Search results for: spectroscopy methods

Authors: Simran Baweja, Bhavika Kalal, Surajit Maity

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Photoinduced tautomerization reactions have been the centre of attention among scientific community over past several decades because of their significance in various biological systems. 7-azaindole (7AI) is considered as a model system for DNA base pairing and to understand the role of such tautomerization reactions in mutations. To the best of our knowledge, extensive studies have been carried on 7-azaindole and its solvent clusters exhibiting proton/ hydrogen transfer in both solution as well as gas phase. Derivatives of above molecule, like 2,7- and 2,6-diazaindoles are proposed to have even better photophysical properties due to the presence of -aza group on the 2nd position. However, there are a few studies in the solution phase which suggest the relevance of these molecules, but there are no experimental studies reported in the gas phase yet. In our current investigation, we present the first gas phase spectroscopic data of 2,7-diazaindole (2,7-DAI) and its solvent cluster (2,7-DAI-H2O). In this, we have employed state-of-the-art laser spectroscopic methods such as fluorescence excitation (LIF), dispersed fluorescence (DF), resonant two-photon ionization time of flight mass spectrometry (2C-R2PI), photoionization efficiency spectroscopy (PIE), IR-UV double resonance spectroscopy i.e. fluorescence-dip infrared spectroscopy (FDIR) and resonant ion-dip infrared spectroscopy (IDIR) to understand the electronic structure of the molecule. The origin band corresponding to S1 ← S0 transition of the bare 2,7-DAI is found to be positioned at 33910 cm-1 whereas the origin band corresponding to S1 ← S0 transition of the 2,7-DAI-H2O is positioned at 33074 cm-1. The red shifted transition in case of solvent cluster suggests the enhanced feasibility of excited state hydrogen/ proton transfer. The ionization potential for the 2,7-DAI molecule is found to be 8.92 eV, which is significantly higher that the previously reported 7AI (8.11 eV) molecule, making it a comparatively complex molecule to study. The ionization potential is reduced by 0.14 eV in case of 2,7-DAI-H2O (8.78 eV) cluster compared to that of 2,7-DAI. Moreover, on comparison with the available literature values of 7AI, we found the origin band of 2,7-DAI and 2,7-DAI-H2O to be red shifted by -729 and -280 cm-1 respectively. The ground and excited state N-H stretching frequencies of the 27DAI molecule were determined using fluorescence-dip infrared spectra (FDIR) and resonant ion dip infrared spectroscopy (IDIR), obtained at 3523 and 3467 cm-1, respectively. The lower value of vNH in the electronic excited state of 27DAI implies the higher acidity of the group compared to the ground state. Moreover, we have done extensive computational analysis, which suggests that the energy barrier in excited state reduces significantly as we increase the number of catalytic solvent molecules (S= H2O, NH3) as well as the polarity of solvent molecules. We found that the ammonia molecule is a better candidate for hydrogen transfer compared to water because of its higher gas-phase basicity. Further studies are underway to understand the excited state dynamics and photochemistry of such N-rich chromophores.

Keywords: photoinduced tautomerization reactions, gas phse spectroscopy, ), IR-UV double resonance spectroscopy, resonant two-photon ionization time of flight mass spectrometry (2C-R2PI)

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Authors: Hyery Kang, Dong-Yeun Koh, Yun-Ho Ahn, Huen Lee

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Terahertz time-domain spectroscopy (THz-TDS) was used to observe the THF clathrate hydrate system with dosage of polyvinylpyrrolidone (PVP) with three different average molecular weights (10,000 g/mol, 40,000 g/mol, 360,000 g/mol). Distinct footprints of phase transition in the THz region (0.4 - 2.2 THz) were analyzed and absorption coefficients and complex refractive indices are obtained and compared in the temperature range of 253 K to 288 K. Along with the optical properties, ring breathing and stretching modes for different molecular weights of PVP in THF hydrate are analyzed by Raman spectroscopy.

