Search results for: KMnO4

Authors: Ashish Kumar, Tejendra Dixit, I. A. Palani, Vipul Singh

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Zinc oxide, with its interesting properties such as large band gap (3.37eV), high exciton binding energy (60 meV) and intense UV absorption has been studied in literature for various applications viz. optoelectronics, biosensors, UV-photodetectors etc. The performance of ZnO devices is highly influenced by morphologies, size, crystallinity of the ZnO active layer and processing conditions. Recently, our group has shown the influence of the in situ addition of KMnO4 in the precursor solution during the hydrothermal growth of ZnO nanorods (NRs) on their near band edge (NBE) emission. In this paper, we have investigated the effect of post-growth annealing on the variations in NBE and deep level (DL) emissions of as grown ZnO nanorods. These observed results have been explained on the basis of X-ray Diffraction (XRD) and Raman spectroscopic analysis, which clearly show that improved crystalinity and quantum confinement in ZnO nanorods.

Keywords: ZnO, nanorods, hydrothermal, KMnO4

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Authors: Mayoorika Shukla, Pramila Jakhar, Tejendra Dixit, I. A. Palani, Vipul Singh

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Biosensors are analytical devices with wide range of applications in biological, chemical, environmental and clinical analysis. It comprises of bio-recognition layer which has biomolecules (enzymes, antibodies, DNA, etc.) immobilized over it for detection of analyte and transducer which converts the biological signal into the electrical signal. The performance of biosensor primarily the depends on the bio-recognition layer and therefore it has to be chosen wisely. In this regard, nanostructures of metal oxides such as ZnO, SnO2, V2O5, and TiO2, etc. have been explored extensively as bio-recognition layer. Recently, ZnO has the attracted attention of researchers due to its unique properties like high iso-electric point, biocompatibility, stability, high electron mobility and high electron binding energy, etc. Although there have been many reports on usage of ZnO as bio-recognition layer but to the authors’ knowledge, none has ever observed correlation between optical properties like defect suppression and biosensing capability of the sensor. Here, ZnO nanorods (ZNR) have been synthesized by a low cost, simple and low-temperature hydrothermal growth process, over Platinum (Pt) coated glass substrate. The ZNR have been synthesized in two steps viz. initially a seed layer was coated over substrate (Pt coated glass) followed by immersion of it into nutrient solution of Zinc nitrate and Hexamethylenetetramine (HMTA) with in situ addition of KMnO4. The addition of KMnO4 was observed to have a profound effect over the growth rate anisotropy of ZnO nanostructures. Clustered and powdery growth of ZnO was observed without addition of KMnO4, although by addition of it during the growth, uniform and crystalline ZNR were found to be grown over the substrate. Moreover, the same has resulted in suppression of defects as observed by Normalized Photoluminescence (PL) spectra since KMnO4 is a strong oxidizing agent which provides an oxygen rich growth environment. Further, to explore the correlation between defect suppression and biosensing capability of the ZNR Glucose oxidase (Gox) was immobilized over it, using physical adsorption technique followed by drop casting of nafion. Here the main objective of the work was to analyze effect of defect suppression over biosensing capability, and therefore Gox has been chosen as model enzyme, and electrochemical amperometric glucose detection was performed. The incorporation of KMnO4 during growth has resulted in variation of optical and charge transfer properties of ZNR which in turn were observed to have deep impact on biosensor figure of merits. The sensitivity of biosensor was found to increase by 12-18 times, due to variations introduced by addition of KMnO4 during growth. The amperometric detection of glucose in continuously stirred buffer solution was performed. Interestingly, defect suppression has been observed to contribute towards the improvement of biosensor performance. The detailed mechanism of growth of ZNR along with the overall influence of defect suppression on the sensing capabilities of the resulting enzymatic electrochemical biosensor and different figure of merits of the biosensor (Glass/Pt/ZNR/Gox/Nafion) will be discussed during the conference.

