Search results for: wet air oxidation

Authors: Kanti Sapkota, Do Hyun Lee, Sung Soo Han

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Nanocomposites have been widely used in various fields such as electronics, catalysis, and in chemical, biological, biomedical and optical fields. They display broad biomedical properties like antidiabetic, anticancer, antioxidant, antimicrobial and antibacterial activities. Moreover, nanomaterials have been used for wastewater treatment. Particularly, bimetallic hybrid nanocomposites exhibit unique features as compared to their monometallic components. Hybrid nanomaterials not only afford the multifunctionality endowed by their constituents but can also show synergistic properties. In addition, these hybrid nanomaterials have noteworthy catalytic and optical properties. Notably, Au−Ag based nanoparticles can be employed in sensor and catalysis due to their characteristic composition-tunable plasmonic properties. Due to their importance and usefulness, various efforts were developed for their preparation. Generally, chemical methods have been described to synthesize such bimetallic nanocomposites. In such chemical synthesis, harmful and hazardous chemicals cause environmental contamination and increase toxicity levels. Therefore, ecologically benevolent processes for the synthesis of nanomaterials are highly desirable to diminish such environmental and safety concerns. In this regard, here we disclose a simple, cost-effective, external additive free and eco-friendly method for the synthesis of Au-Ag@AgCl nanocomposites using Nephrolepis cordifolia root extract. Au-Ag@AgCl NCs were obtained by the simultaneous reduction of cationic Ag and Au into AgCl in the presence of plant extract. The particle size of 10 to 50 nm was observed with the average diameter of 30 nm. The synthesized nanocomposite was characterized by various modern characterization techniques. For example, UV−visible spectroscopy was used to determine the optical activity of the synthesized NCs, and Fourier transform infrared (FT-IR) spectroscopy was employed to investigate the functional groups present in the biomolecules that were responsible for both reducing and capping agents during the formation of nanocomposites. Similarly, powder X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), thermogravimetric analysis (TGA) and energy-dispersive X-ray (EDX) spectroscopy were used to determine crystallinity, size, oxidation states, thermal stability and weight loss of the synthesized nanocomposites. As a synthetic application, the synthesized nanocomposite exhibited excellent catalytic activity for the multicomponent synthesis of biologically interesting quinoline molecules via domino annulation-aromatization reaction of aniline, arylaldehyde, and phenyl acetylene derivatives. Interestingly, the nanocatalyst was efficiently recycled for five times without substantial loss of catalytic properties.

Keywords: nanoparticles, catalysis, multicomponent, quinoline

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Authors: Freja Rydahl Rasmussen, Naja Villadsen, Stig Koust

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Air purifiers have become widely implemented in a wide range of settings, including households, schools, institutions, and hospitals, as they tackle the pressing issue of indoor air pollution. With their ability to enhance indoor air quality and create healthier environments, air purifiers are particularly vital when ventilation options are limited. These devices incorporate a diverse array of technologies, including HEPA filters, active carbon filters, UV-C light, photocatalytic oxidation, and ionizers, each designed to combat specific pollutants and improve air quality within enclosed spaces. However, the safety of air purifiers has not been investigated thoroughly, and many questions still arise when applying them. Certain air purification technologies, such as UV-C light or ionization, can unintentionally generate undesirable byproducts that can negatively affect indoor air quality and health. It is well-established that these technologies can inadvertently generate nanoparticles or convert common gaseous compounds into harmful ones, thus exacerbating air pollution. However, the formation of byproducts can vary across products, necessitating further investigation. There is a particular concern about the formation of the carcinogenic substance formaldehyde from common gases like acetone. Many air purifiers use mechanical filtration to remove particles, dust, and pollen from the air. Filters need to be replaced periodically for optimal efficiency, resulting in an additional cost for end-users. Currently, there are no guidelines for filter lifespan, and replacement recommendations solely rely on manufacturers. A market screening revealed that manufacturers' recommended lifespans vary greatly (from 1 month to 10 years), and there is a need for general recommendations to guide consumers. Activated carbon filters are used to adsorb various types of chemicals that can pose health risks or cause unwanted odors. These filters have a certain capacity before becoming saturated. If not replaced in a timely manner, the adsorbed substances are likely to be released from the filter through off-gassing or losing adsorption efficiency. The goal of this study is to investigate the lifespan of filters as well as investigate the potentially harmful effects of air purifiers. Understanding the lifespan of filters used in air purifiers and the potential formation of harmful byproducts is essential for ensuring their optimal performance, guiding consumers in their purchasing decisions, and establishing industry standards for safer and more effective air purification solutions. At this time, a selection of air purifiers has been chosen, and test methods have been established. In the following 3 months, the tests will be conducted, and the results will be ready for presentation later.

Keywords: air purifiers, activated carbon filters, byproducts, clean air, indoor air quality

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Authors: Rajeev Ravindran, Amit K. Jaiswal

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Lignocellulose is the largest reservoir of inexpensive, renewable source of carbon. It is composed of lignin, cellulose and hemicellulose. Cellulose and hemicellulose is composed of reducing sugars glucose, xylose and several other monosaccharides which can be metabolised by microorganisms to produce several value added products such as biofuels, enzymes, aminoacids etc. Enzymatic treatment of lignocellulose leads to the release of monosaccharides such as glucose and xylose. However, factors such as the presence of lignin, crystalline cellulose, acetyl groups, pectin etc. contributes to recalcitrance restricting the effective enzymatic hydrolysis of cellulose and hemicellulose. In order to overcome these problems, pre-treatment of lignocellulose is generally carried out which essentially facilitate better degradation of lignocellulose. A range of pre-treatment strategy is commonly employed based on its mode of action viz. physical, chemical, biological and physico-chemical. However, existing pretreatment strategies result in lower sugar yield and formation of inhibitory compounds. In order to overcome these problems, we proposes a novel pre-treatment, which utilises the superior oxidising capacity of alkaline potassium permanganate assisted by ultra-sonication to break the covalent bonds in spent coffee waste to remove recalcitrant compounds such as lignin. The pre-treatment was conducted for 30 minutes using 2% (w/v) potassium permanganate at room temperature with solid to liquid ratio of 1:10. The pre-treated spent coffee waste (SCW) was subjected to enzymatic hydrolysis using enzymes cellulase and hemicellulase. Shake flask experiments were conducted with a working volume of 50mL buffer containing 1% substrate. The results showed that the novel pre-treatment strategy yielded 7 g/L of reducing sugar as compared to 3.71 g/L obtained from biomass that had undergone dilute acid hydrolysis after 24 hours. From the results obtained it is fairly certain that ultrasonication assists the oxidation of recalcitrant components in lignocellulose by potassium permanganate. Enzyme hydrolysis studies suggest that ultrasound assisted alkaline potassium permanganate pre-treatment is far superior over treatment by dilute acid. Furthermore, SEM, XRD and FTIR were carried out to analyse the effect of the new pre-treatment strategy on structure and crystallinity of pre-treated spent coffee wastes. This novel one-step pre-treatment strategy was implemented under mild conditions and exhibited high efficiency in the enzymatic hydrolysis of spent coffee waste. Further study and scale up is in progress in order to realise future industrial applications.

Keywords: spent coffee waste, alkaline potassium permanganate, ultra-sonication, physical characterisation

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Authors: Safaa S. Hassan, Mohammed H. Elbakry, Safwat A. Mangoura, Zainab M. Omar

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Background: Liver fibrosis is the main reason for increased mortality in chronic liver disease. It has no standard treatment. Antioxidants from a variety of sources are capable of slowing or preventing oxidation of other molecules. Aim: to evaluate the hepatoprotective effect of vit. C, vit. E and gallic acid in comparison to silymarin in the rat model of carbon tetrachloride induced liver fibrosis and their possible mechanisms of action. Material& Methods: A total number of 60 adult male albino rats 160-200gm were divided into six equal groups; received subcutaneous (s.c) injection for 8 weeks. Group I: as control. Group II: received 1.5 mL/kg of CCL4 .Group III: CCL4 and co- treatment with silymarin 100mg/kg p.o. daily. Group IV: CCL4 and co-treatment with vit. C 50mg/kg p.o. daily. Group V: CCL4 and co-treatment with vit. E 200mg/kg. p.o. Group VI: CCL4 and co-treatment with Gallic acid 100mg/kg. p.o. daily. Liver was processed for histological and immunohistochemical examination. Levels of AST, ALT, ALP, reduced GSH, MDA, SOD and hydroxyproline concentration were measured and evaluated statistically. Results: Light and electron microscopic examination of liver of group II exhibited foci of altered cells with dense nuclei and vacuolated, granular cytoplasm, mononuclear cell infiltration in portal areas, profuse collagen fiber deposits were found around portal tract, more intense staining α-SMA-positive cells occupied most of the liver fibrosis tissue, electron lucent areas in the cytoplasm of the hepatocytes, margination of nuclear chromatin. Treatment by any of the antioxidants variably reduced the hepatic structural changes induced by CCL4. Biochemical analysis showed that carbon tetrachloride significantly increased the levels of serum AST, ALT, ALP, hepatic malondialdehyde and hydroxyproline content. Moreover, it decreased the activities of superoxide dismutase and glutathione. Treatment with silymarin, gallic acid, vit. C and vit. E decreased significantly the AST, ALT, and ALP levels in plasma, MDA and hydroxyproline and increased the activities of SOD and glutathione in liver tissue. The effect of administration of CCl4 was improved with the used antioxidants in variable degrees. The most efficient antioxidant was silymarin followed by gallic acid and vit. C then vit. E. It is possibly due to their antioxidant effect, free radical scavenging properties and the reduction of oxidant dependent activation and proliferation of HSCs. Conclusion: So these antioxidants can be a promising drugs candidate for ameliorating liver fibrosis better than the use of the drugs and their side effects.