Keywords: clathrate hydrate, terahertz, polyvinylpyrrolidone (PVP), THz-TDS, inhibitor

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Authors: Abdulnasser S. Saleh

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The importance of metal-semiconductor interfaces comes from the fact that most electronic devices are interconnected using metallic wiring that forms metal–semiconductor contacts. The properties of these contacts can vary considerably depending on the nature of the interface with the semiconductor. Variable-energy positron annihilation spectroscopy has been applied to study interfaces in Al/Si, Au/Si, and Au/GaAs structures. A computational modeling by ROYPROF program is used to analyze Doppler broadening results in order to determine kinds of regions that positrons are likely to sample. In all fittings, the interfaces are found 1 nm thick and act as an absorbing sink for positrons diffusing towards them and may be regarded as highly defective. Internal electric fields were found to influence positrons diffusing to the interfaces and unable to force them cross to the other side. The materials positron affinities are considered in understanding such motion. The results of these theoretical fittings have clearly demonstrated the sensitivity of interfaces in any fitting attempts of analyzing positron spectroscopy data and gave valuable information about metal-semiconductor interfaces.

Keywords: interfaces, semiconductor, positron, defects

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Authors: K. Petcharaporn, S. Kumchoo

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The acidity (citric acid) is one of the chemical contents that can refer to the internal quality and the maturity index of tomato. The titratable acidity (%TA) can be predicted by a non-destructive method prediction by using the transmittance short wavelength (SW-NIR). Spectroscopy in the wavelength range between 665-955 nm. The set of 167 tomato samples divided into groups of 117 tomatoes sample for training set and 50 tomatoes sample for test set were used to establish the calibration model to predict and measure %TA by partial least squares regression (PLSR) technique. The spectra were pretreated with MSC pretreatment and it gave the optimal result for calibration model as (R = 0.92, RMSEC = 0.03%) and this model obtained high accuracy result to use for %TA prediction in test set as (R = 0.81, RMSEP = 0.05%). From the result of prediction in test set shown that the transmittance SW-NIR spectroscopy technique can be used for a non-destructive method for %TA prediction of tomatoes.

Keywords: tomato, quality, prediction, transmittance, titratable acidity, citric acid

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Authors: Uraib Sharaha, Guy Beck, Joseph Kapelushnik, Adam H. Agbaria, Itshak Lapidot, Shaul Mordechai, Ahmad Salman, Mahmoud Huleihel

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Infectious diseases cause a significant burden on the public health and the economic stability of societies all over the world for several centuries. A reliable detection of the causative agent of infection is not possible based on clinical features, since some of these infections have similar symptoms, including fever, sneezing, inflammation, vomiting, diarrhea, and fatigue. Moreover, physicians usually encounter difficulties in distinguishing between viral and bacterial infections based on symptoms. Therefore, there is an ongoing need for sensitive, specific, and rapid methods for identification of the etiology of the infection. This intricate issue perplex doctors and researchers since it has serious repercussions. In this study, we evaluated the potential of the mid-infrared spectroscopic method for rapid and reliable identification of bacterial and viral infections based on simple peripheral blood samples. Fourier transform infrared (FTIR) spectroscopy is considered a successful diagnostic method in the biological and medical fields. Many studies confirmed the great potential of the combination of FTIR spectroscopy and machine learning as a powerful diagnostic tool in medicine since it is a very sensitive method, which can detect and monitor the molecular and biochemical changes in biological samples. We believed that this method would play a major role in improving the health situation, raising the level of health in the community, and reducing the economic burdens in the health sector resulting from the indiscriminate use of antibiotics. We collected peripheral blood samples from young 364 patients, of which 93 were controls, 126 had bacterial infections, and 145 had viral infections, with ages lower than18 years old, limited to those who were diagnosed with fever-producing illness. Our preliminary results showed that it is possible to determine the infectious agent with high success rates of 82% for sensitivity and 80% for specificity, based on the WBC data.

Keywords: infectious diseases, (FTIR) spectroscopy, viral infections, bacterial infections.

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Authors: A. Guemache, M. Omari

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Oxides with formula Ca1-xSrx MnO3 (0≤x≤0.2) were synthesized using co-precipitation method. The identification of the obtained phase was carried out using infrared spectroscopy and X-ray diffraction. Thermogravimetric and differential analysis was permitted to characterize different transformations of precursors which take place during one heating cycle. The study of electrochemical behavior was carried out by cyclic voltammetry and impedance spectroscopy. The obtained results show that apparent catalytic activity improved when increasing the concentration of strontium. Anodic current densities varies from 1.3 to 5.9 mA/cm2 at the rate scan of 20 mV.s-1 and a potential 0.8 V for oxides with composition x=0 to 0.2.

