Search results for: lifetime spectroscopy

Authors: Raghvendra Singh Yadav, Ivo Kuřitka, Jarmila Vilcakova, Jaromir Havlica, Lukas Kalina, Pavel Urbánek, Michal Machovsky, Milan Masař, Martin Holek

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In this work, CoFe₂₋ₓGdₓO₄ (x=0.00, 0.05, 0.10, 0.15, 0.20) spinel ferrite nanoparticles are synthesized by sonochemical method. The structural properties and cation distribution are investigated using X-ray Diffraction (XRD), Raman Spectroscopy, Fourier Transform Infrared Spectroscopy and X-ray photoelectron spectroscopy. The morphology and elemental analysis are screened using field emission scanning electron microscopy (FE-SEM) and energy dispersive X-ray spectroscopy, respectively. The particle size measured by FE-SEM and XRD analysis confirm the formation of nanoparticles in the range of 7-10 nm. The electrical properties show that the Gd³⁺ doped cobalt ferrite (CoFe₂₋ₓGdₓO₄; x= 0.20) exhibit enhanced dielectric constant (277 at 100 Hz) and ac conductivity (20.17 x 10⁻⁹ S/cm at 100 Hz). The complex impedance measurement study reveals that as Gd³⁺ doping concentration increases, the impedance Z’ and Z’ ’ decreases. The influence of Gd³⁺ doping in cobalt ferrite nanoparticles on the magnetic property is examined by using vibrating sample magnetometer. Magnetic property measurement reveal that the coercivity decreases with Gd³⁺ substitution from 234.32 Oe (x=0.00) to 12.60 Oe (x=0.05) and further increases from 12.60 Oe (x=0.05) to 68.62 Oe (x=0.20). The saturation magnetization decreases with Gd³⁺ substitution from 40.19 emu/g (x=0.00) to 21.58 emu/g (x=0.20). This decrease follows the three-sublattice model suggested by Yafet-Kittel (Y-K). The Y-K angle increases with the increase of Gd³⁺ doping in cobalt ferrite nanoparticles.

Keywords: sonochemical method, nanoparticles, magnetic property, dielectric property, electrical property

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Authors: S. M. Sadrameli, Y. Azizi

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Lithium-ion batteries (LIBs) have shown to be one of the most reliable energy storage systems for electric cars in the recent years. Ambient temperature has a significant impact on the performance, lifetime, safety and cost of such batteries. Increasing the temperature degrade the lithium batteries more quickly while working at low-temperature environment results reducing the power and energy capability of the system. A thermal management system has been designed and setup in laboratory scale for controlling the temperature at optimum conditions using PEG-1000 with the melting point in the range of 33-40 oC as a phase change material. Aluminum plates have been installed in the PCM to increase the thermal conductivity and increasing the heat transfer rate. Experimental tests have been run at different discharge rates and ambient temperatures to investigate the effects of temperature on the efficiency of the batteries. The comparison has been made between the system of 6 batteries with and without PCM and the results show that PCM with aluminum plates decrease the surface temperature of the batteries that would result better performance and longer lifetime of the batteries.

Keywords: lithium-ion batteries, phase change materials, thermal management, temperature control

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Authors: V. P. Muhamed Shajudheen, K. Viswanathan, K. Anitha Rani, A. Uma Maheswari, S. Saravana Kumar

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We are reporting a simple and low-cost chemical precipitation method adopted to prepare zinc oxide nanoparticles (ZnO) using polyvinyl pyrrolidone (PVP) as a capping agent. The Differential Scanning Calorimetry (DSC) and Thermo Gravimetric Analysis (TGA) was applied on the dried gel sample to record the phase transformation temperature of zinc hydroxide Zn(OH)2 to zinc oxide (ZnO) to obtain the annealing temperature of 800C. The thermal, structure, morphology and optical properties have been employed by different techniques such as DSC-TGA, X-Ray Diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Micro Raman spectroscopy, UV-Visible absorption spectroscopy (UV-Vis), Photoluminescence spectroscopy (PL) and Field Effect Scanning Electron Microscopy (FESEM). X-ray diffraction results confirmed the wurtzite hexagonal structure of ZnO nanoparticles. The two intensive peaks at 160 and 432 cm-1 in the Raman Spectrum are mainly attributed to the first order modes of the wurtzite ZnO nanoparticles. The energy band gap obtained from the UV-Vis absorption spectra, shows a blue shift, which is attributed to increase in carrier concentration (Burstein Moss Effect). Photoluminescence studies of the single crystalline ZnO nanoparticles, show a strong peak centered at 385 nm, corresponding to the near band edge emission in ultraviolet range. The mixed shape of grapes, sphere, hexagonal and rock like structure has been noticed in FESEM. The results showed that PVP is a suitable capping agent for the preparation of ZnO nanoparticles by simple chemical precipitation method.

