Search results for: Graphite Furnace Atomic Absorption Spectroscopy

Authors: Majid Afkhami, Maryam Ehsanpour, Zahra Khoshnood

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The concentrations of 10 heavy metals (Cd, Pb, Hg, Cu, Fe, Mn, Al, As, Ni, Zn) were measured in muscle, gill and liver of 6 species from Hormoz Strait in north coast of Persian Gulf in 12 months (April 2009 – March 2010). All samples were analyzed three times for Cd, Pb, Cu, Fe, Mn, Al, As, Ni, Zn by inductively coupled plasma-atomic emission spectrometry (ICP-AES) and for Hg by LECO AMA254 Advanced Mercury Analyzer. Results of this study showed that iron had the highest concentration (total mean concentration) in all species, followed by Zn, Cu, Ni, Al, Pb, Mn, Cd, Hg and lowest concentration in three tissues was As. In addition, the accumulation of metals was species-dependent, and was higher in Scomberomorous commerson and Scomberomorous guttatus (p<0.05) and the lowest concentration was record in Pampus argenteus (p<0.05).

Keywords: Persian Gulf, heavy metals, Hormoz strait, Scomberomorous guttatus, Scomberomorous commerson, Pampus argenteus

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Authors: Harpreet Singh Kainth

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Rubidium salts have been commonly used as an electrolyte to improve the efficiency cycle of Li-ion batteries. In recent years, it has been implemented into the large scale for further technological advances to improve the performance rate and better cyclability in the batteries. X-ray absorption spectroscopy (XAS) is a powerful tool for obtaining the information in the electronic structure which involves the chemical state analysis in the active materials used in the batteries. However, this technique is not well suited for the industrial applications because it needs a synchrotron X-ray source and special sample file for in-situ measurements. In contrast to this, conventional wavelength dispersive X-ray fluorescence (WDXRF) spectrometer is nondestructive technique used to study the chemical shift in all transitions (K, L, M, …) and does not require any special pre-preparation planning. In the present work, the fluorescent Lα, Lβ₁ , Lβ₃,₄ and Lγ₂,₃ X-ray spectra of rubidium in different chemical forms (Rb₂CO₃ , RbCl, RbBr, and RbI) have been measured first time with high resolution wavelength dispersive X-ray fluorescence (WDXRF) spectrometer (Model: S8 TIGER, Bruker, Germany), equipped with an Rh anode X-ray tube (4-kW, 60 kV and 170 mA). In ₃₇Rb compounds, the measured energy shifts are in the range (-0.45 to - 1.71) eV for Lα X-ray peak, (0.02 to 0.21) eV for Lβ₁ , (0.04 to 0.21) eV for Lβ₃ , (0.15 to 0.43) eV for Lβ₄ and (0.22 to 0.75) eV for Lγ₂,₃ X-ray emission lines. The chemical shifts in rubidium compounds have been measured by considering Rb₂CO₃ compounds taking as a standard reference. A Voigt function is used to determine the central peak position of all compounds. Both positive and negative shifts have been observed in L shell emission lines. In Lα X-ray emission lines, all compounds show negative shift while in Lβ₁, Lβ₃,₄, and Lγ₂,₃ X-ray emission lines, all compounds show a positive shift. These positive and negative shifts result increase or decrease in X-ray energy shifts. It looks like that ligands attached with central metal atom attract or repel the electrons towards or away from the parent nucleus. This pulling and pushing character of rubidium affects the central peak position of the compounds which causes a chemical shift. To understand the chemical effect more briefly, factors like electro-negativity, line intensity ratio, effective charge and bond length are responsible for the chemical state analysis in rubidium compounds. The effective charge has been calculated from Suchet and Pauling method while the line intensity ratio has been calculated by calculating the area under the relevant emission peak. In the present work, it has been observed that electro-negativity, effective charge and intensity ratio (Lβ₁/Lα, Lβ₃,₄/Lα and Lγ₂,₃/Lα) are inversely proportional to the chemical shift (RbCl > RbBr > RbI), while bond length has been found directly proportional to the chemical shift (RbI > RbBr > RbCl).

Keywords: chemical shift in L emission lines, bond length, electro-negativity, effective charge, intensity ratio, Rubidium compounds, WDXRF spectrometer

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Authors: Itti Bist, Snehasis Bhakta, Di Jiang, Tia E. Keyes, Aaron Martin, Robert J. Forster, James F. Rusling

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DNA damage from metabolites of lipophilic drugs and pollutants, generated by enzymes, represents a major toxicity pathway in humans. These metabolites can react with DNA to form either 8-oxo-7,8-dihydro-2-deoxyguanosine (8-oxodG), which is the oxidative product of DNA or covalent DNA adducts, both of which are genotoxic and hence considered important biomarkers to detect cancer in humans. Therefore, detecting reactions of metabolites with DNA is an effective approach for the safety assessment of new chemicals and drugs. Here we describe a novel electrochemiluminescent (ECL) sensor array which can detect DNA oxidation and chemical DNA damage in a single array, facilitating a more accurate diagnostic tool for genotoxicity screening. Layer-by-layer assembly of DNA and enzyme are assembled on the pyrolytic graphite array which is housed in a microfluidic device for sequential detection of two type of the DNA damages. Multiple enzyme reactions are run on test compounds using the array, generating toxic metabolites in situ. These metabolites react with DNA in the films to cause DNA oxidation and chemical DNA damage which are detected by ECL generating osmium compound and ruthenium polymer, respectively. The method is further validated by the formation of 8-oxodG and DNA adduct using similar films of DNA/enzyme on magnetic bead biocolloid reactors, hydrolyzing the DNA, and analyzing by liquid chromatography-mass spectrometry (LC-MS). Hence, this combined DNA/enzyme array/LC-MS approach can efficiently explore metabolic genotoxic pathways for drugs and environmental chemicals.

Keywords: biosensor, electrochemiluminescence, DNA damage, microfluidic array

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Authors: Akarsh Verma, Avinash Parashar

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The aim of this article is to study the effects of hydroxyl functional group on the mechanical strength and fracture toughness of graphene. This functional group forms the backbone of intrinsic atomic structure of graphene oxide (GO). Molecular dynamics-based simulations were performed in conjunction with reactive force field (ReaxFF) parameters to capture the mode-I fracture toughness of hydroxyl functionalised graphene. Moreover, these simulations helped in concluding that spatial distribution and concentration of hydroxyl functional group significantly affects the fracture morphology of graphene nanosheet. In contrast to literature investigations, atomistic simulations predicted a transition in the failure morphology of hydroxyl functionalised graphene from brittle to ductile as a function of its spatial distribution on graphene sheet.

