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Sample records for thermogravimetric analysis shows

  1. Thermogravimetric Analysis Laboratory

    Data.gov (United States)

    Federal Laboratory Consortium — At NETL’s Thermogravimetric Analysis Laboratory in Morgantown, WV, researchers study how chemical looping combustion (CLC) can be applied to fossil energy systems....

  2. Thermogravimetric analysis of biowastes during combustion

    International Nuclear Information System (INIS)

    Otero, M.; Sanchez, M.E.; Gomez, X.; Moran, A.

    2010-01-01

    The combustion of sewage sludge (SS), animal manure (AM) and the organic fraction of municipal solid waste (OFMSW) was assessed and compared with that of a semianthracite coal (SC) and of a PET waste by thermogravimetric (TG) analysis. Differences were found in the TG curves obtained for the combustion of these materials accordingly to their respective proximate analysis. Non-isothermal thermogravimetric data were used to assess the kinetics of the combustion of these biowastes. The present paper reports on the application of the Vyazovkin model-free isoconversional method for the evaluation of the activation energy necessary for the combustion of these biowastes. The activation energy related to SS combustion (129.1 kJ/mol) was similar to that corresponding to AM (132.5 kJ/mol) while the OFMSW showed a higher value (159.3 kJ/mol). These values are quite higher than the one determined in the same way for the combustion of SC (49.2 kJ/mol) but lower than that for the combustion of a PET waste (165.6 kJ/mol).

  3. Thermogravimetric analysis in the characterization of colombian coals used in the production of coke

    International Nuclear Information System (INIS)

    Guerrero, Camilo; Salamanca, Monica E; Diaz, Jose de J

    2010-01-01

    Five types of coal from the states of Cundinamarca, Boyaca and Norte de Santander (Colombia) were characterized by proximate, ultimate, rheological, petrographic, calorific and thermogravimetric analysis. The parameters used, especially the ones which determine the rheological properties show that the studied coals and its blends could produce good quality coke. It was observed the inverse relationship between the volatile matter content and the mean vitrinite reflectance, relationship which is attributed to the increase of the aromaticity in the molecular structure of the coal as a consequence of the rank increase. The parameters derived from the thermogravimetric analysis, maximum velocity of de-volatilization and the temperature of maximum velocity of de-volatilization and the media reflectance of the vitrinite showed good correlations. Also was observed an interesting correlation between the velocity of de-volatilization and maximum fluidity. This shows that the thermogravimetric analysis can be a useful tool to characterize in a quick way coals used for metallurgical coke production.

  4. Thermogravimetric analysis and dissociation pressure of caesium trihalides

    International Nuclear Information System (INIS)

    Harris, G.S.; McKechnie, J.S.

    1982-01-01

    We have carried out a thermogravimetric study of caesium trihalides to obtain, from the procedural decomposition temperatures, an order of apparent thermal stability which could be compared with the order of thermodynamic stability obtained from vapour pressure measurements. Thermogravimetric analysis could also prove to be a useful method for rapid analysis of metal polyhalides. The thermograms indicated a one-step decomposition for each compound; the procedural decomposition temperatures and percentage weight losses obtained are given. Dissociation pressures were measured and values of equilibrium constant and enthalpy of dissociation were calculated. The results are given. The 'stability' order obtained is discussed. (U.K.)

  5. Thermogravimetric-quadrupole mass-spectrometric analysis of geochemical samples.

    Science.gov (United States)

    Gibson, E. K., Jr.; Johnson, S. M.

    1972-01-01

    Thermogravimetric-quadrupole mass-spectrometric-analysis techniques can be used to study a wide variety of problems involving decomposition processes and identification of released volatile components. A recording vacuum thermoanalyzer has been coupled with a quadrupole mass spectrometer. The rapid scan capabilities of the quadrupole mass spectrometer are used to identify the gaseous components released. The capability of the thermogravimetric-quadrupole mass spectrometer to provide analytical data for identification of the released volatile components, for determination of their sequence of release and for correlation of thermal-decomposition studies is illustrated by an analysis of the Orgueil carbonaceous chondrite.

