Search results for: SERS spectroscopy

Authors: Sarre Nzaba, Bulelwa Ntsendwana, Bekkie Mamba, Alex Kuvarega

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The discharge of azo dyes such as Brilliant black (BB) into the water bodies has carcinogenic and mutagenic effects on humankind and the ecosystem. Conventional water treatment techniques fail to degrade these dyes completely thereby posing more problems. Advanced oxidation processes (AOPs) are promising technologies in solving the problem. Anatase type nitrogen-platinum (N, Pt) co-doped TiO₂ photocatalysts were prepared by a modified sol-gel method using amine terminated polyamidoamine generation 1 (PG1) as a template and source of nitrogen. The resultant photocatalysts were characterized by X‐ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), X‐ray photoelectron spectroscopy (XPS), UV‐Vis diffuse reflectance spectroscopy, photoluminescence spectroscopy (PL), Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy (RS), thermal gravimetric analysis (TGA). The results showed that the calcination atmosphere played an important role in the morphology, crystal structure, spectral absorption, oxygen vacancy concentration, and visible light photocatalytic performance of the catalysts. Anatase phase particles ranging between 9- 20 nm were also confirmed by TEM, SEM, and analysis. The origin of the visible light photocatalytic activity was attributed to both the elemental N and Pd dopants and the existence of oxygen vacancies. Co-doping imparted a shift in the visible region of the solar spectrum. The visible light photocatalytic activity of the samples was investigated by monitoring the photocatalytic degradation of brilliant black dye. Co-doped TiO₂ showed greater photocatalytic brilliant black degradation efficiency compared to singly doped N-TiO₂ or Pd-TiO₂ under visible light irradiation. The highest reaction rate constant of 3.132 x 10-2 min⁻¹ was observed for N, Pd co-doped TiO₂ (2% Pd). The results demonstrated that the N, Pd co-doped TiO₂ (2% Pd) sample could completely degrade the dye in 3 h, while the commercial TiO₂ showed the lowest dye degradation efficiency (52.66%).

Keywords: brilliant black, Co-doped TiO₂, polyamidoamine generation 1 (PAMAM G1), photodegradation

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

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The structural characterization of silicon nano crystals (SiNCs) have been carried out using transmission electron microscope (TEM) and atomic force microscopy (AFM). SiNCs are crystalline with an average diameter of 65 nm. Erbium trichloride was added to silicon nano crystals using a simple chemical procedure. Erbium is useful in this context because it has a narrow emission band at ⋍1536 nm which corresponds to a standard optical telecommunication wavelength. The optical properties of SiNCs and erbium-mixed SiNCs samples have been characterized using UV-vis spectroscopy, confocal Raman spectroscopy and photoluminescence spectroscopy (PL). SiNCs and erbium-mixed SiNCs samples exhibit an orange PL emission peak at around 595 nm that arise from radiative recombination of Si. Erbium-mixed SiNCs also shows a weak PL emission peak at ⋍1536 nm that attributed to the intra-4f transition in erbium ions. The intensity of the PL peak of Si in erbium-mixed SiNCs is increased in the intensity up to ×3 as compared to pure SiNCs. It was observed that intensity of 1536 nm peak decreased dramatically in the presence of silicon nano crystals and the PL emission peak of silicon nano crystals is increased. Therefore, the resulted data present that the energy transfer from erbium ions to SiNCs due to the chemical mixing method which used in this work.

Keywords: Silicon Nanocrystals (SiNCs), Erbium Ion, photoluminescence, energy transfer

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Authors: G. Balaji, R. Balasundaraprabhu, S. Prasanna, M. D. Kannan, K. Sivakumaran, David Mcilroy

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Copper Zin tin sulphide (Cu2ZnSnS4 or CZTS) is found to be better alternative to Copper Indium gallium diselenide as absorber layers in thin film based solar cells due to the utilisation of earth-abundant materials in the midst of lower toxicity. In the present study, Cu2ZnSnS4 thin films were prepared on soda lime glass using (CuS, ZnS, SnS) targets and were deposited by three different stacking orders, using RF Magnetron sputtering. The substrate temperature was fixed at 300 °C during the depositions. CZTS thin films were characterized using X-ray diffraction, X-ray photoelectron spectroscopy, Raman spectroscopy and UV-Vis-NIR spectroscopy. All the samples exhibited X-ray peaks pertaining to (112) kesterite phase of CZTS, along with the presence of a predominant wurtzite CZTS phase. X-ray photoelectron spectroscopy revealed the presence of all the elements in all the samples. The change in stacking order clearly shows that it affects the structural and phase properties of the films. Relative atomic concentrations of Zn, Cu, Sn and S, which are determined by high-resolution XPS core level spectra integrated peak areas revealed that the CZTS films exhibit inhomogeneity in both stoichiometry and elemental composition. Raman spectroscopy studies on the film showed the presence of CZTS phase. The energy band gap of the CZTS thin films was found to be in the range of 1.5 eV to 1.6 eV. The films were then annealed at 450 °C for 5 hrs and it was found that the predominant nature of the X-ray peaks has transformed from Wurtzite to Kesterite phase which is highly desirable for absorber layers in thin film solar cells. The optimized CZTS layer was used as an absorber layer in thin film solar cells. ZnS and CdS were used as buffer layers which in turn prepared by Hot wall epitaxy technique. Gallium doped Zinc oxide was used as a transparent conducting oxide. The solar cell structure Glass/Mo/CZTS/CdS or ZnS/GZO has been fabricated, and solar cell parameters were measured.