Keywords: graphene, graphene oxide, ReaxFF, molecular dynamics

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Authors: Hadiatullah, T. S. D. Desak Ketut, A. A. Ayu, A. N. Isna, D. P. Ririn

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Spirogyra sp. is genus of microalgae which has a high carbohydrate content that used as a best medium for bacterial fermentation to produce cellulose. This study objective to determine the effect of pulp banana in the fermented paper production process using Spirogyra sp. and characterizing of the paper product. The method includes the production of bacterial cellulose, assay of the effect fermented paper interpolating with banana pulp using Spirogyra sp., and the assay of paper characteristics include gram-mage paper, water assay absorption, thickness, power assay of tensile resistance, assay of tear resistance, density, and organoleptic assay. Experiments were carried out with completely randomized design with a variation of the concentration of sewage treatment in the fermented paper production interpolating banana pulp using Spirogyra sp. Each parameter data to be analyzed by Anova variance that continued by real difference test with an error rate of 5% using the SPSS. Nata production results indicate that different carbon sources (glucose and sugar) did not show any significant differences from cellulose parameters assay. Significantly different results only indicated for the control treatment. Although not significantly different from the addition of a carbon source, sugar showed higher potency to produce high cellulose. Based on characteristic assay of the fermented paper showed that the paper gram-mage indicated that the control treatment without interpolation of a carbon source and a banana pulp have better result than banana pulp interpolation. Results of control gram-mage is 260 gsm that show optimized by cardboard. While on paper gram-mage produced with the banana pulp interpolation is about 120-200 gsm that show optimized by magazine paper and art paper. Based on the density, weight, water absorption assays, and organoleptic assay of paper showing the highest results in the treatment of pulp banana interpolation with sugar source as carbon is 14.28 g/m2, 0.02 g and 0.041 g/cm2.minutes. The conclusion found that paper with nata material interpolating with sugar and banana pulp has the potential formulation to produce super-quality paper.

Keywords: cellulose, fermentation, grammage, paper, Spirogyra sp.

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Authors: A. T. Toci, M. V. B. Zanoni

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The advanced oxidation processes have been defined as destructive technologies treatment of wastewater. These involve the formation of powerful oxidizing agents (usually hydroxyl radical .OH) capable of reacting with organic compounds present in wastewater, transforming damaging substances in CO2 and H2O (mineralization) or other innocuous products. However, the photochemical degradation with singlet oxygen has been little explored as oxidative pathway for the treatment of effluents containing food colorants. The molecular oxygen is an effective suppressor of organic molecules in the triplet excited state. One of the possible results of the physical withdrawal is the formation of singlet oxygen. Studies with singlet oxygen (1O2) show an high reactivity of the excited state of the molecule with olefins, aromatic hydrocarbons and a number of other organic and inorganic compounds. Its reactivity is about 2500 times larger than the oxygen in the ground state. Thus, in this work, it was studied the degradation of some dyes used in food industry (tartrazine, sunset yellow, erythrosine and carmoisine) by singlet oxygen. The sensitizer used for generating the 1O2 was methylene blue, which has a quantum yield generation of 0.50. Samples were prepared in water at a concentration of 5 ppm and irradiated with a sunlight simulator (Newport brand, model no. 67005) by consecutive 8h. The absorption spectra of UV-Vis molecules were made each hour irradiation. The degradation kinetics for each dye was determined using the maximum length of each dye absorption. The analysis by UV-Vis revealed that the processes were very efficient for the colorants sunset yellow and carmoisine. Both presented degradation kinetics of order zero with degradation constants 0.416 and 0.104, respectively. In the case of sunset yellow degradation reached 53% after 7h irradiation, Demonstrating the process efficiency. The erithrosine presented during the period irradiated a oscillating degradation kinetics, which requires further study. In the other hand, tartrazine was stable in the presence of 1O2. The investigation of the dyes degradation products owned degradation by 1O2 are underway, the techniques used for this are MS and NMR. The results of this study will enable the application of the cleanest methods for the treatment of industrial effluents, as there are other non-toxic and polluting molecules to generate 1O2.

Keywords: food colourants, singlet oxygen, degradation, wastewater, oxidative

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Authors: C. Lanzerstorfer

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The off-gas from the basic oxygen furnace (BOF), where pig iron is converted into steel, is treated in the primary ventilation system. This system is in full operation only during oxygen-blowing when the BOF converter vessel is in a vertical position. When pig iron and scrap are charged into the BOF and when slag or steel are tapped, the vessel is tilted. The generated emissions during charging and tapping cannot be captured by the primary off-gas system. To capture these emissions, a secondary ventilation system is usually installed. The emissions are captured by a canopy hood installed just above the converter mouth in tilted position. The aim of this study was to investigate the dependence of Zn and other components on the particle size of BOF secondary ventilation dust. Because of the high temperature of the BOF process it can be expected that Zn will be enriched in the fine dust fractions. If Zn is enriched in the fine fractions, classification could be applied to split the dust into two size fractions with a different content of Zn. For this air classification experiments with dust from the secondary ventilation system of a BOF were performed. The results show that Zn and Pb are highly enriched in the finest dust fraction. For Cd, Cu and Sb the enrichment is less. In contrast, the non-volatile metals Al, Fe, Mn and Ti were depleted in the fine fractions. Thus, air classification could be considered for the treatment of dust from secondary BOF off-gas cleaning.

Keywords: air classification, converter dust, recycling, zinc

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Authors: Naamane Remita, Mohammed laïd Mechri, Nouredine Zekri, Smaïl Chihi

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The goal of this study is the estimation real and imaginary components of both electrical impedance and permittivity z', z'' and ε', ε'' respectively, in Ouargla dunes sand at different temperatures and different frequencies, with alternating current (AC) equal to 1 volt, using the impedance spectroscopy (IS). This method is simple and non-destructive. the results can frequently be correlated with a number of physical properties, dielectric properties and the impacts of the composition on the electrical conductivity of solids. The experimental results revealed that the real part of impedance is higher at higher temperature in the lower frequency region and gradually decreases with increasing frequency. As for the high frequencies, all the values of the real part of the impedance were positive. But at low frequency the values of the imaginary part were positive at all temperatures except for 1200 degrees which were negative. As for the medium frequencies, the reactance values were negative at temperatures 25, 400, 200 and 600 degrees, and then became positive at the rest of the temperatures. At high frequencies of the order of MHz, the values of the imaginary part of the electrical impedance were in contrast to what we recorded for the middle frequencies. The results showed that the electrical permittivity decreases with increasing frequency, at low frequency we recorded permittivity values of 10+ 11, and at medium frequencies it was 10+ 07, while at high frequencies it was 10+ 02. The values of the real part of the electrical permittivity were taken large values at the temperatures of 200 and 600 degrees Celsius and at the lowest frequency, while the smallest value for the permittivity was recorded at the temperature of 400 degrees Celsius at the highest frequency. The results showed that there are large values of the imaginary part of the electrical permittivity at the lowest frequency and then it starts decreasing as the latter increases (the higher the frequency the lower the values of the imaginary part of the electrical permittivity). The character of electrical impedance variation indicated an opportunity to realize the polarization of Ouargla dunes sand and acquaintance if this compound consumes or produces energy. It’s also possible to know the satisfactory of equivalent electric circuit, whether it’s miles induction or capacitance.

