎acids in 75-97 % yield at room ‎temperature. The active species ‎was isolated and characterized by scanning ‎electron ‎microscopy (SEM), ‎‎transmission electron microscopy (TEM), X-ray ‎powder diffraction, EDX and ‎‎FT-IR ‎techniques and identified as NiO₂ nanoparticles (NPNPs). The SEM and ‎TEM images of nickel peroxide samples show a fine spherical-like ‎aggregation of ‎NiO₂ molecules with a nearly homogeneous partial size and confirm the ‎aggregation's size ‎to ‎be in the range of 2-3 nm. The yields, turnover (TO) and turn ‎over frequencies (TOF) were calculated. ‎It was noticed ‎that the aromatic alcohols ‎containing para-substituted electron donation groups gave better ‎‎yields than ‎those having electron-withdrawing groups. The optimum conditions for this ‎‎catalytic reaction ‎were studied using benzyl alcohol as a model. The mechanism ‎of the ‎catalytic conversion reaction was ‎suggested, in which the produced ‎(NPNPs) convert alcohols ‎to acids in two steps through the formation of the ‎‎corresponding aldehyde. The produced ‎NiO, because of this conversion, is ‎converted again to (NPNPs) by ‎an excess of K₂S₂O₈ or KBrO₃. This ‎catalytic cycle continues ‎until all the substrate is oxidized.

Keywords: Nickel, oxidation, catalysts, benzyl alcohol

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Authors: Carla Caiazza, Valentina Preziosi, Giovanna Tomaiuolo, Denis O'Sullivan, Vincenzo Guida, Stefano Guido

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In the last decades, wormlike micellar solutions have been extensively used to tune the rheological behavior of home care and personal care products. This and other successful applications underlie the growing attention that both basic and applied research are devoting to these systems, and to their unique rheological and flow properties. One of the key research topics is the occurrence of flow instabilities at high shear rates (such as shear banding), with the possibility of appearance of flow induced structures. In this scenario, microfluidics is a powerful tool to get a deeper insight into the flow behavior of a wormlike micellar solution, as the high confinement of a microfluidic device facilitates the onset of the flow instabilities; furthermore, thanks to its small dimensions, it can be coupled with optical microscopy, allowing a direct visualization of flow structuring phenomena. Here, the flow of a widely used wormlike micellar solution through a glass capillary has been studied, by coupling the microfluidic device with μPIV techniques. The direct visualization of flow-induced structures and the flow visualization analysis highlight a relationship between solution structuring and the onset of discontinuities in the velocity profile.

Keywords: flow instabilities, flow-induced structures, μPIV, wormlike micelles

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Authors: Raees Khan, Sheikh Z. Ul Abidin, Abdul S. Mumtaz, Jie Liu

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The present study is intended to assess gymnosperms pollen flora of Pakistan using Light Microscope (LM) and Scanning Electron Microscopy (SEM) for its taxonomic significance in identification of gymnosperms. Pollens of 35 gymnosperm species (12 genera and five families) were collected from its various distributional sites of gymnosperms in Pakistan. LM and SEM were used to investigate different palyno-morphological characteristics. Five pollen types (i.e., Inaperturate, Monolete, Monoporate, Vesiculate-bisaccate, and Polyplicate) were observed. In equatorial view seven types of pollens were observed, in which ten species were sub-angular, nine species were triangular, six species were perprolate, three species were rhomboidal, three species were semi-angular, two species were rectangular and two species were prolate. While five types of pollen were observed in polar view, in which ten species were spheroidal, nine species were angular, eight were interlobate, six species were circular, and two species were elliptic. Eighteen species have rugulate and 17 species has faveolate ornamentation. Eighteen species have verrucate and 17 have gemmate type sculpturing. The data was analysed through cluster analysis. The study showed that these palyno-morphological features have significance value in classification and identification of gymnosperms. Based on these different palyno-morphological features, a taxonomic key was proposed for the accurate and fast identifications of gymnosperms from Pakistan.