Keywords: earth-abundant, Kesterite, RF sputtering, thin film solar cells

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Authors: Hilal Kivrak, Aykut ÇağLar, Nahit Aktaş, Ali Osman Solak

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At present, Cd/TiO₂ and CdTe/TiO₂ catalysts are prepared via sodium borohydride (NaBH4) reduction method. These catalysts are characterized by fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). These Cd/TiO₂ and CdTe/TiO₂ are employed as catalysts for the photocatalytic oxidation of glucose. Cyclic voltammetry (CV), chronoamperometry (CA), and electrochemical impedance spectroscopy (EIS) measurements are used to investigate their glucose electrooxidation activities of catalysts at long and under UV illumination (ʎ=354 nm). CdTe/TiO₂ catalyst is showed the best photocatalytic glucose electrooxidation activity compared to Cd/TiO₂ catalyst.

Keywords: cadmium, NaBH4 reduction method, photocatalytic glucose electrooxidation, Tellerium, TiO2

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Authors: M. Bodner, M. Scampicchio

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Fourier Transform Infrared (FT-IR) spectroscopy coupled with chemometrics was used to distinguish between butter samples and non-butter samples. Further, quantification of the content of margarine in adulterated butter samples was investigated. Fingerprinting region (1400-800 cm^–1) was used to develop unsupervised pattern recognition (Principal Component Analysis, PCA), supervised modeling (Soft Independent Modelling by Class Analogy, SIMCA), classification (Partial Least Squares Discriminant Analysis, PLS-DA) and regression (Partial Least Squares Regression, PLS-R) models. PCA of the fingerprinting region shows a clustering of the two sample types. All samples were classified in their rightful class by SIMCA approach; however, nine adulterated samples (between 1% and 30% w/w of margarine) were classified as belonging both at the butter class and at the non-butter one. In the two-class PLS-DA model’s (R² = 0.73, RMSEP, Root Mean Square Error of Prediction = 0.26% w/w) sensitivity was 71.4% and Positive Predictive Value (PPV) 100%. Its threshold was calculated at 7% w/w of margarine in adulterated butter samples. Finally, PLS-R model (R² = 0.84, RMSEP = 16.54%) was developed. PLS-DA was a suitable classification tool and PLS-R a proper quantification approach. Results demonstrate that FT-IR spectroscopy combined with PLS-R can be used as a rapid, simple and safe method to identify pure butter samples from adulterated ones and to determine the grade of adulteration of margarine in butter samples.

Keywords: adulterated butter, margarine, PCA, PLS-DA, PLS-R, SIMCA

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Authors: Bienvenu Gael Fouda Mbanga

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This study reports a new approach of preparation of carbon nanoparticles coated cerium oxide nanorods (CNPs/CeONRs) nanocomposite and reusing the spent adsorbent of Cd2+- CNPs/CeONRs nanocomposite for latent fingerprint detection (LFP) after removing Cd2+ ions from aqueous solution. CNPs/CeONRs nanocomposite was prepared by using CNPs and CeONRs with adsorption processes. The prepared nanocomposite was then characterized by using UV-visible spectroscopy (UV-visible), Fourier transforms infrared spectroscopy (FTIR), X-ray diffraction pattern (XRD), scanning electron microscope (SEM), Transmission electron microscopy (TEM), Energy-dispersive X-ray spectroscopy (EDS), Zeta potential, X-ray photoelectron spectroscopy (XPS). The average size of the CNPs was 7.84nm. The synthesized CNPs/CeONRs nanocomposite has proven to be a good adsorbent for Cd2+ removal from water with optimum pH 8, dosage 0. 5 g / L. The results were best described by the Langmuir model, which indicated a linear fit (R2 = 0.8539-0.9969). The adsorption capacity of CNPs/CeONRs nanocomposite showed the best removal of Cd2+ ions with qm = (32.28-59.92 mg/g), when compared to previous reports. This adsorption followed pseudo-second order kinetics and intra particle diffusion processes. ∆G and ∆H values indicated spontaneity at high temperature (40oC) and the endothermic nature of the adsorption process. CNPs/CeONRs nanocomposite therefore showed potential as an effective adsorbent. Furthermore, the metal loaded on the adsorbent Cd2+- CNPs/CeONRs has proven to be sensitive and selective for LFP detection on various porous substrates. Hence Cd2+-CNPs/CeONRs nanocomposite can be reused as a good fingerprint labelling agent in LFP detection so as to avoid secondary environmental pollution by disposal of the spent adsorbent.