Keywords: electrical impedance, electrical permittivity, temperature, impedance spectroscopy, dunes sand ouargla

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Authors: Vidya Yadav

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Migration is the demographic process that links rural to urban areas, generating or spurring the growth of cities. Evidence shows the role of the city as a production processes. It looks the city as a power of centre, and a centre of change. It has been observed that not only the professionals want to settle down in an urban area but rural labourers are also coming to cities for employment. These are the people who are compelled to migrate to metropolises because of lack of employment opportunities in their place of residence. However, the cities also fail to provide adequate employment because of limited job opportunity creation and capital-intensive industrialization. So these masses of incoming migrants are force to take up whatever employment absorption is available to them particularly in urban informal activities. Ultimately with this informal job they are compelled to stay in the slum areas, which is another form of deprived housing colonies. The paper seeks to examine the evidences of poverty induced migration from rural to urban areas (particularly in urban agglomeration). The present paper utilizes an abundant rich source of census migration data (D-Series) of 1991-2001. Result shows that Mumbai remain as the most attractive place to migrate. The migrants are mainly from the major states like Uttar Pradesh, Bihar, West Bengal, Jharkhand, Odisha, and Rajasthan. Male dominated migration is related mostly for employment and females due to marriages. The picture of occupational absorption of migrants who moved for employment, cross classified with educational status. Result shows that illiterate males are primarily engaged in low grade production processing work. Illiterate’s females engaged in service sectors; but these are actually very low grade services in urban informal sectors in India like maid servants, domestic help, hawkers, vendors or vegetables sellers. Among the higher educational level, a small percentage of males and females got absorbed in professional or clerical work but the percentage has been increased in the period 1991-2001.

Keywords: informal, job, migration, urban

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Authors: Przemyslaw Brzyski, Stanislaw Fic

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Hydrated lime, because of the life cycle (return to its natural form as a result of the setting and hardening) has a positive environmental impact. The lime binder is used in mortars. Lime is a slow setting binder with low mechanical properties. The aim of the study was to evaluate the possibility of improving the properties of the lime binder by using different pozzolanic materials as partial replacement of hydrated lime binder. Pozzolan materials are the natural or industrial waste, so do not affect the environmental impact of the lime binder. The following laboratory tests were performed: the analysis of the physical characteristics of the tested samples of lime mortars (bulk density, porosity), flexural and compressive strength, water absorption and the capillary rise of samples and consistency of fresh mortars. As a partial replacement of hydrated lime (in the amount of 10%, 20%, 30% by weight of lime) a metakaolin, silica fume, and zeolite were used. The shortest setting and hardening time showed mortars with the addition of metakaolin. All additives noticeably improved strength characteristic of lime mortars. With the increase in the amount of additive, the increase in strength was also observed. The highest flexural strength was obtained by using the addition of metakaolin in an amount of 20% by weight of lime (2.08 MPa). The highest compressive strength was obtained by using also the addition of metakaolin but in an amount of 30% by weight of lime (9.43 MPa). The addition of pozzolan caused an increase in the mortar tightness which contributed to the limitation of absorbability. Due to the different surface area, pozzolanic additives affected the consistency of fresh mortars. Initial consistency was assumed as plastic. Only the addition of silica fume an amount of 20 and 30% by weight of lime changed the consistency to the thick-plastic. The conducted study demonstrated the possibility of applying lime mortar with satisfactory properties. The features of lime mortars do not differ significantly from cement-based mortar properties and show a lower environmental impact due to CO₂ absorption during lime hardening. Taking into consideration the setting time, strength and consistency, the best results can be obtained with metakaolin addition to the lime mortar.

Keywords: lime, binder, mortar, pozzolan, properties

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Authors: Peng Hao Wang, Ronald Sterkenburg, Garam Kim, Yuwei He

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As composite materials continue to gain popularity in the aerospace industry; large airframe sections made out of composite materials are becoming the standard for aerospace manufacturers. However, the heavy utilization of these composite materials also increases the importance of the recycling of these composite materials. A team of Purdue University School of Aviation and Transportation Technology (SATT) faculty and students have partnered to investigate the characteristics of 3D printed recycled carbon fiber. A prototype of a 3D printed recycled carbon fiber part was provided by an industry partner and different sections of the prototype were used to create specimens. A furnace was utilized in order to remove the polymer from the specimens and the specimen’s fiber content and fiber length was calculated from the remaining fibers. A differential scanning calorimetry (DSC) and dynamic mechanical analysis (DMA) test was also conducted on the 3D printed recycled carbon fiber prototype in order to determine the prototype’s degree of cure at different locations. The data collected from this study provided valuable information in the process improvement and understanding of 3D printed recycled carbon fiber.

Keywords: 3D printed, carbon fiber, fiber content, recycling

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Authors: Tahani H. Alluhaybi, Leila Mejrissi

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In the present theoretical study, we investigated adiabatically the electronic structure of the (BaNa)+ by the use of the ab initio calculation. We optimized a large atomic GTO basis set for Na and Ba atoms. The (BaNa)+ molecular ion is considered a two-electron thank to a non-empirical pseudo-potentials approach applied to Ba and Na cores with the Core Polarization Potentials operator (CPP). Then, we performed the Full Configuration Interaction (FCI) method. Accordingly, we calculated the adiabatic Potential Energy Curves (PECs) and their spectroscopic constants (well depth De, transition energies Te, the equilibrium distances Re, vibrational constant ⍵e, and anharmonic constant ⍵exe) for 10 electronic states in Σ+ symmetry. Then we determined the vibrational level energies and their spacing, and the electric Permanent Dipole Moments (PDM).

Keywords: Ab initio, dipole moment, non-empirical pseudo-potential, potential energy curves, spectroscopic constants, vibrational energy

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Authors: S. Kohestani, R. Amrollahi, P. Daryabor

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Microwave diagnostics such as reflectometry are receiving growing attention in magnetic confinement fusionresearch. In order to obtain the better understanding of plasma confinement physics, more detailed measurements on density profile and its fluctuations might be required. A 2D full-wave simulation of ordinary mode propagation has been written in an effort to model effects seen in reflectometry experiment. The code uses the finite-difference-time-domain method with a perfectly-matched-layer absorption boundary to solve Maxwell’s equations.The code has been used to simulate the reflectometer measurement in Alborz Tokamak.