  6. Thermogravimetric analysis of forest understory grasses

    Science.gov (United States)

    Thomas Elder; John S. Kush; Sharon M. Hermann

    2011-01-01

    Forest understory grasses are of significance in the initiation, establishment and maintenance of fire, whether used as a management tool or when occurring as wildfire. The fundamental thermal properties of such grasses are critical to their behavior in fire situations and have been investigated in the current work by the application of thermogravimetric analysis (TGA...

  7. Thermogravimetric analysis of the polymer acrylate-vinyl ether mixture cured by radiation

    International Nuclear Information System (INIS)

    Danu, Sugiarto

    1998-01-01

    An experiment on thermal stability of the polymer acrylate-vinyl ether mixture cured by radiation have been done using thermogravimetric analysis. Three kinds of acrylic oligomers i.e., epoxy acrylate, urethane acrylate, and polypropylene glycol diacrylate, and vinyl ether monomers i.e., triethylene glycol divinyl ether (DVE-3), 1,4-cyclohexane dimethanol divinyl ether (CHVE), and butanediol monovinyl ether (HBVE) were used in the experiment. Reaction was taken via radical and cationic polymerisation. In case of cationic polymerisation, diphenyliodonium hexafluorophosphate fotoinisiator was used in the formulation. Thermogravimetric analysis was conducted in a nitrogen atmosphere at a flow rate of 40 ml/minute with a constant heating rate 10 o C and evaluation range were done from 25 to 500 o C. The results of thermogravimetric analysis showed that acrylate and DVE-3 mixture produced the polymer films with higher thermal stability than the mixture of acrylate with CHVE or HBVE. The composition of acrylate-vinyl ether mixture and degree of unsaturation of vinyl ether monomers influenced the thermal stability of polymer. The mixture of epoxy acrylate-vinyl ether and polypropylene glycol diacrylate-vinyl ether have 1 initial decomposition temperature whereas the urethane acrylate-vinyl ether mixture has 2 initial decomposition temperatures. (authors)

  8. Thermogravimetric analysis and thermal degradation behaviour of advanced PMR-X carbon fiber composites

    International Nuclear Information System (INIS)

    Rngie, M.

    2003-01-01

    Thermal degradation behavior of sized and unsized carbon fibers in polyimide matrix was investigated. Degradation of neat resin and unidirectional laminates were investigated by thermogravimetric analysis technique at temperatures between 470 d ig C -650 d ig C and up to 250 h rs. Isothermal ageing of the PMR-X composite samples under different test conditions (i. e. different temperatures and prolonged aging times), showed that oxidation and degradation occurs in stage three different rates. Thermogravimetric analysis showed that the cured PMR-X composite panels are more stable in an inert atmosphere (nitrogen atmosphere)than in air and the degradation of neat resin is much higher than the composite samples. However, the rate of degradation of the unsized untreated carbon fibers in nitrogen environment is much higher than that for the PMR-X composites containing sized fibers

  9. Thermal decomposition characteristics of microwave liquefied rape straw residues using thermogravimetric analysis

    Science.gov (United States)

    Xingyan Huang; Cornelis F. De Hoop; Jiulong Xie; Chung-Yun Hse; Jinqiu Qi; Yuzhu Chen; Feng Li

    2017-01-01

    The thermal decomposition characteristics of microwave liquefied rape straw residues with respect to liquefaction condition and pyrolysis conversion were investigated using a thermogravimetric (TG) analyzer at the heating rates of 5, 20, 50 °C min-1. The hemicellulose decomposition peak was absent at the derivative thermogravimetric analysis (DTG...

  10. Heater-Integrated Cantilevers for Nano-Samples Thermogravimetric Analysis

    OpenAIRE

    Toffoli, Valeria; Carrato, Sergio; Lee, Dongkyu; Jeon, Sangmin; Lazzarino, Marco

    2013-01-01

    The design and characteristics of a micro-system for thermogravimetric analysis (TGA) in which heater, temperature sensor and mass sensor are integrated into a single device are presented. The system consists of a suspended cantilever that incorporates a microfabricated resistor, used as both heater and thermometer. A three-dimensional finite element analysis was used to define the structure parameters. TGA sensors were fabricated by standard microlithographic techniques and tested using mill...

  11. Kinetic parameters from thermogravimetric analysis

    Science.gov (United States)

    Kiefer, Richard L.