Keywords: biosensors, defects, KMnO4, ZnO nanorods

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Authors: T. P. Sathishkumar, P. Navaneethakrishnan

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The research work investigates the variation of tensile properties for the sansevieria ehrenbergii fiber (SEF) and SEF reinforced polyester composites respect to various water absorption time. The experiments were conducted according to ATSM D3379-75 and ASTM D570 standards. The percentage of water absorption for composite specimens was measured according to ASTM D570 standard. The fiber of SE was cut in to 30 mm length for preparation of the composites. The simple hand lay-up method followed by compression moulding process adopted to prepare the randomly oriented SEF reinforced polyester composites at constant fiber weight fraction of 40%. The surface treatment was done on the SEFs with various chemicals such as NaOH, KMnO4, Benzoyl Peroxide, Benzoyl Chloride and Stearic Acid before preparing the composites. NaOH was used for pre-treatment of all other chemical treatments. The morphology of the tensile fractured specimens studied using the Scanning Electron Microscopic. The tensile strength of the SEF and SEF reinforced polymer composites were carried out with various water absorption time such as 4, 8, 12, 16, 20 and 24 hours respectively. The result shows that the tensile strength was drop off with increase in water absorption time for all composites. The highest tensile property of raw fiber was found due to lowest moistures content. Also the chemical bond between the cellulose and cementic materials such as lignin and wax was highest due to lowest moisture content. Tensile load was lowest and elongation was highest for the water absorbed fibers at various water absorption time ranges. During this process, the fiber cellulose inhales the water and expands the primary and secondary fibers walls. This increases the moisture content in the fibers. Ultimately this increases the hydrogen cation and the hydroxide anion from the water. In tensile testing, the water absorbed fibers shows highest elongation by stretching of expanded cellulose walls and the bonding strength between the fiber cellulose is low. The load carrying capability was stable at 20 hours of water absorption time. This could be directly affecting the interfacial bonding between the fiber/matrix and composite strength. The chemically treated fibers carry higher load and lower elongation which is due to removal of lignin, hemicellulose and wax content. The water time absorption decreases the tensile strength of the composites. The chemically SEF reinforced composites shows highest tensile strength compared to untreated SEF reinforced composites. This was due to highest bonding area between the fiber/matrix. This was proven in the morphology at the fracture zone of the composites. The intra-fiber debonding was occurred by water capsulation in the fiber cellulose. Among all, the tensile strength was found to be highest for KMnO4 treated SEF reinforced composite compared to other composites. This was due to better interfacial bonding between the fiber-matrix compared to other treated fiber composites. The percentage of water absorption of composites increased with time of water absorption. The percentage weight gain of chemically treated SEF composites at 4 hours to zero water absorption are 9, 9, 10, 10.8 and 9.5 for NaOH, BP, BC, KMnO4 and SA respectively. The percentage weight gain of chemically treated SEF composites at 24 hours to zero water absorption 5.2, 7.3, 12.5, 16.7 and 13.5 for NaOH, BP, BC, KMnO4 and SA respectively. Hence the lowest weight gain was found for KMnO4 treated SEF composites by highest percentage with lowest water uptake. However the chemically treated SEF reinforced composites is possible materials for automotive application like body panels, bumpers and interior parts, and household application like tables and racks etc.

Keywords: fibres, polymer-matrix composites (PMCs), mechanical properties, scanning electron microscopy (SEM)

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Authors: Aipeng Zhu, Yun Zhang