Keywords: Cd2+-CNPs/CeONRs nanocomposite, cadmium adsorption, isotherm, kinetics, thermodynamics, reusable for latent fingerprint detection

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Authors: J. Belovickis, V. Samulionis, J. Banys, M. V. Silibin, A. V. Solnyshkin, A. V. Sysa

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Ferroelectric polymers exhibit good flexibility, processability and low cost of production. Doping of ferroelectric polymers with nanofillers may modify its dielectric, elastic or piezoelectric properties. Carbon nanotubes are one of the ingredients that can improve the mechanical properties of polymer based composites. In this work, we report on both the ultrasonic and the dielectric properties of the copolymer polyvinylidene fluoride/tetrafluoroethylene (P(VDF-TrFE)) of the composition 70/30 mol% with various concentrations of carbon nanotubes (CNT). Experimental study of ultrasonic wave attenuation and velocity in these composites has been performed over wide temperature range (100 K – 410 K) using an ultrasonic automatic pulse-echo tecnique. The temperature dependences of ultrasonic velocity and attenuation showed anomalies attributed to the glass transition and paraelectric-ferroelectric phase transition. Our investigations showed mechanical losses to be dependent on the volume fraction of the CNTs within the composites. The existence of broad hysteresis of the ultrasonic wave attenuation and velocity within the nanocomposites is presented between cooling and heating cycles. By the means of dielectric spectroscopy, it is shown that the dielectric properties may be tuned by varying the volume fraction of the CNT fillers.

Keywords: carbon nanotubes, polymer composites, PVDF-TrFE, ultrasonic spectroscopy

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Authors: Arifa Batool, Ghulam Hussain Bhatti, Syed Mujtaba Shah

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Inorganic n-type (TiO2, CdO) and p-type (NiO, CuO) metal oxide nanoparticles were synthesized by a facile wet chemical method at room temperature. The morphological, compositional, structural and optical properties were investigated by scanning electron microscopy, energy dispersive X-ray spectroscopy, FT-IR, XRD analysis, UV/Visible and fluorescence spectroscopy. All semiconducting nanoparticles were photosensitized with Ru (II) based Z907 dye in ethanol solvent by grafting. Grafting of dye on the surface of nanoparticles was confirmed by UV/Visible and FT-IR spectroscopy. The synthesized photo-active nanohybrid was thoroughly blended with P3HT, a solid electrolyte and I-V measurements under solar stimulated radiations 1000 W/m2 (AM 1.5) were recorded. Maximum incident photon to current conversion efficiency (IPCE) of 0.9% was achieved with dye functionalized Z907-TiO2 hybrid, IPCE of 0.72% was achieved with bulk-heterojunction of TiO2-Z907-CuO and IPCE of 0.68% was attained with nanocomposite of TiO2-CdO. TiO2 based Solar cells have maximum Jscvalue i.e.4.63 mA/cm2. Dye-functionalized TiO2-based photovoltaic devices were found more efficient than the reference device but the morphology of the device was a major check in progress.

Keywords: solar cell, bulk heterojunction, nanocomposites, photosensitization, dye sensitized solar cell

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Authors: Mohamed Khalifa Zayet, Salma Belal Eiid, Mushira Mohamed Dahaba