Keywords: ZnO nanoparticles, simple chemical precipitation route, mixed shape morphology, UV-visible absorption, photoluminescence, Fourier transform infra-Red spectroscopy

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Authors: Bashar Mudhaffar Abdullah, Hasniza Zaman Huri, Nany Hairunisa

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This study was carried out to determine the thermal properties and spectroscopy study of Malaysian Jatropha curcas seed oil. The J. curcas seed oil physicochemical properties such as free fatty acid (FFA %), acid value, saponification value, iodine value, unsaponifiable matter, and viscosity (cp) gave values of 1.89±0.10%, 3.76±0.07, 203.36±0.36 mg/g, 4.90±0.25, 1.76±0.03%, and 32, respectively. Gas chromatography (GC) was used to determine the fatty acids (FAs) composition. J. curcas seed oil is consisting of saturated FAs (19.55%) such as palmitic (13.19%), palmitoleic (0.40%), and stearic (6.36%) acids and unsaturated FAs (80.42%) such as oleic (43.32%) and linoleic (36.70%) acids. The thermal properties using differential scanning calorimetry (DSC) showed that crystallized TAG was observed at -6.79°C. The melting curves displayed three major exothermic regions of J. curcas seed oil, monounsaturated (lower-temperature peak) at -31.69°C, di-unsaturated (medium temperature peak) at -20.23°C and tri-unsaturated (higher temperature peak) at -12.72°C. The results of this study showed that the J. curcas seed oil is a plausible source of polyunsaturated fatty acid (PUFA) to be developed in the future for pharmaceutical applications.

Keywords: Jatropha curcas seed oil, thermal properties, crystallization, melting, spectroscopy

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Authors: Afiqah Shafify Amran, Siti Aisyah Shamsudin, Nurul Yuziana Mohd Yusof

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Cadmium Sulphide (CdS) from group II-IV quantum dots with good optical properties was successfully synthesized by using the simple colloidal method. Capping them with ligand Polyethylinamine (PEI) alters the surface defect of CdS while, thioglycolic acid (TGA) was added to the reaction as a stabilizer. Due to their cytotoxicity, we decided to conjugate them with the protein cage nanoparticles. In this research, we used capsid of Cowpea Chlorotic Mottle Virus (CCMV) to package the CdS because they have the potential to serve in drug delivery, cell targeting and imaging. Adding Sodium Hydroxide (NaOH) changes the pH of the systems hence the isoelectric charge is adjusted. We have characterized and studied the morphology and the optical properties of CdS and CdS-CCMV by transmitted electron microscopic (TEM), UV-Vis spectroscopy, photoluminescence spectroscopy, UV lamp and Fourier transform infrared spectroscopy (FTIR), respectively. The results obtained suggest that the protein cage nanoparticles do not affect the optical properties of CdS.

Keywords: cadmium sulphide, cowpea chlorotic mottle virus, protein cage nanoparticles, quantum dots

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Authors: Syahira Ibrahim, Herlina Abdul Rahim

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The amylose content is an essential element in determining the texture and taste of rice grains. This paper evaluates the use of VIS-SWNIRS in estimating the amylose content for seven varieties of rice grains available in the Malaysian market. Each type consists of 30 samples and all the samples are scanned using the spectroscopy to obtain a range of values between 680-1000nm. The Savitzky-Golay (SG) smoothing filter is applied to each sample’s data before the Principal Component Regression (PCR) technique is used to examine the data and produce a single value for each sample. This value is then compared with reference values obtained from the standard iodine colorimetric test in terms of its coefficient of determination, R2. Results show that this technique produced low R2 values of less than 0.50. In order to improve the result, the range should include a wavelength range of 1100-2500nm and the number of samples processed should also be increased.

Keywords: amylose content, diffuse reflectance, Malaysia rice grain, principal component regression (PCR), Visible and Shortwave near-infrared spectroscopy (VIS-SWNIRS)

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Authors: Marie Kudrnová, Jana Rejková

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The samples of supplied INCONEL 601, 617, 625, and HASTELLOY C-22 alloys and experimental nickel alloy MoNiCr were examined by XPS (X-ray photoelectron spectroscopy) before and after exposure. The experiment was performed in a mixture of LiCl-KCl salt (58.2-41.8 wt. %). The exposure conditions were 440°C, pressure 0.2 MPa, 500 hours in an inert argon atmosphere. The XPS analysis shows that a thin oxide layer composed of metal oxides such as NiO, Cr₂O₃, and Nb₂O₅ was formed. After sputtering the exposed surface with Ar ions, metals were also detected in the elemental state, indicating a very thin protective oxide layer with a thickness in units of up to tens of nanometers.