    1993-01-01

    High performance polymeric materials are finding increased use in aerospace applications. Proposed high speed aircraft will require materials to withstand high temperatures in an oxidative atmosphere for long periods of time. It is essential that accurate estimates be made of the performance of these materials at the given conditions of temperature and time. Temperatures of 350 F (177 C) and times of 60,000 to 100,000 hours are anticipated. In order to survey a large number of high performance polymeric materials on a reasonable time scale, some form of accelerated testing must be performed. A knowledge of the rate of a process can be used to predict the lifetime of that process. Thermogravimetric analysis (TGA) has frequently been used to determine kinetic information for degradation reactions in polymeric materials. Flynn and Wall studied a number of methods for using TGA experiments to determine kinetic information in polymer reactions. Kinetic parameters, such as the apparent activation energy and the frequency factor, can be determined in such experiments. Recently, researchers at the McDonnell Douglas Research Laboratory suggested that a graph of the logarithm of the frequency factor against the apparent activation energy can be used to predict long-term thermo-oxidative stability for polymeric materials. Such a graph has been called a kinetic map. In this study, thermogravimetric analyses were performed in air to study the thermo-oxidative degradation of several high performance polymers and to plot their kinetic parameters on a kinetic map.

  12. Thermogravimetric Analysis of Single-Wall Carbon Nanotubes

    Science.gov (United States)

    Arepalli, Sivram; Nikolaev, Pavel; Gorelik, Olga

    2010-01-01

    An improved protocol for thermogravimetric analysis (TGA) of samples of single-wall carbon nanotube (SWCNT) material has been developed to increase the degree of consistency among results so that meaningful comparisons can be made among different samples. This improved TGA protocol is suitable for incorporation into the protocol for characterization of carbon nanotube material. In most cases, TGA of carbon nanotube materials is performed in gas mixtures that contain oxygen at various concentrations. The improved protocol is summarized.

  13. Study and Thermogravimetric analysis of Poly N-4 Aminostyrol

    International Nuclear Information System (INIS)

    Meghezzi, A.; Lakhdar, Y.; Saidi, M.; Dadamoussa, B.

    2006-01-01

    The polyaminostyrol samples (PAS) and their copolymers with the styrol differing in position and quantity of amino-group, were obtained by polymerization of monomers on cyclogexan solution. The observed thermal effects were analyzed by the differential thermal analysis combined with a thermogravimetric analysis. It was found that the introduction of amino-groups into the polystyrols increased the temperature of total degradation of polymer from 150 till 260C. The increase in thermostability may be explained by the cohesion of macromolecules with the participation of amino-groups, which results in ammonium evolution, as well as in the decrease of valence area band of -NH2 grouping the region 3370-34440 cm. It was showed that the degree of cohesion formation and thermolysis rate depended on amino-group and their position into the cycle of benzene. (author)

  14. Isothermal thermogravimetric data acquisition analysis system

    Science.gov (United States)

    Cooper, Kenneth, Jr.

    1991-01-01

    The description of an Isothermal Thermogravimetric Analysis (TGA) Data Acquisition System is presented. The system consists of software and hardware to perform a wide variety of TGA experiments. The software is written in ANSI C using Borland's Turbo C++. The hardware consists of a 486/25 MHz machine with a Capital Equipment Corp. IEEE488 interface card. The interface is to a Hewlett Packard 3497A data acquisition system using two analog input cards and a digital actuator card. The system provides for 16 TGA rigs with weight and temperature measurements from each rig. Data collection is conducted in three phases. Acquisition is done at a rapid rate during initial startup, at a slower rate during extended data collection periods, and finally at a fast rate during shutdown. Parameters controlling the rate and duration of each phase are user programmable. Furnace control (raising and lowering) is also programmable. Provision is made for automatic restart in the event of power failure or other abnormal terminations. Initial trial runs were conducted to show system stability.

  15. Heater-Integrated Cantilevers for Nano-Samples Thermogravimetric Analysis

    Science.gov (United States)

    Toffoli, Valeria; Carrato, Sergio; Lee, Dongkyu; Jeon, Sangmin; Lazzarino, Marco

    2013-01-01

    The design and characteristics of a micro-system for thermogravimetric analysis (TGA) in which heater, temperature sensor and mass sensor are integrated into a single device are presented. The system consists of a suspended cantilever that incorporates a microfabricated resistor, used as both heater and thermometer. A three-dimensional finite element analysis was used to define the structure parameters. TGA sensors were fabricated by standard microlithographic techniques and tested using milli-Q water and polyurethane microcapsule. The results demonstrated that our approach provides a faster and more sensitive TGA with respect to commercial systems.