Keywords: oxide, co-precipitation, electrochemical properties, cathode-type

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Authors: Z. Ž. Lazarević, D. L. Sekulić, V. N. Ivanovski, N. Ž. Romčević

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NiFe2O4 (nickel ferrite), ZnFe2O4 (zinc ferrite) and Ni0.5Zn0.5Fe2O4 (nickel-zinc ferrite) were prepared by mechanochemical route in a planetary ball mill starting from mixture of the appropriate quantities of the Ni(OH)2/Fe(OH)3, Zn(OH)2/Fe(OH)3 and Ni(OH)2/Zn(OH)2/Fe(OH)3 hydroxide powders. In order to monitor the progress of chemical reaction and confirm phase formation, powder samples obtained after 25 h, 18 h and 10 h of milling were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), IR, Raman and Mössbauer spectroscopy. It is shown that the soft mechanochemical method, i.e. mechanochemical activation of hydroxides, produces high quality single phase ferrite samples in much more efficient way. From the IR spectroscopy of single phase samples it is obvious that energy of modes depends on the ratio of cations. It is obvious that all samples have more than 5 Raman active modes predicted by group theory in the normal spinel structure. Deconvolution of measured spectra allows one to conclude that all complex bands in the spectra are made of individual peaks with the intensities that vary from spectrum to spectrum. The deconvolution of Raman spectra allows to separate contributions of different cations to a particular type of vibration and to estimate the degree of inversion.

Keywords: ferrites, Raman spectroscopy, IR spectroscopy, Mössbauer measurements

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Authors: C. L. Popa, S. L. Iconaru, A. Costescu, C. S. Ciobanu, M. Motelica Heino, R. Guegan, D. Predoi

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Surface functionalization of ceramic composites with a special focus on tetraethyl orthosilicate (TEOS) and hydroxyapatite (HAp) is discoursed. Mesoporous ceramic HAp-TEOS composites were prepared by the incorporation of hydroxyapatite into tetraethyl orthosilicate by sol-gel method. The resulting samples were analysed by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, and Raman spectroscopy and nitrogen physisorption. The removal of Pb2+ ions from aqueous solutions was evaluated using Atomic Absorbtion Spectroscopy (AAS). Removal experiments of Pb2+ ions were carried out in aqueous solutions with controlled Pb2+ at pH ~ 3 and pH ~ 5. After removal experiment of Pb2+ at pH 3 and pH 5, porous hydroxyapatite nanoparticles is transformed into PbHAp_3 and PbHAp_5 via the adsorption of Pb2+ ions followed by the cation exchange reaction. The diffraction patterns show that THAp nanoparticles were successfully coated with teos without any structural changes. On the other, the AAS analysis showed that THAp can be useful in the removal Pb2+ from water contaminated.

Keywords: teos, hydroxyapatite, environment applications, biosystems engineering

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Authors: Nipin Kohli, Ravi Chand Singh

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Diabetes mellitus is a serious illness and can be life-threatening if left untreated. Acetone present in the exhaled breath of a diabetic person is a biomarker of patients suffering from diabetes mellitus and is higher than its usual concentration present in the breath of healthy people. In the present work, a portable gas sensor system based on chromium oxide (Cr₂O₃) nanoparticles has been developed that can analyze diabetic patient’s breath. Undoped and indium (In) doped Cr₂O₃ nanoparticles were synthesized by a chemical route and characterized by X-ray diffraction, scanning electron microscopy, Raman spectroscopy, UV-visible spectroscopy, and photoluminescence spectroscopy for their structural, morphological and optical properties. Thick film gas sensors were fabricated out of synthesized samples. To diagnose diabetes, the sensors’ response to low concentrations of acetone was measured, and it was found that the addition of indium dramatically enhances the acetone gas sensing response. Moreover, the fabricated sensors were highly stable, reproducible and resistant to humidity. Enhancement of sensor response of doped sensors towards acetone can be ascribed to increase in defects due to addition of a dopant, and it was found that in-doped Cr₂O₃ sensors are more useful for analysis of breath of diabetic patients.

