Search results for: sulfur isotope

Authors: Tshipeng Mwenze, Charles Okujeni, Abdi Siad, Russel Bailie, Dirk Frei, Marcelene Voigt, Petrus Le Roux

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The Platreef is a platinum group element (PGE) deposit in the northern limb of the Bushveld Igneous Complex (BIC) which was emplaced as a series of mafic and ultramafic sills between the Main Zone (MZ) and the country rocks. The PGE mineralisation in the Platreef is hosted in different rock types, and its distribution and style vary with depth and along strike. This study contributes towards understanding the processes involved in the genesis of the Platreef. Twenty-four Platreef (2 harzburgites, 4 olivine pyroxenites, 17 feldspathic pyroxenites and 1 gabbronorite) and few MZ (1 gabbronorite and 1 leucogabbronorite) quarter core samples were collected from four drill cores (e.g., TN754, TN200, SS339, and OY482) and analysed for whole-rock Sr-Nd isotope data. The results show positive ɛNd values (+3.53 to +7.51) for harzburgites suggesting their parental magmas derived from the depleted Mantle. The remaining Platreef rocks have negative ɛNd values (-2.91 to -22.88) and show significant variations in Sr-Nd isotopic compositions. The first group of Platreef samples has relatively high isotopic compositions (ɛNd= -2.91 to -5.68; ⁸⁷Sr/⁸⁶Sri= 0.709177 - 0.711998). The second group of Platreef samples has Sr ratios (⁸⁷Sr/⁸⁶Sri= 0.709816-0.712106) overlapping with samples of the first group but slightly lower ɛNd values (-7.44 to -8.39). Lastly, the third group of Platreef samples has low ɛNd values (-10.82 to -14.32) and low Sr ratios (⁸⁷Sr/⁸⁶Sri= 0.707545-0.710042) than those from samples of the two Platreef groups mentioned above. There is, however, a Platreef sample with ɛNd value (-5.26) in range with the Platreef samples of the first group, but its Sr ratio (0.707281) is the lowest even when compared to samples of the third Platreef group. There are also five other Platreef samples which have either anomalous ɛNd or Sr ratios which make it difficult to assess their isotopic compositions relative to other samples. These isotopic variations for the Platreef samples indicate both multiple sources and multiple magma chambers where varying crustal contamination styles have operated during the evolution of these magmas prior their emplacements into the Platreef setting as sills. Furthermore, the MZ rocks have different Sr-Nd isotopic compositions (For OY482 gabbronorite [ɛNd= +0.65; ⁸⁷Sr/⁸⁶Sri= 0.711746]; for TN754 leucogabbronorite [ɛNd= -7.44; ⁸⁷Sr/⁸⁶Sri= 0.709322]) which do not only indicate different MZ magma chambers, but also different magmas from those of the Platreef. Although the Platreef is still considered a single stratigraphic unit in the northern limb of the BIC, its genesis involved multiple magmatic processes which evolved independently from each other.

Keywords: crustal contamination styles, magma chambers, magma sources, multiple sills emplacement

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Authors: Ajit Singh, Waliur Rahaman, Parmanand Sharma, Laluraj C. M., Lavkush Patel, Bhanu Pratap, Vinay Kumar Gaddam, Meloth Thamban

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The Himalayan glaciers are the potential source of perennial water supply to Asia’s major river systems like the Ganga, Brahmaputra and the Indus. In order to improve our understanding about the source of precipitation and hydrograph components in the interior Himalayan glaciers, it is important to decipher the sources of moisture and their contribution to the glaciers in this river system. In doing so, we conducted an extensive pilot study in a Sutri Dhaka glacier, western Himalaya during 2014-15. To determine the moisture sources, rain, surface snow, ice, and stream meltwater samples were collected and analyzed for stable oxygen (δ¹⁸O) and hydrogen (δD) isotopes. A two-component hydrograph separation was performed for the glacier stream using these isotopes assuming the contribution of rain, groundwater and spring water contribution is negligible based on field studies and available literature. To validate the results obtained from hydrograph separation using above method, snow and ice melt ablation were measured using a network of bamboo stakes and snow pits. The δ¹⁸O and δD in rain samples range from -5.3% to -20.8% and -31.7% to -148.4% respectively. It is noteworthy to observe that the rain samples showed enriched values in the early season (July-August) and progressively get depleted at the end of the season (September). This could be due to the ‘amount effect’. Similarly, old snow samples have shown enriched isotopic values compared to fresh snow. This could because of the sublimation processes operating over the old surface snow. The δ¹⁸O and δD values in glacier ice samples range from -11.6% to -15.7% and -31.7% to -148.4%, whereas in a Sutri Dhaka meltwater stream, it ranges from -12.7% to -16.2% and -82.9% to -112.7% respectively. The mean deuterium excess (d-excess) value in all collected samples exceeds more than 16% which suggests the predominant moisture source of precipitation is from the Western Disturbances. Our detailed estimates of the hydrograph separation of Sutri Dhaka meltwater using isotope hydrograph separation and glaciological field methods agree within their uncertainty; stream meltwater budget is dominated by glaciers ice melt over snowmelt. The present study provides insights into the sources of moisture, controlling mechanism of the isotopic characteristics of Sutri Dhaka glacier water and helps in understanding the snow and ice melt components in Chandra basin, Western Himalaya.

Keywords: D-excess, hydrograph separation, Sutri Dhaka, stable water isotope, western Himalaya

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Authors: Ryan Maclellan

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The nEXO Collaboration is designing a very large detector for neutrinoless double beta decay of Xe-136. The nEXO detector is rooted in the current EXO-200 program, which has reached a sensitivity for the half-life of the decay of 1.9x10^25 years with an exposure of 99.8 kg-y. The baseline nEXO design assumes 5 tonnes of liquid xenon, enriched in the mass 136 isotope, within a time projection chamber. The detector is being designed to reach a half-life sensitivity of > 5x10^27 years covering the inverted neutrino mass hierarchy, with 5 years of data. We present the nEXO detector design, the current status of R&D efforts, and the physics case for the experiment.