Keywords: reflectometry, simulation, ordinary mode, tokamak

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Authors: Mustapha A. Tijjani, Fanna I. Abdulrahman, Irfan Z. Khan, Umar K. Sandabe, Cong Li

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Air dried sample V. doniana after collection and identification was extracted with ethanol and further partition with chloroform, ethyl acetate and n-butanol. Ethanolic extract (11.9g) was fractionated on a silica gel accelerated column chromatography using solvents such as n-hexane, ethyl acetate and methanol. Each eluent fractions (150ml aliquots) were collected and monitored with thin layer chromatography. Fractions with similar Rf values from same solvents system were pooled together. Phytochemical test of all the fractions were performed using standard procedure. Complete elution yielded 48 fractions (150ml/fraction) which were pooled to 24 fractions base on the Rf values. It was further recombined and 12 fractions were obtained on the basis on Rf values and coded Vd1 to Vd12 fractions. Vd8 was further eluted with ethylacetate and methanol and gave fourteen sub fractions Vd8-a, -Vd8-m. Fraction Vd8-a (56mg) gave a white crystal compound coded V1. It was further checked on TLC and observed under ultraviolet lamp and was found to give a single spot. The Rf values were calculated to be 0.433. The melting point was determined using Gallenkamp capillary melting point apparatus and found to be 241-243°C uncorrected. Characterization of the isolated compound coded V1 was done using FT-infra-red spectroscopy, HNMR, 13CNMR(1and 2D) and HRESI-MS. The IR spectrum of compound V1 shows prominent peaks that corresponds to OHstr (3365cm-1) and C=0 (1652cm-1) etc. This spectrum suggests that among the functional moiety in compound V1 are the carbonyl and hydroxyl group. The 1H NMR (400 MHz) spectrum of compound V1 in DMSO-d6 displayed five singlet signals at δ 0.72 (3H, s, H-18), 0.79 (3H, s, H-19), 1.03 (3H, s, H-21), 1.04 (3H, s, H-26), 1.06 (3H, s, H-27) each integrating for three protons indicating the five methyl functional groups present in the compound. It further showed a broad singlet at δ 5.58 integrated for 1 H due to an olefinic H-atom adjacent to the carbonyl carbon atom. Three signals at δ 3.10 (d, J = 9.0 Hz, H-22), 3.59 (m, 1H, 2H-a) and 3.72 (m, 1H, 3H-e), each integrating for one proton is due to oxymethine protons indicating that three oxymethine H-atoms are present in the compound. These all signals are characteristic to the ecdysteroid skeletons. The 13C-NMR spectrum showed the presence of 27 carbon atoms, suggesting that may be steroid skeleton. The DEPT-135 experiment showed the presence of five CH3, eight CH2, and seven CH groups, and seven quaternary C-atoms. The molecular formula was established as C27H44O7 by high resolution electron spray ionization-mass spectroscopy (HRESI-MS) positive ion mode m/z 481.3179. The signals in mass spectrum are 463, 445, and 427 peaks corresponding to losses of one, two, three, or four water molecules characteristic for ecdysterone skeleton reported in the literature. Based on the spectral analysis (HNMR, 13CNMR, DEPT, HMQC, IR, HRESI-MS) the compound V1 is thus concluded to have ecdysteriod skeleton and conclusively conforms with 2β, 3β 14α, 20R, 22R, 25-hexahydroxy-5 β cholest-7-ene-6- one, or 2, 3, 14, 20, 22, 25 hexahydroxy cholest-7-ene-6-one commonly known as 20-hydroxyecdysone.

Keywords: vitex, phytochemical, purification, isolation, chromatography, spectroscopy

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Authors: Moataz Medhat, Essam Khalil, Hatem Haridy

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The present study investigates the flame structure of turbulent diffusion flame of synthesis fuel in a 300 KW swirl-stabilized burner. The three-dimensional model adopts a realizable k-ε turbulent scheme interacting with two-dimensional PDF combustion scheme by applying flamelet concept. The study reveals more characteristics on turbulent diffusion flame of synthesis fuel when changing the inlet air swirl number and the burner quarl angle. Moreover, it concerns with studying the effect of flue gas recirculation and staging with taking radiation effect into consideration. The comparison with natural gas was investigated. The study showed two zones of recirculation, the primary one is at the center of the furnace, and the location of the secondary one varies by changing the quarl angle of the burner. The results revealed an increase in temperature in the external recirculation zone as a result of increasing the swirl number of the inlet air stream. Also, it was found that recirculating part of the combustion products decreases pollutants formation especially nitrogen monoxide. The predicted results showed a great agreement when compared with the experiments.

Keywords: gas turbine, syngas, analysis, recirculation

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Authors: Sheraz Gul

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The requirements for progressing a compound to clinical trials is well established and relies on the results from in-vitro and in-vivo animal tests to indicate that it is likely to be safe and efficacious when testing in humans. The typical data package required will include demonstrating compound safety, toxicity, bioavailability, pharmacodynamics (potential effects of the compound on body systems) and pharmacokinetics (how the compound is potentially absorbed, distributed, metabolised and eliminated after dosing in humans). If the desired criteria are met and the compound meets the clinical Candidate criteria and is deemed worthy of further development, a submission to regulatory bodies such as the US Food & Drug Administration for an exploratory Investigational New Drug Study can be made. The purpose of this study is to collect data to establish that the compound will not expose humans to unreasonable risks when used in limited, early-stage clinical studies in patients or normal volunteer subjects (Phase I). These studies are also designed to determine the metabolism and pharmacologic actions of the drug in humans, the side effects associated with increasing doses, and, if possible, to gain early evidence on their effectiveness. In order to reach the above goals, we have developed a pre-clinical high throughput Absorption, Distribution, Metabolism and Excretion–Toxicity (ADME–Toxicity) panel of assays to identify compounds that are likely to meet the Lead and Candidate compound acceptance criteria. This panel includes solubility studies in a range of biological fluids, cell viability studies in cancer and primary cell-lines, mitochondrial toxicity, off-target effects (across the kinase, protease, histone deacetylase, phosphodiesterase and GPCR protein families), CYP450 inhibition (5 different CYP450 enzymes), CYP450 induction, cardio-toxicity (hERG) and gene-toxicity. This panel of assays has been applied to multiple compound series developed in a number of projects delivering Lead and clinical Candidates and examples from these will be presented.

Keywords: absorption, distribution, metabolism and excretion–toxicity , drug discovery, food and drug administration , pharmacodynamics

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Authors: M. Bahgat, H. Hanafy, H. Al-Tassan

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Cluster formation is an essential phenomenon during direct reduction processes at shaft furnaces. Decreasing the reducing temperature to avoid this problem can cause a significant drop in throughput. In order to prevent sticking of pellets, a coating material basically inactive under the reducing conditions prevailing in the shaft furnace, should be applied to cover the outer layer of the pellets. In the present work, steel dust is used as coating material for iron ore pellets to explore dust coating effectiveness and determines the best coating conditions. Steel dust coating is applied for iron ore pellets in various concentrations. Dust slurry concentrations of 5.0-30% were used to have a coated steel dust amount of 1.0-5.0 kg per ton iron ore. Coated pellets with various concentrations were reduced isothermally in weight loss technique with simulated gas mixture to the composition of reducing gases at shaft furnaces. The influences of various coating conditions on the reduction behavior and the morphology were studied. The optimum reduced samples were comparatively applied for sticking index measurement. It was found that the optimized steel dust coating condition that achieve higher reducibility with lower sticking index was 30% steel dust slurry concentration with 3.0 kg steel dust/ton ore.