Keywords: Diabetes mellitus, nanoparticles, raman spectroscopy, sensor

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Authors: Takashi Kaburagi, Takamasa Komura, Yosuke Kurihara

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Absolute pitch is the ability to identify a musical note without a reference tone. Training for absolute pitch often occurs in preschool education. It is necessary to clarify how well the trainee can make use of synesthesia in order to evaluate the effect of the training. To the best of our knowledge, there are no existing methods for objectively confirming whether the subject is using synesthesia. Therefore, in this study, we present a method to distinguish the use of color-auditory synesthesia from the separate use of color and audition during absolute pitch training. This method measures blood volume in the prefrontal cortex using functional Near-infrared spectroscopy (fNIRS) and assumes that the cognitive step has two parts, a non-linear step and a linear step. For the linear step, we assume a second order ordinary differential equation. For the non-linear part, it is extremely difficult, if not impossible, to create an inverse filter of such a complex system as the brain. Therefore, we apply a method based on a self-organizing map (SOM) and are guided by the available data. The presented method was tested using 15 subjects, and the estimation accuracy is reported.

Keywords: absolute pitch, functional near-infrared spectroscopy, prefrontal cortex, synesthesia

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Authors: A. Guemache, M. Omari

Abstract:

Oxides with formula Ca1-xSrx MnO3(0≤x≤0.2) were synthesized using co precipitation method. The identification of the obtained phase was carried out using infrared spectroscopy and x-ray diffraction. Thermogravimetric and differential analysis was permitted to characterize different transformations of precursors which take place during one heating cycle. The study of electrochemical behavior was carried out by cyclic voltammetry and impedance spectroscopy. The obtained results show that apparent catalytic activity improved when increasing the concentration of strontium. Anodic current densities varies from 1.3 to 5.9 mA/cm2 at the rate scan of 20 mV.s-1 and a potential 0.8 V for oxides with composition x=0 to 0.2.

Keywords: oxide, co-precipitation, thermal analysis, electrochemical properties

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Authors: Lamia L. G. Al-Mahamad, Benjamin R. Horrocks, Andrew Houlton

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Hydrogels based on metal coordination polymers of nucleosides and a range of metal ions (Au, Ag, Cu) have been prepared and characterized by atomic force microscopy (AFM), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy, Fourier transform infrared spectroscopy, ultraviolet-visible absorption spectroscopy, and powder X-ray diffraction. AFM images of the xerogels revealed the formation of extremely long polymer molecules (> 10 micrometers, the maximum scan range). This result is also consistent with TEM images which show a fibrous morphology. Oxidative doping of the Au-nucleoside fibres produces an electrically conductive nanowire. No sharp Bragg peaks were found at the at the X-ray diffraction pattern for metal ions hydrogels indicating that the samples were amorphous, but instead the data showed broad peaks in the range 20 < Q < 40 and correspond to distances d=2μ/Q. The data was analysed using a simplified Rietveld method by fitting a regression model to obtain the distance between atoms.

Keywords: hydrogel, metal ions, nanowire, nucleoside

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Authors: Proficiency Munsaka, Peter Baricholo, Erich Rohwer

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Pulse evolutions along the 5 cm long, 6.0 ×4.2 μm² cross-section silicon germanium (SiGe) photonic waveguides were simulated and compared with experiments. Simulations were carried out by solving a generalized nonlinear Schrodinger equation (GNLSE) for an optical pulse evolution along the length of the SiGe photonic waveguides by the split-step Fourier method (SSFM). The solution obtained from the SSFM gave the pulse envelope in both time and spectral domain calculated at each distance step along the propagation direction. The SiGe photonic waveguides were pumped in an anomalous group velocity dispersion (GVD) regime using a 4.7 μm, 210 fs femtosecond laser to produce a significant supercontinuum (SC). The simulated propagation of ultrafast pulse along the SiGe photonic waveguides produced an SC covering the atmospheric window (2.5-8.5 μm) containing the molecular fingerprints for important gases. Thus, the mid-infrared supercontinuum generation in SiGe photonic waveguides system can be commercialized for gas spectroscopy for detecting gases that include CO₂, CH₄, H₂O, SO₂, SO₃, NO₂, H₂S, CO, and NO at trace level using absorption spectroscopy technique. The simulated profile evolutions are spectrally and temporally similar to those obtained by other researchers. Obtained evolution profiles are characterized by pulse compression, Soliton fission, dispersive wave generation, stimulated Raman Scattering, and Four Wave mixing.