Keywords: antioxidant, ccl4, gallic acid, liver fibrosis

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Authors: A. Kesraoui, M. Seffen

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Applications of adsorption onto activated carbon for water treatment are well known. The process has been demonstrated to be widely effective for removing dissolved organic substances from wastewaters, but this treatment has a major drawback is the high operating cost. The main goal of our research work is to improve the retention capacity of Tunisian biomass for the depollution of industrial wastewater and retention of pollutants considered toxic. The biosorption process is based on the retention of molecules and ions onto a solid surface composed of biological materials. The evaluation of the potential use of these materials is important to propose as an alternative to the adsorption process generally expensive, used to remove organic compounds. Indeed, these materials are very abundant in nature and are low cost. Certainly, the biosorption process is effective to remove the pollutants, but it presents a slow kinetics. The improvement of the biosorption rates is a challenge to make this process competitive with respect to oxidation and adsorption onto lignocellulosic fibers. In this context, the alternating current appears as a new alternative, original and a very interesting phenomenon in the acceleration of chemical reactions. Our main goal is to increase the retention acceleration of dyes (indigo carmine, methylene blue) and phenol by using a new alternative: alternating current. The adsorption experiments have been performed in a batch reactor by adding some of the adsorbents in 150 mL of pollutants solution with the desired concentration and pH. The electrical part of the mounting comprises a current source which delivers an alternating current voltage of 2 to 15 V. It is connected to a voltmeter that allows us to read the voltage. In a 150 mL capacity cell, we plunged two zinc electrodes and the distance between two Zinc electrodes has been 4 cm. Thanks to alternating current, we have succeeded to improve the performance of activated carbon by increasing the speed of the indigo carmine adsorption process and reducing the treatment time. On the other hand, we have studied the influence of the alternating current on the biosorption rate of methylene blue onto Luffa cylindrica fibers and the hybrid material (Luffa cylindrica-ZnO). The results showed that the alternating current accelerated the biosorption rate of methylene blue onto the Luffa cylindrica and the Luffa cylindrica-ZnO hybrid material and increased the adsorbed amount of methylene blue on both adsorbents. In order to improve the removal of phenol, we performed the coupling between the alternating current and the biosorption onto two adsorbents: Luffa cylindrica and the hybrid material (Luffa cylindrica-ZnO). In fact, the alternating current has succeeded to improve the performance of adsorbents by increasing the speed of the adsorption process and the adsorption capacity and reduce the processing time.

Keywords: adsorption, alternating current, dyes, modeling

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Authors: I. Berger, N. Machour, F. Portet-Koltalo

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Polycyclic aromatic hydrocarbons (PAHs) are toxic and carcinogenic pollutants produced in majority by incomplete combustion processes in industrialized and urbanized areas. After being emitted in atmosphere, these persistent contaminants are deposited to soils or sediments. Even if persistent, some can be partially degraded (photodegradation, biodegradation, chemical oxidation) and they lead to oxygenated metabolites (oxy-PAHs) which can be more toxic than their parent PAH. Oxy-PAHs are less measured than PAHs in sediments and this study aims to compare different analytical tools in order to extract and quantify a mixture of four hydroxylated PAHs (OH-PAHs) and four carbonyl PAHs (quinones) in sediments. Methodologies: Two analytical systems – HPLC with on-line UV and fluorescence detectors (HPLC-UV-FLD) and GC coupled to a mass spectrometer (GC-MS) – were compared to separate and quantify oxy-PAHs. Microwave assisted extraction (MAE) was optimized to extract oxy-PAHs from sediments. Results: First OH-PAHs and quinones were analyzed in HPLC with on-line UV and fluorimetric detectors. OH-PAHs were detected with the sensitive FLD, but the non-fluorescent quinones were detected with UV. The limits of detection (LOD)s obtained were in the range (2-3)×10-4 mg/L for OH-PAHs and (2-3)×10-3 mg/L for quinones. Second, even if GC-MS is not well adapted to the analysis of the thermodegradable OH-PAHs and quinones without any derivatization step, it was used because of the advantages of the detector in terms of identification and of GC in terms of efficiency. Without derivatization, only two of the four quinones were detected in the range 1-10 mg/L (LODs=0.3-1.2 mg/L) and LODs were neither very satisfying for the four OH-PAHs (0.18-0.6 mg/L). So two derivatization processes were optimized, comparing to literature: one for silylation of OH-PAHs, one for acetylation of quinones. Silylation using BSTFA/TCMS 99/1 was enhanced using a mixture of catalyst solvents (pyridine/ethyle acetate) and finding the appropriate reaction duration (5-60 minutes). Acetylation was optimized at different steps of the process, including the initial volume of compounds to derivatize, the added amounts of Zn (0.1-0.25 g), the nature of the derivatization product (acetic anhydride, heptafluorobutyric acid…) and the liquid/liquid extraction at the end of the process. After derivatization, LODs were decreased by a factor 3 for OH-PAHs and by a factor 4 for quinones, all the quinones being now detected. Thereafter, quinones and OH-PAHs were extracted from spiked sediments using microwave assisted extraction (MAE) followed by GC-MS analysis. Several mixtures of solvents of different volumes (10-25 mL) and using different extraction temperatures (80-120°C) were tested to obtain the best recovery yields. Satisfactory recoveries could be obtained for quinones (70-96%) and for OH-PAHs (70-104%). Temperature was a critical factor which had to be controlled to avoid oxy-PAHs degradation during the MAE extraction process. Conclusion: Even if MAE-GC-MS was satisfactory to analyze these oxy-PAHs, MAE optimization has to be carried on to obtain a most appropriate extraction solvent mixture, allowing a direct injection in the HPLC-UV-FLD system, which is more sensitive than GC-MS and does not necessitate a previous long derivatization step.

Keywords: derivatizations for GC-MS, microwave assisted extraction, on-line HPLC-UV-FLD, oxygenated PAHs, polluted sediments

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Authors: U. Pruthviraj, Praveen Kumar R. A. K. Athul, K. V. Gangadharan, S. Rao Shrikantha

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An open source based autonomous unmanned marine surface vehicle (UMSV) is developed for some of the marine applications such as pollution control, environmental monitoring and thermal imaging. A double rotomoulded hull boat is deployed which is rugged, tough, quick to deploy and moves faster. It is suitable for environmental monitoring, and it is designed for easy maintenance. A 2HP electric outboard marine motor is used which is powered by a lithium-ion battery and can also be charged from a solar charger. All connections are completely waterproof to IP67 ratings. In full throttle speed, the marine motor is capable of up to 7 kmph. The motor is integrated with an open source based controller using cortex M4F for adjusting the direction of the motor. This UMSV can be operated by three modes: semi-autonomous, manual and fully automated. One of the channels of a 2.4GHz radio link 8 channel transmitter is used for toggling between different modes of the USMV. In this electric outboard marine motor an on board GPS system has been fitted to find the range and GPS positioning. The entire system can be assembled in the field in less than 10 minutes. A Flir Lepton thermal camera core, is integrated with a 64-bit quad-core Linux based open source processor, facilitating real-time capturing of thermal images and the results are stored in a micro SD card which is a data storage device for the system. The thermal camera is interfaced to an open source processor through SPI protocol. These thermal images are used for finding oil spills and to look for people who are drowning at low visibility during the night time. A Real Time clock (RTC) module is attached with the battery to provide the date and time of thermal images captured. For the live video feed, a 900MHz long range video transmitter and receiver is setup by which from a higher power output a longer range of 40miles has been achieved. A Multi-parameter probe is used to measure the following parameters: conductivity, salinity, resistivity, density, dissolved oxygen content, ORP (Oxidation-Reduction Potential), pH level, temperature, water level and pressure (absolute).The maximum pressure it can withstand 160 psi, up to 100m. This work represents a field demonstration of an open source based autonomous navigation system for a marine surface vehicle.

Keywords: open source, autonomous navigation, environmental monitoring, UMSV, outboard motor, multi-parameter probe

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Authors: Nabil Al-Zaqri

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Semiconductor photocatalysts with surface defects display incredible light absorption bandwidth, and these defects function as highly active sites for oxidation processes by interacting with the surface band structure. Accordingly, engineering the photocatalyst with surface oxygen vacancies will enhance the semiconductor nanostructure's photocatalytic efficiency. Herein, a CeO2₋ₓ nanostructure is designed under the influence of low-frequency ultrasonic waves to create surface oxygen vacancies. This approach enhances the photocatalytic efficiency compared to many heterostructures while keeping the intrinsiccrystal structure intact. Ultrasonic waves induce the acoustic cavitation effect leading to the dissemination of active elements on the surface, which results in vacancy formation in conjunction with larger surface area and smaller particle size. The structural analysis of CeO₂₋ₓ revealed higher crystallinity, as well as morphological optimization, and the presence of oxygen vacancies is verified through Raman, X-rayphotoelectron spectroscopy, temperature-programmed reduction, photoluminescence, and electron spinresonance analyses. Oxygen vacancies accelerate the redox cycle between Ce₄+ and Ce₃+ by prolongingphotogenerated charge recombination. The ultrasound-treated pristine CeO₂ sample achieved excellenthydrogen production showing a quantum efficiency of 1.125% and efficient organic degradation. Ourpromising findings demonstrated that ultrasonic treatment causes the formation of surface oxygenvacancies and improves photocatalytic hydrogen evolution and pollution degradation. Conclusion: Defect engineering of the ceria nanoparticles with oxygen vacancies was achieved for the first time using low-frequency ultrasound treatment. The U-CeO₂₋ₓsample showed high crystallinity, and morphological changes were observed. Due to the acoustic cavitation effect, a larger surface area and small particle size were observed. The ultrasound treatment causes particle aggregation and surface defects leading to oxygen vacancy formation. The XPS, Raman spectroscopy, PL spectroscopy, and ESR results confirm the presence of oxygen vacancies. The ultrasound-treated sample was also examined for pollutant degradation, where 1O₂was found to be the major active species. Hence, the ultrasound treatment influences efficient photocatalysts for superior hydrogen evolution and an excellent photocatalytic degradation of contaminants. The prepared nanostructure showed excellent stability and recyclability. This work could pave the way for a unique post-synthesis strategy intended for efficient photocatalytic nanostructures.