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The growing grievous environment problems together with the exhaustion of energy resources put urgent demands for developing high energy density. Considering the factors including capacity, resource and environment, Manganese-based lithium-rich layer-structured cathode materials xLi₂MnO₃⋅(1-x)LiMO₂ (M = Ni, Co, Mn, and other metals) are drawing increasing attention due to their high reversible capacities, high discharge potentials, and low cost. They are expected to be one type of the most promising cathode materials for the next-generation Li-ion batteries (LIBs) with higher energy densities. Unfortunately, their commercial applications are hindered with crucial drawbacks such as poor rate performance, limited cycle life and continuous falling of the discharge potential. With decades of extensive studies, significant achievements have been obtained in improving their cyclability and rate performances, but they cannot meet the requirement of commercial utilization till now. One major problem for lithium-rich layer-structured cathode materials (LLOs) is the side reaction during cycling, which leads to severe surface degradation. In this process, the metal ions can dissolve in the electrolyte, and the surface phase change can hinder the intercalation/deintercalation of Li ions and resulting in low capacity retention and low working voltage. To optimize the LLOs cathode material, the surface coating is an efficient method. Considering the price and stability, Al₂O₃ was used as a coating material in the research. Meanwhile, due to the low initial Coulombic efficiency (ICE), the pristine LLOs was pretreated by KMnO₄ to increase the ICE. The precursor was prepared by a facile coprecipitation method. The as-prepared precursor was then thoroughly mixed with Li₂CO₃ and calcined in air at 500℃ for 5h and 900℃ for 12h to produce Li₁.₂[Ni₀.₂Mn₀.₆]O₂ (LNMO). The LNMO was then put into 0.1ml/g KMnO₄ solution stirring for 3h. The resultant was filtered and washed with water, and dried in an oven. The LLOs obtained was dispersed in Al(NO₃)₃ solution. The mixture was lyophilized to confer the Al(NO₃)₃ was uniformly coated on LLOs. After lyophilization, the LLOs was calcined at 500℃ for 3h to obtain LNMO@LMO@ALO. The working electrodes were prepared by casting the mixture of active material, acetylene black, and binder (polyvinglidene fluoride) dissolved in N-methyl-2-pyrrolidone with a mass ratio of 80: 15: 5 onto an aluminum foil. The electrochemical performance tests showed that the multiple surface modified materials had a higher initial Coulombic efficiency (84%) and better capacity retention (91% after 100 cycles) compared with that of pristine LNMO (76% and 80%, respectively). The modified material suggests that the KMnO₄ pretreat and Al₂O₃ coating can increase the ICE and cycling stability.

Keywords: Li-rich materials, surface coating, lithium ion batteries, Al₂O₃

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Authors: Rashad Al-Gaashani, Muataz A. Atieh

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In this study, the effect of preparation temperature, namely room temperature (RT), 40, 60, and 85°C, on producing of high-quality graphene oxide (GO) has been investigated. GO samples have been prepared by chemical oxidation of graphite via a safe improved chemical technique using a blend of two deferent acids: sulphuric acid (H₂SO₄) and phosphoric acid (H₃PO₄) with volume ratio 4:1, respectively. potassium permanganate (KMnO₄) and hydrogen peroxide (H₂O₂) were applied as oxidizing agents. In this work, sodium nitrate (NaNO₃) was excluded, so the emission of hazardous explosive gases such as NO₂ and N₂O₂ was shunned. Ice and oil baths were used to carefully control the temperature. Several characterization instruments including X-Ray diffraction, transmission electron microscopy, scanning electron microscopy, electron dispersive spectroscopy, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, and UV-vis spectroscopy were used to study and compare the synthesized samples. The results indicated that GO can be prepared at RT with graphite oxide, and the purity of GO increased with rising of the solvent temperature. Optical properties of GO samples were studied using UV-vis absorption spectra.

Keywords: chemical method, graphite, graphene oxide, optical properties

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Authors: Charirat Kusonwiriyawong, Supha Photichan, Wannarut Chutibutr

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Soil test kits for rapid analysis of the organic matter, available phosphorus and exchangeable potassium were developed to drive a low-cost field testing kit to farmers. The objective was to provide a decision tool for improving soil fertility. One aspect of soil test kit development was ease of use which is a time requirement for completing organic matter, available phosphorus and exchangeable potassium test in one soil sample. This testing kit required only two extractions and utilized no filtration consuming approximately 15 minutes per sample. Organic matter was principally created by oxidizing carbon KMnO₄ using the standard color chart. In addition, modified single extractant (Mehlich I) was applied to extract available phosphorus and exchangeable potassium. Molybdenum blue method and turbidimetric method using standard color chart were adapted to analyze available phosphorus and exchangeable potassium, respectively. Modified single extractant using in soil test kits were highly significant matching with analytical laboratory results (r=0.959** and 0.945** for available phosphorus and exchangeable potassium, respectively). Linear regressions were statistically calculated between modified single extractant and standard laboratory analysis (y=0.9581x-12.973 for available phosphorus and y=0.5372x+15.283 for exchangeable potassium, respectively). These equations were calibrated to formulate a fertilizer rate recommendation for specific corps. To validate quality, soil test kits were distributed to farmers and extension workers. We found that the accuracy of soil test kits were 71.0%, 63.9% and 65.5% for organic matter, available phosphorus, and exchangeable potassium, respectively. The quantitative survey was also conducted in order to assess their satisfaction with soil test kits. The survey showed that more than 85% of respondents said these testing kits were more convenient, economical and reliable than the other commercial soil test kits. Based upon the finding of this study, soil test kits can be another alternative for providing soil analysis and fertility recommendations when a soil testing laboratory is not available.

