Search results for: ftir/raman spectra

Authors: Sameena Malik, Ghosh Prakash, Sandeep Mudliar, Vishal Waindeskar, Atul Vaidya

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In this study, the biodegradability enhancement along with COD color and toxicity removal of pharmaceutical effluent by O₃, O₃/Fe²⁺, O₃/nZVI processes has been evaluated. The nZVI particles were synthesized and characterized by XRD and SEM analysis. Kinetic model was reasonably developed to select the ozone doses to be applied based on the ozonation kinetic and mass transfer coefficient values. Nano catalytic ozonation process (O₃/nZVI) effectively enhanced the biodegradability (BI=BOD₅/COD) of pharmaceutical effluent up to 0.63 from 0.18 of control with a COD, color and toxicity removal of 62.3%, 93%, and 75% respectively compared to O₃, O₃/Fe²⁺ pretreatment processes. From the GC-MS analysis, 8 foremost organic compounds were predominantly detected in the pharmaceutical effluent. The disappearance of the corresponding GC-MS spectral peaks during catalyzed ozonation process indicated the degradation of the effluent. The changes in the FTIR spectra confirms the transformation/destruction of the organic compounds present in the effluent to new compounds. Subsequent aerobic biodegradation of pretreated effluent resulted in biodegradation rate enhancement by 5.31, 2.97, and 1.22 times for O₃, O₃/Fe²⁺ and O₃/nZVI processes respectively.

Keywords: iron nanoparticles, pharmaceutical effluent, ozonation, kinetics, mass transfer

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Authors: A. Adelhafidhi, I. M. Babaghayou, S. F. Chabira, M. Sebaa

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This study deals with the photodegradation of unformulated polyethylene films for greenhouse covering. The UV range of solar light appears as the most deleterious factor of plastic degradation in outdoor exposure. The reasons of this photosensitivity are structural defects which are light-absorbing. The use of FTIR as an investigation tool has revealed that the material reacts with surrounding oxygen via a photooxidation process. Although the photochemical process is quite complex, it appears through this study than crosslinking and chain scissions are the most important events taking place during aging These two key reactions change irremediably the average molecular weight affecting thus drastically the mechanical properties and reducing, in the same way, the service lifetime of the films.

Keywords: polyethylene, films, unformulated, FTIR, ageing

Procedia PDF Downloads 337

Authors: Shivani A. Singh, Pravin S. More

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In the present inspection, we indicate the falsification of Fe-doped graphene nanoparticles by modified Hummers method. Structural and physiochemical properties of the resulting pallets were explored with the help of ultraviolet-visible spectroscopy (UV-Vis), Fourier transform infrared spectroscopy (FTIR), X-ray powder diffraction (XRD) and scanning electron microscopy (SEM), Photoluminescence spectroscopy (PL) for graphene sample exhibits absorption peaks ~248nm. Pure graphene shows PL peak at 348 nm. After doping of Fe with graphene the PL peak shifted from 348 nm to 332 nm. The oxidation degree, i.e. the relative amount of oxygen functional groups was estimated from the relative intensities of the oxygen related bands (ORB) in the FTIR measurements. These analyses show that this modified material can be useful for gas sensing applications and to be used in diverse areas.

Keywords: chemical doping, graphene, gas sensing, sensing

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Authors: hassan gheisari

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Ferro silicate calcium nano particles are prepared through the sol-gel method using polyvinyl alcohol (PVA) as a chelating agent. The powder, as prepared, is annealed at three different temperatures (900 ºC, 1000 ºC, and 1100 ºC) for 3 h. The XRD patterns of the samples indicate broad peaks, and the full width at half maximum decreased with increasing annealing temperature. FTIR spectra of the samples confirm the presence of metal - oxygen complexes within the structure. The average particle size obtained from PSA curve demonstrates ultrafine particles. SEM micrographs indicate the particles synthesized have spherical morphology. The saturation magnetization (Ms) and remnant magnetization (Mr) of the samples show dependence on particle size and crystallinity of the samples. The highest saturation magnetization is achieved for the sample annealed at 1100 ºC having maximum average particle size. The high saturation magnetization of the samples suggests the present method is suitable for obtaining nano particles magnetic ferro bioceramic, which is desirable for practical applications such as hyperthermia bone cancer therapy.

Keywords: hyperthermia, bone cancer, bio ceramic; magnetic materials; sol– gel, silicate calcium

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Authors: Hassan Gheisari

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Ferro silicate calcium nano particles are prepared through the sol-gel method using polyvinyl alcohol (PVA) as a chelating agent. The powder as prepared is annealed at three different temperatures (900 ºC, 1000 ºC and 1100 ºC) for 3 h. The XRD patterns of the samples indicate broad peaks and the full width at half maximum decreased with increasing annealing temperature. FTIR spectra of the samples confirm the presence of metal - oxygen complexes within the structure. The average particle size obtained from PSA curve demonstrates ultrafine particles. SEM micrographs indicate the particles synthesized have spherical morphology. The saturation magnetization (Ms) and remnant magnetization (Mr) of the samples show dependence on particle size and crystallinity of the samples. The highest saturation magnetization is achieved for the sample annealed at 1100 ºC having maximum average particle size. The high saturation magnetization of the samples suggests the present method is suitable for obtaining nano particles magnetic ferro bioceramic which is desirable for practical applications such as hyperthermia bone cancer therapy.