Keywords: surface defect, CeO₂₋ₓ, photocatalytic, water treatment, H₂ production

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Authors: Y. Roumila, D. Meziani, R. Bagtache, K. Abdmeziem, M. Trari

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Heterogeneous photocatalysis over semiconductors has proved its effectiveness in the treatment of wastewaters since it works under soft conditions. It has emerged as a promising technique, giving rise to less toxic effluents and offering the opportunity of using sunlight as a sustainable and renewable source of energy. Many compounds have been used as photocatalysts. Though synthesized ones are intensively used, they remain expensive, and their synthesis involves special conditions. We thus thought of implementing a natural material, a phosphate ore, due to its low cost and great availability. Our work is devoted to the removal of hazardous organic pollutants, which cause several environmental problems and health risks. Among them, dye pollutants occupy a large place. This work relates to the study of the photodegradation of methyl violet (MV) and rhodamine B (RhB), in single and binary systems, under UV light and sunlight irradiation. Methyl violet is a triarylmethane dye, while RhB is a heteropolyaromatic dye belonging to the Xanthene family. In the first part of this work, the natural compound was characterized using several physicochemical and photo-electrochemical (PEC) techniques: X-Ray diffraction, chemical, and thermal analyses scanning electron microscopy, UV-Vis diffuse reflectance measurements, and FTIR spectroscopy. The electrochemical and photoelectrochemical studies were performed with a Voltalab PGZ 301 potentiostat/galvanostat at room temperature. The structure of the phosphate material was well characterized. The photo-electrochemical (PEC) properties are crucial for drawing the energy band diagram, in order to suggest the formation of radicals and the reactions involved in the dyes photo-oxidation mechanism. The PEC characterization of the natural phosphate was investigated in neutral solution (Na₂SO₄, 0.5 M). The study revealed the semiconducting behavior of the phosphate rock. Indeed, the thermal evolution of the electrical conductivity was well fitted by an exponential type law, and the electrical conductivity increases with raising the temperature. The Mott–Schottky plot and current-potential J(V) curves recorded in the dark and under illumination clearly indicate n-type behavior. From the results of photocatalysis, in single solutions, the changes in MV and RhB absorbance in the function of time show that practically all of the MV was removed after 240 mn irradiation. For RhB, the complete degradation was achieved after 330 mn. This is due to its complex and resistant structure. In binary systems, it is only after 120 mn that RhB begins to be slowly removed, while about 60% of MV is already degraded. Once nearly all of the content of MV in the solution has disappeared (after about 250 mn), the remaining RhB is degraded rapidly. This behaviour is different from that observed in single solutions where both dyes are degraded since the first minutes of irradiation.

Keywords: environment, organic pollutant, phosphate ore, photodegradation

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Authors: Swati Tomar, Sunil Kumar Gupta

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Anammox is a novel and promising technology that has changed the traditional concept of biological nitrogen removal. The process facilitates direct oxidation of ammonical nitrogen under anaerobic conditions with nitrite as an electron acceptor without the addition of external carbon sources. The present study investigated the feasibility of anammox hybrid reactor (AHR) combining the dual advantages of suspended and attached growth media for biodegradation of ammonical nitrogen in wastewater. The experimental unit consisted of 4 nos. of 5L capacity AHR inoculated with mixed seed culture containing anoxic and activated sludge (1:1). The process was established by feeding the reactors with synthetic wastewater containing NH4-H and NO2-N in the ratio 1:1 at HRT (hydraulic retention time) of 1 day. The reactors were gradually acclimated to higher ammonium concentration till it attained pseudo steady state removal at a total nitrogen concentration of 1200 mg/l. During this period, the performance of the AHR was monitored at twelve different HRTs varying from 0.25-3.0 d with increasing NLR from 0.4 to 4.8 kg N/m3d. AHR demonstrated significantly higher nitrogen removal (95.1%) at optimal HRT of 1 day. Filter media in AHR contributed an additional 27.2% ammonium removal in addition to 72% reduction in the sludge washout rate. This may be attributed to the functional mechanism of filter media which acts as a mechanical sieve and reduces the sludge washout rate many folds. This enhances the biomass retention capacity of the reactor by 25%, which is the key parameter for successful operation of high rate bioreactors. The effluent nitrate concentration, which is one of the bottlenecks of anammox process was also minimised significantly (42.3-52.3 mg/L). Process kinetics was evaluated using first order and Grau-second order models. The first-order substrate removal rate constant was found as 13.0 d-1. Model validation revealed that Grau second order model was more precise and predicted effluent nitrogen concentration with least error (1.84±10%). A new mathematical model based on mass balance was developed to predict N2 gas in AHR. The mass balance model derived from total nitrogen dictated significantly higher correlation (R2=0.986) and predicted N2 gas with least error of precision (0.12±8.49%). SEM study of biomass indicated the presence of the heterogeneous population of cocci and rod shaped bacteria of average diameter varying from 1.2-1.5 mm. Owing to enhanced NRE coupled with meagre production of effluent nitrate and its ability to retain high biomass, AHR proved to be the most competitive reactor configuration for dealing with nitrogen laden wastewater.

Keywords: anammox, filter media, kinetics, nitrogen removal

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Authors: Guanyu Jiang, Donghai Xu, Huanteng Liu

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After the Fukushima-Daiichi accident, the development of accident tolerant fuel cladding materials to improve reactor safety has become a hot topic in the field of nuclear industry. ZrO₂ has a satisfactory neutron economy and can guarantee the fission chain reaction process, which enables it to be a promising coating for zirconium alloy cladding. Maintaining a good corrosion resistance in primary coolant loop during normal operations of Pressurized Water Reactors is a prerequisite for ZrO₂ as a protective coating on zirconium alloy cladding. Research on the corrosion performance of ZrO₂ coating in nuclear water chemistry is relatively scarce, and existing reports failed to provide an in-depth explanation for the failure causes of ZrO₂ coating. Herein, a detailed corrosion process of ZrO₂ coating in lithiated water at 360 °C and 18.5 MPa was proposed based on experimental research and molecular dynamics simulation. Lithiated water with different LiOH solutions in the present work was deaerated and had a dissolved oxygen concentration of < 10 ppb. The concentration of Li (as LiOH) was determined to be 2.3 ppm, 70 ppm, and 500 ppm, respectively. Corrosion tests were conducted in a static autoclave. Modeling and corresponding calculations were operated on Materials Studio software. The calculation of adsorption energy and dynamics parameters were undertaken by the Energy task and Dynamics task of the Forcite module, respectively. The protective effect and failure mechanism of ZrO₂ coating on Zry-4 under varied LiOH concentrations was further revealed by comparison with the coating corrosion performance in pure water (namely 0 ppm Li). ZrO₂ coating provided a favorable corrosion protection with the occurrence of localized corrosion at low LiOH concentrations. Factors influencing corrosion resistance mainly include pitting corrosion extension, enhanced Li+ permeation, short-circuit diffusion of O²⁻ and ZrO₂ phase transformation. In highly-concentrated LiOH solutions, intergranular corrosion, internal oxidation, and perforation resulted in coating failure. Zr ions were released to coating surface to form flocculent ZrO₂ and ZrO₂ clusters due to the strong diffusion and dissolution tendency of α-Zr in the Zry-4 substrate. Considering that primary water of Pressurized Water Reactors usually includes 2.3 ppm Li, the stability of ZrO₂ make itself a candidate fuel cladding coating material. Under unfavorable conditions with high Li concentrations, more boric acid should be added to alleviate caustic corrosion of ZrO₂ coating once it is used. This work can provide some references to understand the service behavior of nuclear coatings under variable water chemistry conditions and promote the in-pile application of ZrO₂ coating.

Keywords: ZrO₂ coating, Zry-4, corrosion behavior, failure mechanism, LiOH concentration

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Authors: Kalu Uka Orji, Nasiman Sapari, Khamaruzaman W. Yusof

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Exposure of galena (PbS), tealite (PbSnS2), and other associated minerals during mining activities release lead (Pb) and other heavy metals into the mining water through oxidation and dissolution. Heavy metal pollution has become an environmental challenge. Lead, for instance, can cause toxic effects to human health, including brain damage. Ex-mining pond water was reported to contain lead as high as 69.46 mg/L. Conventional treatment does not easily remove lead from water. A promising and emerging treatment technology for lead removal is the application of the electrocoagulation (EC) process. However, some of the problems associated with EC are systematic reactor design, selection of maximum EC operating parameters, scale-up, among others. This study investigated an EC process for the removal of lead from synthetic ex-mining pond water using a batch reactor and Fe electrodes. The effects of various operating parameters on lead removal efficiency were examined. The results obtained indicated that the maximum removal efficiency of 98.6% was achieved at an initial PH of 9, the current density of 15mA/cm2, electrode spacing of 0.3cm, treatment time of 60 minutes, Liquid Motion of Magnetic Stirring (LM-MS), and electrode arrangement = BP-S. The above experimental data were further modeled and optimized using a 2-Level 4-Factor Full Factorial design, a Response Surface Methodology (RSM). The four factors optimized were the current density, electrode spacing, electrode arrangements, and Liquid Motion Driving Mode (LM). Based on the regression model and the analysis of variance (ANOVA) at 0.01%, the results showed that an increase in current density and LM-MS increased the removal efficiency while the reverse was the case for electrode spacing. The model predicted the optimal lead removal efficiency of 99.962% with an electrode spacing of 0.38 cm alongside others. Applying the predicted parameters, the lead removal efficiency of 100% was actualized. The electrode and energy consumptions were 0.192kg/m3 and 2.56 kWh/m3 respectively. Meanwhile, the adsorption kinetic studies indicated that the overall lead adsorption system belongs to the pseudo-second-order kinetic model. The adsorption dynamics were also random, spontaneous, and endothermic. The higher temperature of the process enhances adsorption capacity. Furthermore, the adsorption isotherm fitted the Freundlish model more than the Langmuir model; describing the adsorption on a heterogeneous surface and showed good adsorption efficiency by the Fe electrodes. Adsorption of Pb2+ onto the Fe electrodes was a complex reaction, involving more than one mechanism. The overall results proved that EC is an efficient technique for lead removal from synthetic mining pond water. The findings of this study would have application in the scale-up of EC reactor and in the design of water treatment plants for feed-water sources that contain lead using the electrocoagulation method.