Keywords: gymnosperms, palynology, Pakistan, taxonomy

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Authors: Rym Taktak, Achwek Elghazel, Jamel Bouaziz

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In the present work, we explored the potential of tribological behavior of tricalcium phosphate-Fluorapatite (β Tcp-Fap) bioceramic which has attracted considerable attention for orthopedics and dental applications. The approximate representatives Fap-βTcp were respectively [{13.26 wt%, 86.74 wt%} {19.9 wt%, 80.1 wt%},{ 26.52 wt%, 73.48 wt%}, {33.16 wt%, 66.84 wt%} and {40 wt%, 60 wt%}. The effects of Fluorapatite additives on friction and wear behavior were studied and discussed. The wear test was conducted using pion-disk tribometer at room temperature under dry condition using a constant sliding speed of 0,063 m/s, and three loads 3, 5 and 8 N. The wear rate and friction coefficient of β Tcp with different additive amounts were compared. An Alumina ball specimens were used as the pin and flat surface β Tcp-Fap specimens as the antagonist counterface. The results show a huge difference between the wear rate of β TCP samples and the other β TCP-Fap composites for all normal forces applied. This result shows the beneficial effect of fluorapatite on the tribological behavior of the β TCP. Moreover, we note that β Tcp-26% Fap specimens exhibit, under dry condition, the lower friction coefficient and the smaller wear rate than other biocomposites. Thereby, the friction and wear behavior is influenced by the addition of fluorapatite, the applied normal force, and the sliding velocity. To extend the understanding of the wear process, the surface topography of β Tcp-26% Fap specimens and the wear track obtained during the wear tests were studied using a surface profilometer, optical microscopy, and scanning electron microscopy.

Keywords: alumina, bioceramic, friction and wear test, tricalcium phosphate

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Authors: Marcelle Muriel Domkam Tchunkam, Rolin Feudjio

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This work investigates the ultrastructure, physicochemical and thermal properties evaluation of Palm Kernel Shells (PKS). PKS Tenera waste samples were obtained from a palm oil mill in Dizangué Sub-Division, Littoral region of Cameroon, while PKS Dura waste samples were collected from the Institute of Agricultural Research for Development (IRAD) of Mbongo. A sodium hydroxide solution was used to wash the shells. They were then rinsed by demineralised water and dried in an oven at 70 °C during 72 hours. They were then grounded and sieved to obtained powders from 0.04 mm to 0.45 mm in size. Transmission Electron Microscopy (TEM) and Surface Electron Microscopy (SEM) were used to characterized powder samples. Chemical compounds and elemental constituents, as well as thermal performance were evaluated by Van Soest Method, TEM/EDXA and SEM/EDS techniques. Thermal characterization was also performed using Differential Scanning Calorimetry (DSC) and Thermogravimetric Analysis (TGA). Our results from microstructural analysis revealed that most of the PKS material is made of particles with irregular morphology, mainly amorphous phases of carbon/oxygen with small amounts of Ca, K, and Mg. The DSC data enabled the derivation of the materials’ thermal transition phases and the relevant characteristic temperatures and physical properties. Overall, our data show that PKS have nanopores and show potential in 3D printing and membrane filtration applications.

Keywords: DSC, EDXA, palm kernel shells, SEM, TEM

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Authors: Amine Harrane, Mahmoud Belalia

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During the last decade, polymer layered silicate nanocomposites have received increasing attention from scientists and industrial researchers because they generally exhibit greatly improved mechanical, thermal, barrier and flame-retardant properties at low clay content in comparison with unfilled polymers or more conventional micro composites. Poly(ε-caprolactone) (PCL)-layered silicate nanocomposites have the advantage of adding biocompatibility and biodegradability to the traditional properties of nanocomposites. They can be prepared by in situ ring-opening polymerization of ε-caprolactone using a conventional initiator to induce polymerization in the presence of an organophilic clay, such as organomodified montmorillonite. Messersmith and Giannelis used montmorillonite exchanged with protonated 12-amino dodecanoic acid and Cr3+ exchanged fluorohectorite, a synthetic mica type of silicate. Sn-based catalysts such as tin (II) octoate and dibutyltin (IV) dimethoxide have been reported to efficiently promote the polymerization of ε-caprolactone in the presence of organomodified clays. In this work, we have used an alternative method to prepare PCL/montmorillonite nanocomposites. The cationic polymerization of ε-caprolactone was initiated directly by Maghnite-TOA, organomodified montmorillonite clay, to produce nanocomposites (Scheme 1). Resulted from nanocomposites were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), force atomic microscopy (AFM) and thermogravimetry.