Keywords: hyperthermia, bone cancer, bio ceramic, magnetic materials, sol– gel, silicate calcium

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Authors: Mohamed Izzharif Abdul Halim, Niamh Nic Daeid

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Determining the source of pen inks used on a variety of documents is impartial for forensic document examiners. The examination of inks is often performed to differentiate between inks in order to evaluate the authenticity of a document. A ballpoint pen ink consists of synthetic dyes in (acidic and/or basic), pigments (organic and/or inorganic) and a range of additives. Inks of similar color may consist of different composition and are frequently the subjects of forensic examinations. This study emphasizes on blue ballpoint pen inks available in the market because it is reported that approximately 80% of questioned documents analysis involving ballpoint pen ink. Analytical techniques such as thin layer chromatography, high-performance liquid chromatography, UV-vis spectroscopy, luminescence spectroscopy and infrared spectroscopy have been used in the analysis of ink samples. In this study, application of Diamond Attenuated Total Reflectance (ATR) FTIR is straightforward but preferable in forensic science as it offers no sample preparation and minimal analysis time. The data obtained from these techniques were further analyzed using multivariate chemometric methods which enable extraction of more information based on the similarities and differences among samples in a dataset. It was indicated that some pens from the same manufactures can be similar in composition, however, discrete types can be significantly different.

Keywords: ATR FTIR, ballpoint, multivariate chemometric, PCA

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Authors: N. Azouaou, H. Mokaddem, D. Senadjki, K. Kedjit, Z. Sadaoui

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Introduction: Water contamination caused by dye industries, including food, leather, textile, plastic, cosmetics, paper-making, printing and dye synthesis, has caused more and more attention, since most dyes are harmful to human being and environments. Untreated coffee grounds were used as a high-efficiency adsorbent for the removal of a cationic dye (methylene blue, MB) from aqueous solution. Characterization of the adsorbent was performed using several techniques such as SEM, surface area (BET), FTIR and pH zero charge. The effects of contact time, adsorbent dose, initial solution pH and initial concentration were systematically investigated. Results showed the adsorption kinetics followed the pseudo-second-order kinetic model. Langmuir isotherm model is in good agreement with the experimental data as compared to Freundlich and D–R models. The maximum adsorption capacity was found equal to 52.63mg/g. In addition, the possible adsorption mechanism was also proposed based on the experimental results. Experimental: The adsorption experiments were carried out in batch at room temperature. A given mass of adsorbent was added to methylene blue (MB) solution and the entirety was agitated during a certain time. The samples were carried out at quite time intervals. The concentrations of MB left in supernatant solutions after different time intervals were determined using a UV–vis spectrophotometer. The amount of MB adsorbed per unit mass of coffee grounds (qt) and the dye removal efficiency (R %) were evaluated. Results and Discussion: Some chemical and physical characteristics of coffee grounds are presented and the morphological analysis of the adsorbent was also studied. Conclusions: The good capacity of untreated coffee grounds to remove MB from aqueous solution was demonstrated in this study, highlighting its potential for effluent treatment processes. The kinetic experiments show that the adsorption is rapid and maximum adsorption capacities qmax= 52.63mg/g achieved in 30min. The adsorption process is a function of the adsorbent concentration, pH and metal ion concentration. The optimal parameters found are adsorbent dose m=5g, pH=5 and ambient temperature. FTIR spectra showed that the principal functional sites taking part in the sorption process included carboxyl and hydroxyl groups.

Keywords: adsorption, methylene blue, coffee grounds, kinetic study

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Authors: Rebecca Thombre, Aishwarya Borate

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Chemical synthesis of nanoparticles produces toxic by-products, as a result of which eco-friendly methods of synthesis are gaining importance. The synthesis of nanoparticles using plant derived extracts is economical, safe and eco-friendly. Biostabilized gold nanoparticles were synthesized using extracts of Garcinia indica. The gold nanoparticles were characterized using UV-Vis spectrophotometry and demonstrated a peak at 527 nm. The presence of plant derived peptides and phytoconstituents was confirmed using the FTIR spectra. TEM analysis revealed formation of gold nanopyramids and nanorods. The SAED analysis confirmed the crystalline nature of nanoparticles. The gold nanoparticles demonstrated antibacterial and antifungal activity against Escherichia coli, Staphylococcus aureus, Bacillus subtilis, Aspergillus niger and Pichia pastoris. The cytotoxic activity of gold nanoparticles was studied using HEK, Hela and L929 cancerous cell lines and the apoptosis of cancerous cells were observed using propidium iodide staining. Thus, a simple and eco-friendly method for synthesis of biostabilized gold nanoparticles using fruit extracts of Garcinia indica was developed and the nanoparticles had potent antibacterial, antifungal and anticancer properties.