Keywords: ex-mining water, electrocoagulation, lead, adsorption kinetics

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Authors: P. D. Pedrosa, J. M. A. Rebello, M. P. Cindra Fonseca

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Duplex stainless steels (DSS) exhibit a biphasic microstructure consisting of austenite and delta ferrite. Their high resistance to oxidation, and corrosion, even in H2S containing environments, allied to low cost when compared to conventional stainless steel, are some properties which make this material very attractive for several industrial applications. However, several of these industrial applications imposes cyclic loading to the equipments and in consequence fatigue damage needs to be a concern. A well-known way of improving the fatigue life of a component is by introducing compressive residual stress in its surface. Shot peening is an industrial working process which brings the material directly beneath component surface in a high mechanical compressive state, so inhibiting fatigue crack initiation. However, one must take into account the fact that the cyclic loading itself can reduce and even suppress these residual stresses, thus having undesirable consequences in the process of improving fatigue life by the introduction of compressive residual stresses. In the present work, shot peening was used to introduce residual stresses in several DSS samples. These were thereafter submitted to three different fatigue regimes: low, medium and high cycle fatigue. The evolution of the residual stress during loading were then examined on both surface and subsurface of the samples. It was used the DSS UNS S31803, with microstructure composed of 49% austenite and 51% ferrite. The treatment of shot peening was accomplished by the application of blasting in two Almen intensities of 0.25 and 0.39A. The residual stresses were measured by X-ray diffraction using the double exposure method and a portable equipment with CrK radiation and the (211) diffracting plane for the austenite phase and the (220) plane for the ferrite phase. It is known that residual stresses may arise when two regions of the same material experienced different degrees of plastic deformation. When these regions are separated in respect to each other on a scale that is large compared to the material's microstructure they are called macro stresses. In contrast, microstresses can largely vary over distances which are small comparable to the scale of the material's microstructure and must balance zero between the phases present. In the present work, special attention will be paid to the measurement of residual microstresses. Residual stress measurements were carried out in test pieces submitted to low, medium and high-cycle fatigue, in both longitudinal and transverse direction of the test pieces. It was found that after shot peening, the residual microstress is tensile in the austenite and compressive in the ferrite phases. It was hypothesized that the hardening behavior of the austenite after shot peening was probably due to its higher nitrogen content. Fatigue cycling can effectively change this stress state but this effect was found to be dependent of the shot peening intensity was well as the fatigue range.

Keywords: residual stresses, fatigue, duplex steel, shot peening

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Authors: Barrera C. Monserrat, Sierra-Alvarez Reyes, Pat-Espadas Aurora, Moreno Andrade Ivan

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Antimony is a toxic and carcinogenic metalloid considered a pollutant of priority interest by the United States Environmental Protection Agency. It is present in the environment in two oxidation states: antimonite (Sb (III)) and antimony (Sb (V)). Sb (III) is toxic to several aquatic organisms, but the potential inhibitory effect of Sb species for microorganisms has not been extensively evaluated. The fate and possible toxic impact of antimony on aerobic and anaerobic wastewater treatment systems are unknown. For this reason, the objective of this study was to evaluate the microbial toxicity of Sb (V) and Sb (III) in aerobic and anaerobic environments. Sb(V) and Sb(III) were used as potassium hexahydroxoantimonate (V) and potassium antimony tartrate, respectively (Sigma-Aldrich). The toxic effect of both Sb species in anaerobic environments was evaluated on methanogenic activity and the inhibition of hydrogen production of microorganisms from a wastewater treatment bioreactor. For the methanogenic activity, batch experiments were carried out in 160 mL serological bottles; each bottle contained basal mineral medium (100 mL), inoculum (1.5 g of VSS/L), acetate (2.56 g/L) as substrate, and variable concentrations of Sb (V) or Sb (III). Duplicate bioassays were incubated at 30 ± 2°C on an orbital shaker (105 rpm) in the dark. Methane production was monitored by gas chromatography. The hydrogen production inhibition tests were carried out in glass bottles with a working volume of 0.36 L. Glucose (50 g/L) was used as a substrate, pretreated inoculum (5 g VSS/L), mineral medium and varying concentrations of the two species of antimony. The bottles were kept under stirring and at a temperature of 35°C in an AMPTSII device that recorded hydrogen production. The toxicity of Sb on aerobic microorganisms (from a wastewater activated sludge treatment plant) was tested with a Microtox standardized toxicity test and respirometry. Results showed that Sb (III) is more toxic than Sb (V) for methanogenic microorganisms. Sb (V) caused a 50% decrease in methanogenic activity at 250 mg/L. In contrast, exposure to Sb (III) resulted in a 50% inhibition at a concentration of only 11 mg/L, and an almost complete inhibition (95%) at 25 mg/L. For hydrogen-producing microorganisms, Sb (III) and Sb (V) inhibited 50% of this production with 12.6 mg/L and 87.7 mg/L, respectively. The results for aerobic environments showed that 500 mg/L of Sb (V) do not inhibit the Allivibrio fischeri (Microtox) activity or specific oxygen uptake rate of activated sludge. In the case of Sb (III), this caused a loss of 50% of the respiration of the microorganisms at concentrations below 40 mg/L. The results obtained indicate that the toxicity of the antimony will depend on the speciation of this metalloid and that Sb (III) has a significantly higher inhibitory potential compared to Sb (V). It was shown that anaerobic microorganisms can reduce Sb (V) to Sb (III). Acknowledgments: This work was funded in part by grants from the UA-CONACYT Binational Consortium for the Regional Scientific Development and Innovation (CAZMEX), the National Institute of Health (NIH ES- 04940), and PAPIIT-DGAPA-UNAM (IN105220).

Keywords: aerobic inhibition, antimony reduction, hydrogen inhibition, methanogenic toxicity

Procedia PDF Downloads 166

Authors: Kristina Zuzek, Xuan Xu, Awais Ikram, Richard Sheridan, Allan Walton, Saso Sturm

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Recycling of end-of-life REEs based Nd-Fe-B magnets is an important strategy for reducing the environmental dangers associated with rare-earth mining and overcoming the well-documented supply risks related to the REEs. However, challenges on their reprocessing still remain. We report on the possibility of direct electrochemical recycling and reprocessing of Nd-Fe(B)-based magnets. In this investigation, we were able first to electrochemically leach the end-of-life NdFeB magnet and to electrodeposit Nd–Fe using a 1-ethyl-3-methyl imidazolium dicyanamide ([EMIM][DCA]) ionic liquid-based electrolyte. We observed that Nd(III) could not be reduced independently. However, it can be co-deposited on a substrate with the addition of Fe(II). Using advanced TEM techniques of electron-energy-loss spectroscopy (EELS) it was shown that Nd(III) is reduced to Nd(0) during the electrodeposition process. This gave a new insight into determining the Nd oxidation state, as X-ray photoelectron spectroscopy (XPS) has certain limitations. This is because the binding energies of metallic Nd (Nd0) and neodymium oxide (Nd₂O₃) are very close, i. e., 980.5-981.5 eV and 981.7-982.3 eV, respectively, making it almost impossible to differentiate between the two states. These new insights into the electrodeposition process represent an important step closer to efficient recycling of rare piles of earth in metallic form at mild temperatures, thus providing an alternative to high-temperature molten-salt electrolysis and a step closer to deposit Nd-Fe-based magnetic materials. Further, we propose a new concept of recycling the sintered Nd-Fe-B magnets by direct recovering the 2:14:1 matrix phase. Via an electrochemical etching method, we are able to recover pure individual 2:14:1 grains that can be re-used for new types of magnet production. In the frame of physical reprocessing, we have successfully synthesized new magnets out of hydrogen (HDDR)-recycled stocks with a contemporary technique of pulsed electric current sintering (PECS). The optimal PECS conditions yielded fully dense Nd-Fe-B magnets with the coercivity Hc = 1060 kA/m, which was boosted to 1160 kA/m after the post-PECS thermal treatment. The Br and Hc were tackled further and increased applied pressures of 100 – 150 MPa resulted in Br = 1.01 T. We showed that with a fine tune of the PECS and post-annealing it is possible to revitalize the Nd-Fe-B end-of-life magnets. By applying advanced TEM, i.e. atomic-scale Z-contrast STEM combined with EDXS and EELS, the resulting magnetic properties were critically assessed against various types of structural and compositional discontinuities down to atomic-scale, which we believe control the microstructure evolution during the PECS processing route.