Keywords: polycaprolactone, polycaprolactone/clay nanocomposites, biodegradables nanocomposites, Maghnite, Insitu polymeriation

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Authors: Bunty Tomar, Shiva S.

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Fabrication of steel and copper-based functionally graded material (FGM) through cold metal transfer-based wire arc additive manufacturing is a novel exploration. Components combining Cu and steel show significant usage in many industrial applications as they combine high corrosion resistance, ductility, thermal conductivity, and wear resistance to excellent mechanical properties. Joining steel and copper is challenging due to the mismatch in their thermo-mechanical properties. In this experiment, a functionally graded material (FGM) structure of pure copper (Cu) and 316L stainless steel (SS) was successfully developed using cold metal transfer-based wire arc additive manufacturing (CMT-WAAM). The interface of the fabricated samples was characterized under optical microscopy, field emission scanning electron microscopy, and X-ray diffraction techniques. Detailed EBSD and TEM analysis was performed to analyze the grain orientation, strain distribution, grain boundary misorientations, and formation of metastable and intermetallic phases. Mechanical characteristics of deposits was also analyzed using tensile and wear testing. This works paves the way to use CMT-WAAM to fabricate steel/copper FGMs.

Keywords: wire arc additive manufacturing (waam), cold metal transfer (cmt), metals and alloys, mechanical properties, characterization

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Authors: Azeez O. Idris, Benjamin O. Orimolade, Potlako J. Mafa, Alex T. Kuvarega, Usisipho Feleni, Bhekie B. Mamba

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We report a simple and cheaper method for the electrochemical detection of Se(IV) using carbon nanodots (CNDTs) prepared from oat. The carbon nanodots were synthesised by green and facile approach and characterised using scanning electron microscopy, high-resolution transmission electron microscopy, Fourier transform infrared spectroscopy, X-ray diffraction, and Raman spectroscopy. The CNDT was used to fabricate an electrochemical sensor for the quantification of Se(IV) in water. The modification of glassy carbon electrode (GCE) with carbon nanodots led to an increase in the electroactive surface area of the electrode, which enhances the redox current peak of [Fe(CN)₆]₃₋/₄‒ in comparison to the bare GCE. Using the square wave voltammetry, the detection limit and quantification limit of 0.05 and 0.167 ppb were obtained under the optimised parameters using deposition potential of -200 mV, 0.1 M HNO₃ electrolyte, electrodeposition time of 60 s, and pH 1. The results further revealed that the GCE-CNDT was not susceptible to many interfering cations except Cu(II) and Pb(II), and Fe(II). The sensor fabrication involves a one-step electrode modification and was used to detect Se(IV) in a real water sample, and the result obtained is in agreement with the inductively coupled plasma technique. Overall, the electrode offers a cheap, fast, and sensitive way of detecting selenium in environmental matrices.

Keywords: carbon nanodots, square wave voltammetry, nanomaterials, selenium, sensor

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Authors: H. Beisch, J. Marx, S. Garlof, R. Shvets, I. I. Grygorchak, A. Kityk, B. Fiedler

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Carbon materials, especially three-dimensional carbon foams, show very high potential in the application as electrode material for energy storage systems such as batteries and supercapacitors with unique fast charging and discharging times. Regarding their high specific surface areas (SSA) high specific capacities can be reached. Globugraphite is a newly developed carbon foam with an interconnected globular carbon morphology. Especially, this foam has a statistically distributed hierarchical pore structure resulting from the manufacturing process based on sintered ceramic templates which are synthetized during a final chemical vapor deposition (CVD) process. For morphology characterization scanning electron (SEM) and transmission electron microscopy (TEM) is used. In addition, the SSA is carried out by nitrogen adsorption combined with the Brunauer–Emmett–Teller (BET) theory. Electrochemical measurements in organic and inorganic electrolyte provide high energy densities and power densities resulting from ion absorption by forming an electrochemical double layer. All values are summarized in a Ragone Diagram. Finally, power densities up to 833 W/kg and energy densities up to 48 Wh/kg could be achieved. The corresponding SSA is between 376 m²/g and 859 m²/g. For organic electrolyte a specific capacity of 71 F/g at a density of 20 mg/cm³ was achieved.