Keywords: double-beta, Majorana, neutrino, neutrinoless

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Authors: Medhanie Gebremedhin Gebru, Alex Schechter

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Dimethyl ether (DME) possesses several advantages over other small organic molecules such as methanol, ethanol, and ammonia in terms of providing higher energy density, being less toxic, and having lower Nafion membrane crossover. However, the absence of an active and stable catalyst has been the bottleneck that hindered the commercialization of direct DME fuel cells. A Vulcan XC72 carbon-supported ternary metal catalyst, Pt₃Pd₃Sn₂/C is reported to have yielded the highest specific power density (90 mW mg-¹PGM) as compared to other catalysts tested fordirect DME fuel cell (DDMEFC). However, the micropores and sulfur groups present in Vulcan XC72 hinder the fuel utilization by causing Pt agglomeration and sulfur poisoning. Vulcan XC72 having a high carbon sp³ hybridization content, is also prone to corrosion. Therefore, carbon supports such as multi-walled carbon nanotube (MWCNT), black pearl 2000 (BP2000), and their cold N2 plasma-treated counterpartswere tested to further enhance the activity of the catalyst, and the outputs with these carbons were compared with the originally used support. Detailed characterization of the pristine and carbon supports was conducted. Electrochemical measurements in three-electrode cells and laboratory prototype fuel cells were conducted.Pt₃Pd₃Sn₂/BP2000 exhibited excellent performance in terms of electrochemical active surface area (ECSA), peak current density (jp), and DME oxidation charge (Qoxi). The effect of the plasma activation on the activity improvement was observed only in the case of MWCNT while having little or no effect on the other carbons. A Pt₃Pd₃Sn₂ supported on the optimized mixture of carbons containing 75% plasma-activated MWCNT and 25% BP2000 (Pt₃Pd₃Sn₂/75M25B) provided the highest reported power density of 117 mW mg-1PGM using an anode loading of1.55 mgPGMcm⁻².

Keywords: DME, DDMEFC, ternary metal catalyst, carbon support, plasma activation

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Authors: Lijuan Li

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Nitric oxide (NO) has become a fascinating entity in biological chemistry over the past few years. It is a gaseous lipophilic radical molecule that plays important roles in several physiological and pathophysiological processes in mammals, including activating the immune response, serving as a neurotransmitter, regulating the cardiovascular system, and acting as an endothelium-derived relaxing factor. NO functions in eukaryotes both as a signal molecule at nanomolar concentrations and as a cytotoxic agent at micromolar concentrations. The latter arises from the ability of NO to react readily with a variety of cellular targets leading to thiol S-nitrosation, amino acid N-nitrosation, and nitrosative DNA damage. Nitric oxide can readily bind to metals to give metal-nitrosyl (M-NO) complexes. Some of these species are known to play roles in biological NO storage and transport. These complexes have different biological, photochemical, or spectroscopic properties due to distinctive structural features. These recent discoveries have spawned a great interest in the development of transition metal complexes containing NO, particularly its iron complexes that are central to the role of nitric oxide in the body. Spectroscopic evidence would appear to implicate species of “Fe(NO)2+” type in a variety of processes ranging from polymerization, carcinogenesis, to nitric oxide stores. Our research focuses on isolation and structural studies of non-heme iron nitrosyls that mimic biologically active compounds and can potentially be used for anticancer drug therapy. We have shown that reactions between Fe(NO)2(CO)2 and a series of imidazoles generated new non-heme iron nitrosyls of the form Fe(NO)2(L)2 [L = imidazole, 1-methylimidazole, 4-methylimidazole, benzimidazole, 5,6-dimethylbenzimidazole, and L-histidine] and a tetrameric cluster of [Fe(NO)2(L)]4 (L=Im, 4-MeIm, BzIm, and Me2BzIm), resulted from the interactions of Fe(NO)2 with a series of substituted imidazoles was prepared. Recently, a series of sulfur bridged iron di nitrosyl complexes with the general formula of [Fe(µ-RS)(NO)2]2 (R = n-Pr, t-Bu, 6-methyl-2-pyridyl, and 4,6-dimethyl-2-pyrimidyl), were synthesized by the reaction of Fe(NO)2(CO)2 with thiols or thiolates. Their structures and properties were studied by IR, UV-vis, 1H-NMR, EPR, electrochemistry, X-ray diffraction analysis and DFT calculations. IR spectra of these complexes display one weak and two strong NO stretching frequencies (νNO) in solution, but only two strong νNO in solid. DFT calculations suggest that two spatial isomers of these complexes bear 3 Kcal energy difference in solution. The paramagnetic complexes [Fe2(µ-RS)2(NO)4]-, have also been investigated by EPR spectroscopy. Interestingly, the EPR spectra of complexes exhibit an isotropic signal of g = 1.998 - 2.004 without hyperfine splitting. The observations are consistent with the results of calculations, which reveal that the unpaired electron dominantly delocalize over the two sulfur and two iron atoms. The difference of the g values between the reduced form of iron-sulfur clusters and the typical monomeric di nitrosyl iron complexes is explained, for the first time, by of the difference in unpaired electron distributions between the two types of complexes, which provides the theoretical basis for the use of g value as a spectroscopic tool to differentiate these biologically active complexes.

Keywords: di nitrosyl iron complex, metal nitrosyl, non-heme iron, nitric oxide

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Authors: Flora Elvistia Firdaus

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The chemical structure of soybean oils have to be chemically modified through its tryglyceride to attain resemblance properties with petrochemicals. Sulfur acid catalyst in peracetic acid co-reagent has good performance on modified soybean oil strucutures through its unsaturated fatty acid moiety to the desired hydroxyl functional groups. A series of screening reactions have indicated that the ratio of acetic/peroxide acid 1:7.25 (mol/mol) with temperature of 600°C for soy-epoxide synthesis are prevailed for up-scaling of bodied soybean into 10 and 20 folds from initials. A two-step process was conducted for the preparation of soy-polyol in designated temperatures.