Keywords: available phosphorus, exchangeable potassium, modified single extractant, organic matter, soil test kits

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Authors: Neeraj Neeraj, Soumen Basu, Banibrata Maity

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Glutathione (GSH) is one of the most important biomolecules having small molecular weight, which helps in various cellular functions like regulation of gene, xenobiotic metabolism, preservation of intracellular redox activities, signal transduction, etc. Therefore, the detection of GSH requires huge attention by using extremely selective and sensitive techniques. Herein, a rapid fluorometric nanosensor is designed by combining carbon dots (Cdots) and MnO₂ nanoparticles of different sizes for the detection of GSH. The bottom-up approach, i.e., microwave method, was used for the preparation of the water soluble and greatly fluorescent Cdots by using ascorbic acid as a precursor. MnO₂ nanospheres of different sizes (large, medium, and small) were prepared by varying the ratio of concentration of methionine and KMnO₄ at room temperature, which was confirmed by HRTEM analysis. The successive addition of MnO₂ nanospheres in Cdots results fluorescence quenching. From the fluorescence intensity data, Stern-Volmer quenching constant values (KS-V) were evaluated. From the fluorescence intensity and lifetime analysis, it was found that the degree of fluorescence quenching of Cdots followed the order: large > medium > small. Moreover, fluorescence recovery studies were also performed in the presence of GSH. Fluorescence restoration studies also show the order of turn on follows the same order, i.e., large > medium > small, which was also confirmed by quantum yield and lifetime studies. The limits of detection (LOD) of GSH in presence of Cdots@different sized MnO₂ nanospheres were also evaluated. It was observed thatLOD values were in μM region and lowest in case of large MnO₂ nanospheres. The separation distance (d) between Cdots and the surface of different MnO₂ nanospheres was determined. The d values increase with increase in the size of the MnO₂ nanospheres. In summary, the synthesized Cdots@MnO₂ nanocomposites acted as a rapid, simple, economical as well as environmental-friendly nanosensor for the detection of GSH.

Keywords: carbon dots, fluorescence, glutathione, MnO₂ nanospheres, turn off-on

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Authors: Saeed Bagherifam, Trevor Brown, Chris Fellows, Ravi Naidu

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Over the last century, rapid urbanization, industrial emissions, and mining activities have resulted in widespread contamination of the environment by heavy metal(loid)s. Arsenic (As) is a toxic metalloid belonging to group 15 of the periodic table, which occurs naturally at low concentrations in soils and the earth’s crust, although concentrations can be significantly elevated in natural systems as a result of dispersion from anthropogenic sources, e.g., mining activities. Bioavailability is the fraction of a contaminant in soils that is available for uptake by plants, food chains, and humans and therefore presents the greatest risk to terrestrial ecosystems. Numerous attempts have been made to establish in situ and ex-situ technologies of remedial action for remediation of arsenic-contaminated soils. In situ stabilization techniques are based on deactivation or chemical immobilization of metalloid(s) in soil by means of soil amendments, which consequently reduce the bioavailability (for biota) and bioaccessibility (for humans) of metalloids due to the formation of low-solubility products or precipitates. This study investigated the effectiveness of two different types of synthetic manganese and iron oxides (birnessite and goethite) for stabilization of As in a soil spiked with 1000 mg kg⁻¹ of As and treated with 10% dosages of soil amendments. Birnessite was made using HCl and KMnO₄, and goethite was synthesized by the dropwise addition of KOH into Fe(NO₃) solution. The resulting contaminated soils were subjected to a series of chemical extraction studies including sequential extraction (BCR method), single-step extraction with distilled (DI) water, 2M HNO₃ and simplified bioaccessibility extraction tests (SBET) for estimation of bioaccessible fractions of As in two different soil fractions ( < 250 µm and < 2 mm). Concentrations of As in samples were measured using inductively coupled plasma mass spectrometry (ICP-MS). The results showed that soil with birnessite reduced bioaccessibility of As by up to 92% in both soil fractions. Furthermore, the results of single-step extractions revealed that the application of both birnessite and Goethite reduced DI water and HNO₃ extractable amounts of arsenic by 75, 75, 91, and 57%, respectively. Moreover, the results of the sequential extraction studies showed that both birnessite and goethite dramatically reduced the exchangeable fraction of As in soils. However, the amounts of recalcitrant fractions were higher in birnessite, and Goethite amended soils. The results revealed that the application of both birnessite and goethite significantly reduced bioavailability and the exchangeable fraction of As in contaminated soils, and therefore birnessite and Goethite amendments might be considered as promising adsorbents for stabilization and remediation of As contaminated soils.