Keywords: XPS, MSR, nickel alloy, metal oxides

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Authors: Carolin Lutz, Jörg Matthes, Patrick Waibel, Ulrich Precht, Krassimir Garbev, Günter Beuchle, Uwe Schweike, Peter Stemmermann, Hubert B. Keller

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Online measurement of the product quality is a challenging task in cement production, especially in the production of Celitement, a novel environmentally friendly hydraulic binder. The mineralogy and chemical composition of clinker in ordinary Portland cement production is measured by X-ray diffraction (XRD) and X ray fluorescence (XRF), where only crystalline constituents can be detected. But only a small part of the Celitement components can be measured via XRD, because most constituents have an amorphous structure. This paper describes the development of algorithms suitable for an on-line monitoring of the final processing step of Celitement based on NIR-data. For calibration intermediate products were dried at different temperatures and ground for variable durations. The products were analyzed using XRD and thermogravimetric analyses together with NIR-spectroscopy to investigate the dependency between the drying and the milling processes on one and the NIR-signal on the other side. As a result, different characteristic parameters have been defined. A short overview of the Celitement process and the challenging tasks of the online measurement and evaluation of the product quality will be presented. Subsequently, methods for systematic development of near-infrared calibration models and the determination of the final calibration model will be introduced. The application of the model on experimental data illustrates that NIR-spectroscopy allows for a quick and sufficiently exact determination of crucial process parameters.

Keywords: calibration model, celitement, cementitious material, NIR 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: Ishrat Jahan Saifi, Sheelu Shafiq Siddiqi, M. R. Ajmal

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Glycation of protein is very important as well as a harmful process, which may lead to develop DM in human body. Human Serum Albumin (HSA) is the most abundant protein in blood and it is highly prone to glycation by the reducing sugars. 2-¬deoxy d-¬Ribose (dRib) is a highly reactive reducing sugar which is produced in cells as a product of the enzyme thymidine phosphorylase. It is generated during the degradation of DNA in human body. It may cause glycation in HSA rapidly and is involved in the development of DM. In present study, we did in¬vitro glycation of HSA with different concentrations of 2-¬deoxy d-¬ribose and found that dRib glycated HSA rapidly within 4h incubation at 37◦C. UV¬ Spectroscopy, Fluorescence spectroscopy, Fourier transform infrared spectroscopy (FTIR) and Circular Dichroism (CD) technique have been done to determine the structural changes in HSA upon glycation. Results of this study suggested that dRib is the potential glycating agent and it causes alteration in protein structure and biophysical properties which may lead to development and progression of Diabetes mellitus.

Keywords: 2-deoxy D-ribose, human serum albumin, glycation, diabetes mellitus

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Authors: Kim Kennedy, Daren Gibson, Stephanie Flukes, Chandra Diwakarla, Lisa Spalding, Leanne Pilkington, Andrew Redfern

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Introduction: Head and neck cancers (HNC) are often associated with the development of non-HNC primaries, as the risk factors that predispose patients to HNC are often risk factors for other cancers. Aim: We sought to evaluate whether there was an increased risk of smoking and alcohol-related cancers and also other cancers in HNC patients and to evaluate whether there is a difference between the rates of non-HNC primaries in Aboriginal compared with non-Aboriginal HNC patients. Methods: We performed a retrospective cohort analysis of 320 HNC patients from a single center in Western Australia, identifying 80 Aboriginal and 240 non-Aboriginal patients matched on a 1:3 ratio by sites, histology, rurality, and age. We collected data on the patient characteristics, tumour features, treatments, outcomes, and past and subsequent HNCs and non-HNC primaries. Results: In the overall study population, there were 86 patients (26.9%) with a metachronous or synchronous non-HNC primary. Non-HNC primaries were actually significantly more common in the non-Aboriginal population compared with the Aboriginal population (30% vs. 17.5%, p=0.02); however, half of these were patients with cutaneous squamous or basal cell carcinomas (cSCC/BCC) only. When cSCC/BCCs were excluded, non-Aboriginal patients had a similar rate as Aboriginal patients (16.7% vs. 15%, p=0.73). There were clearly more cSCC/BCCs in non-Aboriginal patients compared with Aboriginal patients (16.7% vs. 2.5%, p=0.001) and more patients with melanoma (2.5% vs. 0%, p value not significant (p=NS). Rates of most cancers were similar between non-Aboriginal and Aboriginal patients, including prostate (2.9% vs. 3.8%), colorectal (2.9% vs. 2.5%), kidney (1.2% vs. 1.2%), and these rates appeared comparable to Australian Age Standardised Incidence Rates (ASIR) in the general community. Oesophageal cancer occurred at double the rate in Aboriginal patients (3.8%) compared with non-Aboriginal patients (1.7%), which was far in excess of ASIRs which estimated a lifetime risk of 0.59% in the general population. Interestingly lung cancer rates did not appear to be significantly increased in our cohort, with 2.5% of Aboriginal patients and 3.3% of non-Aboriginal patients having lung cancer, which is in line with ASIRs which estimates a lifetime risk of 5% (by age 85yo). Interestingly the rate of Glioma in the non-Aboriginal population was higher than the ASIR, with 0.8% of non-Aboriginal patients developing Glioma, with Australian averages predicting a 0.6% lifetime risk in the general population. As these are small numbers, this finding may well be due to chance. Unsurprisingly, second HNCs occurred at an increased incidence in our cohort, in 12.5% of Aboriginal patients and 11.2% of non-Aboriginal patients, compared to an ASIR of 17 cases per 100,000 persons, estimating a lifetime risk of 1.70%. Conclusions: Overall, 26.9% of patients had a non-HNC primary. When cSCC/BCCs were excluded, Aboriginal and non-Aboriginal patients had similar rates of non-HNC primaries, although non-Aboriginal patients had a significantly higher rate of cSCC/BCCs. Aboriginal patients had double the rate of oesophageal primaries; however, this was not statistically significant, possibly due to small case numbers.