Keywords: cytotoxic, gold nanoparticles, green synthesis, Garcinia indica, anticancer

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Authors: Friday Godwin Okibe, Christian Chinweuba Onoyima, Edith Bolanle Agbaji, Victor Olatunji Ajibola

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Polymer-inorganic nanocomposites are presently impacting diverse areas, specifically in biomedical sciences. In this research, hydroxyapatite-sodium alginate has been prepared, and characterized, with emphasis on the influence of sodium alginate on its characteristics. In situ wet chemical precipitation method was used in the preparation. The prepared nanocomposite was characterized with Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), with image analysis, and X-Ray Diffraction (XRD). The FTIR study shows peaks characteristics of hydroxyapatite and confirmed formation of the nanocomposite via chemical interaction between sodium alginate and hydroxyapatite. Image analysis shows the nanocomposites to be of irregular morphologies which did not show significant change with increasing sodium alginate addition, while particle size decreased with increase in sodium alginate addition (359.46 nm to 109.98 nm). From the XRD data, both the crystallite size and degree of crystallinity also decreased with increasing sodium alginate composition (32.36 nm to 9.47 nm and 72.87% to 1.82% respectively), while the specific surface area and microstrain increased with increasing sodium alginate composition (0.0041 to 0.0139 and 58.99 m²/g to 201.58 m²/g respectively). The results show that the formulation with 50%wt of sodium alginate (HASA-50%wt), possess exceptional characteristics for biomedical applications such as drug delivery.

Keywords: nanocomposite, sodium alginate, hydroxyapatite, biomedical, FTIR, XRD, SEM

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Authors: Sara Mercedes Barroso Pinzón, Álvaro Jesús Caicedo Castro, Antonio Javer Sánchez Herencia

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In recent years there has been increased academic and industrial research into the development of orthopaedic implants with structural properties and functionality similar to mechanical strength, osseointegration, thermal stability and antibacterial capacity similar to bone structure. Hydroxyapatite has been considered for decades as an ideal biomaterial for bone regeneration due to its chemical and crystallographic similarity to the mineral structure bioapatites. However, the lack of trace elements in the hydroxyapatite structure confers very low mechanical and biological properties. Under this scenario, the objective of the research is the synthesis of hydroxyapatite with Mg from the francolite mineral present in phosphate rock from the central-eastern region of Colombia, taking advantage of the extraction of mineral species as natural precursors of Ca, P and Mg. The minerals present were studied, fluorapatite as the mineral of interest associated with magnesium carbonates and quartz. The chemical and mineralogical composition was determined by X-ray fluorescence (XRF) and X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX); the optimum conditions were established using the acid leaching mechanism in the wet concentration process. From the products obtained and characterised by XRD, XRF, SEM, FTIR, RAMAN, HAp-Mg biocomposite scaffolds are fabricated and the influence of Mg on morphometric parameters, mechanical and biological properties in the formed materials is evaluated.

Keywords: phosphate rock, hydroxyapatite, magnesium, biomaterials

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Authors: Khamael M. Abualnaja, Lidija Šiller, Benjamin R. Horrocks

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Alkylated silicon nanocrystals (C11-SiNCs) were prepared successfully by galvanostatic etching of p-Si(100) wafers followed by a thermal hydrosilation reaction of 1-undecene in refluxing toluene in order to extract C11-SiNCs from porous silicon. Erbium trichloride was added to alkylated SiNCs using a simple mixing chemical route. To the best of our knowledge, this is the first investigation on mixing SiNCs with erbium ions (III) by this chemical method. The chemical characterization of C11-SiNCs and their mixtures with Er3+ (Er/C11-SiNCs) were carried out using X-ray photoemission spectroscopy (XPS). The optical properties of C11-SiNCs and their mixtures with Er3+ were investigated using Raman spectroscopy and photoluminescence (PL). The erbium-mixed alkylated SiNCs shows an orange PL emission peak at around 595 nm that originates from radiative recombination of Si. Er/C11-SiNCs mixture also exhibits a weak PL emission peak at 1536 nm that originates from the intra-4f transition in erbium ions (Er3+). The PL peak of Si in Er/C11-SiNCs mixture is increased in the intensity up to three times as compared to pure C11-SiNCs. The collected data suggest that this chemical mixing route leads instead to a transfer of energy from erbium ions to alkylated SiNCs.

Keywords: photoluminescence, silicon nanocrystals, erbium, Raman spectroscopy

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Authors: Marcia Silva, Jayme Kolarik, Brennon Garthwait, William Lee, Hai-Feng Zhang

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Adsorption of lead by a natural porous material was studied to establish a baseline for the removal of heavy metals from drinking and waste water. Samples were examined under different conditions such as solution pH, solution concentration, solution temperature, and exposure time. New materials with potentially enhanced adsorption properties were developed by functionalizing the surface of the natural porous material to fabricate graphene based coated and sulfide based treated porous material. The functionalized materials were characterized with Fourier Transform Infrared Spectroscopy (FTIR), Raman, Thermogravimetric Analysis (TGA) and Scanning Electron Microscopy (SEM) and Energy Dispersive Spectroscopy (EDS) techniques. Solution pH effect on removal efficiency has been investigated in acidic (pH = 4), neutral (pH = 6) and basic (pH = 10) pH levels. All adsorbent materials showed highest adsorption capacities at neutral pH levels. Batch experiment was employed to assess the efficacy for the removal of lead with the sorption kinetics and the adsorption isotherms being determined for the natural and treated porous materials. The addition of graphene-based and sulfide-based materials increased the lead removal capacity of the natural clean porous material. Theoretical calculations confirmed pseudo-second order model as kinetic mechanism for lead adsorption for all adsorbents.