  16. Thermogravimetric analysis-mass spectrometry (TG-MS) of selected Chinese palygorskites-Implications for structural water

    International Nuclear Information System (INIS)

    Cheng, Hongfei; Yang, Jing; Frost, Ray L.

    2011-01-01

    Four Chinese palygorskites clay minerals have been analysed by thermogravimetric analysis-mass spectrometry and X-ray diffraction. The structural water of the palygorskite dehydrates in the temperature range of 30-625 o C, as shown in the thermogravimetric analysis and mass spectrometric curves. The mass spectrometric curves combined the differential thermogravimetric curves enable the detailed determination of the main dehydration steps. The results show that the dehydration occurs in four main steps: (a) elimination of interparticle water and partial zeolitic water at below 110 o C, (b) release of the rest part of zeolitic water from the structural layer of palygorskite at about 160 o C, (c) dehydration of one part of bound water at about 340 o C and (d) loss of the rest part of bound water at around 450 o C. The temperatures of dehydration of the palygorskite minerals are found to be influenced by the geological environment and the amount and kind of impurities. The evolved gases in the decomposition process are various because of the different amounts and kind of impurities. It is also found that decarbonization takes place at around 600 o C due to the decomposition of calcite and dolomite impurities in these minerals. It is evident by the mass spectrometric curve that the water is given out from the samples and carbon dioxide originates from the impurity calcite and dolomite.

  17. Thermal analysis of thermo-gravimetric measurements of spent nuclear fuel oxidation rates

    International Nuclear Information System (INIS)

    Cramer, E.R.

    1997-01-01

    A detailed thermal analysis was completed of the sample temperatures in the Thermo-Gravimetric Analysis (TGA) system used to measure irradiated N Reactor fuel oxidation rates. Sample temperatures during the oxidation process did not show the increase which was postulated as a result of the exothermic reactions. The analysis shows the axial conduction of heat in the sample holder effectively removes the added heat and only a very small, i.e., <10 C, increase in temperature is calculated. A room temperature evaporation test with water showed the sample thermocouple sensitivity to be more than adequate to account for a temperature change of approximately 5 C. Therefore, measured temperatures in the TGA are within approximately 10 C of the actual sample temperatures and no adjustments to reported data to account for the heat input from the oxidation process are necessary

  18. Characterization and thermogravimetric analysis of lanthanide hexafluoroacetylacetone chelates.

    Science.gov (United States)

    Shahbazi, Shayan; Stratz, S Adam; Auxier, John D; Hanson, Daniel E; Marsh, Matthew L; Hall, Howard L

    2017-01-01

    This work reports the thermodynamic characterizations of organometallic species as a vehicle for the rapid separation of volatile nuclear fission products via gas chromatography due to differences in adsorption enthalpy. Because adsorption and sublimation thermodynamics are linearly correlated, there is considerable motivation to determine sublimation enthalpies. A method of isothermal thermogravimetric analysis, TGA-MS and melting point analysis are employed on thirteen lanthanide 1,1,1,5,5,5-hexafluoroacetylacetone complexes to determine sublimation enthalpies. An empirical correlation is used to estimate adsorption enthalpies of lanthanide complexes on a quartz column from the sublimation data. Additionally, four chelates are characterized by SC-XRD, elemental analysis, FTIR and NMR.

  19. Thermogravimetric analysis of reactor-neutrons-irradiated LEXAN polycarbonate film

    International Nuclear Information System (INIS)

    Kalsi, P.C.