Keywords: head and neck cancer, synchronous and metachronous primaries, other primaries, Aboriginal

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Authors: A. Sakavičius, A. Lukša, V. Nargelienė, V. Bukauskas, G. Astromskas, A. Šetkus

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We investigate the influence of annealing on the properties of a contact between graphene and metal (Au and Ni), using circular transmission line model (CTLM) contact geometry. Kelvin probe force microscopy (KPFM) and Raman spectroscopy are applied for characterization of the surface and interface properties. Annealing causes a decrease of the metal-graphene contact resistance for both Ni and Au.

Keywords: Au/Graphene contacts, graphene, Kelvin force probe microscopy, NiC/Graphene contacts, Ni/Graphene contacts, Raman spectroscopy

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Authors: Yunwei Zhang, Qiaochu Tang, Yao Zhang, Jiabin Wang, Ulrich Stimming, Alpha Lee

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Forecasting the state of health and remaining useful life of Li-ion batteries is an unsolved challenge that limits technologies such as consumer electronics and electric vehicles. Here we build an accurate battery forecasting system by combining electrochemical impedance spectroscopy (EIS) -- a real-time, non-invasive and information-rich measurement that is hitherto underused in battery diagnosis -- with Gaussian process machine learning. We collect over 20,000 EIS spectra of commercial Li-ion batteries at different states of health, states of charge and temperatures -- the largest dataset to our knowledge of its kind. Our Gaussian process model takes the entire spectrum as input, without further feature engineering, and automatically determines which spectral features predict degradation. Our model accurately predicts the remaining useful life, even without complete knowledge of past operating conditions of the battery. Our results demonstrate the value of EIS signals in battery management systems.

Keywords: battery degradation, machine learning method, electrochemical impedance spectroscopy, battery diagnosis

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Authors: Abdulqader Alkhouzaam, Hazim Qiblawey, Majeda Khraisheh

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Membrane treatment for desalination and wastewater treatment is one of the promising solutions to affordable clean water. It is a developing technology throughout the world and considered as the most effective and economical method available. However, the limitations of membranes’ mechanical and chemical properties restrict their industrial applications. Hence, developing novel membranes was the focus of most studies in the water treatment and desalination sector to find new materials that can improve the separation efficiency while reducing membrane fouling, which is the most important challenge in this field. Graphene oxide (GO) is one of the materials that have been recently investigated in the membrane water treatment sector. In this work, ultrafiltration polysulfone (PSF) membranes with high antifouling properties were synthesized by incorporating different loadings of GO. High-oxidation degree GO had been synthesized using a modified Hummers' method. The synthesized GO was characterized using different analytical techniques including elemental analysis, Fourier transform infrared spectroscopy - universal attenuated total reflectance sensor (FTIR-UATR), Raman spectroscopy, and CHNSO elemental analysis. CHNSO analysis showed a high oxidation degree of GO represented by its oxygen content (50 wt.%). Then, ultrafiltration PSF membranes incorporating GO were fabricated using the phase inversion technique. The prepared membranes were characterized using scanning electron microscopy (SEM) and atomic force microscopy (AFM) and showed a clear effect of GO on PSF physical structure and morphology. The water contact angle of the membranes was measured and showed better hydrophilicity of GO membranes compared to pure PSF caused by the hydrophilic nature of GO. Separation properties of the prepared membranes were investigated using a cross-flow membrane system. Antifouling properties were studied using bovine serum albumin (BSA) and humic acid (HA) as model foulants. It has been found that GO-based membranes exhibit higher antifouling properties compared to pure PSF. When using BSA, the flux recovery ratio (FRR %) increased from 65.4 ± 0.9 % for pure PSF to 84.0 ± 1.0 % with a loading of 0.05 wt.% GO in PSF. When using HA as model foulant, FRR increased from 87.8 ± 0.6 % to 93.1 ± 1.1 % with 0.02 wt.% of GO in PSF. The pure water permeability (PWP) decreased with loadings of GO from 181.7 L.m⁻².h⁻¹.bar⁻¹ of pure PSF to 181.1, and 157.6 L.m⁻².h⁻¹.bar⁻¹ with 0.02 and 0.05 wt.% GO respectively. It can be concluded from the obtained results that incorporating low loading of GO could enhance the antifouling properties of PSF hence improving its lifetime and reuse.

Keywords: antifouling properties, GO based membranes, hydrophilicity, polysulfone, ultrafiltration

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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: Hossain A, Hossain S.