Keywords: soybean, polyol, up-scaling, polyurethane

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Authors: F. Zouai, F. Z. Benabid, S. Bouhelal, D. Benachour

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Nanocomposite polymer / clay are relatively important area of research. These reinforced plastics have attracted considerable attention in scientific and industrial fields because a very small amount of clay can significantly improve the properties of the polymer. The polymeric matrices used in this work are two saturated polyesters ie polyethylene terephthalate (PET) and polyethylene naphthalate (PEN).The success of processing compatible blends, based on poly(ethylene terephthalate) (PET)/ poly(ethylene naphthalene) (PEN)/clay nanocomposites in one step by reactive melt extrusion is described. Untreated clay was first purified and functionalized ‘in situ’ with a compound based on an organic peroxide/ sulfur mixture and (tetramethylthiuram disulfide) as the activator for sulfur. The PET and PEN materials were first separately mixed in the molten state with functionalized clay. The PET/4 wt% clay and PEN/7.5 wt% clay compositions showed total exfoliation. These compositions, denoted nPET and nPEN, respectively, were used to prepare new n(PET/PEN) nanoblends in the same mixing batch. The n(PET/PEN) nanoblends were compared to neat PET/PEN blends. The blends and nanocomposites were characterized using various techniques. Microstructural and nanostructural properties were investigated. Fourier transform infrared spectroscopy (FTIR) results showed that the exfoliation of tetrahedral clay nanolayers is complete and the octahedral structure totally disappears. It was shown that total exfoliation, confirmed by wide angle X-ray scattering (WAXS) measurements, contributes to the enhancement of impact strength and tensile modulus. In addition, WAXS results indicated that all samples are amorphous. The differential scanning calorimetry (DSC) study indicated the occurrence of one glass transition temperature Tg, one crystallization temperature Tc and one melting temperature Tm for every composition. This was evidence that both PET/PEN and nPET/nPEN blends are compatible in the entire range of compositions. In addition, the nPET/nPEN blends showed lower Tc and higher Tm values than the corresponding neat PET/PEN blends. In conclusion, the results obtained indicate that n(PET/PEN) blends are different from the pure ones in nanostructure and physical behavior.

Keywords: blends, exfoliation, DRX, DSC, montmorillonite, nanocomposites, PEN, PET, plastograph, reactive melt-mixing

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Authors: Gulmira Umarova

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The data on the assessment of the influence of environmental risk to the health of the population of Uralsk in the West region of Kazakhstan were presented. Calculation of non-carcinogenic risks was performed for such air pollutants as sulfur dioxide, nitrogen oxides, hydrogen sulfide, carbon monoxide. Here with the critical organs and systems, which are affected by the above-mentioned substances were taken into account. As well as indicators of primary and general morbidity by classes of diseases among the population were considered. The quantitative risk of the influence of substances on organs and systems is established by results of the calculation.

Keywords: environment, health, morbidity, non-carcinogenic risk

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Authors: Salehi Zahabi Saleh, Rajabi Hosaien, Rasaneh Samira

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Yttrium-90 (90Y) radioembolisation(RE) is increasingly used for the treatment of patients with unresectable primary or metastatic liver tumours. Image-based approaches to assess microsphere distribution after RE have gained interest but are mostly hampered by the limited imaging possibilities of the Isotope 90Y. Quantitative 90Y-SPECT imaging has limited spatial resolution because it is based on 90Y Bremsstrahlung whereas 90Y-PET has better spatial resolution but low sensitivity. As a consequence, new alternative methods of visualizing the microspheres have been investigated, such as MR imaging of iron-labelled microspheres. It was also shown that MRI combines high sensitivity with high spatial and temporal resolution and with superior soft tissue contrast and thus can be used to cover a broad range of clinically interesting imaging parameters.The aim of the study in this article was to investigate the capability of MRI to measure the intrahepatic microsphere distribution in order to quantify the absorbed radiation dose in RE.

Keywords: radioembolisation, MRI, imaging, dosimetry

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Authors: Allagui Mohamed

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The study of the concentrations of atmospheric pollutants is analyzed during two days of sea breeze (April 26, 2010, and January 11, 2008) on the Mediterranean coasts, just in front of Gabès (33 ° 53 'N, 10 ° 07' E), Tunisia. During these two cases, we found that Gabès was contaminated by a coastal sea breeze. On April 26, 2010, the terrestrial synoptic wind admitted a maximum speed of about 6 m / s and was approximately perpendicular to the coast and making the breeze easier. On January 11, 2008, the terrestrial wind was local. Under these conditions, O3 and, therefore, the concentrations were multiplied by the factors 0.1 and 2, respectively. The episodes of ozone concentrations faithfully follow the sea breeze circulation. These sea breeze events can be responsible for high concentrations of NO, NO2, and SO2 as air pollutants in this area.

Keywords: sea breeze, O3, cost town, air quality

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Authors: Nicolaas Unland, John Webb

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The acidification and mobilisation of metals during the oxidation of acid sulfate soils exposed during lake bed drying is an increasingly common phenomenon under climate scenarios with reduced rainfall. In order to assess the risk of generating high concentrations of acidity and dissolved metals, chromium suite analysis are fundamental, but sometimes limited in characterising the potential risks they pose. This study combines such fundamental test work, along with incubation tests and 1D modelling to investigate the risks associated with the drying of Third Reedy Lake in South East Australia. Core samples were collected from a variable depth of 0.5 m below the lake bed, at 19 locations across the lake’s footprint, using a boat platform. Samples were subjected to a chromium suite of analysis, including titratable actual acidity, chromium reducible sulfur and acid neutralising capacity. Concentrations of reduced sulfur up to 0.08 %S and net acidities up to 0.15 %S indicate that acid sulfate soils have formed on the lake bed during permanent inundation over the last century. A further sub-set of samples were prepared in 7 columns and subject to accelerated heating, drying and wetting over a period of 64 days in laboratory. Results from the incubation trial indicate that while pyrite oxidation proceeded, minimal change to soil pH or the acidity of leachate occurred, suggesting that the internal buffering capacity of lake bed sediments was sufficient to neutralise a large proportion of the acidity produced. A 1D mass balance model was developed to assess potential changes in lake water quality during drying based on the results of chromium suite and incubation tests. Results from the above test work and modelling suggest that acid sulfate soils pose a moderate to low risk to the Third Reedy Lake system. Further, the risks can be effectively managed during the initial stages of lake drying via flushing with available mildly alkaline water. The study finds that while test work such as chromium suite analysis are fundamental in characterizing acid sulfate soil environments, they can the overestimate risks associated with the soils. Subsequent incubation test work may more accurately characterise such soils and lead to better-informed management strategies.

Keywords: acid sulfate soil, incubation, management, model, risk

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Authors: Abhishek Kumar

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X70 pipeline steel was electrochemically charged with hydrogen for different durations in order to find crack nucleation and propagation sites. After 3 hours charging, suitable regions for crack initiation and propagation were found. These regions were studied by OM, SEM, EDS and later Vicker hardness test was done. The results brought out that HIC cracks nucleated from regions rich of inclusions and further propagated through the segregation area of some elements, such as manganese, carbon, silicon and sulfur. It is worth-mentioning that all these potential sites for crack nucleation and propagation appeared at the centre of cross section of the specimens. Additionally, cracked area has harder phase than the non-cracked area which was confirmed by hardness test.