    2000-01-01

    The effects of reactor-neutrons irradiation on the thermogravimetric (TG) analysis of LEXAN polycarbonate film in air were studied. Irradiation enhances the degradation rate and the effect increases further with increasing neutron fluence. The kinetics of the different steps of degradation were also evaluated from the TG curves. The activation energy values calculated for all the degradation stages decrease on irradiation. (author)

  20. Heater-Integrated Cantilevers for Nano-Samples Thermogravimetric Analysis

    Directory of Open Access Journals (Sweden)

    Valeria Toffoli

    2013-12-01

    Full Text Available The design and characteristics of a micro-system for thermogravimetric analysis (TGA in which heater, temperature sensor and mass sensor are integrated into a single device are presented. The system consists of a suspended cantilever that incorporates a microfabricated resistor, used as both heater and thermometer. A three-dimensional finite element analysis was used to define the structure parameters. TGA sensors were fabricated by standard microlithographic techniques and tested using milli-Q water and polyurethane microcapsule. The results demonstrated that our approach provides a faster and more sensitive TGA with respect to commercial systems.

  1. Thermogravimetric analysis coupled with chemometrics as a powerful predictive tool for ß-thalassemia screening.

    Science.gov (United States)

    Risoluti, Roberta; Materazzi, Stefano; Sorrentino, Francesco; Maffei, Laura; Caprari, Patrizia

    2016-10-01

    β-Thalassemia is a hemoglobin genetic disorder characterized by the absence or reduced β-globin chain synthesis, one of the constituents of the adult hemoglobin tetramer. In this study the possibility of using thermogravimetric analysis (TGA) followed by chemometrics as a new approach for β-thalassemia detection is proposed. Blood samples from patients with β-thalassemia were analyzed by the TG7 thermobalance and the resulting curves were compared to those typical of healthy individuals. Principal Component Analysis (PCA) was used to evaluate the correlation between the hematological parameters and the thermogravimetric results. The thermogravimetric profiles of blood samples from β-thalassemia patients were clearly distinct from those of healthy individuals as result of the different quantities of water content and corpuscular fraction. The hematological overview showed significant decreases in the values of red blood cell indices and an increase in red cell distribution width value in thalassemia subjects when compared with those of healthy subjects. The implementation of a predictive model based on Partial Least Square Discriminant Analysis (PLS-DA) for β-thalassemia diagnosis, was performed and validated. This model permitted the discrimination of anemic patients and healthy individuals and was able to detect thalassemia in clinically heterogeneous patients as in the presence of δβ-thalassemia and β-thalassemia combined with Hb Lepore. TGA and Chemometrics are capable of predicting ß-thalassemia syndromes using only a few microliters of blood without any pretreatment and with an hour of analysis time. A fast, rapid and cost-effective diagnostic tool for the β-thalassemia screening is proposed. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Thermogravimetric analysis of the gasification of microalgae Chlorella vulgaris.

    Science.gov (United States)

    Figueira, Camila Emilia; Moreira, Paulo Firmino; Giudici, Reinaldo

    2015-12-01

    The gasification of microalgae Chlorella vulgaris under an atmosphere of argon and water vapor was investigated by thermogravimetric analysis. The data were interpreted by using conventional isoconversional methods and also by the independent parallel reaction (IPR) model, in which the degradation is considered to happen individually to each pseudo-component of biomass (lipid, carbohydrate and protein). The IPR model allows obtaining the kinetic parameters of the degradation reaction of each component. Three main stages were observed during the gasification process and the differential thermogravimetric curve was satisfactorily fitted by the IPR model considering three pseudocomponents. The comparison of the activation energy values obtained by the methods and those found in the literature for other microalgae was satisfactory. Quantification of reaction products was performed using online gas chromatography. The major products detected were H2, CO and CH4, indicating the potential for producing fuel gas and syngas from microalgae. Copyright © 2015 Elsevier Ltd. All rights reserved.

  3. Curie temperature determination via thermogravimetric and continuous wavelet transformation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Hasier, John; Nash, Philip [Thermal Processing Technology Center, IIT, Chicago, IL (United States); Riolo, Maria Annichia [University of Michigan, Center for the Study of Complex Systems, Ann Arbor, MI (United States)

    2017-12-15

    A cost effective method for conversion of a vertical tube thermogravimetric analysis system into a magnetic balance capable of measuring Curie Temperatures is presented. Reference and preliminary experimental data generated using this system is analyzed via a general-purpose wavelet based Curie point edge detection technique allowing for enhanced speed, ease and repeatability of magnetic balance data analysis. The Curie temperatures for a number of Heusler compounds are reported. (orig.)