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Introduction: Malignant tumors may not be easily detected by traditional radiographic techniques especially in an anatomically complex area like maxillofacial region. At the same time, the advent of biological functional MRI was a significant footstep in the diagnostic imaging field. Objective: The purpose of this study was to define the malignant metabolic profile of maxillofacial lesions using diffusion MRI and magnetic resonance spectroscopy, as adjunctive aids for diagnosing of such lesions. Subjects and Methods: Twenty-one patients with twenty-two lesions were enrolled in this study. Both morphological and functional MRI scans were performed, where T1, T2 weighted images, diffusion-weighted MRI with four apparent diffusion coefficient (ADC) maps were constructed for analysis, and magnetic resonance spectroscopy with qualitative and semi-quantitative analyses of choline and lactate peaks were applied. Then, all patients underwent incisional or excisional biopsies within two weeks from MR scans. Results: Statistical analysis revealed that not all the parameters had the same diagnostic performance, where lactate had the highest areas under the curve (AUC) of 0.9 and choline was the lowest with insignificant diagnostic value. The best cut-off value suggested for lactate was 0.125, where any lesion above this value is supposed to be malignant with 90 % sensitivity and 83.3 % specificity. Despite that ADC maps had comparable AUCs still, the statistical measure that had the final say was the interpretation of likelihood ratio. As expected, lactate again showed the best combination of positive and negative likelihood ratios, whereas for the maps, ADC map with 500 and 1000 b-values showed the best realistic combination of likelihood ratios, however, with lower sensitivity and specificity than lactate. Conclusion: Diffusion weighted imaging and magnetic resonance spectroscopy are state-of-art in the diagnostic arena and they manifested themselves as key players in the differentiation process of orofacial tumors. The complete biological profile of malignancy can be decoded as low ADC values, high choline and/or high lactate, whereas that of benign entities can be translated as high ADC values, low choline and no lactate.

Keywords: diffusion magnetic resonance imaging, magnetic resonance spectroscopy, malignant tumors, maxillofacial

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Authors: Hamsasew Hankebo Lemago, Dóra Hessz, Tamás Igricz, Zoltán Erdélyi, , Imre Miklós Szilágyi

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Metal oxide inverse opals are a promising class of photocatalysts with a unique hierarchical structure. Atomic layer deposition (ALD) is a versatile technique for the synthesis of high-precision metal oxide thin films, including inverse opals. In this study, we report the synthesis of TiO₂, ZnO, and Al₂O₃ inverse opal and their composites photocatalysts using thermal or plasma-enhanced ALD. The synthesized photocatalysts were characterized using a variety of techniques, including scanning electron microscopy (SEM)-energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Raman spectroscopy, photoluminescence (PL), ellipsometry, and UV-visible spectroscopy. The results showed that the ALD-synthesized metal oxide inverse opals had a highly ordered structure and a tunable pore size. The PL spectroscopy results showed low recombination rates of photogenerated electron-hole pairs, while the ellipsometry and UV-visible spectroscopy results showed tunable optical properties and band gap energies. The photocatalytic activity of the samples was evaluated by the degradation of methylene blue under visible light irradiation. The results showed that the ALD-synthesized metal oxide inverse opals exhibited high photocatalytic activity, even under visible light irradiation. The composites photocatalysts showed even higher activity than the individual metal oxide inverse opals. The enhanced photocatalytic activity of the composites can be attributed to the synergistic effect between the different metal oxides. For example, Al₂O₃ can act as a charge carrier scavenger, which can reduce the recombination of photogenerated electron-hole pairs. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production. The ALD-synthesized metal oxide inverse opals and their composites are promising photocatalysts for a variety of applications, such as wastewater treatment, air purification, and energy production.

Keywords: ALD, metal oxide inverse opals, photocatalysis, composites

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Authors: Sergey A. Burikov, Tatiana A. Dolenko, Kirill A. Gushchin, Sergey A. Dolenko

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The paper presents the results of clusterization by Kohonen self-organizing maps (SOM) applied for analysis of array of Raman spectra of multi-component solutions of inorganic salts, for determination of types of salts present in the solution. It is demonstrated that use of SOM is a promising method for solution of clusterization and classification problems in spectroscopy of multi-component objects, as attributing a pattern to some cluster may be used for recognition of component composition of the object.

Keywords: Kohonen self-organizing maps, clusterization, multi-component solutions, Raman spectroscopy

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Authors: Fatma Gülden Şi̇mşek, Osman Meli̇h Can, Mehmet Yumak, Bora Gari̇pcan, Yekta Ülgen

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In this study, the impedance spectroscopy is used as a detection tool in order to characterize surface coating with graphene oxide. Gold electrodes are produced by standard lithography procedures and then coated with graphene oxide using self-assembly method. The impedance of redox solution through bare gold electrodes and graphene oxide coated gold electrodes is measured in the low and high frequency range. The graphene oxide coating reduces the impedance value of the gold electrode and this reduction is distinguishable in the low-frequency range.

Keywords: bioimpedance, electrode characterization, graphene oxide, gold electrodes, impedance spectroscopy

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Authors: Bodhayan Nandi, Shubhajit Roy Chowdhury

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This paper presents the development of a portable blood glucose monitoring device based on Near-Infrared Spectroscopy. The system supports Internet connectivity through WiFi and uploads the time series data of glucose concentration of patients to a server. In addition, the server is given sufficient intelligence to predict the future pathophysiological state of a patient given the current and past pathophysiological data. This will enable to prognosticate the approaching critical condition of the patient much before the critical condition actually occurs.The server hosts web applications to allow authorized users to monitor the data remotely.