Keywords: X70 steel, morphology of inclusions, SEM/EDS/OM, simulation, statistical data

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Authors: Mouna Mesbahi, M. Loutfi Benkhedir

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In CZTS films solar cell, the preferable reaction between Cu and sulfur vapor was likely to be induced by out diffusion of the bottom Cu component to the surface; this would lead to inhomogeneous distribution of the Cu component to form the Cu2SnS3 secondary phase and formation of many voids and crevices in the resulting CZTS film; which is also the cause of the decline in performance. In this work we study the electronic and optical properties of Cu2SnS3. For this purpose we used the Wien2k code based on the theory of density functional theory (DFT) with the modified Becke-Johnson exchange potential mBJ and the Hubbard potential individually or combined. We have found an energy gap 0.92 eV. The results are in good agreement with experimental results.

Keywords: Cu2SnS3, DFT, electronic and optical properties, mBJ+U, WIEN2K

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Authors: Gabi N. Nehme

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The reduction of phosphorus and sulfur in engine oil are the main topics of this paper. Very reproducible boundary lubrication tests were conducted as part of Design of Experiment software (DOE) to study the behavior of fluorinated catalyst iron fluoride (FeF3), and polutetrafluoroethylene or Teflon (PTFE) in developing environmentally friendly (reduced P and S) anti-wear additives for future engine oil formulations. Multi-component Chevron fully formulated oil (GF3) and Chevron plain oil were used with the addition of PTFE and catalyst to characterize and analyze their performance. Lower phosphorus blends were the goal of the model solution. Experiments indicated that new sub-micron FeF3 catalyst played an important role in preventing breakdown of the tribofilm.

Keywords: wear, SEM, EDS, friction, lubricants

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Authors: M. Fares, S. Mameri, I. Abdlani, K. Negara

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Neutron detectors in general, proportional counters gas filling based isotope 3He in particular are going to be essential for monitoring and control of certain nuclear facilities, monitoring of experimentation around neutron beams and channels nuclear research reactors, radiation protection instruments and other tools multifaceted exploration and testing of materials, etc. This work consists of a measurement campaign features two Proportional Counters 3He (3He: LND252/USA CP, CP prototype: 3He LND/DDM). This is to make a comparison study of a CP 3He LND252/USA reference one hand, and in the context of routine periodic monitoring of the characteristics of the detectors for controlling the operation especially for laboratory prototypes. In this paper, we have described the different characteristics of the detectors and the experimental protocols used. Tables of measures have been developed and the different curves were plotted. The experimental campaign at stake: 2 PC 3He were thus characterized: Their characteristics (sensitivity, energy pulse height distribution spectra, gas amplification etc.) Were identified: 01 PC 3He 1'' Type: prototype DEDIN/DDM, 01 PC 3He 1'' Type: LND252/USA.

Keywords: PC 3He, sensitivity, pulse height distribution spectra, gas amplification

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Authors: Izza Hidaya, Korichi Mourad

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Solvent extraction is an affective method for reduction of aromatic content of lube oil. Frequently with phenol, furfural, NMP(N-methyl pyrrolidone). The solvent power and selectivity can be further increased by using surfactant as additive which facilitate phase separation and to increase raffinate yield. The aromatics in lube oil were extracted at different temperatures (ranging from 333.15 to 343.15K) and different concentration of surfactant (ranging from 0.01 to 0.1% wt).The extraction temperature and the amount of sulfate lauryl éther de sodium In phenoll were investigated systematically in order to determine their optimum values. The amounts of aromatic, paraffinic and naphthenic compounds were determined using ASTM standards by measuring refractive index (RI), viscosity, molecular weight and sulfur content. It was found that using 0,01%wt. surfactant at 343.15K yields the optimum extraction conditions.

Keywords: extraction, lubricating oil, aromatics, hydrocarbons

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Authors: Jessica Vasil'chuk, Elena Ivanova, Pavel Krechetov, Vladimir Litvinsky, Nadine Budantseva, Julia Chizhova, Yurij Vasil'chuk

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Carbonate minerals’ isotopic composition is widely used as a proxy for environmental parameters of the past. Pedogenic carbonate coatings on lower surfaces of coarse rock fragments are studied in order to indicate the climatic conditions and predominant vegetation under which they were formed. The purpose of the research is to characterize the isotopic composition of carbonate pedofeatures in soils of Minusink Hollow and estimate its correlation with isotopic composition of soil pore water, precipitation, vegetation and parent material. The samples of pedogenic carbonates, vegetation, carbonate parent material, soil water and precipitation water were analyzed using the Delta-V mass spectrometer with options of a gas bench and element analyser. The soils we studied are mainly Kastanozems that are poorly moisturized, therefore soil pore water was extracted by ethanol. Oxygen and carbon isotopic composition of pedogenic carbonates was analyzed in 3 key sites. Kazanovka Khakass state national reserve, Hankul salt lake, region of Sayanogorsk aluminum smelter. Vegetation photosynthetic pathway in the region is mainly C3. δ18O values of carbonate coatings in soils of Kazanovka vary in a range from −7.49 to −10.5‰ (vs V-PDB), and the smallest value −13.9‰ corresponds the coatings found between two buried soil horizons which 14C dates are 4.6 and 5.2 kyr BP. That may indicate cooler conditions of late Holocene than nowadays. In Sayanogorsk carbonates’ δ18O range is from −8.3 to −11.1‰ and near the Hankul Lake is from −9.0 to −10.2‰ all ranges are quite similar and may indicate coatings’ uniform formation conditions. δ13C values of carbonate coatings in Kazanovka vary from −2.5 to −6.7‰, the highest values correspond to the soils of Askiz and Syglygkug rivers former floodplains. For Sayanogorsk the range is from −4.9 to −6.8‰ and for Hankul from −2.3 to −5.7‰, where the highest value is for the modern salt crust. δ13C values of coatings strongly decrease from inner (older) to outer (younger) layers of coatings, that can indicate differences connected with the diffusion of organic material. Carbonate parent material δ18O value in the region vary from −11.1 to −12.0‰ and δ13C values vary from −4.9 to −5.7‰. Soil pore water δ18O values that determine the oxygen isotope composition of carbonates vary due to the processes of transpiration and mixing in the studied sites in a wide range of −2.0 to −13.5‰ (vs V-SMOW). Precipitation waters show δ18O values from -6.6‰ in May and -19.0‰ in January (snow) due to the temperature difference. The main conclusions are as follows: pedogenic carbonates δ13C values (−7…−2,5‰) show no correlation with modern C3 vegetation δ13C values (−30…−26‰), expected values under such vegetation are (−19…−15‰) but are closer to C4 vegetation. Late Holocene climate for the Minusinsk Hollow according to obtained data on isotope composition of carbonates and soil pore water chemical composition was dryer and cooler than present, that does not contradict with paleocarpology data obtained for the region. The research was supported by Russian Science Foundation (grant №14-27-00083).