  4. A simple, sensitive graphical method of treating thermogravimetric analysis data

    Science.gov (United States)

    Abraham Broido

    1969-01-01

    Thermogravimetric Analysis (TGA) is finding increasing utility in investigations of the pyrolysis and combustion behavior of materuals. Although a theoretical treatment of the TGA behavior of an idealized reaction is relatively straight-forward, major complications can be introduced when the reactions are complex, e.g., in the pyrolysis of cellulose, and when...

  5. Thermogravimetric analysis and fast pyrolysis of Milkweed.

    Science.gov (United States)

    Kim, Seung-Soo; Agblevor, Foster A

    2014-10-01

    Pyrolysis of Milkweed was carried out in a thermogravimetric analyzer and a bubbling fluidized bed reactor. Total liquid yield of Milkweed pyrolysis was between 40.74% and 44.19 wt% between 425 °C and 550 °C. The gas yield increased from 27.90 wt% to 33.33 wt% with increasing reaction temperature. The higher heating values (HHV) of the Milkweed bio-oil were relatively high (30.33-32.87 MJ/kg) and varied with reaction temperature, feeding rate and fluidization velocity. The selectivity for CO2 was highest within non-condensable gases, and the molar ratio of CO2/CO was about 3 at the different reaction conditions. The (13)C NMR analysis, of the bio-oil showed that the relative concentration carboxylic group and its derivatives was higher at 425 °C than 475 °C, which resulted in slightly higher oxygen content in bio-oil. The pH of aqueous phase obtained at 475 °C was 7.37 which is the highest reported for any lignocellulosic biomass pyrolysis oils. Copyright © 2014 Elsevier Ltd. All rights reserved.

  6. Mechanism study on cellulose pyrolysis using thermogravimetric analysis coupled with infrared spectroscopy

    Institute of Scientific and Technical Information of China (English)

    WANG Shurong; LIU Qian; LUO Zhongyang; WEN Lihua; CEN Kefa

    2007-01-01

    Based on the investigation of the polysaccharide structure of cellulose by using Fourier transform spectrum analysis,the pyrolysis behaviour of cellulose was studied at a heating rate of 20 K/min by thermogravimetric (TG) analysis coupled with Fourier transform infrared (FTIR) spectroscopy.Experimental results show that the decomposition of cellulose mainly occurs at the temperature range of 550-670 K.The weight loss becomes quite slow when the temperature increases further up to 680 K and the amount of residue reaches a mass percent of 14.7%.The FTIR analysis shows that free water is released first during cellulose pyrolysis,followed by depolymerization and dehydration.Glucosidic bond and carbon-carbon bond break into a series of hydrocarbons,alcohols,aldehydes,acids,etc.Subsequently these large-molecule compounds decompose further into gases,such as methane and carbon monoxide.

  7. Thermogravimetric analysis of silicon carbide-silicon nitride fibers at ambient to 1000 C in air

    Science.gov (United States)

    Daniels, J. G.; Ledbetter, F. E., III; Clemons, J. M.; Penn, B. G.

    1984-01-01

    Thermogravimetric analysis of silicon carbide-silicon nitride fibers was carried out at ambient to 1000 C in air. The weight loss over this temperature range was negligible. In addition, the oxidative stability at high temperature for a short period of time was determined. Fibers heated at 1000 C in air for fifteen minutes showed negligible weight loss (i.e., less than 1 percent).

  8. Thermogravimetric analysis of fuel film evaporation

    Institute of Scientific and Technical Information of China (English)

    HU Zongjie; LI Liguang; YU Shui

    2006-01-01

    Thermogravimetric analysis (TGA) was compared with the petrochemical distillation measurement method to better understand the characteristics of fuel film evaporation at different wall tem- peratures. The film evaporation characteristics of 90# gasoline, 93# gasoline and 0# diesel with different initial thicknesses were investigated at different environmental fluxes and heating rates. The influences of heating rate, film thickness and environmental flux on fuel film evaporation for these fuels were found. The results showed that the environmental conditions in TGA were similar to those for fuel films in the internal combustion engines, so data from TGA were suitable for the analysis of fuel film evaporation. TGA could simulate the key influencing factors for fuel film evaporation and could investigate the basic quantificational effect of heating rate and film thickness. To get a rapid and sufficient fuel film evaporation, sufficiently high wall temperature is necessary. Evaporation time decreases at a high heating rate and thin film thickness, and intense gas flow is important to promoting fuel film evaporation. Data from TGA at a heating rate of 100℃/min are fit to analyze the diesel film evaporation during cold-start and warming-up. Due to the tense molecular interactions, the evaporation sequence could not be strictly divided according to the boiling points of each component for multicomponent dissolved mixture during the quick evaporation process, and the heavier components could vaporize before reaching their boiling points. The 0# diesel film would fully evaporate when the wall temperature is beyond 250℃.