Keywords: non invasive, blood glucose concentration, microcontroller, IoT, application server, database server

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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: Tshaiya Devi Thandauthapani, Adam J. Reeve, Adam S. Long, Ian J. Turner, James S. Sharp

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Fingermarks are a crucial form of evidence for identifying a person at a crime scene. However, visualising latent (hidden) fingermarks can be difficult, and the correct choice of techniques is essential to develop and preserve any fingermarks that might be present. Knives, firearms and other metal weapons have proven to be challenging substrates (stainless steel in particular) from which to reliably obtain fingermarks. In this study, time of flight secondary ion mass spectroscopy (ToF-SIMS) was used to image fingermarks on metal surfaces. This technique was compared to a conventional superglue based fuming technique that was accompanied by a series of contrast enhancing dyes (basic yellow 40 (BY40), crystal violet (CV) and Sudan black (SB)) on three different metal surfaces. The conventional techniques showed little to no evidence of fingermarks being present on the metal surfaces after a few days. However, ToF-SIMS images revealed fingermarks on the same and similar substrates with an exceptional level of detail demonstrating clear ridge definition as well as detail about sweat pore position and shape, that persist for over 26 days after deposition when the samples were stored under ambient conditions.

Keywords: conventional techniques, latent fingermarks, metal substrates, time of flight secondary ion mass spectroscopy

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Authors: N. Ammouchi

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We have studied the effect of milling time on the structural and hyperfine properties of Ni45Al45Fe10 compound elaborated by mechanical alloying. The elaboration was performed by using the planetary ball mill at different milling times. The as milled powders were characterized by X-ray diffraction (XRD) and Mӧssbauer spectroscopy. From XRD diffraction spectra, we show that the β NiAl(Fe) was completely formed after 24 h of milling time. When the milling time increases, the lattice parameter increases, whereas the grain size decreases to a few nanometres and the mean level of microstrains increases. The analysis of Mӧssbauer spectra indicates that, in addition to a ferromagnetic phase, α-Fe, a paramagnetic disordered phase Ni Al (Fe) solid solution is observed after 2h and only this phase is present after 12h.

Keywords: NiAlFe, nanostructured powders, X-ray diffraction, Mӧssbauer spectroscopy

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Authors: Vivek Kumar, Alexander M. Zaitsev

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A study on chemical sensing properties of carbon nanofilms on diamond for developing all-carbon chemical sensors is presented. The films were obtained by high temperature graphitization of diamond followed by successive plasma etchings. Characterization of the films was done by Raman spectroscopy, atomic force microscopy, and electrical measurements. Fast and selective response to common organic vapors as seen as sensitivity of electrical conductance was observed. The phenomenological description of the chemical sensitivity is proposed as a function of the surface and bulk material properties of the films.

Keywords: chemical sensor, carbon nanofilm, graphitization of diamond, plasma etching, Raman spectroscopy, atomic force microscopy

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Authors: Keiji Komatsu, Hayato Maruyama, Ariyuki Kato, Atsushi Nakamura, Shigeo Ohshio, Hiroki Akasaka, Hidetoshi Saitoh

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Violet Sr–Al–O:Eu2+ phosphor particles were synthesized from a metal–ethylenediaminetetraacetic acid (EDTA) solution of Sr, Al, Eu, and particulate alumina via spray drying and sintering in a reducing atmosphere. The crystal structures and emission properties at 85–300 K were investigated. The composition of the violet Sr–Al–O:Eu2+ phosphor particles was determined from various Sr–Al–O:Eu2+ phosphors by their emission properties’ dependence on temperature. The highly crystalline SrAl12O19:Eu2+ emission phases were confirmed by their crystallite sizes and the activation energies for the 4f5d–8S7/2 transition of the Eu2+ ion. These results showed that the material identification for the violet Sr–Al–O:Eu2+ phosphor was accomplished by the low-temperature luminescence measurements.