Keywords: BET, CVD process, electron microscopy, Ragone diagram

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Authors: Suresh Vidyasagar Chevuri, D. B. Karunakar Chevuri

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The main advantages of 'Metal Matrix Nano Composites (MMNCs)' include excellent mechanical performance, good wear resistance, low creep rate, etc. The method of fabrication of MMNCs is quite a challenge, which includes processing techniques like Spark Plasma Sintering (SPS), etc. The objective of the present work is to fabricate aluminum based MMNCs with the addition of small amounts of yttrium using Spark Plasma Sintering and to evaluate their mechanical and microstructure properties. Samples of 2024 AA with yttrium ranging from 0.1% to 0.5 wt% keeping 1 wt% TiB2 constant are fabricated by Spark Plasma Sintering (SPS). The mechanical property like hardness is determined using Vickers hardness testing machine. The metallurgical characterization of the samples is evaluated by Optical Microscopy (OM), Field Emission Scanning Electron Microscopy (FE-SEM) and X-Ray Diffraction (XRD). Unreinforced 2024 AA sample is also fabricated as a benchmark to compare its properties with that of the composite developed. It is found that the yttrium addition increases the above-mentioned properties to some extent and then decreases gradually when yttrium wt% increases beyond a point between 0.3 and 0.4 wt%. High density is achieved in the samples fabricated by spark plasma sintering when compared to any other fabrication route, and uniform distribution of yttrium is observed.

Keywords: spark plasma sintering, 2024 AA, yttrium addition, microstructure characterization, mechanical properties

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Authors: Patcharee Pripdeevech, Sarunpron Khruengsai

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Thirty fungi were tested for their degradation ability on low-density polyethylene (LDPE) plastic film. Biodegradation of all fungi was screened in mineral salt medium broth containing LDPE film as the sole carbon source for 30 days. Diaporthe italiana, Thyrostroma jaczewskii, Colletotrichum fructicola, and Stagonosporopsis citrulli were able to colonize and cover the surface of LDPE film in media. The degradation test result was compared to those obtained from Aspergillus niger. LDPE films cocultured with D. italiana, T. jaczewskii, C. fructicola, S. citrulli, A. niger, and control showed weight loss of 43.90%, 46.34%, 48.78%, 45.12%, 28.78%, and 10.85%, respectively. The tensile strength of degraded LDPE films cocultured with D. italiana, T. jaczewskii, C. fructicola, S. citrulli, A. niger, and control also reduced significantly by 1.56 MPa, 1.78 MPa, 0.43 MPa, 1.86 MPa, 3.34 MPa, and 9.98 MPa, respectively. Analysis of LDPE films by Fourier transform infrared spectroscopy and scanning electron microscopy confirmed the biodegradation by the presence of morphological changes such as cracks, scions, and holes on the surface of the film. These fungi have the ability to break down and consume the LDPE film, especially C. fructicola. These findings showed the potential of fungi in Thailand that play an important role in LDPE film degradation.

Keywords: plastic biodegradation, LDPE film, fungi, Fourier transform infrared, scanning electron microscopy

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Authors: Masaki Ohno, Cervinia Manalo, Tetsuji Okuda, Satoshi Nakai, Wataru Nishijima