Keywords: electrochemistry, Nd-Fe-B, pulsed electric current sintering, recycling, reprocessing

Procedia PDF Downloads 156

Authors: Lina Wu

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The excessive discharge of nitrogen in sewage greatly intensifies the eutrophication of water bodies and poses a threat to water quality. Nitrogen pollution control has become a global concern. Currently, the problem of water pollution in China is still not optimistic. As a typical high ammonia nitrogen organic wastewater, landfill leachate is more difficult to treat than domestic sewage because of its complex water quality, high toxicity, and high concentration.Many studies have shown that the autotrophic anammox bacteria in nature can combine nitrous and ammonia nitrogen without carbon source through functional genes to achieve total nitrogen removal, which is very suitable for the removal of nitrogen from leachate. In addition, the process also saves a lot of aeration energy consumption than the traditional nitrogen removal process. Therefore, anammox plays an important role in nitrogen conversion and energy saving. The process composed of short-range nitrification and denitrification coupled an ammo ensures the removal of total nitrogen and improves the removal efficiency, meeting the needs of the society for an ecologically friendly and cost-effective nutrient removal treatment technology. Continuous flow process for treating late leachate [an up-flow anaerobic sludge blanket reactor (UASB), anoxic/oxic (A/O)–anaerobic ammonia oxidation reactor (ANAOR or anammox reactor)] has been developed to achieve autotrophic deep nitrogen removal. In this process, the optimal process parameters such as hydraulic retention time and nitrification flow rate have been obtained, and have been applied to the rapid start-up and stable operation of the process system and high removal efficiency. Besides, finding the characteristics of microbial community during the start-up of anammox process system and analyzing its microbial ecological mechanism provide a basis for the enrichment of anammox microbial community under high environmental stress. One research developed partial nitrification-Anammox (PN/A) using an internal circulation (IC) system and a biological aerated filter (BAF) biofilm reactor (IBBR), where the amount of water treated is closer to that of landfill leachate. However, new high-throughput sequencing technology is still required to be utilized to analyze the changes of microbial diversity of this system, related functional genera and functional genes under optimal conditions, providing theoretical and further practical basis for the engineering application of novel anammox system in biogas slurry treatment and resource utilization.

Keywords: nutrient removal and recovery, leachate, anammox, partial nitrification

Procedia PDF Downloads 50

Authors: Thomas S. Abia II

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Intel Chandler Site has internally developed its first-of-kind (FOK) facility-scale wastewater treatment system to achieve multi-metal ion exchange. The process was carried out using a serial process train of carbon filtration, pH / ORP adjustment, and cationic exchange purification to treat dilute metal wastewater (DMW) discharged from a substrate packaging factory. Spanning a trial period of 10 months, a total of 3,271 samples were collected and statistically analyzed (average baseline + standard deviation) to evaluate the performance of a 95-gpm, multi-reactor continuous copper ion exchange treatment system that was consequently retrofitted for manganese ion exchange to meet environmental regulations. The system is also equipped with an inline acid and hot caustic regeneration system to rejuvenate exhausted IX resins and occasionally remove surface crud. Data generated from lab-scale studies was transferred to system operating modifications following multiple trial-and-error experiments. Despite the DMW treatment system failing to meet internal performance specifications for manganese output, it was observed to remove the cation notwithstanding the prevalence of copper in the waste stream. Accordingly, the average manganese output declined from 6.5 + 5.6 mg¹L⁻¹ at pre-pilot to 1.1 + 1.2 mg¹L⁻¹ post-pilot (83% baseline reduction). This milestone was achieved regardless of the average influent manganese to DMW increasing from 1.0 + 13.7 mg¹L⁻¹ at pre-pilot to 2.1 + 0.2 mg¹L⁻¹ post-pilot (110% baseline uptick). Likewise, the pre-trial and post-trial average influent copper values to DMW were 22.4 + 10.2 mg¹L⁻¹ and 32.1 + 39.1 mg¹L⁻¹, respectively (43% baseline increase). As a result, the pre-trial and post-trial average copper output values were 0.1 + 0.5 mg¹L⁻¹ and 0.4 + 1.2 mg¹L⁻¹, respectively (300% baseline uptick). Conclusively, the operating pH range upstream of treatment (between 3.5 and 5) was shown to be the largest single point of influence for optimizing manganese uptake during multi-metal ion exchange. However, the high variability of the influent copper-to-manganese ratio was observed to adversely impact the system functionality. The journal herein intends to discuss the operating parameters such as pH and oxidation-reduction potential (ORP) that were shown to influence the functional versatility of the ion exchange system significantly. The literature also proposes to discuss limitations of the treatment system such as influent copper-to-manganese ratio variations, operational configuration, waste by-product management, and system recovery requirements to provide a balanced assessment of the multi-metal ion exchange process. The take-away from this literature is intended to analyze the overall feasibility of ion exchange for metals manufacturing facilities that lack the capability to expand hardware due to real estate restrictions, aggressive schedules, or budgetary constraints.

Keywords: copper, industrial wastewater treatment, multi-metal ion exchange, manganese

Procedia PDF Downloads 143

Authors: Temitope L. Baiyegunhi, Christopher Baiyegunhi, Kuiwu Liu, Oswald Gwavava

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Diagenesis is the most important factor that affects or impact the reservoir property. Despite the fact that published data gives a vast amount of information on the geology, sedimentology and lithostratigraphy of the Ecca Group in the Karoo Basin of South Africa, little is known of the diagenesis of the potentially feasible shales and sandstones of the Ecca Group. The study aims to provide a general account of the diagenesis of sandstones and mudstone of the Ecca Group. Twenty-five diagenetic textures and structures are identified and grouped into three regimes or stages that include eogenesis, mesogenesis and telogenesis. Clay minerals are the most common cementing materials in the Ecca sandstones and mudstones. Smectite, kaolinite and illite are the major clay minerals that act as pore lining rims and pore-filling cement. Most of the clay minerals and detrital grains were seriously attacked and replaced by calcite. Calcite precipitates locally in pore spaces and partly or completely replaced feldspar and quartz grains, mostly at their margins. Precipitation of cements and formation of pyrite and authigenic minerals as well as little lithification occurred during the eogenesis. This regime was followed by mesogenesis which brought about an increase in tightness of grain packing, loss of pore spaces and thinning of beds due to weight of overlying sediments and selective dissolution of framework grains. Compaction, mineral overgrowths, mineral replacement, clay-mineral authigenesis, deformation and pressure solution structures occurred during mesogenesis. During rocks were uplifted, weathered and unroofed by erosion, this resulted in additional grain fracturing, decementation and oxidation of iron-rich volcanic fragments and ferromagnesian minerals. The rocks of Ecca Group were subjected to moderate-intense mechanical and chemical compaction during its progressive burial. Intergranular pores, matrix micro pores, secondary intragranular, dissolution and fractured pores are the observed pores. The presence of fractured and dissolution pores tend to enhance reservoir quality. However, the isolated nature of the pores makes them unfavourable producers of hydrocarbons, which at best would require stimulation. The understanding of the space and time distribution of diagenetic processes in these rocks will allow the development of predictive models of their quality, which may contribute to the reduction of risks involved in their exploration.

Keywords: diagenesis, reservoir quality, Ecca Group, Karoo Supergroup

Procedia PDF Downloads 148

Authors: Agne Jucyte Cicine, Vytautas Abromaitis, Zita Rasuole Gasiunaite, I. Vybernaite-Lubiene, D. Overlinge, K. Vilke

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Pharmaceutical pollution in aquatic environments has become a growing concern. Various active pharmaceutical ingredient (API) residues, hormones, antibiotics, or/and psychiatric drugs, have already been discovered in different environmental compartments. Due to existing ineffective wastewater treatment technologies to remove APIs, an underestimated amount can enter the ecosystem by discharged treated wastewater. Especially, psychiatric compounds, such as carbamazepine (CBZ) and venlafaxine (VNX), persist in effluent even post-treatment. Therefore, these pharmaceuticals usually exceed safe environmental levels and pose risks to the aquatic environment, particularly to sensitive ecosystems such as the Baltic Sea. CBZ, known for its chemical stability and long biodegradation time, accumulates in the environment, threatening aquatic life and human health through the food chain. As the use of medication rises, there is an urgent need for advanced wastewater treatment to reduce pharmaceutical contamination and meet future regulatory requirements. In this study, we tested advanced oxidation technology using ozone to remove two commonly used psychiatric drugs (carbamazepine and venlafaxine) from biologically treated wastewater effluent. Additionally, general water quality parameters (suspended matter (SPM), dissolved organic carbon (DOC), chemical oxygen demand (COD), and bacterial presence were analyzed. Three wastewater treatment plants (WWTPs) representing different anthropogenic pressures were selected: 1) resort, 2) resort and residential, and 3) residential, industrial, and resort. Wastewater samples for the experiment were collected during the summer season after mechanical and biological treatment and ozonated for 5, 10, and 15 minutes. The initial dissolved ozone concentration of 7,3±0,7 mg/L was held constant during all the experiments. Pharmaceutical levels in this study exceeded the predicted no-effect concentration (PNEC) of 500 and 90 ng L⁻¹ for CBZ and VNX, respectively, in all WWTPs, except CBZ in WWTP 1. Initial CBZ contamination was found to be lower in WWTP 1 (427.4 ng L⁻¹), compared with WWTP 2 (1266.5 ng L⁻¹) and 3 (119.2 ng L⁻¹). VNX followed a similar trend with concentrations of 341.2 ng L⁻¹, 361.4 ng L⁻¹, and 390.0 ng L⁻¹, respectively, for WWTPs 1, 2, and 3. It was determined that CBZ was not detected in the effluent after 5 minutes of ozonation in any of the WWTPs. Contrarily, VNX was still detected after 5, 10, and 15 minutes of treatment with ozone, however, under the limits of quantification (LOD) (<5ng L⁻¹). Additionally, general pollution of SPM, DOC, COD, and bacterial contamination was reduced notably after 5 minutes of treatment with ozone, while no bacterial growth was obtained. Although initial pharmaceutical levels exceeded PNECs, indicating ongoing environmental risks, ozonation demonstrated high efficiency in reducing pharmaceutical and general contamination in wastewater with different pollution matrices.