Keywords: arsenic, bioavailability, in situ stabilisation, metalloid(s) contaminated soils

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Authors: S. J. Kim, Y. J. Yoo

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Slack-tide sampling was carried out at seven stations at high and low tides for a tidal cycle, in summer (7, 8, 9) and fall (10), 2016 to determine the differences of water quality according to tides in Masan Bay. The data were analyzed by Pearson correlation and factor analysis. The mixing state of all the water quality components investigated is well explained by the correlation with salinity (SAL). Turbidity (TURB), dissolved silica (DSi), nitrite and nitrate nitrogen (NNN) and total nitrogen (TN), which find their way into the bay from the streams and have no internal source and sink reaction, showed a strong negative correlation with SAL at low tide, indicating the property of conservative mixing. On the contrary, in summer and fall, dissolved oxygen (DO), hydrogen sulfide (H2S) and chemical oxygen demand with KMnO4 (CODMn) of the surface and bottom water, which were sensitive to an internal source and sink reaction, showed no significant correlation with SAL at high and low tides. The remaining water quality parameters showed a conservative or a non-conservative mixing pattern depending on the mixing characteristics at high and low tides, determined by the functional relationship between the changes of the flushing time and the changes of the characteristics of water quality components of the end-members in the bay. Factor analysis performed on the concentration difference data sets between high and low tides helped in identifying the principal latent variables for them. The concentration differences varied spatially and temporally. Principal factors (PFs) scores plots for each monitoring situation showed high associations of the variations to the monitoring sites. At sampling station 1 (ST1), temperature (TEMP), SAL, DSi, TURB, NNN and TN of the surface water in summer, TEMP, SAL, DSi, DO, TURB, NNN, TN, reactive soluble phosphorus (RSP) and total phosphorus (TP) of the bottom water in summer, TEMP, pH, SAL, DSi, DO, TURB, CODMn, particulate organic carbon (POC), ammonia nitrogen (AMN), NNN, TN and fecal coliform (FC) of the surface water in fall, TEMP, pH, SAL, DSi, H2S, TURB, CODMn, AMN, NNN and TN of the bottom water in fall commonly showed up as the most significant parameters and the large concentration differences between high and low tides. At other stations, the significant parameters showed differently according to the spatial and temporal variations of mixing pattern in the bay. In fact, there is no estuary that always maintains steady-state flow conditions. The mixing regime of an estuary might be changed at any time from linear to non-linear, due to the change of flushing time according to the combination of hydrogeometric properties, inflow of freshwater and tidal action, And furthermore the change of end-member conditions due to the internal sinks and sources makes the occurrence of concentration difference inevitable. Therefore, when investigating the water quality of the estuary, it is necessary to take a sampling method considering the tide to obtain average water quality data.

Keywords: conservative mixing, end-member, factor analysis, flushing time, high and low tide, latent variables, non-conservative mixing, slack-tide sampling, spatial and temporal variations, surface and bottom water

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