Keywords: carbon, oxygen, pedogenic carbonates, South Siberia, stable isotopes

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Authors: Yalçın Kılıç, İbrahim Kani

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In recent years, interest in the synthesis of coordination compounds has greatly increased due to various application areas (such as catalysis, gas storage, luminescence). Dicarboxylic acids are often used in the synthesis of metal complexes. Bis-thiosalicylate derivative ligands contribute to the synthesis of structures of crystal engineering interest, as they can have both rigid and flexible properties. In addition, these ligands have great potential in terms of catalytic applications with the sulfur and oxygen donor atoms in their structures. In this study, we synthesized a Cu(II) complex [Cu(tsaxyl)(phen)2]•CH3OH (where tsaxyl = 2,2'-(1,2-phylenebis(methylene))bis(sulfanedyl)dibenzoate, phen = 1,10-phenantroline) and characterized through X-ray crystallography. The catalytic activities of Cu(II) complex on oxidation of ethylbenzene, cyclohexane, diphenylmethane, p-xylene were performed in acetonitrile with t-BuOOH as the source of oxygen.

Keywords: complex, crystallography, catalysis, oxidation

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Authors: Jenson George, Thoa Nguyen, Garth Sanewski, Craig Hardner, Heather Eunice Smyth

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Pineapple (Ananas comosus), with its unique sweet flavour, is one of the most popular tropical, non-climacteric fruits consumed worldwide. It is also the third most important tropical fruit in world production. In Australia, 99% of the pineapple production is from the Queensland state due to the favourable subtropical climatic conditions. The flavourful fruit is known to contain around 500 volatile organic compounds (VOC) at varying concentrations and greatly contribute to the flavour quality of pineapple fruit by providing distinct aroma sensory properties that are sweet, fruity, tropical, pineapple-like, caramel-like, coconut-like, etc. The aroma of pineapple is one of the important factors attracting consumers and strengthening the marketplace. To better understand the aroma of Australian-grown pineapples, the matrix-matched Gas chromatography–mass spectrometry (GC-MS), Head Space - Solid-phase microextraction (HS-SPME), Stable-isotope dilution analysis (SIDA) method was developed and validated. The developed method represents a significant improvement over current methods with the incorporation of multiple external reference standards, multiple isotopes labeled internal standards, and a matching model system of pineapple fruit matrix. This method was employed to quantify 28 key aroma compounds in more than 200 genetically diverse pineapple varieties from a breeding program. The Australian pineapple cultivars varied in content and composition of free volatile compounds, which were predominantly comprised of esters, followed by terpenes, alcohols, aldehydes, and ketones. Using selected commercial cultivars grown in Australia, and by employing the sensorial analysis, the appearance (colour), aroma (intensity, sweet, vinegar/tang, tropical fruits, floral, coconut, green, metallic, vegetal, fresh, peppery, fermented, eggy/sulphurous) and texture (crunchiness, fibrousness, and juiciness) were obtained. Relationships between sensory descriptors and volatiles were explored by applying multivariate analysis (PCA) to the sensorial and chemical data. The key aroma compounds of pineapple exhibited a positive correlation with corresponding sensory properties. The sensory and volatile data were also used to explore genetic diversity in the breeding population. GWAS was employed to unravel the genetic control of the pineapple volatilome and its interplay with fruit sensory characteristics. This study enhances our understanding of pineapple aroma (flavour) compounds, their biosynthetic pathways and expands breeding option for pineapple cultivars. This research provides foundational knowledge to support breeding programs, post-harvest and target market studies, and efforts to optimise the flavour of commercial pineapple varieties and their parent lines to produce better tasting fruits for consumers.

Keywords: Ananas comosus, pineapple, flavour, volatile organic compounds, aroma, Gas chromatography–mass spectrometry (GC-MS), Head Space - Solid-phase microextraction (HS-SPME), Stable-isotope dilution analysis (SIDA).

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Authors: Michael Huber, Maximilian J. Poller, Jens Tochtermann, Wolfgang Korth, Andreas Jess, Jakob Albert

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Aside from the desulfurisation, the denitrogenation of fuels is of great importance to minimize the environmental impact of transport emissions. The oxidative reaction pathway of organic nitrogen in the catalytic oxidative denitrogenation could be successfully elucidated. This is the first time such a pathway could be traced in detail in non-microbial systems. It was found that the organic nitrogen is first oxidized to nitrate, which is subsequently reduced to molecular nitrogen via nitrous oxide. Hereby, the organic substrate serves as a reducing agent. The discovery of this pathway is an important milestone for the further development of fuel denitrogenation technologies. The United Nations aims to counteract global warming with Net Zero Emissions (NZE) commitments; however, it is not yet foreseeable when crude oil-based fuels will become obsolete. In 2021, more than 50 million barrels per day (mb/d) were consumed for the transport sector alone. Above all, heteroatoms such as sulfur or nitrogen produce SO₂ and NOx during combustion in the engines, which is not only harmful to the climate but also to health. Therefore, in refineries, these heteroatoms are removed by hy-drotreating to produce clean fuels. However, this catalytic reaction is inhibited by the basic, nitrogenous reactants (e.g., quinoline) as well as by NH3. The ion pair of the nitrogen atom forms strong pi-bonds to the active sites of the hydrotreating catalyst, which dimin-ishes its activity. To maximize the desulfurization and denitrogenation effectiveness in comparison to just extraction and adsorption, selective oxidation is typically combined with either extraction or selective adsorption. The selective oxidation produces more polar compounds that can be removed from the non-polar oil in a separate step. The extraction step can also be carried out in parallel to the oxidation reaction, as a result of in situ separation of the oxidation products (ECODS; extractive catalytic oxidative desulfurization). In this process, H8PV5Mo7O40 (HPA-5) is employed as a homogeneous polyoxometalate (POM) catalyst in an aqueous phase, whereas the sulfur containing fuel components are oxidized after diffusion from the organic fuel phase into the aqueous catalyst phase, to form highly polar products such as H₂SO₄ and carboxylic acids, which are thereby extracted from the organic fuel phase and accumulate in the aqueous phase. In contrast to the inhibiting properties of the basic nitrogen compounds in hydrotreating, the oxidative desulfurization improves with simultaneous denitrification in this system (ECODN; extractive catalytic oxidative denitrogenation). The reaction pathway of ECODS has already been well studied. In contrast, the oxidation of nitrogen compounds in ECODN is not yet well understood and requires more detailed investigations.