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Reverse osmosis (RO) membranes have been widely used for desalination to purify water for drinking and other purposes. Although at present most RO membranes have no resistance to chlorine, chlorine-resistant membranes are being developed. Therefore, direct chlorine treatment or chlorine washing will be an option in preventing biofouling on chlorine-resistant membranes. Furthermore, if particle accumulation control is possible by using chlorine washing, expensive pretreatment for particle removal can be removed or simplified. The objective of this study was to determine the effective hypochlorite washing condition required for controlling biofilm formation and inorganic particle accumulation on RO membrane in a continuous flow channel with RO membrane and spacer. In this study, direct chlorine washing was done by soaking fouled RO membranes in hypochlorite solution and fluorescence intensity was used to quantify biofilm on the membrane surface. After 48 h of soaking the membranes in high fouling potential waters, the fluorescence intensity decreased to 0 from 470 using the following washing conditions: 10 mg/L chlorine concentration, 2 times/d washing interval, and 30 min washing time. The chlorine concentration required to control biofilm formation decreased as the chlorine concentration (0.5–10 mg/L), the washing interval (1–4 times/d), or the washing time (1–30 min) increased. For the sample solutions used in the study, 10 mg/L chlorine concentration with 2 times/d interval, and 5 min washing time was required for biofilm control. The optimum chlorine washing conditions obtained from soaking experiments proved to be applicable also in controlling biofilm formation in continuous flow experiments. Moreover, chlorine washing employed in controlling biofilm with suspended particles resulted in lower amounts of organic (0.03 mg/cm²) and inorganic (0.14 mg/cm²) deposits on the membrane than that for sample water without chlorine washing (0.14 mg/cm² and 0.33 mg/cm², respectively). The amount of biofilm formed was 79% controlled by continuous washing with 10 mg/L of free chlorine concentration, and the inorganic accumulation amount decreased by 58% to levels similar to that of pure water with kaolin (0.17 mg/cm²) as feed water. These results confirmed the acceleration of particle accumulation due to biofilm formation, and that the inhibition of biofilm growth can almost completely reduce further particle accumulation. In addition, effective hypochlorite washing condition which can control both biofilm formation and particle accumulation could be achieved.

Keywords: reverse osmosis, washing condition optimization, hypochlorous acid, biofouling control

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Authors: Juiwen Liang, Choliang Chung

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In this study, the silicon-base oxide nanofibers with hollow structure were prepared using single-nozzle electrospinning and heat treatment. Firstly, precursor solution was prepared: the Polyvinylpyrrolidone (PVP) and Tetraethyl orthosilicate (TEOS) dissolved in ethanol and to make sure the concentration of solution in appropriate using single-nozzle electrospinning to produce the nanofibers. Secondly, control morphology of the electrostatic spinning nanofibers was conducted, and design the temperature profile to created hollow nanofibers, exploring the morphology and properties of nanofibers. The characterized of nanofibers, following instruments were used: Atomic force microscopy (AFM), Field Emission Scanning Electron Microscope (FE-SEM), Transmission electron microscopy (TEM), Photoluminescence (PL), X-ray Diffraction (XRD). The AFM was used to scan the nanofibers, and 3D Graphics were applied to explore the surface morphology of fibers. FE-SEM and TEM were used to explore the morphology and diameter of nanofibers and hollow nanofiber. The excitation and emission spectra explored by PL. Finally, XRD was used for identified crystallization of ceramic nanofibers. Using electrospinning technique followed by subsequent heat treatment, we have successfully prepared silicon-base oxide nanofibers with hollow structure. Thus, the microstructure and morphology of electrostatic spinning silicon-base oxide hollow nanofibers were explored. Major characteristics of the nanofiber in terms of crystalline, optical properties and crystal structure were identified.

Keywords: electrospinning, single-nozzle, hollow, nanofibers

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Authors: Fani Sakellariadou, Danae Antivachis

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Purpose of this paper is to evaluate the environmental status of a coastal Mediterranean lake, named Koumoundourou, located in the northeastern coast of Elefsis Bay, in the western region of Attiki in Greece, 15 km far from Athens. It is preserved from ancient times having an important archaeological interest. Koumoundourou lake is also considered as a valuable wetland accommodating an abundant flora and fauna, with a variety of bird species including a few world’s threatened ones. Furthermore, it is a heavily modified lake, affected by various anthropogenic pollutant sources which provide industrial, urban and agricultural contaminants. The adjacent oil refineries and the military depot are the major pollution providers furnishing with crude oil spills and leaks. Moreover, the lake accepts a quantity of groundwater leachates from the major landfill of Athens. The environmental status of the lake results from the intensive land uses combined with the permeable lithology of the surrounding area and the existence of karstic springs which discharge calcareous mountains. Sediment samples were collected along the shoreline of the lake using a Van Veen grab stainless steel sampler. They were studied for the determination of the total metal content and the metal fractionation in geochemical phases as well as the characterization of the dissolved organic matter (DOM). These constituents have a significant role in the ecological consideration of the lake. Metals may be responsible for harmful environmental impacts. The metal partitioning offers comprehensive information for the origin, mode of occurrence, biological and physicochemical availability, mobilization and transport of metals. Moreover, DOM has a multifunctional importance interacting with inorganic and organic contaminants leading to biogeochemical and ecological effects. The samples were digested using microwave heating with a suitable laboratory microwave unit. For the total metal content, the samples were treated with a mixture of strong acids. Then, a sequential extraction procedure was applied for the removal of exchangeable, carbonate hosted, reducible, organic/sulphides and residual fractions. Metal content was determined by an ICP-MS (Perkin Elmer, ICP MASS Spectrophotometer NexION 350D). Furthermore, the DOM was removed via a gentle extraction procedure and then it was characterized by fluorescence spectroscopy using a Perkin-Elmer LS 55 luminescence spectrophotometer equipped with the WinLab 4.00.02 software for data processing (Agilent, Cary Eclipse Fluorescence). Mono dimensional emission, excitation, synchronous-scan excitation and total luminescence spectra were recorded for the classification of chromophoric units present in the aqueous extracts. Total metal concentrations were determined and compared with those of the Elefsis gulf sediments. Element partitioning showed the anthropogenic sources and the contaminant bioavailability. All fluorescence spectra, as well as humification indices, were evaluated in detail to find out the nature and origin of DOM. All the results were compared and interpreted to evaluate the environmental quality of Koumoundourou lake and the need for environmental management and protection.