Keywords: heavy metals, ion exchange, adsorption, water remediation

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Authors: Hina Verma, Karine Le Guen, Renaud Dalaunay, Iyas Ismail, Vita Ilakovac, Jean Pascal Rueff, Yunlin Jacques Zheng, Philippe Jonnard

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To the extent of our knowledge, X-ray emission spectroscopy (XES) has been applied in the soft x-ray region (photon energy ≤ 2 keV) to study the buried layers and interfaces of stacks of nanometer-thin films. Now we extend the methodology to study the buried interfaces in the hard X-ray region (i.e., ≥ five keV). The emission spectra allow us to study the interactions between elements in the buried layers from the analysis of their valence states, thereby providing sensitive information about the physical-chemical environment of the emitting element in multilayers. We exploit the chemical sensitivity of XES to study the interfaces between Fe and Si layers in the Fe/Si multilayer from the Fe Kβ₂,₅ emission spectra (7108 eV). The Fe Kβ₅ emission line results from the electronic transition from occupied 3d to 1s levels (i.e., valence to core transition) and is hence sensitive to the chemical state of emitting Fe atoms. The comparison of emission spectra recorded for Fe/Si multilayer with Fe and FeSi₂ references reveal the formation of FeSi₂ at the Fe-Si interfaces inside the multilayer stack. The interfacial thickness was calculated to be 1.4 ± 0.2 nm by taking into consideration the intensity of Fe atoms emitted from the interface and the Fe layer. The formation of FeSi₂ at the interface was further confirmed by the X-ray diffraction and X-ray photoelectron spectroscopy done on the Fe/Si multilayer. Hence, we can conclude that the XES in the hard X-ray range could be used to study multilayers and their interfaces and obtain information both qualitatively and quantitatively.

Keywords: buried interfaces, hard X-ray emission spectroscopy, X-ray diffraction, X-ray photoelectron spectroscopy

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Authors: Lea Lenhardt, Ivana Zeković, Tatjana Dramićanin, Miroslav D. Dramićanin

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Fluorescence spectroscopy coupled with parallel factor analysis (PARAFAC) and artificial neural networks (ANN) were used for characterization and classification of honey. Excitation emission spectra were obtained for 95 honey samples of different botanical origin (acacia, sunflower, linden, meadow, and fake honey) by recording emission from 270 to 640 nm with excitation in the range of 240-500 nm. Fluorescence spectra were described with a six-component PARAFAC model, and PARAFAC scores were further processed with two types of ANN’s (feed-forward network and self-organizing maps) to obtain algorithms for classification of honey on the basis of their botanical origin. Both ANN’s detected fake honey samples with 100% sensitivity and specificity.

Keywords: honey, fluorescence, PARAFAC, artificial neural networks

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Authors: Mohd Sukri Hassan, Ahlam Inayatullah Badrul Munir, M. Husaini A. Rahman

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Halal authentication and verification in supplement capsules are highly required as the gelatine available in the market can be from halal or non-halal sources. It is an obligation for Muslim to consume and use the halal consumer goods. At present, real-time polymerase chain reaction (RT-PCR) is the most common technique being used for the detection of porcine and bovine DNA in gelatine due to high sensitivity of the technique and higher stability of DNA compared to protein. In this study, twenty samples of supplements capsules from different products with different Halal logos were analyzed for porcine and bovine DNA using RT-PCR. Standard bovine and porcine gelatine from eurofins at a range of concentration from 10^-1 to 10^-5 ng/µl were used to determine the linearity range, limit of detection and specificity on RT-PCR (SYBR Green method). RT-PCR detected porcine (two samples), bovine (four samples) and mixture of porcine and bovine (six samples). The samples were also tested using FT-IR technique where normalized peak of IR spectra were pre-processed using Savitsky Golay method before Principal Components Analysis (PCA) was performed on the database. Scores plot of PCA shows three clusters of samples; bovine, porcine and mixture (bovine and porcine). The RT-PCR and FT-IR with chemometrics technique were found to give same results for porcine gelatine samples which can be used for Halal authentication.