Keywords: Baltic Sea, ozonation, pharmaceuticals, wastewater treatment plants

Procedia PDF Downloads 19

Authors: Alessio Varotto, Lorenzo Freschi, Umberto Pasqual Laverdura, Anastasia Moschovi, Davide Pumiglia, Iakovos Yakoumis, Marta Feroci, Maria Luisa Grilli

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Dry reforming of Methane (DRM) is considered one of the most valuable technologies for green-house gas valorization thanks to the fact that through this reaction, it is possible to obtain syngas, a mixture of H₂ and CO in an H₂/CO ratio suitable for utilization in the Fischer-Tropsch process of high value-added chemicals and fuels. Challenges of the DRM process are the reduction of costs due to the high temperature of the process and the high cost of precious metals of the catalyst, the metal particles sintering, and carbon deposition on the catalysts’ surface. The aim of this study is to demonstrate the feasibility of the synthesis of catalysts using a leachate solution containing Pt coming directly from the recovery of spent diesel oxidation catalysts (DOCs) without further purification. An unusual perovskite support for DRM, the BaCe₁₋ₓ₋ᵧZrₓGdᵧO₃ (BCZG) perovskite, has been chosen as the catalyst support because of its high thermal stability and capability to produce oxygen vacancies, which suppress the carbon deposition and enhance the catalytic activity of the catalyst. BCZG perovskite has been synthesized by a sol-gel modified Pechini process and calcinated in air at 1100 °C. BCZG supports have been impregnated with a Pt-containing leachate solution of DOC, obtained by a mild hydrometallurgical recovery process, as reported elsewhere by some of the authors of this manuscript. For comparison reasons, a synthetic solution obtained by digesting commercial Pt-black powder in aqua regia was used for BCZG support impregnation. Pt nominal content was 2% in both BCZG-based catalysts formed by real and synthetic solutions. The structure and morphology of catalysts were characterized by X-Ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). Thermogravimetric Analysis (TGA) was used to study the thermal stability of the catalyst’s samples. Brunauer-Emmett-Teller (BET) analysis provided a high surface area of the catalysts. H₂-TPR (Temperature Programmed Reduction) analysis was used to study the consumption of hydrogen for reducibility, and it was associated with H₂-TPD characterization to study the dispersion of Pt on the surface of the support and calculate the number of active sites used by the precious metal. Dry reforming of methane (DRM) reaction, carried out in a fixed bed reactor, showed a high conversion efficiency of CO₂ and CH4. At 850°C, CO₂ and CH₄ conversion were close to 100% for the catalyst obtained with the aqua regia-based solution of commercial Pt-black, and ~70% (for CH₄) and ~80 % (for CO₂) in the case of real HCl-based leachate solution. H₂/CO ratios were ~0.9 and ~0.70 in the first and latter cases, respectively. As far as we know, this is the first pioneering work in which a BCGZ catalyst and a real Pt-containing leachate solution were successfully employed for DRM reaction.

Keywords: dry reforming of methane, perovskite, PGM, recycled Pt, syngas

Procedia PDF Downloads 37

Authors: Patrícia Severino, Luciana Nalone, Daniele Martins, Marco Chaud, Classius Ferreira, Cristiane Bani, Ricardo Albuquerque

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Hydrogels produced with polymers have been used in the development of dressings for wound treatment and tissue revitalization. Our study on polymer nanocomposites containing silver nanoparticles shows antimicrobial activity and applications in wound healing. The effects are linked with the slow oxidation and Ag⁺ liberation to the biological environment. Furthermore, bacterial cell membrane penetration and metabolic disruption through cell cycle disarrangement also contribute to microbial cell death. The silver antimicrobial activity has been known for many years, and previous reports show that low silver concentrations are safe for human use. This work aims to develop a hydrogel using natural polymers (sodium alginate and gelatin) combined with silver nanoparticles for wound healing and with antimicrobial properties in cutaneous lesions. The hydrogel development utilized different sodium alginate and gelatin proportions (20:80, 50:50 and 80:20). The silver nanoparticles incorporation was evaluated at the concentrations of 1.0, 2.0 and 4.0 mM. The physico-chemical properties of the formulation were evaluated using ultraviolet-visible (UV-Vis) absorption spectroscopy, Fourier transform infrared (FTIR) spectroscopy, differential scanning calorimetry (DSC), and thermogravimetric (TG) analysis. The morphological characterization was made using transmission electron microscopy (TEM). Human fibroblast (L2929) viability assay was performed with a minimum inhibitory concentration (MIC) assessment as well as an in vivo cicatrizant test. The results suggested that sodium alginate and gelatin in the (80:20) proportion with 4 mM of AgNO₃ in the (UV-Vis) exhibited a better hydrogel formulation. The nanoparticle absorption spectra of this analysis showed a maximum band around 430 - 450 nm, which suggests a spheroidal form. The TG curve exhibited two weight loss events. DSC indicated one endothermic peak at 230-250 °C, due to sample fusion. The polymers acted as stabilizers of a nanoparticle, defining their size and shape. Human fibroblast viability assay L929 gave 105 % cell viability with a negative control, while gelatin presented 96% viability, alginate: gelatin (80:20) 96.66 %, and alginate 100.33 % viability. The sodium alginate:gelatin (80:20) exhibited significant antimicrobial activity, with minimal bacterial growth at a ratio of 1.06 mg.mL⁻¹ in Pseudomonas aeruginosa and 0.53 mg.mL⁻¹ in Staphylococcus aureus. The in vivo results showed a significant reduction in wound surface area. On the seventh day, the hydrogel-nanoparticle formulation reduced the total area of injury by 81.14 %, while control reached a 45.66 % reduction. The results suggest that silver-hydrogel nanoformulation exhibits potential for wound dressing therapeutics.

Keywords: nanocomposite, wound healing, hydrogel, silver nanoparticle

Procedia PDF Downloads 101

Authors: Andrea Dragu, Solen Kinayyigit, Valerie Colliere, Karin Karin Philippot, Camelia Bala, Vasile I. Parvulescu

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The production of transportation fuels from biomass has gained a growing attention due to diminishing fossil fuel reserves, rising petroleum prices and increasing concern about global warming. In recent years, renewable hydrocarbons that are completely fungible with fossil fuels have been suggested to be efficiently produced by catalytic deoxygenation of fatty acids and their derivatives viadecarboxylation / decarbonylation. Several triglycerides (tall oil fatty acids) and saturated/unsaturated fatty acids and their corresponding esters were used as feedstocks. Their impact together with the influence of the reaction conditions and the catalyst composition on the nature of the reaction pathways of the deoxygenation of vegetable oils and their derivatives were recently reviewed. Following this state of the art the aim of the present study was the investigation of Pd NPs deposited onto mesoporous carbon supports as active and stable catalysts for the deoxygenation of oleic acid. The catalysts were prepared by the deposition of Pd NPs synthesised following an organometallic route on mesoporous carbons with different characteristics. Experiments were carried out under both batch and flow conditions. They demonstrated that under batch conditions (200 atm; 573K), the extent of the reaction depended, firstly, on the Pd loading and then on the metal dispersion and the oxidation state of palladium, both influenced by the way the support has been treated before the NPs deposition and by the preparation/stabilization methodology of Pd NPs. No aromatic compounds were detected in the reaction products but octadecanol and octadecane were observed in large extents. Under flow conditions (4 atm; 573 K), the conversion of stearic acid was superior to that observed in batch conditions. The product mixture contained over 20% heptadecane. No octadecanol, octadecane, and aromatic compounds were detected. The maxima in performances are obtained after only 0.5 h. After that, the yields in heptadecane suffer from a severe decrease until 3h reaction time. However, at that time, stopping feeding the reactor with oleic acid and flushing the catalyst only with mesitylene recovered the activity and the selectivity of the catalysts. With the complete removal of H2, the analysis revealed the presence of heptadecene in high excess compared to heptadecane (almost 7 to 1), thus suggesting decarbonylation as the main route. ICP-OES measurements indicated no leaching of palladium and simple washing of catalysts with mesitylene allowed recycling without any change in conversion or product distribution. Noteworthy, mesitylene as solvent exhibited no effect in this reaction. In conclusion, this study demonstrates the feasibility of such catalysts for the green production of fuels from biomass.

Keywords: fuels from biomass, green catalyst, Pd nano-particles , recycble catalyst

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Authors: Vinu Viswanath, Lawrence Dsouza, Ugo Ravon

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Syngas typically and intermediary gas product has a wide range of application of producing various chemical products, such as mixed alcohols, hydrogen, ammonia, Fischer-Tropsch products methanol, ethanol, aldehydes, alcohols, etc. There are several technologies available for the syngas production. An alternative to the conventional processes an attractive route of utilizing carbon dioxide and methane in equimolar ratio to generate syngas of ratio close to one has been developed which is also termed as Dry Reforming of Methane technology. It also gives the privilege to utilize the greenhouse gases like CO2 and CH4. The dry reforming process is highly endothermic, and indeed, ΔG becomes negative if the temperature is higher than 900K and practically, the reaction occurs at 1000-1100K. At this temperature, the sintering of the metal particle is happening that deactivate the catalyst. However, by using this strategy, the methane is just partially oxidized, and some cokes deposition occurs that causing the catalyst deactivation. The current research work was focused to mitigate the main challenges of dry reforming process such coke deposition, and metal sintering at high temperature.To achieve these objectives, we employed three different strategies of catalyst development. 1) Use of bulk catalysts such as olivine and pyrochlore type materials. 2) Use of metal doped support materials, like spinel and clay type material. 3) Use of core-shell model catalyst. In this approach, a thin layer (shell) of redox metal oxide is deposited over the MgAl2O4 /Al2O3 based support material (core). For the core-shell approach, an active metal is been deposited on the surface of the shell. The shell structure formed is a doped metal oxide that can undergo reduction and oxidation reactions (redox), and the core is an alkaline earth aluminate having a high affinity towards carbon dioxide. In the case of metal-doped support catalyst, the enhanced redox properties of doped CeO2 oxide and CO2 affinity property of alkaline earth aluminates collectively helps to overcome coke formation. For all of the mentioned three strategies, a systematic screening of the metals is carried out to optimize the efficiency of the catalyst. To evaluate the performance of them, the activity and stability test were carried out under reaction conditions of temperature ranging from 650 to 850 ̊C and an operating pressure ranging from 1 to 20 bar. The result generated infers that the core-shell model catalyst showed high activity and better stable DR catalysts under atmospheric as well as high-pressure conditions. In this presentation, we will show the results related to the strategy.