Keywords: oxidative reaction pathway, denitrogenation of fuels, molecular catalysis, polyoxometalate

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Authors: Seema Kothari, Dinesh Panday

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An observed correlation of the reaction rates with the changes in the nature of substituent present on one of the reactants often reveals the nature of transition state. Selective oxidation of organic compounds under non-aqueous media is an important transformation in synthetic organic chemistry. Inorganic chromates and dichromates being drastic oxidant and are generally insoluble in most organic solvents, a number of different chromium (VI) derivatives have been synthesized. Benzimidazolium dichromate (BIDC) is one of the recently reported Cr(VI) reagents which is neither hygroscopic nor light sensitive being, therefore, much stable. Not many reports on the kinetics of the oxidations by BIDC are seemed to be available in the literature. In the present investigation, the kinetics and mechanism of benzyl alcohol (BA) and a number of para- and meta-substituted benzyl alcohols by benzimidazolium dichromate (BIDC), in dimethyl sulphoxide, is reported. The reactions were followed spectrophotometrically at 364 nm by monitoring the decrease in [BIDC] for up to 85-90% reaction, the temperature being constant. The observed oxidation product is the corresponding benzaldehyde. The reactions were of first order with respect to each the alcohol and BIDC. The reactions are catalyzed by proton, and the dependence is of the form: kobs = a + b[H+]. The reactions thus follow both, an acid-dependent and acid-independent paths. The oxidation of [1,1 2H2]benzyl alcohol exhibited the presence of a substantial kinetic isotope effect ( kH/kD = 6.20 at 298 K ). This indicated the cleavage of a α-C-H bond in the rate-determining step. An analysis of the temperature dependence of the deuterium isotope effect showed that the loss of hydrogen proceeds through a concerted cyclic process. The rate of oxidation of BA was determined in 19 organic solvents. An analysis of the solvent effect by Swain’s equation indicated that though both the anion and cation-solvating powers of the solvent contribute to the observed solvent effect, the role of cation-solvation is major. The rates of the para and meta compounds, at 298 K, failed to exhibit a significant correlation in terms of Hammett or Brown's substituent constants. The rates were then subjected to analyses in terms of dual substituent parameter (DSP) equations. The rates of oxidation of the para-substituted benzyl alcohols show an excellent correlation with Taft's σI and σRBA values. However, the rates for the meta-substituted benzyl alcohols show an excellent correlation with σI and σR0. The polar reaction constants are negative indicating an electron-deficient transition state. Hence the overall mechanism is proposed to involve the formation of a chromate ester in a fast pre-equilibrium and then a decomposition of the ester in a subsequent slow step via a cyclic concerted symmetrical transition state, involving hydride-ion transfer, leading to the product. The first order dependence on alcohol may be accounted in terms of the small value of the formation constant of the ester intermediate. An another reaction mechanism accounting the acid-catalysis involve the formation of a protonated BIDC prior to formation of an ester intermediate which subsequently decomposes in a slow step leading to the product.

Keywords: benzimidazolium dichromate, benzyl alcohols, correlation analysis, kinetics, oxidation

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Authors: Mohamed Khedr, Ahmed Farghali, Waleed El Rouby, Abdelrhman Hamdeldeen

Abstract:

Pure CeO2, Sm and Gd doped CeO2 were successfully prepared via hydrothermal method. The effect of hydrothermal temperature, reaction time and precursors were investigated. The prepared nanoparticles were characterized using X-ray diffraction (XRD), FT-Raman Spectroscopy, transmission electron microscope (TEM) and field emission scanning electron microscope (FESEM). The prepared pure and doped CeO2 nanoparticles were used as photo-catalyst for the degradation of Methylene blue (MB) dye under UV light irradiation. The results showed that Gd doped CeO2 nano-particles have the best catalytic degradation effect for MB under UV irradiation. The degradation pathways of MB were followed using liquid chromatography (LC/MS) and it was found that Gd doped CeO2 was able to oxidize MB dye with a complete mineralization of carbon, nitrogen and sulfur heteroatoms into CO2, NH4+, NO3- and SO42-.

Keywords: CeO2, doped CeO2, photocatalysis, methylene blue

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Authors: Mina Naeini, Thomas A. Adams II