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Introduction: In a small cohort, we sought to assess the magnetic resonance spectroscopy's (MRS) ability to predict the presence of metastatic lesions. Method: A Popular Diagnostic Centre Limited enrolled patients with neuroepithelial tumors. The 1H CSI MRS of the brain allows us to detect changes in the concentration of specific metabolites caused by metastatic lesions. Among these metabolites are N-acetyl-aspartate (NNA), creatine (Cr), and choline (Cho). For Cho, NAA, Cr, and Cr₂, the metabolic ratio was calculated using the division method. Results: The NAA values were 0.63 and 5.65 for tumor cells, 1.86 and 5.66 for normal cells, and 1.86 and 5.66 for normal cells 2. NAA values for normal cells 1 were 1.84, 10.6, and 1.86 for normal cells 2, respectively. Cho levels were as low as 0.8 and 10.53 in the tumor cell, compared to 1.12 and 2.7 in the normal cell 1 and 1.24 and 6.36 in the normal cell 2. Cho/Cr₂ barely distinguished itself from the other ratios in terms of significance. For tumor cells, the ratios of Cho/NAA, Cho/Cr₂, NAA/Cho, and NAA/Cr₂ were significant. Normal cell 1 had significant Cho/NAA, Cho/Cr, NAA/Cho, and NAA/Cr ratios. Conclusion: The clinical result can be improved by using 1H-MRSI to guide the size of resection for metastatic lesions. Even though it is non-invasive and doesn't present any difficulties during the procedure, MRS has been shown to predict the detection of metastatic lesions.

Keywords: metabolite ratio, MRI images, metastatic lesion, MR spectroscopy, N-acetyl-aspartate

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Authors: Ashish Kumar Singh, Preeti Tiwari, Shubham Srivastava, Rajiv Prakash, Herman Terryn, Gopal Ji

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Corrosion inhibition potential of azo dyes namely Allura red (AR), Sunset Yellow (SY) and Amaranth (AN) have been investigated in 0.5 M H2SO4 solutions by electrochemical impedance spectroscopy (EIS), Tafel polarization curves, linear polarization curves, open circuit potential (ocp) curves, UV-Visible spectroscopy, Fourier Transform Infrared spectroscopy (FTIR) and scanning electron microscopy (SEM) techniques. Amaranth dye is found to provide highest corrosion inhibition (90 %) against mild steel corrosion in sulfuric acid solutions among all the tested dyes; while SY and AR dye shows 80% and 78% corrosion inhibition efficiency respectively. The electrochemical measurements and surface morphology analysis reveal that molecular adsorption of dyes at metal acid interface is accountable for inhibition of mild steel corrosion in H2SO4 solutions. The adsorption behavior of dyes has been investigated by various isotherms models, which verifies that it is in accordance with Langmuir isotherm.

Keywords: mild steel, Azo dye, EIS, Langmuir isotherm

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Authors: Jan Luxa, Vlastimil Mazanek, Petr Malinsky, Alexander Romanenko, Mariapompea Cutroneo, Vladimir Havranek, Josef Novak, Eva Stepanovska, Anna Mackova, Zdenek Sofer

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Using accelerated energetic ions is an interesting method for the introduction of structural changes in various carbon-based materials. This way, the properties can be altered in two ways: a) the ions lead to the formation of conductive pathways in graphene oxide structures due to the elimination of oxygen functionalities and b) doping with selected ions to form metal nanoclusters, thus increasing the conductivity. In this work, energetic beams were employed in two ways to prepare capacitor structures in graphene oxide (GO), reduced graphene oxide (rGO) and polyimide (PI) on a micro-scale. The first method revolved around using ion beam writing with a focused ion beam, and the method involved ion implantation via a polymeric mask. To prepare the polymeric mask, a direct spin-coating of PMMA on top of the foils was used. Subsequently, proton beam writing and development in isopropyl alcohol were employed. Finally, the mask was removed using acetone solvent. All three materials were exposed to ion beams with an energy of 2.5-5 MeV and an ion fluence of 3.75x10¹⁴ cm-² (1800 nC.mm-²). Thus, prepared microstructures were thoroughly characterized by various analytical methods, including Scanning electron microscopy (SEM) with Energy-Dispersive X-ray spectroscopy (EDS), X-ray Photoelectron spectroscopy (XPS), micro-Raman spectroscopy, Rutherford Back-scattering Spectroscopy (RBS) and Elastic Recoil Detection Analysis (ERDA) spectroscopy. Finally, these materials were employed and tested as sensors for humidity using electrical conductivity measurements. The results clearly demonstrate that the type of ions, their energy and fluence all have a significant influence on the sensory properties of thus prepared sensors.