Keywords: carbon dioxide, dry reforming, supports, core shell catalyst

Procedia PDF Downloads 176

Authors: Lekgowa Collen Makola, Cecil Naphtaly Moro Ouma, Sharon Moeno, Langelihle Dlamini

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In recent years, advancement in the field of nanotechnology has evolved new strategies to address energy and environmental issues. Amongst the developing technologies, visible-light-driven photocatalysis is regarded as a sustainable approach for energy production and environmental detoxifications, where transition metal oxides (TMOs) and metal-free carbon-based semiconductors such as graphitic carbon nitride (CN) evidenced notable potential in this matter. Herein, g-C₃N₄@WO₃@Ti₃C₂Tx three-component multijunction photocatalyst was fabricated via facile ultrasonic-assisted self-assembly, followed by calcination to facilitate extensive integrations of the materials. A series of different Ti₃C₂ wt% loading in the g-C₃N4@WO₃@Ti₃C₂Tx were prepared and represented as 1-CWT, 3-CWT, 5-CWT, and 7-CWT corresponding to 1, 3, 5, and 7wt%, respectively. Systematic characterization using spectroscopic and microscopic techniques were employed to validate the successful preparation of the photocatalysts. Enhanced optoelectronic and photoelectrochemical properties were observed for the WO₃@Ti₃C2@g-C₃N4 heterostructure with respect to the individual materials. Photoluminescence spectra and Nyquist plots show restrained recombination rates and improved photocarrier conductivities, respectively, and this was credited to the synergistic coupling effect and the presence of highly conductive Ti₃C2 MXene. The strong interfacial contact surfaces upon the formation of the composite were confirmed using XPS. Multiple charge transfer mechanisms were proposed for the WO3@Ti3C₂@g-C3N4, which couples Z-scheme and Schottky-junction mediated with Ti3C2 MXene. Bode phase plots show improved charge carrier life-times upon the formation of the multijunctional photocatalyst. Moreover, transient photocurrent density of 7-CWT is 40 and seven (7) times higher compared to that of g-C₃N4 and WO3, correspondingly. Unlike in the traditional Z-Scheme, the formed ternary heterostructure possesses interfaces through the metallic 2D Ti₃C₂ MXene, which provided charge transfer channels for efficient photocarrier transfers with carrier concentrations (ND) of 17.49×1021 cm-3 and 4.86% photo-to-chemical conversion efficiency. The as-prepared ternary g-C₃N₄@WO₃@Ti₃C₂Tx exhibited excellent photoelectrochemical properties with reserved redox band potential potencies to facilitate efficient photo-oxidation and -reduction reactions. The fabricated multijunction photocatalyst exhibits potentials to be used in an extensive range of photocatalytic process vis., production of valuable hydrocarbons from CO₂, production of H₂, and degradation of a plethora of pollutants from wastewater.

Keywords: photocatalysis, Z-scheme, multijunction heterostructure, Ti₃C₂ MXene, g-C₃N₄

Procedia PDF Downloads 123

Authors: Abhishek Sraw, Amit Sobti, Yamini Pandey, R. K. Wanchoo, Amrit Pal Toor

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Monocrotophos (MCP) is a widely used pesticide in India, which belong to an extremely toxic organophosphorus family, is persistent in nature and its toxicity is widely reported in all environmental segments in the country. Advanced Oxidation Process (AOP) is a promising solution to the problem of water pollution. TiO₂ is being widely used as a photocatalyst because of its many advantages, but it has a large band gap, due to which it is modified using metal and nonmetal dopant to make it active under sunlight and visible light. The use of nanosized powdered catalysts makes the recovery process extremely complicated. Hence the aim is to use low cost, easily available, eco-friendly clay material in form of bead as the support for the immobilization of catalyst, to solve the problem of post-separation of suspended catalyst from treated water. A recirculation type photocatalytic reactor (RTPR), using ultraviolet light emitting source (blue black lamp) was designed which work effectively for both suspended catalysts and catalyst coated clay beads. The bare, TiO₂ and W-TiO₂ coated clay beads were characterized by scanning electron microscopy (SEM), electron dispersive spectroscopy (EDS) and N₂ adsorption–desorption measurements techniques (BET) for their structural, textural and electronic properties. The study involved variation of different parameters like light conditions, recirculation rate, light intensity and initial MCP concentration under UV and sunlight for the degradation of MCP. The degradation and mineralization studies of the insecticide solution were performed using UV-Visible spectrophotometer, and COD vario-photometer and GC-MS analysis respectively. The main focus of the work lies in checking the recyclability of the immobilized TiO₂ over clay beads in the developed RTPR up to 30 continuous cycles without reactivation of catalyst. The results demonstrated the economic feasibility of the utilization of developed RTPR for the efficient purification of pesticide polluted water. The prepared TiO₂ clay beads delivered 75.78% degradation of MCP under UV light with negligible catalyst loss. Application of W-TiO₂ coated clay beads filled RTPR for the degradation of MCP under sunlight, however, shows 32% higher degradation of MCP than the same system based on undoped TiO₂. The COD measurements of TiO₂ coated beads led to 73.75% COD reduction while W-TiO₂ resulted in 87.89% COD reduction. The GC-MS analysis confirms the efficient breakdown of complex MCP molecules into simpler hydrocarbons. This supports the promising application of clay beads as a support for the photocatalyst and proves its eco-friendly nature, excellent recyclability, catalyst holding capacity, and economic viability.

Keywords: immobilized clay beads, monocrotophos, recirculation type photocatalytic reactor, TiO₂

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Authors: Sanchita Baitalik, Nijhuma Kayal, Omprakash Chakrabarti

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Recently SiC ceramics have been a focus of interest in the field of porous materials due to their unique combination of properties and hence they are considered as an ideal candidate for catalyst supports, thermal insulators, high-temperature structural materials, hot gas particulate separation systems etc. in different industrial processes. Several processing methods are followed for fabrication of porous SiC at low temperatures but all these methods are associated with several disadvantages. Therefore processing of porous SiC ceramics at low temperatures is still challenging. Concerning that of incorporation of secondary bond phase additives by an infiltration technique should result in a homogenous distribution of bond phase in the final ceramics. Present work is aimed to synthesis cordierite (2MgO.2Al2O3.5SiO2) bonded porous SiC ceramics following incorporation of sol-gel bond phase precursor into powder compacts of SiC and heat treating the infiltrated body at 1400 °C. In this paper the primary aim was to study the effect of infiltration of a precursor sol of cordierite into a porous SiC powder compact prepared with pore former of different particle sizes on the porosity, pore size, microstructure and the mechanical properties of the porous SiC ceramics. Cordierite sol was prepared by mixing a solution of magnesium nitrate hexahydrate and aluminium nitrate nonahydrate in 2:4 molar ratio in ethanol another solution containing tetra-ethyl orthosilicate and ethanol in 1:3 molar ratio followed by stirring for several hours. Powders of SiC (α-SiC; d50 =22.5 μm) and 10 wt. % polymer microbead of two sizes 8 and 50µm as the pore former were mixed in a suitable liquid medium, dried and pressed in the form of bars (50×20×16 mm3) at 23 MPa pressure. The well-dried bars were heat treated at 1100° C for 4 h with a hold at 750 °C for 2 h to remove the pore former. Bars were evacuated for 2 hr upto 0.3 mm Hg pressure into a vacuum chamber and infiltrated with cordierite precursor sol. The infiltrated samples were dried and the infiltration process was repeated until the weight gain became constant. Finally the infiltrated samples were sintered at 1400 °C to prepare cordierite bonded porous SiC ceramics. Porous ceramics prepared with 8 and 50 µm sized microbead exhibited lower oxidation degrees of respectively 7.8 and 4.8 % than the sample (23 %) prepared with no microbead. Depending on the size of pore former, the porosity of the final ceramic varied in the range of 36 to 40 vol. % with a variation of flexural strength from 33.7 to 24.6 MPa. XRD analysis showed major crystalline phases of the ceramics as SiC, SiO2 and cordierite. Two forms of cordierite, α-(hexagonal) and µ-(cubic), were detected by the XRD analysis. The SiC particles were observed to be bonded both by cristobalite with fish scale morphology and cordierite with rod shape morphology and thereby formed a porous network. The material and mechanical properties of cordierite bonded porous SiC ceramics are good in agreement to carry out further studies like thermal shock, corrosion resistance etc.