Keywords: silicon germanium photonic waveguide, supercontinuum generation, spectroscopy, mid infrared

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

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Metal-enhanced luminescence of silicon nano crystals (SiNCs) was determined using two different particle sizes of silver nano particles (AgNPs). SiNCs have been characterized by scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), Fourier transform infrared spectroscopy (FTIR) and X-ray photo electron spectroscopy (XPS). It is found that the SiNCs are crystalline with an average diameter of 65 nm and FCC lattice. AgNPs were synthesized using photochemical reduction of AgNO3 with sodium dodecyl sulphate (SDS). The enhanced luminescence of SiNCs by AgNPs was evaluated by confocal Raman microspectroscopy. Enhancement up to ×9 and ×3 times were observed for SiNCs that mixed with AgNPs which have an average particle size of 100 nm and 30 nm, respectively. Silver NPs-enhanced luminescence of SiNCs occurs as a result of the coupling between the excitation laser light and the plasmon bands of AgNPs; thus this intense field at AgNPs surface couples strongly to SiNCs.

Keywords: silver nanoparticles, surface enhanced raman spectroscopy (SERS), silicon nanocrystals, luminescence

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Authors: J. Mona, R. R. da Silva, C.-L.Cheng, Y. Kopelevich

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We report on a possible occurrence of superconductivity in 5 nm particle size diamond powders treated with sulfur (S) at 500 o C for 10 hours in ~10-2 Torr vacuum. Superconducting-like magnetization hysteresis loops M(H) have been measured up to ~ 50 K by means of the SQUID magnetometer (Quantum Design). Both X-ray (Θ-2Θ geometry) and Raman spectroscopy analyses revealed no impurity or additional phases. Nevertheless, the measured Raman spectra are characteristic to the diamond with embedded disordered carbon and/or graphitic fragments suggesting a link to the previous reports of the local or surface superconductivity in graphite- and amorphous carbon–sulfur composites.

Keywords: nanodiamond, sulfur, superconductivity, Raman spectroscopy

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Authors: Isao Tomita

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The detection of environmental gases, 12CO_2, 13CO_2, and CH_4, using near-infrared semiconductor lasers with a short laser path length is studied by means of wavelength-modulation spectroscopy. The developed system is compact and has high sensitivity enough to detect the absorption peaks of isotopic 13CO_2 of a 3-% CO_2 gas at 2 um with a path length of 2.4 m, where its peak size is two orders of magnitude smaller than that of the ordinary 12CO_2 peaks. In addition, the detection of 12CO_2 peaks of a 385-ppm (0.0385-%) CO_2 gas in the air is made at 2 um with a path length of 1.4 m. Furthermore, in pursuing the detection of an ancient environmental CH_4 gas confined to a bubble in ice at the polar regions, measurements of the absorption spectrum for a trace gas of CH_4 in a small area are attempted. For a 100-% CH_4 gas trapped in a 1 mm^3 glass container, the absorption peaks of CH_4 are obtained at 1.65 um with a path length of 3 mm, and also the gas pressure is extrapolated from the measured data.

Keywords: environmental gases, Near-Infrared Laser Detection, Wavelength-Modulation Spectroscopy, gas pressure

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Authors: Nisrine Benzbiria, Abderrahmane Thoume, Mustapha Zertoubi

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The goal of this research is to investigate the corrosion inhibition potential of functionalized graphene oxide (GO) with oxime derivative on AA2024-T3 surface in synthetic seawater. The utilization of functionalized graphene oxide is creating a category of corrosion inhibitors known as organically modified nanomaterials. In our work, the functionalization of GO by chalcone oxime enables graphene oxide to have enhanced water solubility and a good corrosion mitigation capacity. Fourier-transform infrared (FT-IR) spectroscopy was utilized to evaluate the main functional groups of the inhibitor. Electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization curves (PDP) showed that the inhibitor acts as a mixed-type inhibitor. The inhibitory efficiency (IE) improved as the concentration increased to a value of 96% after one hour of exposure to a medium containing 60 mg/L ppm of the inhibitor. According to thermodynamic calculations, the adsorption of the inhibitor on the AA2024-T3 surface in 3% NaCl followed the Langmuir isotherm. The formation of a barrier layer was further confirmed by surface analysis. The protective film prevented the alloy dissolution and limited the accessibility of attacking ions, as evinced by solution analysis techniques.

Keywords: AA2024-T3, NaCl, electrochemical methods, FT-IR, SEM/AFM, DFT, MC simulation

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Authors: Dauda G., Bila Ha Sani Y. M., Magaji M. G., Musa A. M., Hassan H. S.