Keywords: reduction, ironmaking, steel dust, coating

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Authors: Nurudeen Afolami Ayeni, Kasali Adewale Bello

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Study of the effect of dye-resin complexation on the degree of dye absorption were carried out using Procion Blue MX-R to dye cotton fabric in the presence hexamethylol melamine (MR6) and its phosphate derivative (MPR4) for resination. The highest degree of dye exhaustion was obtained at 400C for 1 hour with the resinated fabric showing more affinity for the dye than the ordinary fibre. Improved fastness properties was recorded which show a relatively higher stability of dye-resin complex formed in the fibre.

Keywords: affinity, cotton, dyeing, reactive dye, resination

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Authors: Mercedes Bertotto, Marcelo Bello, Hector Goicoechea, Veronica Fusca

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The National Service of Agri-Food Health and Quality (SENASA), controls honey to detect contamination by synthetic or natural chemical substances and establishes and controls the traceability of the product. The utility of near-infrared spectroscopy for the detection of adulteration of honey with high fructose corn syrup (HFCS) was investigated. First of all, a mixture of different authentic artisanal Argentinian honey was prepared to cover as much heterogeneity as possible. Then, mixtures were prepared by adding different concentrations of high fructose corn syrup (HFCS) to samples of the honey pool. 237 samples were used, 108 of them were authentic honey and 129 samples corresponded to honey adulterated with HFCS between 1 and 10%. They were stored unrefrigerated from time of production until scanning and were not filtered after receipt in the laboratory. Immediately prior to spectral collection, honey was incubated at 40°C overnight to dissolve any crystalline material, manually stirred to achieve homogeneity and adjusted to a standard solids content (70° Brix) with distilled water. Adulterant solutions were also adjusted to 70° Brix. Samples were measured by NIR spectroscopy in the range of 650 to 7000 cm⁻¹. The technique of specular reflectance was used, with a lens aperture range of 150 mm. Pretreatment of the spectra was performed by Standard Normal Variate (SNV). The ant colony optimization genetic algorithm sample selection (ACOGASS) graphical interface was used, using MATLAB version 5.3, to select the variables with the greatest discriminating power. The data set was divided into a validation set and a calibration set, using the Kennard-Stone (KS) algorithm. A combined method of Potential Functions (PF) was chosen together with Partial Least Square Linear Discriminant Analysis (PLS-DA). Different estimators of the predictive capacity of the model were compared, which were obtained using a decreasing number of groups, which implies more demanding validation conditions. The optimal number of latent variables was selected as the number associated with the minimum error and the smallest number of unassigned samples. Once the optimal number of latent variables was defined, we proceeded to apply the model to the training samples. With the calibrated model for the training samples, we proceeded to study the validation samples. The calibrated model that combines the potential function methods and PLSDA can be considered reliable and stable since its performance in future samples is expected to be comparable to that achieved for the training samples. By use of Potential Functions (PF) and Partial Least Square Linear Discriminant Analysis (PLS-DA) classification, authentic honey and honey adulterated with HFCS could be identified with a correct classification rate of 97.9%. The results showed that NIR in combination with the PT and PLS-DS methods can be a simple, fast and low-cost technique for the detection of HFCS in honey with high sensitivity and power of discrimination.

Keywords: adulteration, multivariate analysis, potential functions, regression

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Authors: Josef Fládr, Jiří Němeček, Veronika Koudelková, Petr Bílý

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Mechanical parameters of cementitious composites differ quite significantly based on the composition of cement matrix. They are also influenced by mixing times and procedure. The research presented in this paper was aimed at identification of differences in microstructure of normal strength (NSC) and differently mixed high strength (HSC) cementitious composites. Scanning electron microscopy (SEM) investigation together with energy dispersive X-ray spectroscopy (EDX) phase analysis of NSC and HSC samples was conducted. Evaluation of interfacial transition zone (ITZ) between the aggregate and cement matrix was performed. Volume share, thickness, porosity and composition of ITZ were studied. In case of HSC, samples obtained by several different mixing procedures were compared in order to find the most suitable procedure. In case of NSC, ITZ was identified around 40-50% of aggregate grains and its thickness typically ranged between 10 and 40 µm. Higher porosity and lower share of clinker was observed in this area as a result of increased water-to-cement ratio (w/c) and the lack of fine particles improving the grading curve of the aggregate. Typical ITZ with lower content of Ca was observed only in one HSC sample, where it was developed around less than 15% of aggregate grains. The typical thickness of ITZ in this sample was similar to ITZ in NSC (between 5 and 40 µm). In the remaining four HSC samples, no ITZ was observed. In general, the share of ITZ in HSC samples was found to be significantly smaller than in NSC samples. As ITZ is the weakest part of the material, this result explains to large extent the improved mechanical properties of HSC compared to NSC. Based on the comparison of characteristics of ITZ in HSC samples prepared by different mixing procedures, the most suitable mixing procedure from the point of view of properties of ITZ was identified.

Keywords: electron diffraction spectroscopy, high strength concrete, interfacial transition zone, normal strength concrete, scanning electron microscopy

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Authors: Rosemary Anibogwu, Kavita Sharma, Karl De Jesus

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Sagebrush is an abundant and naturally occurring plant in the Intermountain West region of the United States. The plant contains an array of bioactive compounds such as flavonoids, terpenoids, sterols, and phenolic acids. It is important to identify and characterize these compounds because Native Americans use sagebrush as herbal medicine. These compounds are also utilized for preventing infection in wounds, treating headaches and colds, and possess antitumor properties. This research is an exploratory study on the sesquiterpene present in the leaves of sagebrush. The leaf foliage was extracted with 100 % chloroform and 100 % methanol. The percentage yield for the crude was considerably higher in chloroform. The Thin Layer Chromatography (TLC) analysis of the crude extracted unveiled a brown band at Rf = 0.25 and a dark brown band at Rf = 0.74, along with three unknown faint bands the 254 nm UV lamp. Furthermore, the two distinct brown (Achillin) and dark brown band (Hydroxyachillin) in TLC were further utilized in the isolation of pure compounds with column chromatography. The structures of Achillin and Hydroxyachillin were elucidated based on extensive spectroscopic analysis, including TLC, High-Performance Liquid Chromatography (HPLC), 1D- and 2D-Nuclear Magnetic Resonance (NMR), and Mass Spectroscopy (MS). The antioxidant activities of crude extract and three pure compounds were evaluated in terms of their peroxyl radical scavenging by Ferric Reducing Ability of Plasma (FRAP) and 1,1-Diphenyl-2-picryl-hydrazyl (DPPH) methods. The crude extract showed the antioxidant activity of 18.99 ± 0.51 µmol TEg -1 FW for FRAP and 11.59 ± 0.38 µmol TEg -1 FW for DPPH. The activities of Achillin, Hydroxyachillin, and Quercetagetin trimethyl ether were 13.03, 15.90 and 14.02 µmol TEg -1 FW respectively for the FRAP assay. The three purified compounds have been submitted to the National Cancer Institute 60 cancer cell line for further study.