Keywords: cordierite, infiltration technique, porous ceramics, sol-gel

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Authors: Dorottya Guban, Irina Borbath, Istvan Bakos, Peter Nemeth, Andras Tompos

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One of the greatest challenges of the implementation of polymer electrolyte membrane fuel cells (PEMFCs) is to find active and durable electrocatalysts. The cell performance is always limited by the oxygen reduction reaction (ORR) on the cathode since it is at least 6 orders of magnitude slower than the hydrogen oxidation on the anode. Therefore high loading of Pt is required. Catalyst corrosion is also more significant on the cathode, especially in case of mobile applications, where rapid changes of loading have to be tolerated. Pt-Sn bulk alloys and SnO2-decorated Pt3Sn nanostructures are among the most studied bimetallic systems for fuel cell applications. Exclusive formation of supported Sn-Pt alloy phases with different Pt/Sn ratios can be achieved by using controlled surface reactions (CSRs) between hydrogen adsorbed on Pt sites and tetraethyl tin. In this contribution our results for commercial and a home-made 20 wt.% Pt/C catalysts modified by tin anchoring via CSRs are presented. The parent Pt/C catalysts were synthesized by modified NaBH4-assisted ethylene-glycol reduction method using ethanol as a solvent, which resulted either in dispersed and highly stable Pt nanoparticles or evenly distributed raspberry-like agglomerates according to the chosen synthesis parameters. The 20 wt.% Pt/C catalysts prepared that way showed improved electrocatalytic performance in the ORR and stability in comparison to the commercial 20 wt.% Pt/C catalysts. Then, in order to obtain Sn-Pt/C catalysts with Pt/Sn= 3 ratio, the Pt/C catalysts were modified with tetraethyl tin (SnEt4) using three and five consecutive tin anchoring periods. According to in situ XPS studies in case of catalysts with highly dispersed Pt nanoparticles, pre-treatment in hydrogen even at 170°C resulted in complete reduction of the ionic tin to Sn0. No evidence of the presence of SnO2 phase was found by means of the XRD and EDS analysis. These results demonstrate that the method of CSRs is a powerful tool to create Pt-Sn bimetallic nanoparticles exclusively, without tin deposition onto the carbon support. On the contrary, the XPS results revealed that the tin-modified catalysts with raspberry-like Pt agglomerates always contained a fraction of non-reducible tin oxide. At the same time, they showed increased activity and long-term stability in the ORR than Pt/C, which was assigned to the presence of SnO2 in close proximity/contact with Pt-Sn alloy phase. It has been demonstrated that the content and dispersion of the fcc Pt3Sn phase within the electrocatalysts can be controlled by tuning the reaction conditions of CSRs. The bimetallic catalysts displayed an outstanding performance in the ORR. The preparation of a highly dispersed 20Pt/C catalyst permits to decrease the Pt content without relevant decline in the electrocatalytic performance of the catalysts.

Keywords: anode catalyst, cathode catalyst, controlled surface reactions, oxygen reduction reaction, PtSn/C electrocatalyst

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Authors: Ana Flavia Belchior De Andrade

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Forensic laboratories all over the world face a great challenge to overcame waiting time and backlog in many different areas. Many aspects contribute to this situation, such as an increase in drug complexity, increment in the number of exams requested and cuts in funding limiting laboratories hiring capacity. Altogether, those facts pose an essential challenge for forensic chemistry laboratories to keep both quality and time of response within an acceptable period. In this paper we will analyze how the backlog affects test results and, in the end, the whole judicial system. In this study data from marijuana samples seized by the Federal District Civil Police in Brazil between the years 2013 and 2017 were tabulated and the results analyzed and discussed. In the last five years, the number of petitioned exams increased from 822 in February 2013 to 1358 in March 2018, representing an increase of 32% in 5 years, a rise of more than 6% per year. Meanwhile, our data shows that the number of performed exams did not grow at the same rate. Product numbers are stationed as using the actual technology scenario and analyses routine the laboratory is running in full capacity. Marijuana detection is the most prevalence exam required, representing almost 70% of all exams. In this study, data from 7,110 (seven thousand one hundred and ten) marijuana samples were analyzed. Regarding waiting time, most of the exams were performed not later than 60 days after receipt (77%). Although some samples waited up to 30 months before being examined (0,65%). When marijuana´s exam is delayed we notice the enlargement of inconclusive results using thin-layer chromatography (TLC). Our data shows that if a marijuana sample is stored for more than 18 months, inconclusive results rise from 2% to 7% and when if storage exceeds 30 months, inconclusive rates increase to 13%. This is probably because Cannabis plants and preparations undergo oxidation under storage resulting in a decrease in the content of Δ9-tetrahydrocannabinol ( Δ9-THC). An inconclusive result triggers other procedures that require at least two more working hours of our analysts (e.g., GC/MS analysis) and the report would be delayed at least one day. Those new procedures increase considerably the running cost of a forensic drug laboratory especially when the backlog is significant as inconclusive results tend to increase with waiting time. Financial aspects are not the only ones to be observed regarding backlog cases; there are also social issues as legal procedures can be delayed and prosecution of serious crimes can be unsuccessful. Delays may slow investigations and endanger public safety by giving criminals more time on the street to re-offend. This situation also implies a considerable cost to society as at some point, if the exam takes a long time to be performed, an inconclusive can turn into a negative result and a criminal can be absolved by flawed expert evidence.

Keywords: backlog, forensic laboratory, quality management, accreditation

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Authors: Totsaporn Suwannaruang, Kitirote Wantala

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The purposes of this research were to synthesize titanium dioxide photocatalyst doped with nitrogen (N-doped TiO₂) by hydrothermal method and to test the photocatalytic degradation of paraquat under UV and visible light illumination. The effect of calcination treatment temperature on their physical and chemical properties and photocatalytic efficiencies were also investigated. The characterizations of calcined N-doped TiO₂ photocatalysts such as specific surface area, textural properties, bandgap energy, surface morphology, crystallinity, phase structure, elements and state of charges were investigated by Brunauer, Emmett, Teller (BET) and Barrett, Joyner, Halenda (BJH) equations, UV-Visible diffuse reflectance spectroscopy (UV-Vis-DRS) by using the Kubelka-Munk theory, Wide-angle X-ray scattering (WAXS), Focussed ion beam scanning electron microscopy (FIB-SEM), X-ray photoelectron spectroscopy (XPS) and X-ray absorption spectroscopy (XAS), respectively. The results showed that the effect of calcination temperature was significant on surface morphology, crystallinity, specific surface area, pore size diameter, bandgap energy and nitrogen content level, but insignificant on phase structure and oxidation state of titanium (Ti) atom. The N-doped TiO₂ samples illustrated only anatase crystalline phase due to nitrogen dopant in TiO₂ restrained the phase transformation from anatase to rutile. The samples presented the nanorice-like morphology. The expansion on the particle was found at 650 and 700°C of calcination temperature, resulting in increased pore size diameter. The bandgap energy was determined by Kubelka-Munk theory to be in the range 3.07-3.18 eV, which appeared slightly lower than anatase standard (3.20 eV), resulting in the nitrogen dopant could modify the optical absorption edge of TiO₂ from UV to visible light region. The nitrogen content was observed at 100, 300 and 400°C only. Also, the nitrogen element disappeared at 500°C onwards. The nitrogen (N) atom can be incorporated in TiO₂ structure with the interstitial site. The uncalcined (100°C) sample displayed the highest percent paraquat degradation under UV and visible light irradiation due to this sample revealed both the highest specific surface area and nitrogen content level. Moreover, percent paraquat removal significantly decreased with increasing calcination treatment temperature. The nitrogen content level in TiO₂ accelerated the rate of reaction with combining the effect of the specific surface area that generated the electrons and holes during illuminated with light. Therefore, the specific surface area and nitrogen content level demonstrated the important roles in the photocatalytic activity of paraquat under UV and visible light illumination.

Keywords: restraining phase transformation, interstitial site, chemical charge state, photocatalysis, paraquat degradation

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Authors: A. Chiker, A. Benamor, A. Haddad, Y. Hadji, M. Hadji

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Metal matrix composites (MMCs) have been of big interest for a few decades. Their major drawback lies in their enhanced mechanical performance over unreinforced alloys. They found ground in many engineering fields, such as aeronautics, aerospace, automotive, and other structural applications. One of the most used alloys as a matrix is nickel alloys, which meet the need for high-temperature mechanical properties; some attempts have been made to develop nickel base composites reinforced by high melt point and high modulus particulates. Among the carbides used as reinforcing particulates, chromium carbide is interesting for wear applications; it is widely used as a tribological coating material in high-temperature applications requiring high wear resistance and hardness. Moreover, a set of properties make it suitable for use in MMCs, such as toughness, the good corrosion and oxidation resistance of its three polymorphs -the cubic (Cr23C6), the hexagonal (Cr7C3), and the orthorhombic (Cr3C2)-, and it’s coefficient of thermal expansion that is almost equal to that of metals. The in-situ synthesis of CrC-reinforced Ni matrix composites could be achieved by the powder metallurgy route. To ensure the in-situ reactions during the sintering process, the use of phase precursors is necessary. Recently, new precursor materials have been proposed; these materials are called MAX phases. The MAX phases are thermodynamically stable nano-laminated materials displaying unusual and sometimes unique properties. These novel phases possess Mn+1AXn chemistry, where n is 1, 2, or 3, M is an early transition metal element, A is an A-group element, and X is C or N. Herein, the pressureless sintering method is used to elaborate Ni/Cr2AlC composites. Four composites were elaborated from 5, 10, 15 and 20 wt% of Cr2AlC MAX phase precursor which fully reacted with Ni-matrix at 1100 °C sintering temperature for 4 h in argon atmosphere. XRD results showed that Cr2AlC MAX phase was totally decomposed forming chromium carbide Cr7C3, and the released Al and Cr atoms diffused in Ni matrix giving rise to γ-Ni(Al,Cr) solid solution and γ’-Ni3(Al,Cr) intermetallic. Scanning Electron Microscopy (SEM) of the elaborated samples showed the presence of nanosized Cr7C3 reinforcing particles embedded in the Ni metal matrix, which have a direct impact on the tribological properties of the composites and their hardness. All the composites exhibited higher hardness than pure Ni; whereas adding 15 wt% of Cr2AlC gives the highest hardness (1.85 GPa). Using a ball-on-disc tribometer, dry sliding tests for the elaborated composites against 100Cr6 steel ball were studied under different applied loads. The microstructures and worn surface characteristics were then analyzed using SEM and Raman spectroscopy. The results show that all the composites exhibited better wear resistance compared to pure Ni, which could be explained by the formation of a lubricious tribo-layer during sliding and the good bonding between the Ni matrix and the reinforcing phases.

Keywords: composites, microscopy, sintering, wear

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