Keywords: anthropogenic contaminant, dissolved organic matter, lake, metal, pollution

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Authors: Shweta Maheshwari, Anish Dua

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Hematological changes reflect the adverse effects of heavy metals on fish. Hematology is a valuable tool to evaluate pathological condition of the fish. It helps in diagnosing the structural and functional status of fish exposed to toxicants. Morphological alteration in erythrocytes due to environmental stress can be studied through ultra-structural analysis. The aim of the present study was to assess the toxicity of mercuric chloride on red blood cells of an air breathing fish, Channa punctatus. Fish were subjected to chronic experiments using three sublethal concentration of mercuric chloride (0.020mg/L, 0.027mg/L, 0.040mg/L) for a period of 15, 30 and 60 days. Exposed fish of all the three concentrations were subjected to a recovery period of 30 days. A control was maintained in tap water simultaneously. For SEM analysis, blood from caudal vein of fish was taken and examined at an accelerating voltage of 20kV. Scanning electron micrographs revealed elliptical shaped erythrocytes of control fish. Alterations in the erythrocyte morphology such as presence of spherocytes, membrane internalization, crenation of membrane and development of lobopodial projections were observed in the exposed fish. The study revealed that ultra-structural analysis appears to be a sensitive method to evaluate the toxicity of various toxicants to fish.

Keywords: Channa punctatus, erythrocytes, mercuric chloride, scanning electron microscopy

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Authors: Manel Bouloudenine, Karima Djeddou, Hadjer Ben Manser, Hana Soualah Alila, Mohmed Bououdina

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This survey research involves the elaboration and characterization of silver nanoparticles for therapeutic and environmental applications. The silver nanoparticles "Ag NPs" were synthesized by reducing AgNO3 with microwaves. The characterization of nanoparticles was done by using Transmission Electron Microscopy " TEM ", Energy Dispersive Spectroscopy "EDS", Selected Area Electron Diffraction "SEAD", UV-Visible Spectroscopy and Dynamic Light Scattering "DLS". Transmission Electron Microscopy and Electron Diffraction have confirmed the nanoscale, the shape, and the crystalline quality of as synthesized silver nanoparticles. Elementary analysis has proved the purity of Ag NPs and the presence of the Surface Plasmon Resonance phenomenon "SPR". A strong absorption shift was observed in the visible range of the UV-visible spectrum of as synthesized Ag NPs, which indicates the presence of metallic silver. When the strong absorption in the ultraviolet range of the spectrum has revealed the presence of ionic Ag NPs ionic Ag aggregates species. The autocorrelation function measured by the Dynamic Light Scattering has shown a strong monodispersed character of Ag NPs, which is indicated by the presence of a single size population, with a minima and a maxima laying between 40 and 111 nm. Related to other research, our results confirm the performance properties of as synthesized Ag NPs, which allows them to be performing in many technological applications, including therapeutic and environmental ones.

Keywords: silvers nanoparticles, microwaves, EDS, TEM

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