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Introduction: Globimetula oreophila is a parasitic plant with a known therapeutic value that is widely used in the treatment of various ailments, including malaria, hypertension, cancer, diabetes, epilepsy and as a diuretic agent. Objectives: The present study is aimed at analyzing and documenting the level of trace and toxic metals in the crude ethanol leaf extract of G. oreophila. Methods: After collection and authentication, the leaves were air-dried, mashed into powder, weighed and extracted using aqueous ethanol (70%). The crude extract (0.5g) was digested with HNO₃: HCl (3:1); then heated to 2000C and analyzed for its metal content by atomic absorption spectroscopy (AAS). Results: Fe had the highest concentration (32.73mg/kg), while Pb was not detected. The concentrations of Co, Cu, Ni, Zn and Cd detected were 5.97, 10.8, 8.01 and 0.9mg/kg, respectively. The concentration of Cd, Fe and Ni were above the permissible limit of FAO/WHO. Conclusion: The results also show that the analyzed plant is a beneficial source of appropriate and essential trace metals. However, the leaf of G. oreophila in the present study was probably unsafe for long-term use because of the level of Fe, Ni, and Cd concentration.

Keywords: Globimetula oreophila, minerals, trace element, crude extract

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Authors: Ayten Ekin Meşe, Selahattin Şentürk, Melike Duvanoğlu

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Petroleum refineries are a highly complex process industry with continuous production and high operating costs. Physical separation of crude oil starts with the crude oil distillation unit, continues with various conversion and purification units, and passes through many stages until obtaining the final product. To meet the desired product specification, process parameters are strictly followed. To be able to ensure the quality of distillates, routine analyses are performed in quality control laboratories based on appropriate international standards such as American Society for Testing and Materials (ASTM) standard methods and European Standard (EN) methods. The cut point of distillates in the crude distillation unit is very crucial for the efficiency of the upcoming processes. In order to maximize the process efficiency, the determination of the quality of distillates should be as fast as possible, reliable, and cost-effective. In this sense, an alternative study was carried out on the crude oil distillation unit that serves the entire refinery process. In this work, studies were conducted with three different crude oil distillates which are Light Straight Run Naphtha (LSRN), Heavy Straight Run Naphtha (HSRN), and Kerosene. These products are named after separation by the number of carbons it contains. LSRN consists of five to six carbon-containing hydrocarbons, HSRN consist of six to ten, and kerosene consists of sixteen to twenty-two carbon-containing hydrocarbons. Physical properties of three different crude distillation unit products (LSRN, HSRN, and Kerosene) were determined using Near-Infrared Spectroscopy with multivariate calibration. The absorbance spectra of the petroleum samples were obtained in the range from 10000 cm⁻¹ to 4000 cm⁻¹, employing a quartz transmittance flow through cell with a 2 mm light path and a resolution of 2 cm⁻¹. A total of 400 samples were collected for each petroleum sample for almost four years. Several different crude oil grades were processed during sample collection times. Extended Multiplicative Signal Correction (EMSC) and Savitzky-Golay (SG) preprocessing techniques were applied to FT-NIR spectra of samples to eliminate baseline shifts and suppress unwanted variation. Two different multivariate calibration approaches (Partial Least Squares Regression, PLS and Genetic Inverse Least Squares, GILS) and an ensemble model were applied to preprocessed FT-NIR spectra. Predictive performance of each multivariate calibration technique and preprocessing techniques were compared, and the best models were chosen according to the reproducibility of ASTM reference methods. This work demonstrates the developed models can be used for routine analysis instead of conventional analytical methods with over 90% accuracy.

Keywords: crude distillation unit, multivariate calibration, near infrared spectroscopy, data preprocessing, refinery

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Authors: Olga Długosz, Jolanta Pulit-Prociak, Marcin Banach

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The paper presents a process to obtain glutathione-modified titanium oxide nanoparticles. The processes were carried out in a microwave radiation field. The influence of the molar ratio of glutathione to titanium oxide and the effect of the fold of NaOH vs. stoichiometric amount on the size of the formed TiO₂ nanoparticles was determined. The physicochemical properties of the obtained products were evaluated using dynamic light scattering (DLS), transmission electron microscope- energy-dispersive X-ray spectroscopy (TEM-EDS), low-temperature nitrogen adsorption method (BET), X-Ray Diffraction (XRD) and Fourier-transform infrared spectroscopy (FTIR) microscopy methods. The size of TiO₂ nanoparticles was characterized from 30 to 336 nm. The release of titanium ions from the prepared products was evaluated. These studies were carried out using different media in which the powders were incubated for a specific time. These were water, SBF and Ringer's solution. The release of titanium ions from modified products is weaker compared to unmodified titanium oxide nanoparticles. The reduced release of titanium ions may allow the use of such modified materials as substances in drug delivery systems.