Keywords: halal, real-time PCR, gelatine, chemometrics

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Authors: Gina Zavaleta-Espejo, Segundo R. Jáuregui-Rosas, Fanny V. Samanamud-Moreno, José Saldaña Jiménez, Anibal Felix-Quintero, Víctor Montero-Del Aguila, Elsi Mejía-Uriarte

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Vicugnapacos "alpaca" fabrics are considered special for their finesse, and the garments in the textile market are very luxurious. It has many special characteristics such as antiallergic, soft, hygroscopic, among others. In this sense, the research aimed to evaluate the antimicrobial activity of alpaca fabrics functionalized with silver nanoparticles on the bacteria Escherichia coli ATCC 25922 and Staphylococcus aureus ATCC 25923. For the functionalization of the fabrics, AgNO3 and different concentrations of trisodium citrate (TSC) 2, 6, and 10 mg. Tissue characterization was performed using Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). The determination of the antimicrobial activity of the alpaca tissues was made by the Kirby-Bauer method with alpaca tissue discs functionalized with silver nanoparticles, an experimental design was made in completely randomized blocks with three treatments and a negative control with three repetitions. The results showed that inhibition halos were formed for both bacteria, therefore, the functionalized tissues have a high antimicrobial activity, whose mechanism of action is attributed to the free radicals (ROS) generated by the nanoparticles that cause oxidative damage to the bacteria. proteins and lipids of the bacterial cell wall.

Keywords: antimicrobial, animal fibers, fabrics, functionalization, trisodium citrate

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Authors: L. Chevez, A. Apaza, J. Rodriguez, R. Puga, H. Loro, Juan Z. Davalos

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Virtual Dimension (VD) procedure is used to analyze Hyperspectral Image (HIS) treatment-data in order to estimate the abundance of mineral components of a mining sample. Hyperspectral images coming from reflectance spectra (NIR region) are pre-treated using Standard Normal Variance (SNV) and Minimum Noise Fraction (MNF) methodologies. The endmember components are identified by the Simplex Growing Algorithm (SVG) and after adjusted to the reflectance spectra of reference-databases using Simulated Annealing (SA) methodology. The obtained abundance of minerals of the sample studied is very near to the ones obtained using XRD with a total relative error of 2%.

Keywords: hyperspectral imaging, minimum noise fraction, MNF, simplex growing algorithm, SGA, standard normal variance, SNV, virtual dimension, XRD

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Authors: Loredana Elena Nita, Maria Bercea, Aurica P. Chiriac, Iordana Neamtu

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The paper is devoted to the behavior of gels based on poly(itaconic anhydride-co-3, 9-divinyl-2, 4, 8, 10-tetraoxaspiro (5.5) undecane) copolymers, with different ratio between the comonomers, and hyaluronic acid (HA). The gel formation was investigated by small-amplitude oscillatory shear measurements following the viscoelastic behavior as a function of gel composition, temperature and shear conditions. Hyaluronic acid was investigated in the same conditions and its rheological behavior is typical to viscous fluids. In the case of the copolymers, the ratio between the two comonomers influences the viscoelastic behavior, a higher content of itaconic anhydride favoring the gel formation. Also, the sol-gel transition was evaluated according to Winter-Chambon criterion that identifies the gelation point when the viscoelastic moduli (G’ and G”) behave similarly as a function of oscillation frequency. From rheological measurements, an optimum composition was evidenced for which the system presents a typical gel-like behavior at 37 °C: the elastic modulus is higher than the viscous modulus and they are not dependent on the oscillation frequency. The formation of the 3D macroporous network was also evidenced by FTIR spectra, SEM microscopy and chemical imaging. These hydrogels present a high potential as drug delivery systems.

Keywords: copolymer, viscoelasticity, gelation, 3D network

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Authors: Yasir Ali Arfat

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Composite films based on fish protein isolate (FPI) and fish skin gelatin (FSG) blend incorporated with 50 and 100% (w/w, protein) basil leaf essential oil (BEO) in the absence and presence of 3% (w/w, protein) ZnO nanoparticles (ZnONP) were prepared and characterised. Tensile strength (TS) decreased, whilst elongation at break (EAB) increased as BEO level increased (p < 0.05). However, ZnONP addition resulted in higher TS but lower EAB (p < 0.05). The lowest water vapour permeability (WVP) was observed for the film incorporated with 100% BEO and 3% ZnONP (p < 0.05). BEO and ZnONP incorporation decreased transparency of FPI/FSG films (p < 0.05). FTIR spectra indicated that films added with BEO exhibited higher hydrophobicity. Both BEO and ZnONP had a marked impact on thermal stability of the films. Microstructural study revealed that presence of ZnONP prevented bilayer formation of film containing 100% BEO. FPI/FSG films incorporated with 100% BEO, especially in combination with ZnONP, exhibited strong antibacterial activity against food pathogenic and spoilage bacteria and thus could be used as an active food packaging material to ensure safety and to extend the shelf-life of packaged foods.