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Solid Oxide Fuel Cells (SOFCs) feature high electrical efficiency and generate substantial amounts of waste heat that make them suitable for integrated community energy systems (ICEs). By harvesting and distributing the waste heat through hot water pipelines, SOFCs can meet thermal demand of the communities. Therefore, they can replace traditional gas boilers and reduce greenhouse gas (GHG) emissions. Despite these advantages of SOFCs over competing power generation units, this technology has not been successfully commercialized in large-scale to replace traditional generators in ICEs. One reason is that SOFC performance deteriorates over long-term operation, which makes it difficult to find the proper sizing of the cells for a particular ICE system. In order to find the optimal sizing and operating conditions of SOFCs in a community, a proper knowledge of degradation mechanisms and effects of operating conditions on SOFCs long-time performance is required. The simplified SOFC models that exist in the current literature usually do not provide realistic results since they usually underestimate rate of performance drop by making too many assumptions or generalizations. In addition, some of these models have been obtained from experimental data by curve-fitting methods. Although these models are valid for the range of operating conditions in which experiments were conducted, they cannot be generalized to other conditions and so have limited use for most ICEs. In the present study, a general, detailed degradation-based model is proposed that predicts the performance of conventional SOFCs over a long period of time at different operating conditions. Conventional SOFCs are composed of Yttria Stabilized Zirconia (YSZ) as electrolyte, Ni-cermet anodes, and LaSr₁₋ₓMnₓO₃ (LSM) cathodes. The following degradation processes are considered in this model: oxidation and coarsening of nickel particles in the Ni-cermet anodes, changes in the pore radius in anode, electrolyte, and anode electrical conductivity degradation, and sulfur poisoning of the anode compartment. This model helps decision makers discover the optimal sizing and operation of the cells for a stable, efficient performance with the fewest assumptions. It is suitable for a wide variety of applications. Sulfur contamination of the anode compartment is an important cause of performance drop in cells supplied with hydrocarbon-based fuel sources. H₂S, which is often added to hydrocarbon fuels as an odorant, can diminish catalytic behavior of Ni-based anodes by lowering their electrochemical activity and hydrocarbon conversion properties. Therefore, the existing models in the literature for H₂-supplied SOFCs cannot be applied to hydrocarbon-fueled SOFCs as they only account for the electrochemical activity reduction. A regression model is developed in the current work for sulfur contamination of the SOFCs fed with hydrocarbon fuel sources. The model is developed as a function of current density and H₂S concentration in the fuel. To the best of authors' knowledge, it is the first model that accounts for impact of current density on sulfur poisoning of cells supplied with hydrocarbon-based fuels. Proposed model has wide validity over a range of parameters and is consistent across multiple studies by different independent groups. Simulations using the degradation-based model illustrated that SOFCs voltage drops significantly in the first 1500 hours of operation. After that, cells exhibit a slower degradation rate. The present analysis allowed us to discover the reason for various degradation rate values reported in literature for conventional SOFCs. In fact, the reason why literature reports very different degradation rates, is that literature is inconsistent in definition of how degradation rate is calculated. In the literature, the degradation rate has been calculated as the slope of voltage versus time plot with the unit of voltage drop percentage per 1000 hours operation. Due to the nonlinear profile of voltage over time, degradation rate magnitude depends on the magnitude of time steps selected to calculate the curve's slope. To avoid this issue, instantaneous rate of performance drop is used in the present work. According to a sensitivity analysis, the current density has the highest impact on degradation rate compared to other operating factors, while temperature and hydrogen partial pressure affect SOFCs performance less. The findings demonstrated that a cell running at lower current density performs better in long-term in terms of total average energy delivered per year, even though initially it generates less power than if it had a higher current density. This is because of the dominant and devastating impact of large current densities on the long-term performance of SOFCs, as explained by the model.

Keywords: degradation rate, long-term performance, optimal operation, solid oxide fuel cells, SOFCs

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Authors: Muhammad Mufakkar, Ghulam Hussain Bhatti, Maryem Rana

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The study of the coordination behavior of thiones is of considerable interest due to the similarity of their binding sites to those in living systems. The complexation of thiones towards Copper(I) has also received considerable attraction in view of their variable bonding modes, structural diversity and promising biological implications. Copper (I) complexes of thioureas of the general formula: CuLCl, CuL2Cl and CuL3Cl [where L= Thiourea and its N- and N, N/- mono and di alkyl and phenyl derivatives] have been prepared using Cu(I)CN in the presence of HCl. The complexes have been characterized by thermal, IR and NMR(1H and 13C) spectroscopy. An upfield shift in 13C NMR and downfield shifts in 1H NMR are consistent with the sulfur coordination to Copper(I). The disappearance of a band around 2200 cm⁻¹ in IR and a resonance around 146 ppm in 13C NMR indicates that during the course of reaction the cyanide group of the Copper(I) salt has been replaced by chloride leading to the formation of chlorido complexes.

Keywords: Thiones, complexation, spectra, TGA, thermogram, chemical shifts, deshielding, resonance

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Authors: Bo Yang, Hali̇l Ceylan, Ali Ulvi̇ Uzer

Abstract:

This experimental study was performed to investigate the effect of biofuel co-products (BCPs) with sulfur-free lignin addition on the unconsolidated on strength and durability behavior in pavement soil stabilization subjected to freezing–thawing cycles. For strength behavior, a series of unconfined compression tests were conducted. Mass losses were also calculated after freezing–thawing cycles as criteria for durability behavior. To investigate the effect of the biofuel co-products on the durability behavior of the four type’s soils, mass losses were calculated after 12 freezing–thawing cycles. The co-products tested are promising additives for improving durability under freeze-thaw conditions, and each type has specific advantages.

Keywords: durability, mass lose, freezing–thawing test, bio-energy co-product, soil stabilization

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Authors: Nina Sankat, Gerd Wilsch, Cassian Gottlieb, Steven Millar, Tobias Guenther

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Laser-Induced Breakdown Spectroscopy (LIBS) is a combination of laser ablation and optical emission spectroscopy, which in principle can simultaneously analyze all elements on the periodic table. Materials can be analyzed in terms of chemical composition in a two-dimensional, time efficient and minor destructive manner. These advantages predestine LIBS as a monitoring technique in the field of civil engineering. The decreasing service life of concrete infrastructures is a continuously growing problematic. A variety of intruding, harmful substances can damage the reinforcement or the concrete itself. To insure a sufficient service life a regular monitoring of the structure is necessary. LIBS offers many applications to accomplish a successful examination of the conditions of concrete structures. A selection of those applications are the 2D-evaluation of chlorine-, sodium- and sulfur-concentration, the identification of carbonation depths and the representation of the heterogeneity of concrete. LIBS obtains this information by using a pulsed laser with a short pulse length (some mJ), which is focused on the surfaces of the analyzed specimen, for this only an optical access is needed. Because of the high power density (some GW/cm²) a minimal amount of material is vaporized and transformed into a plasma. This plasma emits light depending on the chemical composition of the vaporized material. By analyzing the emitted light, information for every measurement point is gained. The chemical composition of the scanned area is visualized in a 2D-map with spatial resolutions up to 0.1 mm x 0.1 mm. Those 2D-maps can be converted into classic depth profiles, as typically seen for the results of chloride concentration provided by chemical analysis like potentiometric titration. However, the 2D-visualization offers many advantages like illustrating chlorine carrying cracks, direct imaging of the carbonation depth and in general allowing the separation of the aggregates from the cement paste. By calibrating the LIBS-System, not only qualitative but quantitative results can be obtained. Those quantitative results can also be based on the cement paste, while excluding the aggregates. An additional advantage of LIBS is its mobility. By using the mobile system, located at BAM, onsite measurements are feasible. The mobile LIBS-system was already used to obtain chloride, sodium and sulfur concentrations onsite of parking decks, bridges and sewage treatment plants even under hard conditions like ongoing construction work or rough weather. All those prospects make LIBS a promising method to secure the integrity of infrastructures in a sustainable manner.