Keywords: titanium dioxide, nanoparticles, drug carrier, glutathione

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Authors: Olga Długosz, Jolanta Pulit-Prociak, Marcin Banach

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The paper presents a process to obtain glutathione-modified titanium oxide nanoparticles. The processes were carried out in a microwave radiation field. The influence of the molar ratio of glutathione to titanium oxide and the effect of the fold of NaOH vs. stoichiometric amount on the size of the formed TiO₂ nanoparticles was determined. The physicochemical properties of the obtained products were evaluated using dynamic light scattering (DLS), transmission electron microscope- energy-dispersive X-ray spectroscopy (TEM-EDS), low-temperature nitrogen adsorption method (BET), X-Ray Diffraction (XRD), and Fourier-transform infrared spectroscopy (FTIR) microscopy methods. The size of TiO₂ nanoparticles was characterized from 30 to 336 nm. The release of titanium ions from the prepared products was evaluated. These studies were carried out using different media in which the powders were incubated for a specific time. These were: water, SBF, and Ringer's solution. The release of titanium ions from modified products is weaker compared to unmodified titanium oxide nanoparticles. The reduced release of titanium ions may allow the use of such modified materials as substances in drug delivery systems.

Keywords: titanium dioxide, nanoparticles, drug carrier, glutathione

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Authors: Sabir Hussain, Mujtaba Hassan, Kashif Rasool, Asif Shahzad

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Fine particulate matter with an aerodynamic diameter of less than 2.5 μm (PM2.5) was collected in Islamabad from November 2022 to January 2023, at urban sites. The average mass concentrations of PM2.5 varied, ranging from 90.5 to 133 μg m−3 in urban areas. Environmental scanning electron microscopy (ESEM) analysis revealed that Islamabad's PM2.5 comprised soot aggregates, ashes, minerals, bio-particles, and unidentified particles. Results from inductively coupled plasma atomic emission spectroscopy (ICP-OES) indicated a gradual increase in total elemental concentrations in Islamabad PM2.5 in winter, with relatively high levels in December. Significantly different elemental compositions were observed in urban PM2.5. Enrichment factor (EF) analysis suggested that elements such as K, Na, Ca, Mg, Al, Fe, Ba, and Sr were of natural origin, while As, Cu, Zn, Pb, Cd, Mn, Ni, and Se originated from anthropogenic sources. Plasmid DNA assays demonstrated varying levels of potential toxicity in Islamabad PM2.5 collected from urban sites, as well as across different seasons. Notably, the urban winter PM2.5 sample exhibited much stronger toxicity compared to other samples. The presence of heavy metals in Islamabad PM2.5, including Cu, Zn, Pb, Cd, Cr, Mn, and Ni, may have synergistic effects on human health.

Keywords: islamabad particulate matter pm2.5, scanning electron microscopy with energy-dispersive x-ray spectroscopy(sem-eds), fourier transform infrared spectroscopy(ftir), inductively coupled plasma optical emission spectroscopy(icp-oes)

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

Abstract:

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: Vusumzi E. Pakade, Themba D. Ntuli, Augustine E. Ofomaja

Abstract:

Macadamia nutshell biosorbents treated in three different methods (raw Macadamia nutshell powder (RMN), acid-treated Macadamia nutshell (ATMN) and base-treated Macadamia nutshell (BTMN)) were investigated for the adsorption of Cr(VI) from aqueous solutions. Fourier transform infrared spectroscopy (FT-IR) spectra of free and Cr(VI)-loaded sorbents as well as thermogravimetric analysis (TGA) revealed that the acid and base treatments modified the surface properties of the sorbents. The optimum conditions for the adsorption of Cr(VI) by sorbents were pH 2, contact time 10 h, adsorbent dosage 0.2 g L-1, and concentration 100 mg L-1. The different treatment methods altered the surface characteristics of the sorbents and produced different maximum binding capacities of 42.5, 40.6 and 37.5 mg g-1 for RMN, ATMN and BTMN, respectively. The data was fitted into the Langmuir, Freundlich, Redlich-Peterson and Sips isotherms. No single model could clearly explain the data perhaps due to the complexity of process taking place. The kinetic modeling results showed that the process of Cr(VI) biosorption with Macadamia sorbents was better described by a process of chemical sorption in pseudo-second order. These results showed that the three treatment methods yielded different surface properties which then influenced adsorption of Cr(VI) differently.