Keywords: bionanocomposite, fish protein isolate, fish skin gelatin, basil essential oil, ZnO nanoparticles, antimicrobial packaging

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Authors: Ruolan Zhang, Ryo Imai, Naoko Senda, Tomoyuki Sakai

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Enzymes have attracted increasing attentions in industrial manufacturing for their applicability in catalyzing complex chemical reactions under mild conditions. Directed evolution has become a powerful approach to optimize enzymes and exploit their full potentials under the circumstance of insufficient structure-function knowledge. With the incorporation of cell-free synthetic biotechnology, rapid enzyme synthesis can be realized because no cloning procedure such as transfection is needed. Its open environment also enables direct enzyme measurement. These properties of cell-free biotechnology lead to excellent throughput of enzymes generation. However, the capabilities of current screening methods have limitations. Fluorescence-based assay needs applicable fluorescent label, and the reliability of acquired enzymatic activity is influenced by fluorescent label’s binding affinity and photostability. To acquire the natural activity of an enzyme, another method is to combine pre-screening step and high-performance liquid chromatography (HPLC) measurement. But its throughput is limited by necessary time investment. Hundreds of variants are selected from libraries, and their enzymatic activities are then identified one by one by HPLC. The turn-around-time is 30 minutes for one sample by HPLC, which limits the acquirable enzyme improvement within reasonable time. To achieve the real high-throughput enzyme screening, i.e., obtain reliable enzyme improvement within reasonable time, a widely applicable high-throughput measurement of enzymatic reactions is highly demanded. Here, a high-throughput screening method using broadband coherent anti-Stokes Raman spectroscopy (CARS) was proposed. CARS is one of coherent Raman spectroscopy, which can identify label-free chemical components specifically from their inherent molecular vibration. These characteristic vibrational signals are generated from different vibrational modes of chemical bonds. With the broadband CARS, chemicals in one sample can be identified from their signals in one broadband CARS spectrum. Moreover, it can magnify the signal levels to several orders of magnitude greater than spontaneous Raman systems, and therefore has the potential to evaluate chemical's concentration rapidly. As a demonstration of screening with CARS, alcohol dehydrogenase, which converts ethanol and nicotinamide adenine dinucleotide oxidized form (NAD+) to acetaldehyde and nicotinamide adenine dinucleotide reduced form (NADH), was used. The signal of NADH at 1660 cm⁻¹, which is generated from nicotinamide in NADH, was utilized to measure the concentration of it. The evaluation time for CARS signal of NADH was determined to be as short as 0.33 seconds while having a system sensitivity of 2.5 mM. The time course of alcohol dehydrogenase reaction was successfully measured from increasing signal intensity of NADH. This measurement result of CARS was consistent with the result of a conventional method, UV-Vis. CARS is expected to have application in high-throughput enzyme screening and realize more reliable enzyme improvement within reasonable time.

Keywords: Coherent Anti-Stokes Raman Spectroscopy, CARS, directed evolution, enzyme screening, Raman spectroscopy

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Authors: Kumbharkhane Ashok

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The time domain dielectric relaxation spectroscopy (TDRS) probes the interaction of a macroscopic sample with a time-dependent electrical field. The resulting complex permittivity spectrum, characterizes amplitude (voltage) and time scale of the charge-density fluctuations within the sample. These fluctuations may arise from the reorientation of the permanent dipole moments of individual molecules or from the rotation of dipolar moieties in flexible molecules, like polymers. The time scale of these fluctuations depends on the sample and its relative relaxation mechanism. Relaxation times range from some picoseconds in low viscosity liquids to hours in glasses, Therefore the DRS technique covers an extensive dynamical process, its corresponding frequency range from 10-4 Hz to 1012 Hz. This inherent ability to monitor the cooperative motion of molecular ensemble distinguishes dielectric relaxation from methods like NMR or Raman spectroscopy which yield information on the motions of individual molecules. An experimental set up for Time Domain Reflectometry (TDR) technique from 10 MHz to 30 GHz has been developed for the aqueous solutions. This technique has been very simple and covers a wide band of frequencies in the single measurement. Dielectric Relaxation Spectroscopy is especially sensitive to intermolecular interactions. The complex permittivity spectra of aqueous solutions have been fitted using Cole-Davidson (CD) model to determine static dielectric constants and relaxation times for entire concentrations. The heterogeneous molecular interactions in aqueous solutions have been discussed through Kirkwood correlation factor and excess properties.

Keywords: liquid, aqueous solutions, time domain reflectometry

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Authors: Sahar Heidary, Ramin Ghasemi Shayan

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The overall goal Monte Carlo N-atom radioactivity transference PC program (MCNP4C) was done for the regeneration of x-ray groups in diagnostic radiology and mammography. The electrons were transported till they slow down and stopover in the target. Both bremsstrahlung and characteristic x-ray creation were measured in this study. In this issue, the x-ray spectra forecast by several computational models recycled in the diagnostic radiology and mammography energy kind have been calculated by appraisal with dignified spectra and their outcome on the scheming of absorbed dose and effective dose (ED) told to the adult ORNL hermaphroditic phantom quantified. This comprises practical models (TASMIP and MASMIP), semi-practical models (X-rayb&m, X-raytbc, XCOMP, IPEM, Tucker et al., and Blough et al.), and Monte Carlo modeling (EGS4, ITS3.0, and MCNP4C). Images got consuming synchrotron radiation (SR) and both screen-film and the CR system were related with images of the similar trials attained with digital mammography equipment. In sight of the worthy feature of the effects gained, the CR system was used in two mammographic inspections with SR. For separately mammography unit, the capability acquiesced bilateral mediolateral oblique (MLO) and craniocaudal(CC) mammograms attained in a woman with fatty breasts and a woman with dense breasts. Referees planned the common groups and definite absences that managed to a choice to miscarry the part that formed the scientific imaginings.