Keywords: concrete, damage assessment, harmful substances, LIBS

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Authors: Sukla Saha, Alok Sinha

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Acid mine drainage (AMD) refers to the production of acidified water from abandoned mines and active mines as well. The reason behind the generation of this kind of acidified water is the oxidation of pyrites present in the rocks in and around mining areas. Thiobacillus ferrooxidans, which is a sulfur oxidizing bacteria, helps in the oxidation process. AMD is extremely acidic in nature, (pH 2-3) with high concentration of several trace and heavy metals such as Fe, Al, Zn, Mn, Cu and Co and anions such as chloride and sulfate. AMD has several detrimental effect on aquatic organism and environment. It can directly or indirectly contaminate the ground water and surface water as well. The present study considered the treatment of AMD with metallurgical slag, which is a waste material. Slag helped to enhance the pH of AMD to 8.62 from 1.5 with 99% removal of trace metals such as Fe, Al, Mn, Cu and Co. Metallurgical slag was proven as efficient neutralizing material for the treatment of AMD.

Keywords: acid mine drainage, Heavy metals, metallurgical slag, Neutralization

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Authors: Bosung Kim, Youngmok Yun, Sungho Lee, Chanseok Park

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There is a limitation to power supply and operation by the chemical or physical battery in the space environment. Therefore, research for utilizing nuclear energy in the universe has been in progress since the 1950s, around the major industrialized countries. In this study, the self-rechargeable battery having a long life relative to the half-life of the radioisotope is suggested. The hybrid system is composed of betavoltaic battery, all solid battery and energy harvesting board. Betavoltaic battery can produce electrical power at least 10 years over using the radioisotope from Ni-63 and the silicon-based semiconductor. The electrical power generated from the betavoltaic battery is stored in the all-solid battery and stored power is used if necessary. The hybrid system board is composed of input terminals, boost circuit, charging terminals and output terminals. Betavoltaic and all solid batteries are connected to the input and output terminal, respectively. The electric current of 10 µA is applied to the system board by using the high-resolution power simulator. The system efficiencies are measured from a boost up voltage of 1.8 V, 2.4 V and 3 V, respectively. As a result, the efficiency of system board is about 75% after boosting up the voltage from 1V to 3V.

Keywords: isotope, betavoltaic, nuclear, battery, energy harvesting

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Authors: L. Asaro, M. Gratton, S. Seghar, N. Poirot, N. Ait Hocine

Abstract:

Rubber waste disposal is an environmental problem. Particularly, many researches are centered in the management of discarded tires. In spite of all different ways of handling used tires, the most common is to deposit them in a landfill, creating a stock of tires. These stocks can cause fire danger and provide ambient for rodents, mosquitoes and other pests, causing health hazards and environmental problems. Because of the three-dimensional structure of the rubbers and their specific composition that include several additives, their recycling is a current technological challenge. The technique which can break down the crosslink bonds in the rubber is called devulcanization. Strictly, devulcanization can be defined as a process where poly-, di-, and mono-sulfidic bonds, formed during vulcanization, are totally or partially broken. In the recent years, super critical carbon dioxide (scCO₂) was proposed as a green devulcanization atmosphere. This is because it is chemically inactive, nontoxic, nonflammable and inexpensive. Its critical point can be easily reached (31.1 °C and 7.38 MPa), and residual scCO₂ in the devulcanized rubber can be easily and rapidly removed by releasing pressure. In this study thermomechanical devulcanization of ground tire rubber (GTR) was performed in a twin screw extruder under diverse operation conditions. Supercritical CO₂ was added in different quantities to promote the devulcanization. Temperature, screw speed and quantity of CO₂ were the parameters that were varied during the process. The devulcanized rubber was characterized by its devulcanization percent and crosslink density by swelling in toluene. Infrared spectroscopy (FTIR) and Gel permeation chromatography (GPC) were also done, and the results were related with the Mooney viscosity. The results showed that the crosslink density decreases as the extruder temperature and speed increases, and, as expected, the soluble fraction increase with both parameters. The Mooney viscosity of the devulcanized rubber decreases as the extruder temperature increases. The reached values were in good correlation (R= 0.96) with de the soluble fraction. In order to analyze if the devulcanization was caused by main chains or crosslink scission, the Horikx's theory was used. Results showed that all tests fall in the curve that corresponds to the sulfur bond scission, which indicates that the devulcanization has successfully happened without degradation of the rubber. In the spectra obtained by FTIR, it was observed that none of the characteristic peaks of the GTR were modified by the different devulcanization conditions. This was expected, because due to the low sulfur content (~1.4 phr) and the multiphasic composition of the GTR, it is very difficult to evaluate the devulcanization by this technique. The lowest crosslink density was reached with 1 cm³/min of CO₂, and the power consumed in that process was also near to the minimum. These results encourage us to do further analyses to better understand the effect of the different conditions on the devulcanization process. The analysis is currently extended to monophasic rubbers as ethylene propylene diene monomer rubber (EPDM) and natural rubber (NR).

Keywords: devulcanization, recycling, rubber, waste

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Authors: Pankaj Pathak, Susmita Sharma

Abstract:

Incessant industrial growth fulfill the energy demand of present day society, at the same time it produces huge amount of waste which could be hazardous or non-hazardous in nature. These wastes are coming out from different sources viz, nuclear power, thermal power, coal mines which contain different types of contaminants and one of the emergent contaminant is strontium, used in the present study. The isotope of strontium (Sr90) is radioactive in nature with half-life of 28.8 years and permissible limit of strontium in drinking water is 1.5 ppm. Above the permissible limit causes several types of diseases in human being. Therefore, safe disposal of strontium into ground becomes a biggest challenge for the researchers. In this context, bentonite is being used as an efficient material to retain strontium onto ground due to its specific physical, chemical and mineralogical properties which exhibits higher cation exchange capacity and specific surface area. These properties influence the interaction between strontium and bentonite, which is quantified by employing a parameter known as distribution coefficient. Batch test was conducted, and sorption isotherms were modelled at different interaction time. The pseudo first-order and pseudo second order kinetic models have been used to fit experimental data, which helps to determine the sorption rate and mechanism.

Keywords: bentonite, interaction time, sorption, strontium

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