Keywords: biosorption, chromium(VI), isotherms, Macadamia, reduction, treatment

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Authors: Siva Chander Chabattula, Piyush Kumar Gupta, Debashis Chakraborty, Rama Shanker Verma

Abstract:

Green nanoparticles have gotten a lot of attention because of their potential applications in tissue regeneration, bioimaging, wound healing, and cancer therapy. The physical and chemical methods to synthesize metal oxide nanoparticles have an environmental impact, necessitating the development of an environmentally friendly green strategy for nanoparticle synthesis. In this study, we used Annona muricata plant leaf extract to synthesize Zinc Oxide nanoparticles (Am-ZnO NPs), which were evaluated using UV/Visible spectroscopy, FTIR spectroscopy, X-Ray Diffraction, DLS, and Zeta potential. Nanoparticles had an optical absorbance of 355 nm and a net negative surface charge of ~ - 2.59 mV. Transmission Electron Microscope characterizes the Shape and size of the nanoparticles. The obtained Am-ZnO NPs are biocompatible and hemocompatible in nature. These nanoparticles caused an anti-cancer therapeutic effect in MIA PaCa2 and MOLT4 cancer cells by inducing oxidative stress, and a change in mitochondrial membrane potential leads to programmed cell death. Further, we observed a reduction in the size of lung cancer spheroids (act as tumor micro-environment) with doxorubicin as a positive control.

Keywords: Biomaterials, nanoparticle, anticancer activity, ZnO nanoparticles

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

Abstract:

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

Abstract:

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

Abstract:

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: E. Gil, A. Zepeda, J. Rivera, C. Ben-Youssef, S. Rincón

Abstract:

Water pollution has become one of the most serious environmental problems. Multiple methods have been proposed for the removal of Pb(II) from contaminated water. Among these, adsorption processes have shown to be more efficient, cheaper and easier to handle with respect to other treatment methods. However, research for adsorbents with high adsorption capacities is still necessary. For this purpose, we proposed in this work the study of metal-organic Framework [Co2(btec)(bipy)(DMF)2]n (MOF-Co) as adsorbent material of Pb (II) in aqueous media. MOF-Co was synthesized by a simple method. Firstly 4, 4’ dipyridyl, 1,2,4,5 benzenetetracarboxylic acid, cobalt (II) and nitrate hexahydrate were first mixed each one in N,N dimethylformamide (DMF) and then, mixed in a reactor altogether. The obtained solution was heated at 363 K in a muffle during 68 h to complete the synthesis. It was washed and dried, obtaining MOF-Co as the final product. MOF-Co was characterized before and after the adsorption process by Fourier transforms infrared spectra (FTIR) and X-ray photoelectron spectroscopy (XPS). The Pb(II) in aqueous media was detected by Absorption Atomic Spectroscopy (AA). In order to evaluate the adsorption process in the presence of Pb(II) in aqueous media, the experiments were realized in flask of 100 ml the work volume at 200 rpm, with different MOF-Co quantities (0.0125 and 0.025 g), pH (2-6), contact time (0.5-6 h) and temperature (298,308 and 318 K). The kinetic adsorption was represented by pseudo-second order model, which suggests that the adsorption took place through chemisorption or chemical adsorption. The best adsorption results were obtained at pH 5. Langmuir, Freundlich and BET equilibrium isotherms models were used to study the adsorption of Pb(II) with 0.0125 g of MOF-Co, in the presence of different concentration of Pb(II) (20-200 mg/L, 100 mL, pH 5) with 4 h of reaction. The correlation coefficients (R2) of the different models show that the Langmuir model is better than Freundlich and BET model with R2=0.97 and a maximum adsorption capacity of 833 mg/g. Therefore, the Langmuir model can be used to best describe the Pb(II) adsorption in monolayer behavior on the MOF-Co. This value is the highest when compared to other materials such as the graphene/activated carbon composite (217 mg/g), biomass fly ashes (96.8 mg/g), PVA/PAA gel (194.99 mg/g) and MOF with Ag12 nanoparticles (120 mg/g).

Keywords: adsorption, heavy metals, metal-organic frameworks, Pb(II)

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