Keywords: mammography, monte carlo, effective dose, radiology

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Authors: Khalidou Ba, Abdelkrim Chahine, Mohamed Ebn Touhami

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A strong industrial interest is focused on the development of coatings for anticorrosion protection. In this context, phosphate composite materials are expanding strongly due to their chemical characteristics and their interesting physicochemical properties. Sol-gel coatings offer high homogeneity and purity that may lead to obtain coating presenting good adhesion to metal surface. The goal behind this work is to develop efficient coatings for corrosion protection of steel to extend its life. In this context, a sol gel process allowing to obtain thin film coatings on carbon steel with high resistance to corrosion has been developed. The optimization of several experimental parameters such as the hydrolysis time, the temperature, the coating technique, the molar ratio between precursors, the number of layers and the drying mode has been realized in order to obtain a coating showing the best anti-corrosion properties. The effect of these parameters on the microstructure and anticorrosion performance of the films sol gel coating has been investigated using different characterization methods (FTIR, XRD, Raman, XPS, SEM, Profilometer, Salt Spray Test, etc.). An optimized coating presenting good adhesion and very stable anticorrosion properties in salt spray test, which consists of a corrosive attack accelerated by an artificial salt spray consisting of a solution of 5% NaCl, pH neutral, under precise conditions of temperature (35 °C) and pressure has been obtained.

Keywords: sol gel, coating, corrosion, XPS

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Authors: Lee Chiau Yeng, Norhayani Othman

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Regenerated cellulose fiber is fabricated in the NaOH/urea aqueous solution. In this work, cellulose is dissolved in 7 .wt% NaOH/12 .wt% urea in the temperature of -12 °C to prepare regenerated cellulose. Thermal and structure properties of cellulose and regenerated cellulose was compared and investigated by Field Emission Scanning Electron Microscopy (FeSEM), Fourier Transform Infrared Spectroscopy (FTIR), X-Ray Diffraction (XRD), Thermogravimetric analysis (TGA), and Differential Scanning Calorimetry. Results of FeSEM revealed that the regenerated cellulose fibers showed a more circular shape with irregular size due to fiber agglomeration. FTIR showed the difference in between the structure of cellulose and the regenerated cellulose fibers. In this case, regenerated cellulose fibers have a cellulose II crystalline structure with lower degree of crystallinity. Regenerated cellulose exhibited better thermal stability than the cellulose.

Keywords: regenerated cellulose, cellulose, NaOH, urea

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Authors: Jan Karl, Ondrej Suchy, Eliska Fiserova, Milan Ruzicka

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The evolving electromobility and all the electronics also bring an increase of danger with used Li-batteries. Li-batteries have been used in many industries, and currently many types of the batteries are available. Batteries have different compositions that affect their behavior. In the field of Li-battery safety, there are some areas of little discussion, such as extinguishing of fires caused by Li-batteries as well as toxicity of gaseous compounds released from Li batteries, transport or storage. Technical Institute of Fire Protection, which is a part of Fire Brigades of the Czech Republic, is dealing with the safety of Li batteries. That is the reason why we are dealing with toxicity of gaseous compounds released under conditions of fire, mechanical damage, overcharging and other emergencies that may occur. This is necessary for protection of intervening of fire brigade units, people in the vicinity and other envirnomental consequences. In this work, different types of batteries (Li-ion, Li-Po, LTO, LFP) with different kind of damage were tested, and the toxicity and total amount of released gases were studied. These values were evaluated according to their environmental hazard. FTIR spectroscopy was used for the evaluation of toxicity. We used a FTIR gas cell for continuous measurement. The total amount of released gases was determined by collecting the total gas phase through the absorbers and then determining the toxicants absorbed into the solutions. Based on the obtained results, it is possible to determine the protective equipment necessary for the event of an emergency with a Li-battery, to define the environmental load and the immediate danger in an emergency.

Keywords: Li-battery, toxicity, gaseous toxic compounds, FTIR spectroscopy

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Authors: Gonzalez Carlos, Martinez Fransisco

Abstract:

The creation of a seismic prediction model that considers all the regional variations and perfectly adjusts its results to the response spectra is very complicated. To achieve statistically acceptable results, it is necessary to process a sufficiently robust data set, and even if high efficiencies are achieved, this model will only work properly in this region. However, when using it in other regions, differences are found due to different parameters that have not been calibrated to other regions, such as the site effect. The fact that impedance contrasts, as well as other factors belonging to the site, have a great influence on the local response is well known, which is why this work, using the residual method, is intended to establish a regional calibration of the corresponding parameters site effect for the Spain region in the global GMPM BSSA 14.

Keywords: GMPM, seismic prediction equations, residual method, response spectra, impedance contrast

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Authors: Abdallah F. Abd El-Mohsen, Ahmed A. Abdelsamee, Nouby M. Ghazaly

Abstract:

Engine exhaust noise is considered one of the largest sources of vehicle exterior noise. Further reduction of noise from the vehicle exhaust system will be required, as the vehicle exterior noise regulations become stricter. Therefore, the present study has been carried out to illustrate the role of engine operating parameters and exhaust system construction factors on exhaust noise emitted. The measurements carried out using different exhaust systems, which are mainly used in today’s vehicle. The effect of engine speed on the spectra level of exhaust noise is recorded at engine speeds of 900 rpm, 1800 rpm, 2700, rpm 3600 rpm and 4500 rpm. The results indicate that the increase of engine speed causes a significant increase in the spectrum level of exhaust noise. The increase in the number of the outlet of the expansion chamber also reduces the overall level of exhaust noise.