Keywords: low temperature luminescence spectroscopy, material identification, strontium aluminates phosphor, emission properties

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Authors: A. P. Srivastava, D. Srivastava, D. J. Browne

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Relaxation dynamics of Zr44Cu40Al8Ag8 bulk metallic glass (BMG) has been probed using dynamic mechanical analyzer. The BMG sample was casted in the form of a plate of dimension 55 mm x 40 mm x 3 mm using tilt casting technique. X-ray diffraction and transmission electron microscope have been used for the microstructural characterization of as-cast BMG. For the mechanical spectroscopy study, samples in the form of a bar of size 55 mm X 2 mm X 3 mm were machined from the BMG plate. The mechanical spectroscopy was performed on dynamic mechanical analyzer (DMA) by 50 mm 3-point bending method in a nitrogen atmosphere. It was observed that two glass transition process were competing in supercooled liquid region around temperature 390°C and 430°C. The supercooled liquid state was completely characterized using DMA and differential scanning calorimeter (DSC). In addition to the main α-relaxation process, presence of β relaxation process around temperature 360°C; below the glass transition temperature was also observed. The β relaxation process could be described by Arrhenius law with the activation energy of 160 kJ/mole. The volume of the flow unit associated with this relaxation process has been estimated. The results from DMA study has been used to characterize the shear transformation zone in terms of activation volume and size. High fragility parameter value of 34 and higher activation volume indicates that this alloy could show good plasticity in supercooled liquid region. The possible mechanism for the relaxation processes has been discussed.

Keywords: DMA, glass transition, metallic glass, thermoplastic forming

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Authors: Amanda M. Tadini, Houssam Hajjoul, Gustavo Nicolodelli, Stéphane Mounier, Célia R. Montes, Débora M. B. P. Milori

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Soil organic matter (SOM) plays an important role in maintaining soil productivity and accounting for the promotion of biological diversity. The main components of the SOM are the humic substances which can be fractionated according to its solubility in humic acid (HA), fulvic acids (FA) and humin (HU). The determination of the chemical properties of organic matter as well as its interaction with metallic species is an important tool for understanding the structure of the humic fractions. Fluorescence spectroscopy has been studied as a source of information about what is happening at the molecular level in these compounds. Specially, soils of Amazon region are an important ecosystem of the planet. The aim of this study is to understand the molecular and structural composition of HA samples from Spodosol of Amazonia using the fluorescence Emission-Excitation Matrix (EEM) and Time Resolved Fluorescence Spectroscopy (TRFS). The results showed that the samples of HA showed two fluorescent components; one has a more complex structure and the other one has a simpler structure, which was also seen in TRFS through the evaluation of each sample lifetime. Thus, studies of this nature become important because it aims to evaluate the molecular and structural characteristics of the humic fractions in the region that is considered as one of the most important regions in the world, the Amazon.

Keywords: Amazonian soil, characterization, fluorescence, humic acid, lifetime

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Authors: Satish Kolli, Adriana Ferancova, David Porter, Jukka Kömi

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Electrochemical impedance spectroscopy (EIS) has been used to detect sensitization in austenitic stainless steels that are heat treated in the temperature regime 600-820 °C to produce different degrees of sensitization in the material. The tests were conducted at five different DC potentials in the transpassive region. The quantitative determination of degree of sensitization has been done using double loop electrochemical potentiokinetic reactivation tests (DL-EPR). The correlation between EIS Nyquist diagrams and DL-EPR degree of sensitization values has been studied. The EIS technique can be used as a qualitative tool in determining the intergranular corrosion in austenitic stainless steels that are heat treated at a given temperature.

Keywords: electrochemical technique, intergranular corrosion, sensitization, stainless steels

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Authors: I. Ben Kaddour, S. Larbaoui

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Since their first synthesis, the Silicoaluminophosphates materials have proved their efficiency as a good adsorbent and catalyst in several environmental and energetic applications. In this work, the photocatalytic hydrogen production from water splitting reactions has been conducted under visible radiations in the presence of a series of iron and/or titanium-containing microporous silico-alumino-phosphates materials synthesized by hydrothermal method, using triethylamine as an organic structuring agent to obtain the AFI structure type. These photo-catalysts were then characterized by various physicochemical methods to determine their structural, textural and morphological properties such as X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), scanning electron microscopy (SEM) coupled with X rays microanalysis, nitrogen adsorption measurements, UV-visible diffuse reflectance spectroscopy (UV-Vis-DRS), and X-rays photoelectron spectroscopy (XPS) and the analysis revealed that these materials have significant photocatalytic properties. The hydrogen production process has been followed by photoelectrochemical characterization (PEC). The results showed that hydrogen is the only gas produced, and the reaction takes place in the conduction band where water is reduced to hydrogen. The electron recombination has also been avoided, as holes are entrapped using hole scavengers. In addition, these catalysts have been shown to remain stable during reuse for up to five cycles.