Keywords: graphene, graphene oxide, polyimide, ion implantation, sensors

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Authors: Yen-Ping Peng, Ku-Fan Chen, Ken-Lin Chang, Jian Sun

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In this study, palladium loaded titanium dioxide nanotube arrays (Pd/TNAs) was successfully synthesized by anodic oxidation etching method combined with microwave hydrothermal method, using tea or coffee as a green reductant. Pd/TNAs was employed as an electrode in a photoelectrochemcial (PEC) system to simultaneously remove azo-dye and to generate hydrogen in the anodic and cathodic chamber, respectively. The chemical and physical properties of as-synthesized Pd/TNAs were characterized by scanning electron microscopy (SEM), ultraviolet–visible spectroscopy (UV-vis), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). SEM image indicates the diameter and the length of Pd/TNAs were approximately 300 nm and 2.5 μm, respectively. XPS analyses indicate that 1.13% (atomic %) of Pd was loaded onto the surface of TNAs. UV-vis results show that the band gap of TNAs was reduced from 3.2 eV to 2.37 eV after Pd loading. In addition, the electrochemical performances of Pd/TNAs were investigated by photocurrent density test and electrochemical impedance spectroscopy (EIS). The photocurrent (4.0 mA/cm²) of Pd /TNAs was higher than that of the uncoated TNAs (1.4 mA/cm²) at a bias potential of 1 V (vs. Ag/AgCl), indicating that Pd/TNAs-C can effectively separate photogenerated electrons and holes. The mechanism of our PEC system was proposed and discussed in detail in this study.

Keywords: Pd/TNAs, photoelectrochemical, azo-dye degradation, hydrogen generation

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Authors: Christine Fräulin, Daniela Schurr, Hamed Shahidi Rad, Gerrit Waters, Günter Rinke, Roland Dittmeyer, Michael Nilles

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The reaction mechanisms of many liquid-phase reactions in organic chemistry have not yet been sufficiently clarified. Process conditions of several hundred degrees celsius and pressures to ten megapascals complicate the sampling and the determination of kinetic data. Space resolved in-situ measurements promises new insights. A non-invasive in-situ measurement technique has the advantages that no sample preparation is necessary, there is no change in sample mixture before analysis and the sampling do no lead to interventions in the flow. Thus, the goal of our research was the development of a contact-free spatially resolved measurement technique for kinetic studies of liquid phase reaction under process conditions. Therefore we used laser Raman spectroscopy combined with an optical transparent microchannel reactor. To show the performance of the system we choose the oxidation of cyclohexane as sample reaction. Cyclohexane oxidation is an economically important process. The products are intermediates for caprolactam and adipic acid, which are starting materials for polyamide 6 and 6.6 production. To maintain high selectivities of 70 to 90 %, the reaction is performed in industry at a low conversion of about six percent. As Raman spectroscopy is usually very selective but not very sensitive the detection of the small product concentration in cyclohexane oxidation is quite challenging. To meet these requirements, an optical experimental setup was optimized to determine the concentrations by laser Raman spectroscopy with respect to good detection sensitivity. With this measurement technique space resolved kinetic studies of uncatalysed and homogeneous catalyzed cyclohexane oxidation were carried out to obtain details about the reaction mechanism.

Keywords: in-situ laser raman spectroscopy, space resolved kinetic measurements, homogeneous catalysis, chemistry

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Authors: Carol Yue-En Ong, Angelina Hui-Min Tan, Quan Liu, Paul Chi-Lui Ho

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A public general hospital in Singapore has recently implemented an automated unit-dose machine in their inpatient dispensary, Swisslog, with the objective of reducing human error and improving patient safety. However, a concern in stability arises as tablets are removed from their original packaging (bottled loose tablets/capsules) and are repackaged into individual, clear plastic wrappers as unit doses in the system. Drugs that are light-sensitive and hygroscopic would be more susceptible to degradation as the wrapper does not offer full protection. Hence, this study was carried out to study the stability of haloperidol tablets and phenytoin capsules that are light-sensitive and hygroscopic respectively. Validated HPLC-UV assays were first established for quantification of these two compounds. The medications involved were put in the Swisslog and sampled every week for one month. The collected data was analysed and showed no degradation over time. This study also explored an alternative approach for drug stability determination-Raman spectroscopy. The advantage of Raman spectroscopy is its high time efficiency and non-destructive nature. The results suggest that drug degradation can indeed be detected using Raman microscopy, but further research is needed to establish this approach for quantification or qualification of compounds. NanoRam®, a portable Raman spectrocope was also used alongside Raman microscopy but was unsuccessful in detecting degradation in this study.

Keywords: drug stability, haloperidol, HPLC, phenytoin, raman spectroscopy, Swisslog

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Authors: Mandana Amiri, Sima Nouhi, Yashar Azizan-Kalandaragh

Abstract:

Silver nanostructures have been successfully fabricated by using electrodeposition method onto indium-tin-oxide (ITO) substrate. Scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS) and ultraviolet-visible spectroscopy (UV-Vis) techniques were employed for characterization of silver nanostructures. The results show nanostructures with different morphology and electrochemical properties can be obtained by various the deposition potentials and times. Electrochemical behavior of the nanostructures has been studied by using cyclic voltammetry. Silver nanostructures exhibits good electrocatalytic activity towards the reduction of H₂O₂. The presented electrode can be employed as sensing element for hydrogen peroxide.