Keywords: exhaust system, expansion chamber, engine speed, spectra

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Authors: Ahmad Umar, Sheikh Akbar, Ahmed A. Ibrahim, Mohsen A. Alhamami

Abstract:

The development of advanced materials for energy storage and gas sensing applications has gained significant attention in recent years. In this study, we synthesized and characterized PANI@MnO2@rGO ternary nanocomposites (NCs) to explore their potential in supercapacitors and gas sensing devices. The ternary NCs were synthesized through a multi-step process involving the hydrothermal synthesis of MnO2 nanoparticles, preparation of PANI@rGO composites and the assembly to the ternary PANI@MnO2@rGO ternary NCs. The structural, morphological, and compositional characteristics of the materials were thoroughly analyzed using techniques such as XRD, FESEM, TEM, FTIR, and Raman spectroscopy. In the realm of gas sensing, the ternary NCs exhibited excellent performance as NH3 gas sensors. The optimized operating temperature of 100 °C yielded a peak response of 15.56 towards 50 ppm NH3. The nanocomposites demonstrated fast response and recovery times of 6 s and 10 s, respectively, and displayed remarkable selectivity for NH3 gas over other tested gases. For supercapacitor applications, the electrochemical performance of the ternary NCs was evaluated using cyclic voltammetry and galvanostatic charge-discharge techniques. The composites exhibited pseudocapacitive behavior, with the capacitance reaching up to 185 F/g at 1 A/g and excellent capacitance retention of approximately 88.54% over 4000 charge-discharge cycles. The unique combination of rGO, PANI, and MnO2 nanoparticles in these ternary NCs offer synergistic advantages, showcasing their potential to address challenges in energy storage and gas sensing technologies.

Keywords: paniI@mnO2@rGO ternary NCs, synergistic effects, supercapacitors, gas sensing, energy storage

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Authors: Anna Drzewicz, Marzena Tykarska

Abstract:

The chiral liquid crystal phases form the helicoidal structure, which is characterized by the helical pitch and the helical twist sense. In anticlinic smectic phase with antiferroelectric properties three types of helix temperature dependence have been obtained: increased helical pitch with temperature and right-handed helix, decreased helical pitch with temperature and left-handed helix and the inversion of both. The change of helical twist sense may be observed during the transition from one liquid crystal phase to another or within one phase for the same substance. According to Gray and McDonnell theory, the helical handedness depends on the absolute configuration of the assymetric carbon atom and its position related to the rigid core of the molecule. However, this theory does not explain the inversion of helical twist sense phenomenon. It is supposed, that it may be caused by the presence of different conformers with opposite handendess, which concentration may change with temperature. In this work, the inversion of helical twist sense in the chiral liquid crystals differing in the length of alkyl chain, in the substitution the benzene ring by fluorine atoms and in the type of helix handedness was tested by vibrational spectroscopy (infrared and raman spectroscopy) and by nuclear magnetic resonance spectroscopy. The results obtained from the vibrational spectroscopy confirm the presence of different conformers. Moreover, the analysis of nuclear magnetic resonance spectra is very useful to check, on which structural fragments the change of conformations are important for the change of helical twist sense.

Keywords: helical twist sense, liquid crystals, nuclear magnetic resonance spectroscopy, vibrational spectroscopy

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Authors: Hamid Merzouk, Djahida Touati-Talantikite, Amina Zaabar

Abstract:

New nanosized materials are in huge expansion worldwide. They play a fundamental role in various industrial applications thanks their unique and functional properties. Moreover, in recent years, a great effort has been made to the design and control fabrication of nanostructured semiconductors such zinc sulphide. In recent years, much attention has been accorded in doped and co-doped ZnS to improve the ZnS films quality. We present in this work the preparation and characterization of ZnS and Al doped ZnS thin films. Nanoparticles ZnS and Al doped ZnS films are prepared by chemical bath deposition method (CBD), for various dopant concentrations. Thin films are deposed onto commercial microscope glass slides substrates. Thiourea is used as sulfide ion source, zinc acetate as zinc ion source and manganese acetate as manganese ion source in alkaline bath at 90 °C. X-ray diffraction (XRD) analyses are carried out at room temperature on films and powders with a powder diffractometer, using CuKα radiation. The average grain size obtained from the Debye–Scherrer’s formula is around 10 nm. Films morphology is examined by scanning electron microscopy. IR spectra of representative sample are recorded with the FTIR between 400 and 4000 cm-1.The transmittance (70 %) is performed with the UV–VIS spectrometer in the wavelength range 200–800 nm. This value is enhanced by Al doping.

Keywords: ZnS, nanostructured semiconductors, thin films, chemical bath deposition

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