Keywords: photocatalysis, SAPO-5, hydrothermal synthesis, hydrogen production

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Authors: Shahriar Ghammamy, Mehrnoosh Saboony

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Purpose: To evaluate the spectral specification (IR-XRD and SEM) of nano-ciprofloxacin that prepared by up-down method (satellite mill). Methods: the ciprofloxacin was minimized to nano-scale with satellite mill and its characterization evaluated by Infrared spectroscopy, XRD diffraction and semi electron microscope (SEM). Expectation enhances the antibacterial property of nano-ciprofloxacin in comparison to ciprofloxacin. IR spectrum of nano-ciprofloxacin compared with spectrum of ciprofloxacin, and both of them were almost agreement with a difference: the peaks in spectrum of nano-ciprofloxacin were sharper than peaks in spectrum of ciprofloxacin. X-Ray powder diffraction analysis of nano-ciprofloxacin shows the diameter of particles equal to 90.9nm. (on the basis of Scherer Equation). SEM image shows the global shape for nano-ciprofloxacin.

Keywords: antibiotic, ciprofloxacin, nano, IR, XRD, SEM

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Authors: Shahriar Ghammamy, Mehrnoosh Saboony

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Purpose: to evaluate the spectral specification(IR-XRD and SEM) of nano ciprofloxacin that prepared by up-down method (satellite mill). Methods: the ciprofloxacin was minimized to nano-scale with satellite mill and it,s characterization evaluated by Infrared spectroscopy, XRD diffraction and semi electron microscope (SEM). Expectation: to enhance the antibacterial property of nano ciprofloxacin in comparison to ciprofloxacin.IR spectrum of nano ciprofloxacin compared with spectrum of ciprofloxacin, and both of them were almost agreement with a difference: the peaks in spectrum of nano ciprofloxacin was sharper than peaks in spectrum of ciprofloxacin. X-Ray powder diffraction analysis of nano ciprofloxacin showes the diameter of particles equal to 90.9 nm (on the basis of scherrer equation). SEM image showes the global shape for nano ciprofloxacin.

Keywords: antibiotic, ciprofloxacin, nano, IR, XRD, SEM

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Authors: Aria Vitkova, Hanna Sykulska-Lawrence

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In recent years, Europa has been one of the major focus points in astrobiology due to its high potential of harbouring life in the vast ocean underneath its icy crust. However, the detection of life on Europa faces many challenges due to the harsh environmental conditions and mission constraints. Raman spectroscopy is a highly capable and versatile in-situ characterisation technique that does not require any sample preparation. It has only been used on Earth to date; however, recent advances in optical and laser technology have also allowed it to be considered for extraterrestrial exploration. So far, most efforts have been focused on the exploration of Mars, the most imminent planetary target. However, as an emerging technology with high miniaturization potential, Raman spectroscopy also represents a promising tool for the exploration of Europa. In this study, the capabilities of Raman technology in terms of life detection on Europa are explored and assessed. Spectra of biosignatures identified as high priority molecular targets for life detection on Europa were acquired at various excitation wavelengths and conditions analogous to Europa. The effects of extremely low temperatures and low concentrations in water ice were explored and evaluated in terms of the effectiveness of various configurations of Raman instruments. Based on the findings, a design of a miniaturized Raman instrument optimized for in-situ detection of life on Europa is proposed.

Keywords: astrobiology, biosignatures, Europa, life detection, Raman Spectroscopy

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Authors: Emily Awuor, Helga Huszar, Zoltan Bozoki

Abstract:

Isotope analysis has found numerous applications in the environmental science discipline, most common being the tracing of environmental contaminants on both regional and global scales. Many environmental contaminants contain ammonia (NH₃) since it is the most abundant gas in the atmosphere and its largest sources are from agricultural and industrial activities. NH₃ isotopes (¹⁴NH₃ and ¹⁵NH₃) are therefore important and can be used in the traceability studies of these atmospheric pollutants. The goal of the project is the construction of a photoacoustic spectroscopy system that is capable of measuring ¹⁵NH₃ isotope selectively in terms of its concentration. A further objective is for the system to be robust, easy-to-use, and automated. This is provided by using two telecommunication type near-infrared distributed feedback (DFB) diode lasers and a laser coupler as the light source in the photoacoustic measurement system. The central wavelength of the lasers in use was 1532 nm, with the tuning range of ± 1 nm. In this range, strong absorption lines can be found for both ¹⁴NH₃ and ¹⁵NH₃. For the selective measurement of ¹⁵NH₃, wavelengths were chosen where the cross effect of ¹⁴NH₃ and water vapor is negligible. We completed the calibration of the photoacoustic system, and as a result, the lowest detectable concentration was 3.32 ppm (3Ϭ) in the case of ¹⁵NH₃ and 0.44 ppm (3Ϭ) in the case of ¹⁴NH₃. The results are most useful in the environmental pollution measurement and analysis.