Keywords: electrochemical sensor, electrodeposition, hydrogen peroxide, silver nanostructures

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Authors: Chaluntorn Vichasilp, Sutee Wangtueai

Abstract:

This study aims to develop a new method to detect active compounds in Thai herbs (1-deoxynojirimycin (DNJ) in mulberry leave, anthocyanin in Mao and curcumin in turmeric) using near infrared spectroscopy (NIRs). NIRs is non-destructive technique that rapid, non-chemical involved and low-cost determination. By NIRs and chemometrics technique, it was found that the DNJ prediction equation conducted with partial least square regression with cross-validation had low accuracy R2 (0.42) and SEP (31.87 mg/100g). On the other hand, the anthocyanin prediction equation showed moderate good results (R2 and SEP of 0.78 and 0.51 mg/g) with Multiplication scattering correction at wavelength of 2000-2200 nm. The high absorption could be observed at wavelength of 2047 nm and this model could be used as screening level. For curcumin prediction, the good result was obtained when applied original spectra with smoothing technique. The wavelength of 1400-2500 nm was created regression model with R2 (0.68) and SEP (0.17 mg/g). This model had high NIRs absorption at a wavelength of 1476, 1665, 1986 and 2395 nm, respectively. NIRs showed prospective technique for detection of some active compounds in Thai herbs.

Keywords: anthocyanin, curcumin, 1-deoxynojirimycin (DNJ), near infrared spectroscopy (NIRs)

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Authors: Dhanashree Aole, V. Hariharan, Swati Surushe

Abstract:

Corrosion can cause serious and expensive damage to the automobile components. Various proven techniques for controlling and preventing corrosion depend on the specific material to be protected. Electrochemical Impedance Spectroscopy (EIS) and salt spray tests are commonly used to assess the corrosion degradation mechanism of coatings on metallic surfaces. While, the only test which monitors the corrosion rate in real time is known as Linear Polarisation Resistance (LPR). In this study, electrochemical tests (EIS & LPR) and spray test are reviewed to assess the corrosion resistance and durability of different coatings. The main objective of this study is to correlate the test results obtained using linear polarization resistance (LPR) and Electrochemical Impedance Spectroscopy (EIS) with the results obtained using standard salt spray test. Another objective of this work is to evaluate the performance of various coating systems- CED, Epoxy, Powder coating, Autophoretic, and Zn-trivalent coating for vehicle underbody application. The corrosion resistance coating are assessed. From this study, a promising correlation between different corrosion testing techniques is noted. The most profound observation is that electrochemical tests gives quick estimation of corrosion resistance and can detect the degradation of coatings well before visible signs of damage appear. Furthermore, the corrosion resistances and salt spray life of the coatings investigated were found to be according to the order as follows- CED> powder coating > Autophoretic > epoxy coating > Zn- Trivalent plating.

Keywords: Linear Polarization Resistance (LPR), Electrochemical Impedance Spectroscopy (EIS), salt spray test, sacrificial and barrier coatings

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Authors: Issam Alnader, Aboubaker Lasebae, Rand Raheem

Abstract:

Wireless sensor networks (WSNs) are distributed network systems used in a wide range of applications, including safety-critical systems. The latter provide critical services, often concerned with human life or assets. Therefore, ensuring the dependability requirements of Safety critical systems is of paramount importance. The purpose of this paper is to utilize the Hidden Markov Model (HMM) to elongate the service availability of WSNs by increasing the time it takes a node to become obsolete via optimal load balancing. We propose an HMM algorithm that, given a WSN, analyses and predicts undesirable situations, notably, nodes dying unexpectedly or prematurely. We apply this technique to improve on C. Lius’ algorithm, a scheduling-based algorithm which has served to improve the lifetime of WSNs. Our experiments show that our HMM technique improves the lifetime of the network, achieved by detecting nodes that die early and rebalancing their load. Our technique can also be used for diagnosis and provide maintenance warnings to WSN system administrators. Finally, our technique can be used to improve algorithms other than C. Liu’s.

Keywords: wireless sensor networks, IoT, dependability of safety WSNs, energy conservation, sleep awake schedule

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Authors: Zeynep Dikmen, Vural Bütün

Abstract:

Electron donor or acceptor capability to participate in electron conjugation is the requirement for an electroactive material. Conjugated molecules and polymers bearing heterocyclic units have potential as optically electroactive materials. Thiazolo thiazole based compounds have attention for last two decades, because they have attractive electronic and optical properties, these compounds are useful for electronic application areas such as dye sentisized solar cells (DSSCs), organic light emitting diodes (OLEDs) and field effect transistors (FETs). Thiazolo[5,4-d]thiazole is bicyclic aromatic structure contains N and S atoms which act as electron donor. A new electron accepting or donating group bound to thiazolo [5,4-d] thiazole fused ring can change the electronic, spectroscopic, stability and dyeing properties of the new material. Polyphenylene(thiazolo [5,4-d] thiazole) (p-PhTT) compound was synthesized via condensation reaction of terephthalaldehyde with dithiooxamide. The chemical structure was determined with solid state 13C NMR spectroscopy. Optical properties (i.e. absorbance and band gap) was determined via solid UV-vis spectroscopy. The insoluble polymer was quarternized with 4-vinylbenzyl chloride (VBC). Colorless VBC changed into a yellow liquid. AgNO3 complex were prepared and optical properties were investigated with UV-Vis, fluorescence spectroscopy and X-ray spectroscopy and cyclic voltammetry studies were examined in this research. This structure exhibits good absorbance and fluorescence in UV-vis region. Synthesis scheme of PyTT and preparation of metal complexes are given. PyTT has absorbance at ~360 nm and fluorescence at ~420 nm.