  9. Purity Evaluation of Single-Walled Carbon Nanotubes Using Thermogravimetric Analysis

    International Nuclear Information System (INIS)

    Goak, Jeung Choon; Kim, Tae Yang; Jung, Jongwan; Seo, Young-Soo; Lee, Naesung; Sok, Junghyun

    2013-01-01

    This study evaluated the purity of single-walled carbon nanotubes (SWCNTs) in the arc-synthesized SWCNT samples by using thermogravimetric analysis (TGA). The as-produced SWCNT samples were heat-treated in air for 20 h at 275-475°C and characterized by scanning and transmission electron microscopes and TGA to establish oxidation temperature ranges of SWCNTs and carbonaceous impurities comprising the samples. Based on these oxidation temperature ranges, derivative thermogravimetric curves were deconvoluted, and differentiated peaks were assigned to SWCNTs and carbonaceous impurities. The compositions and the SWCNT purities of the samples were obtained simply by calculating the areal ratios under the deconvoluted curves. TGA studies on purity evaluation and thermal stabilities of SWCNTs and carbonaceous impurities are likely to provide us with a simple route of thermal oxidation purification to acquire high-purity SWCNT samples.

  10. Strategy for thermo-gravimetric analysis of K East fuel samples

    International Nuclear Information System (INIS)

    Lawrence, L.A.

    1997-01-01

    A strategy was developed for the Thermo-Gravimetric Analysis (TGA) testing of K East fuel samples for oxidation rate determinations. Tests will first establish if there are any differences for dry air oxidation between the K West and K East fuel. These tests will be followed by moist inert gas oxidation rate measurements. The final series of tests will consider pure water vapor i.e., steam

  11. Pyrolysis of coal, biomass and their blends: performance assessment by thermogravimetric analysis.

    Science.gov (United States)

    Ferrara, Francesca; Orsini, Alessandro; Plaisant, Alberto; Pettinau, Alberto

    2014-11-01

    With the aim to support the experimental tests in a gasification pilot plant, the thermal decomposition of coal, biomass and their mixtures has been carried out through a thermogravimetric analysis (TGA) and a simplified kinetic analysis. The TGA of pure fuels indicates the low reactivity of South African coal and the relatively high reactivity of Sardinian Sulcis coal during pyrolysis. Among the tested fuels, biomass (stone pine wood chips) is the most reactive one. These results fully confirm those obtained during the experimental tests in the gasification pilot plant. As for the fuel blends, the analysis shows that the synergic effects between the considered coals and biomass are negligible when they are co-pyrolyzed. The results of the analysis confirm that TGA could be very useful to generally predict the gasification performance and to optimize the experimental campaigns in pilot-scale gasification plants. Copyright © 2014 Elsevier Ltd. All rights reserved.

  12. Characteristics and kinetic studies of Hydrilla verticillata pyrolysis via thermogravimetric analysis.

    Science.gov (United States)

    Hu, Zhiquan; Chen, Zhihua; Li, Genbao; Chen, Xiaojuan; Hu, Mian; Laghari, Mahmood; Wang, Xun; Guo, Dabin

    2015-10-01

    The pyrolysis characteristics and kinetic of Hydrilla verticillata (HV) have been investigated using non-isothermal thermogravimetric analysis. The results showed that the pyrolysis behavior of HV can be divided into two independent stages. The kinetics of Stage I was investigated using a distributed activation energy model (DAEM) with discrete 99 first-order reactions. Stage II was an independent stage which corresponds to the decomposition of calcium oxalate, whose kinetics was studied using iso-conversional method together with compensation effect and master-plots method. The activation energies ranged from 92.39 to 506.17 and 190.42 to 222.48 kJ/mol for the first and second stages respectively. Calculated data gave very good fit to the experimental data. Copyright © 2015 Elsevier Ltd. All rights reserved.