Keywords: HPLC, nuclear magnetic resonance spectroscopy, sagebrush, sesquiterpene lactones

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Authors: Haiming Wen, Isabella J. Van Rooyen

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Tristructural isotropic (TRISO)-coated fuel particles are designed as nuclear fuel for high-temperature gas reactors. TRISO coating consists of layers of carbon buffer, inner pyrolytic carbon (IPyC), SiC, and outer pyrolytic carbon. The TRISO coating, especially the SiC layer, acts as a containment system for fission products produced in the kernel. However, release of certain metallic fission products across intact TRISO coatings has been observed for decades. Despite numerous studies, mechanisms by which fission products migrate across the coating layers remain poorly understood. In this study, scanning transmission electron microscopy (STEM), energy dispersive X-ray spectroscopy (EDS), high-resolution transmission electron microscopy (HRTEM) and electron energy loss spectroscopy (EELS) were used to examine the distribution, composition and structure of fission products in a TRISO coated particle neutron irradiated to 3.6 x 1021 n/cm² fast fluence at 1040 ⁰C. Precession electron diffraction was used to investigate characters of grain boundaries where specific fission product precipitates are located. The retention fraction of 110mAg in the investigated TRISO particle was estimated to be 0.19. A high density of nanoscale fission product precipitates was observed in the SiC layer close to the SiC-IPyC interface, most of which are rich in Pd, while Ag was not identified. Some Pd-rich precipitates contain U. Precipitates tend to have complex structure and composition. Although a precipitate appears to have uniform contrast in STEM, EDS indicated that there may be composition variations throughout the precipitate, and HRTEM suggested that the precipitate may have several parts different in crystal structure or orientation. Attempts were made to measure charge states of precipitates using EELS and study their possible effect on precipitate transport.

Keywords: TRISO particle, fission product, nuclear fuel, electron microscopy, neutron irradiation

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Authors: A. Elsayed, M. H. Dewaidar, M. Ghali, M. Elkemary

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The high production cost of the conventional solar cells requires the search for economic methods suitable for solar energy conversion. Cadmium Sulfide (CdS) is one of the most important semiconductors used in photovoltaics, especially in large area solar cells; and can be prepared in a thin film form by a wide variety of deposition techniques. The preparation techniques include vacuum evaporation, sputtering and molecular beam epitaxy. Other techniques, based on chemical solutions, are also used for depositing CdS films with dramatically low-cost compared to other vacuum-based methods. Although this technique is widely used during the last decades, due to simplicity and low-deposition temperature (~100°C), there is still a strong need for more information on the growth process and its relation with the quality of the deposited films. Here, we report on deposition of high-quality CdS thin films; with low-surface roughness ( < 3.0 nm) and sharp optical absorption edge; on low-temperature glass substrates (70°C) using a new method based on the room-temperature chemical solution. In this method, a mixture solution of cadmium acetate and thiourea at room temperature was used under special growth conditions for deposition of CdS films. X-ray diffraction (XRD) measurements were used to examine the crystal structure properties of the deposited CdS films. In addition, UV-VIS transmittance and low-temperature (4K) photoluminescence (PL) measurements were performed for quantifying optical properties of the deposited films. The deposited films show high optical quality as confirmed by observation of both, sharp edge in the transmittance spectra and strong PL intensity at room temperature. Furthermore, we found a strong effect of the growth conditions on the optical band gap of the deposited films; where remarkable red-shift in the absorption edge with temperature is clearly seen in both transmission and PL spectra. Such tuning of both optical band gap of the deposited CdS films can be utilized for tuning the electronic bands' alignments between CdS and other light-harvesting materials, like CuInGaSe or CdTe, for potential improvement in the efficiency of solar cells devices based on these heterostructures.

Keywords: chemical deposition, CdS, optical properties, surface, thin film

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Authors: Paweł Strzępek, Małgorzata Zasadzińska, Szymon Kordaszewski, Wojciech Ściężor

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The constant tendency toward the materials properties improvement nowadays creates opportunities for the scientists, and furthermore the manufacturers all over the world to design, form and produce new alloys almost every day. Considering the fact that companies all over the world look for alloys with the highest values of mechanical properties coexisting with a reasonable electrical conductivity made it necessary to develop new materials based on copper, such as copper magnesium alloys with over 2 wt. % of Mg. Though, before such new material may be mass produced it must undergo a series of tests in order to determine the production technology and its parameters. The presented study is based on the numerical simulations calculated with the use of finite element method analysis, where the geometry of the cooling system, the material used to produce the cooling system and the surface quality of the graphite crystallizer at the place of contact with the cooling system and its influence on the temperatures throughout the continuous casting process is being investigated. The calculated simulations made it possible to propose the optimal set of equipment necessary for the continuous casting process to be carried out in laboratory conditions with various casting parameters and to determine basic materials properties of the obtained alloys such as hardness, electrical conductivity and homogeneity of the chemical composition. The authors are grateful for the financial support provided by The National Centre for Research and Development – Research Project No. LIDER/33/0121/L-11/19/NCBR/2020.

Keywords: CuMg alloys, continuous casting, temperature analysis, finite element method

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Authors: Ana Maria Igual-Munoz, Juan Gilabert, Marta Garcia, Alfredo Quijano-Lopez

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Nowadays, several lithium-ion battery technologies are being commercialized. These chemistries present different properties that make them more suitable for different purposes. However, comparative studies showing the advantages and disadvantages of different chemistries are incomplete or scarce. Different non-destructive techniques are currently being employed to detect how ageing affects the active materials of lithium-ion batteries (LIBs). For instance, electrochemical impedance spectroscopy (EIS) is one of the most employed ones. This technique allows the user to identify the variations on the different resistances present in LIBs. On the other hand, differential voltage analysis (DVA) has shown to be a powerful technique to detect the processes affecting the different capacities present in LIBs. This technique shows variations in the state of health (SOH) and the capacities for one or both electrodes depending on their chemistry. Finally, incremental capacity analysis (ICA) is a widely known technique for being capable of detecting phase equilibria. It reminds of the commonly used cyclic voltamperometry, as it allows detecting some reactions taking place in the electrodes. In these studies, a set of ageing procedures have been applied to commercial batteries of different chemistries (NCA, NMC, and LFP). Afterwards, results of EIS, DVA, and ICA have been used to correlate them with the processes affecting each cell. Ciclability, overpotential, and temperature cycling studies envisage how the charge-discharge rates, cut-off voltage, and operation temperatures affect each chemistry. These studies will serve battery pack manufacturers, as for common battery users, as they will determine the different conditions affecting cells for each of the chemistry. Taking this into account, each cell could be adjusted to the final purpose of the battery application. Last but not least, all the degradation parameters observed are focused to be integrated into degradation models in the future. This fact will allow the implementation of the widely known digital twins to the degradation in LIBs.