Keywords: thiazolo thiazole, quarternized polymers, polymeric ligands, Ag complexes

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Authors: V. Sivakumar, R. Neelakantan

Abstract:

Mineral mapping on the Moon surface provides the clue to understand the origin, evolution, stratigraphy and geological history of the Moon. Recently, reflectance imaging spectroscopy plays a significant role in identifying minerals on the planetary surface in the Visible to NIR region of the electromagnetic spectrum. The Moon Mineralogy Mapper (M3) onboard Chandrayaan-1 provides unprecedented spectral data of lunar surface to study about the Moon surface. Here we used the M3 sensor data (hyperspectral imaging spectroscopy) for analysing mineralogy of Orientale basin region on the Moon surface. Reflectance spectrums were sampled from different locations of the basin and continuum was removed using ENvironment for Visualizing Images (ENVI) software. Reflectance spectra of unknown mineral composition were compared with known Reflectance Experiment Laboratory (RELAB) spectra for discriminating mineralogy. Minerals like olivine, Low-Ca Pyroxene (LCP), High-Ca Pyroxene (HCP) and plagioclase were identified. In addition to these minerals, an unusual type of spectral signature was identified, which indicates the probable Fe-Mg-spinel lithology in the basin region.

Keywords: chandryaan-1, moon mineralogy mapper, mineral, mare orientale, moon

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Authors: A. Attaf, I. Bouhaf Kharkhachi

Abstract:

Hexagonal tin disulfide (SnS2) films were deposited by spray ultrasonic technique on glass substrates at different experimental conditions. The effect of deposition time (2, 4, 6, and 7 min) on different properties of SnS2 thin films was investigated by XRD and UV spectroscopy visible spectrum. X-ray diffraction study detected the preferential orientation growth of SnS2 compound having structure along (001) plane increased with the deposition time. The results of UV spectroscopy visible spectrum showed that films deposited at 4 min have high transmittance, up to 60%, in the visible region.

Keywords: structural and optical properties, tin sulfide, thin films, ultrasonic spray

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Authors: Rafiuddin

Abstract:

Solid polymer electrolytes have emerged as an area of interest in the field of solid state chemistry owing to their facile and cost-effective synthesis and number of applications in different areas of chemistry, extending over a wide range of temperatures. In the present work, polymer composite solid electrolyte comprising of Polyaniline (PANI) as polymer and potassium silver iodide (KAg4I5) using alumina (Al2O3) of different compositions having the formula (1-x) PANI- KAg4I5. x Al2O3 with x ranging from 0.0 to 0.5 was prepared by solid state reaction method. The structural elucidation and characterization was done by X- Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Thermogravimetric- Differential Thermal Analysis (TG-DTA) and Impedance Spectroscopy. The thermal analysis shows a phase transition at 147°C attributed to β-α phase transition of AgI due to the disproportionation of KAg4I5 to AgI and KAg2I3 at temperatures higher than 36°C. The X Ray diffraction analysis also confirms the presence of both AgI and KAg2I3 in the samples. The conductivities recorded over a temperature range of 40-250° C lie in the range of 10-1 to 10-3 S cm-1. Maximum conductivity was seen in the compositon x = 0.4 i.e. 1.84 × 10-2 Scm-1 at 313 K and 1.38 × 10-1 Scm-1 at 513 K, with a minimum activation energy of 0.14 eV.

Keywords: polymer solid electrolytes, XRD, DTA, electrical conductivity, impedance spectroscopy

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Authors: N. H. Alias, S. A. Aziz, Y. Abdullah, H. M. Kamari, S. Sani, M. P. Ismail, N. U. Saidin, N. A. A. Salim, N. E. E. Abdullah

Abstract:

Gamma (γ) irradiation study has been investigated on the 6 rectangular shape of the standard X-Ray lead glass with 5/16” thick, providing 2.00 mm lead shielding value; at selected Sievert doses (C1; 0, C2; 0.07, C3; 0.035, C4; 0.07, C5; 0.105 and C6; 0.14) by using (XRD) X-ray Diffraction techniques, ultrasonic and (UV-VIS) Ultraviolet-Visible Spectroscopy. Concentration of lead in 0.5 N acid nitric (HNO3) environments is then studied by means of Atomic Absorption Spectroscopy (AAS) as to observe the glass corrosion behavior after irradiation at room temperature. This type of commercial glass is commonly used as radiation shielding glass in medical application.

Keywords: gamma irradiation, lead glass, leaching, structural

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