Keywords: ammonia isotope, near-infrared DFB diode laser, photoacoustic spectroscopy, environmental monitoring

Procedia PDF Downloads 120

Authors: Oluwole Opeyemi Dina, Saheed E. Elugoke, Peter Olutope Fayemi, Omolola E. Fayemi

Abstract:

This study presents the detection of epinephrine (EP) at Fe₃O₄ modified screen printed silver electrode (SPSE). The iron oxide (Fe₃O₄) nanoparticles were characterized with UV-visible spectroscopy, Fourier-Transform infrared spectroscopy (FT-IR) and Scanning electron microscopy (SEM) prior to the modification of the SPSE. The EP oxidation peak current (Iap) increased with an increase in the concentration of EP as well as the scan rate (from 25 - 400 mVs⁻¹). Using cyclic voltammetry (CV), the relationship between Iap and EP concentration was linear over a range of 3.8 -118.9 µM and 118.9-175 µM with a detection limit of 41.99 µM and 83.16 µM, respectively. Selective detection of EP in the presence of ascorbic acid was also achieved at this electrode.

Keywords: screenprint electrode, iron oxide nanoparticle, epinephrine, serum, cyclic voltametry

Procedia PDF Downloads 134

Authors: Dina Ahmed Selim, Eman Shawky Anwar, Rasha Mohamed Abu El-Khair

Abstract:

A rapid, simple and efficient method with minimal sample treatment was developed for authentication of Garcinia cambogia fruit peel powder, along with determining undeclared active pharmaceutical ingredients (APIs) in its herbal slimming dietary supplements using near infrared spectroscopy combined with chemometrics. Five featured adulterants, including sibutramine, metformin, orlistat, ephedrine, and theophylline are selected as target compounds. The Near infrared spectral data matrix of authentic Garcinia cambogia fruit peel and specimens degraded by intentional contamination with the five selected APIs was subjected to hierarchical clustering analysis to investigate their bundling figure. SIMCA models were established to ensure the genuiness of Garcinia cambogia fruit peel which resulted in perfect classification of all tested specimens. Adulterated samples were utilized for construction of PLSR models based on different APIs contents at minute levels of fraud practices (LOQ < 0.2% w/w).The suggested approach can be applied to enhance and guarantee the safety and quality of Garcinia fruit peel powder as raw material and in dietary supplements.

Keywords: Garcinia cambogia, Quality control, NIR spectroscopy, Chemometrics

Procedia PDF Downloads 54

Authors: Asiful Hossain Seikh, Mohammad Asif Alam, Ubair Abdus Samad, Jabair A. Mohammed, S. M. Al-Zahrani, El-Sayed M. Sherif

Abstract:

In this current investigation, aliphatic amine-cured diglycidyl ether of bisphenol-A (DGEBA) based epoxy coating was mixed with certain weight % hardener polyaminoamide (1:2) and was coated on carbon steel panels with and without 1% nano crystalline Al powder. The corrosion behavior of the coated samples were investigated by exposing them in the salt spray chamber, for 500 hours. According to ASTM-B-117, the bath was kept at 35 °C and 5% NaCl containing mist was sprayed at 1.3 bars pressure. Composition of coatings was confirmed using Fourier-transform infrared spectroscopy (FTIR). Electrochemical characterization of the coated samples was also performed using potentiodynamic polarization technique and electrochemical impedance spectroscopy (EIS) technique. All the experiments were done in 3.5% NaCl solution. The nano Al coated sample shows good corrosion resistance property compared to bare Al sample. In fact after salt spray exposure no pitting or local damage was observed for nano coated sample and the coating gloss was negligibly affected. The surface morphology of coated and corroded samples was studied using scanning electron microscopy (SEM).

Keywords: epoxy, nano aluminium, potentiodynamic polarization, salt spray, electrochemical impedence spectroscopy

Procedia PDF Downloads 119

Authors: Akhtar Rasool, Tasneem Zahra Rizvi

Abstract:

In this study, a series of the cadmium sulphide quantum dots/polyaniline nanocomposites with varying compositions were prepared by in-situ polymerization technique and were characterized using X-ray diffraction and Fourier transform infrared spectroscopy. The surface morphology was studied by scanning electron microscopy. UV-Visible spectroscopy was used to find out the energy band gap of the nanoparticles and the nanocomposites. Temperature dependence of DC electrical conductivity and temperature and frequency dependence of AC conductivity were investigated to study the charge transport mechanism in the nanocomposites. DC conductivity was found to be a typical for a semiconducting behavior following Mott’s 1D variable range hoping model. The frequency dependent AC conductivity followed the universal power law.

Keywords: conducting polymers, nanocomposites, polyaniline composites, quantum dots

Procedia PDF Downloads 227