Keywords: lithium ion batteries, non-destructive analysis, different chemistries, ante-mortem studies, ICA, DVA, EIS

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Authors: Sevda Engin, Ugur Buyuk, Necmettin Marasli

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Directional solidification of eutectic alloys attracts considerable attention because of microhardness, tensile strength, and electrical resistivity influenced by eutectic structures. In this research, we examined processing of Al–Si–Fe (Al–11.7wt.%Si–1wt.%Fe) eutectic by directional solidification. The alloy was prepared by vacuum furnace and directionally solidified in Bridgman-type equipment. During the directional solidification process, the growth rates utilized varied from 8.25 m/s to 164.80 m/s. The Al–Si–Fe system showed an eutectic transformation, which resulted in the matrix Al, Si and Al5SiFe plate phases. The eutectic spacing between (λ_Si-λ_Si, λ_(Al_5 SiFe)-λ_(Al_5 SiFe)) was measured. Additionally, the microhardness, tensile strength, and electrical resistivity of the alloy were determined using directionally solidified samples. The effects of growth rates on microhardness, tensile strength, and electrical resistivity for directionally solidified Al–Si–Fe eutectic alloy were investigated, and the relationships between them were experimentally obtained. It was found that the microhardness, tensile strength, and electrical resistivity were affected by both eutectic spacing and the solidification parameter.

Keywords: directional solidification, aluminum alloy, microstructure, electrical properties, tensile test, hardness test

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Authors: Mariana-Dana Damaceanu

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Electrochemical oxidation is one of the most convenient ways to obtain conjugated polymer films as polypyrrole, polyaniline, polythiophene or polycarbazole. The research in the field has been mainly directed to the study of electrical conduction properties of the materials obtained by electropolymerization, often the main reason being their use as electroconducting electrodes, and very little attention has been paid to the morphological and optical quality of the films electrodeposited on flat surfaces. Electropolymerization of the monomer solution was scarcely used in the past to manufacture polymer-based light-emitting diodes (PLED), most probably due to the difficulty of obtaining defectless polymer films with good mechanical and optical properties, or conductive polymers with well controlled molecular weights. Here we report our attempts in using electrochemical deposition as appropriate method for preparing ultrathin films of fluorene-based polymers for PLED applications. The properties of these films were evaluated in terms of structural morphology, optical properties, and electrochemical conduction. Thus, electropolymerization of 4,4'-(9-fluorenylidene)-dianiline was performed in dichloromethane solution, at a concentration of 10-2 M, using 0.1 M tetrabutylammonium tetrafluoroborate as electrolyte salt. The potential was scanned between 0 and 1.3 V on the one hand, and 0 - 2 V on the other hand, when polymer films with different structures and properties were obtained. Indium tin oxide-coated glass substrate of different size was used as working electrode, platinum wire as counter electrode and calomel electrode as reference. For each potential range 100 cycles were recorded at a scan rate of 100 mV/s. The film obtained in the potential range from 0 to 1.3 V, namely poly(FDA-NH), is visible to the naked eye, being light brown, transparent and fluorescent, and displays an amorphous morphology. Instead, the electrogrowth poly(FDA) film in the potential range of 0 - 2 V is yellowish-brown and opaque, presenting a self-assembled structure in aggregates of irregular shape and size. The polymers structure was identified by FTIR spectroscopy, which shows the presence of broad bands specific to a polymer, the band centered at approx. 3443 cm-1 being ascribed to the secondary amine. The two polymer films display two absorption maxima, at 434-436 nm assigned to π-π* transitions of polymers, and another at 832 and 880 nm assigned to polaron transitions. The fluorescence spectra indicated the presence of emission bands in the blue domain, with two peaks at 422 and 488 nm for poly (FDA-NH), and four narrow peaks at 422, 447, 460 and 484 nm for poly(FDA), peaks originating from fluorene-containing segments of varying degrees of conjugation. Poly(FDA-NH) exhibited two oxidation peaks in the anodic region and the HOMO energy value of 5.41 eV, whereas poly(FDA) showed only one oxidation peak and the HOMO level localized at 5.29 eV. The electrochemical data are discussed in close correlation with the proposed chemical structure of the electrogrowth films. Further research will be carried out to study their use and performance in light-emitting devices.

Keywords: electrogrowth polymer films, fluorene, morphology, optical properties

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Authors: M. Naveed Yasin, Robert Brooke, Andrew Chan, Geoffrey I. N. Waterhouse, Drew Evans, Darren Svirskis, Ilva D. Rupenthal

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Poly(3,4-ethylenedioxythiophene) (PEDOT) is a robust conducting polymer (CP) exhibiting high conductivity and environmental stability. It can be synthesized by either chemical, electrochemical or vapour phase polymerization (VPP). Dexamethasone sodium phosphate (dexP) is an anionic drug molecule which has previously been loaded onto PEDOT as a dopant via electrochemical polymerisation; however this technique requires conductive surfaces from which polymerization is initiated. On the other hand, VPP produces highly organized biocompatible CP structures while polymerization can be achieved onto a range of surfaces with a relatively straight forward scale-up process. Following VPP of PEDOT, dexP can be loaded and subsequently released via ion-exchange. This study aimed at preparing and characterising both non-porous and porous VPP PEDOT structures including examining drug loading and release via ion-exchange. Porous PEDOT structures were prepared by first depositing a sacrificial polystyrene (PS) colloidal template on a substrate, heat curing this deposition and then spin coating it with the oxidant solution (iron tosylate) at 1500 rpm for 20 sec. VPP of both porous and non-porous PEDOT was achieved by exposing to monomer vapours in a vacuum oven at 40 mbar and 40 °C for 3 hrs. Non-porous structures were prepared similarly on the same substrate but without any sacrificial template. Surface morphology, compositions and behaviour were then characterized by atomic force microscopy (AFM), scanning electron microscopy (SEM), x-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV) respectively. Drug loading was achieved by 50 CV cycles in a 0.1 M dexP aqueous solution. For drug release, each sample was exposed to 20 mL of phosphate buffer saline (PBS) placed in a water bath operating at 37 °C and 100 rpm. Film was stimulated (continuous pulse of ± 1 V at 0.5 Hz for 17 mins) while immersed into PBS. Samples were collected at 1, 2, 6, 23, 24, 26 and 27 hrs and were analysed for dexP by high performance liquid chromatography (HPLC Agilent 1200 series). AFM and SEM revealed the honey comb nature of prepared porous structures. XPS data showed the elemental composition of the dexP loaded film surface, which related well with that of PEDOT and also showed that one dexP molecule was present per almost three EDOT monomer units. The reproducible electroactive nature was shown by several cycles of reduction and oxidation via CV. Drug release revealed success in drug loading via ion-exchange, with stimulated porous and non-porous structures exhibiting a proof of concept burst release upon application of an electrical stimulus. A similar drug release pattern was observed for porous and non-porous structures without any significant statistical difference, possibly due to the thin nature of these structures. To our knowledge, this is the first report to explore the potential of VPP prepared PEDOT for stimuli-responsive drug delivery via ion-exchange. The produced porous structures were ordered and highly porous as indicated by AFM and SEM. These porous structures exhibited good electroactivity as shown by CV. Future work will investigate porous structures as nano-reservoirs to increase drug loading while sealing these structures to minimize spontaneous drug leakage.

Keywords: PEDOT for ion-exchange drug delivery, stimuli-responsive drug delivery, template based porous PEDOT structures, vapour phase polymerization of PEDOT

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Authors: Ramzi Farra, Detre Teschner, Marc Willinger, Robert Schlögl

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Introduction: The conventional approach of characterizing solid catalysts under static conditions, i.e., before and after reaction, does not provide sufficient knowledge on the physicochemical processes occurring under dynamic conditions at the molecular level. Hence, the necessity of improving new in situ characterizing techniques with the potential of being used under real catalytic reaction conditions is highly desirable. In situ Prompt Gamma Activation Analysis (PGAA) is a rapidly developing chemical analytical technique that enables us experimentally to assess the coverage of surface species under catalytic turnover and correlate these with the reactivity. The catalytic HCl oxidation (Deacon reaction) over bulk ceria will serve as our example. Furthermore, the in situ Transmission Electron Microscopy is a powerful technique that can contribute to the study of atmosphere and temperature induced morphological or compositional changes of a catalyst at atomic resolution. The application of such techniques (PGAA and TEM) will pave the way to a greater and deeper understanding of the dynamic nature of active catalysts. Experimental/Methodology: In situ Prompt Gamma Activation Analysis (PGAA) experiments were carried out to determine the Cl uptake and the degree of surface chlorination under reaction conditions by varying p(O2), p(HCl), p(Cl2), and the reaction temperature. The abundance and dynamic evolution of OH groups on working catalyst under various steady-state conditions were studied by means of in situ FTIR with a specially designed homemade transmission cell. For real in situ TEM we use a commercial in situ holder with a home built gas feeding system and gas analytics. Conclusions: Two complimentary in situ techniques, namely in situ PGAA and in situ FTIR were utilities to investigate the surface coverage of the two most abundant species (Cl and OH). The OH density and Cl uptake were followed under multiple steady-state conditions as a function of p(O2), p(HCl), p(Cl2), and temperature. These experiments have shown that, the OH density positively correlates with the reactivity whereas Cl negatively. The p(HCl) experiments give rise to increased activity accompanied by Cl-coverage increase (opposite trend to p(O2) and T). Cl2 strongly inhibits the reaction, but no measurable increase of the Cl uptake was found. After considering all previous observations we conclude that only a minority of the available adsorption sites contribute to the reactivity. In addition, the mechanism of the catalysed reaction was proposed. The chlorine-oxygen competition for the available active sites renders re-oxidation as the rate-determining step of the catalysed reaction. Further investigations using in situ TEM are planned and will be conducted in the near future. Such experiments allow us to monitor active catalysts at the atomic scale under the most realistic conditions of temperature and pressure. The talk will shed a light on the potential and limitations of in situ PGAA and in situ TEM in the study of catalyst dynamics.

Keywords: CeO2, deacon process, in situ PGAA, in situ TEM, in situ FTIR

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Authors: Anil Saini, Jatinder Kumar Ratan

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Now a day, the key issue for the scientific community is to devise the innovative technologies for sustainable control of urban pollution. In urban cities, a large surface area of the masonry structures, buildings, and pavements is exposed to the open environment, which may be utilized for the control of air pollution, if it is built from the photocatalytically active cement-based constructional materials such as concrete, mortars, paints, and blocks, etc. The photocatalytically active cement is formulated by incorporating a photocatalyst in the cement matrix, and such cement is generally known as self-cleaning cement In the literature, self-cleaning cement has been synthesized by incorporating nanosized-TiO₂ (n-TiO₂) as a photocatalyst in the formulation of the cement. However, the utilization of n-TiO₂ for the formulation of self-cleaning cement has the drawbacks of nano-toxicity, higher cost, and agglomeration as far as the commercial production and applications are concerned. The use of microsized-TiO₂ (m-TiO₂) in place of n-TiO₂ for the commercial manufacture of self-cleaning cement could avoid the above-mentioned problems. However, m-TiO₂ is less photocatalytically active as compared to n- TiO₂ due to smaller surface area, higher band gap, and increased recombination rate. As such, the use of m-TiO₂ in the formulation of self-cleaning cement may lead to a reduction in photocatalytic activity, thus, reducing the self-cleaning, depolluting, and antimicrobial abilities of the resultant cement material. So improvement in the photoactivity of m-TiO₂ based self-cleaning cement is the key issue for its practical applications in the present scenario. The current work proposes the use of surface-fluorinated m-TiO₂ for the formulation of self-cleaning cement to enhance its photocatalytic activity. The calcined dolomite, a constructional material, has also been utilized as co-adsorbent along with the surface-fluorinated m-TiO₂ in the formulation of self-cleaning cement to enhance the photocatalytic performance. The surface-fluorinated m-TiO₂, calcined dolomite, and the formulated self-cleaning cement were characterized using diffuse reflectance spectroscopy (DRS), X-ray diffraction analysis (XRD), field emission-scanning electron microscopy (FE-SEM), energy dispersive x-ray spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), BET (Brunauer–Emmett–Teller) surface area, and energy dispersive X-ray fluorescence spectrometry (EDXRF). The self-cleaning property of the as-prepared self-cleaning cement was evaluated using the methylene blue (MB) test. The depolluting ability of the formulated self-cleaning cement was assessed through a continuous NOX removal test. The antimicrobial activity of the self-cleaning cement was appraised using the method of the zone of inhibition. The as-prepared self-cleaning cement obtained by uniform mixing of 87% clinker, 10% calcined dolomite, and 3% surface-fluorinated m-TiO₂ showed a remarkable self-cleaning property by providing 53.9% degradation of the coated MB dye. The self-cleaning cement also depicted a noteworthy depolluting ability by removing 5.5% of NOx from the air. The inactivation of B. subtiltis bacteria in the presence of light confirmed the significant antimicrobial property of the formulated self-cleaning cement. The self-cleaning, depolluting, and antimicrobial results are attributed to the synergetic effect of surface-fluorinated m-TiO₂ and calcined dolomite in the cement matrix. The present study opens an idea and route for further research for acile and economical formulation of self-cleaning cement.

Keywords: microsized-titanium dioxide (m-TiO₂), self-cleaning cement, photocatalysis, surface-fluorination

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