  13. A comprehensive physicochemical, thermal, and spectroscopic characterization of zinc (II) chloride using X-ray diffraction, particle size distribution, differential scanning calorimetry, thermogravimetric analysis/differential thermogravimetric analysis, ultraviolet-visible, and Fourier transform-infrared spectroscopy.

    Science.gov (United States)

    Trivedi, Mahendra Kumar; Sethi, Kalyan Kumar; Panda, Parthasarathi; Jana, Snehasis

    2017-01-01

    Zinc chloride is an important inorganic compound used as a source of zinc and has other numerous industrial applications. Unfortunately, it lacks reliable and accurate physicochemical, thermal, and spectral characterization information altogether. Hence, the authors tried to explore in-depth characterization of zinc chloride using the modern analytical technique. The analysis of zinc chloride was performed using powder X-ray diffraction (PXRD), particle size distribution, differential scanning calorimetry (DSC), thermogravimetric analysis/differential thermogravimetric analysis (TGA/DTG), ultraviolet-visible spectroscopy (UV-vis), and Fourier transform-infrared (FT-IR) analytical techniques. The PXRD patterns showed well-defined, narrow, sharp, and the significant peaks. The crystallite size was found in the range of 14.70-55.40 nm and showed average crystallite size of 41.34 nm. The average particle size was found to be of 1.123 ( d 10 ), 3.025 ( d 50 ), and 6.712 ( d 90 ) μm and average surface area of 2.71 m 2 /g. The span and relative span values were 5.849 μm and 1.93, respectively. The DSC thermogram showed a small endothermic inflation at 308.10°C with the latent heat (ΔH) of fusion 28.52 J/g. An exothermic reaction was observed at 449.32°C with the ΔH of decomposition 66.10 J/g. The TGA revealed two steps of the thermal degradation and lost 8.207 and 89.72% of weight in the first and second step of degradation, respectively. Similarly, the DTG analysis disclosed T max at 508.21°C. The UV-vis spectrum showed absorbance maxima at 197.60 nm (λ max ), and FT-IR spectrum showed a peak at 511/cm might be due to the Zn-Cl stretching. These in-depth, comprehensive data would be very much useful in all stages of nutraceuticals/pharmaceuticals formulation research and development and other industrial applications.

  14. Characterization of an alkali-treated grass fiber by thermogravimetric and X-ray crystallographic analysis

    NARCIS (Netherlands)

    De, D.; De, Debapriya

    2008-01-01

    The thermal behavior of grass fiber was characterized by means of thermogravimetric analysis and differential scanning calorimetry analysis. The results proved that the removal of water-soluble matter improved the thermal behavior of grass fiber over that of unleached fiber, and this was further

  15. Combustion behavior and kinetics of low-lipid microalgae via thermogravimetric analysis.

    Science.gov (United States)

    Gai, Chao; Liu, Zhengang; Han, Guanghua; Peng, Nana; Fan, Aonan

    2015-04-01

    Thermogravimetric analysis and differential thermal analysis were employed to investigate combustion characteristics of two low-lipid microalgae, Chlorella pyrenoidosa (CP) and Spirulina platensis (SP) and iso-conversional Starink approach was used to calculate the kinetic parameters in the present study. The results showed that three stages of mass loss, including dehydration, devolatilization and char oxidation, were observed during combustion of both of two low-lipid microalgae. The whole weight loss of combustion of two microalgae was both shifted to higher temperature zones with increased heating rates from 10 to 40 K/min. In the 0.1-0.9 conversion range, the apparent activation energy of CP increased first from 51.96 to 79.53 kJ/mol, then decreased to 55.59 kJ/mol. Finally, it slightly increased to 67.27 kJ/mol. In the case of SP, the apparent activation energy gradually increased from 68.51 to 91.06 kJ/mol. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Quantitation of Surface Coating on Nanoparticles Using Thermogravimetric Analysis.

    Science.gov (United States)

    Dongargaonkar, Alpana A; Clogston, Jeffrey D

    2018-01-01

    Nanoparticles are critical components in nanomedicine and nanotherapeutic applications. Some nanoparticles, such as metallic nanoparticles, consist of a surface coating or surface modification to aid in its dispersion and stability. This surface coating may affect the behavior of nanoparticles in a biological environment, thus it is important to measure. Thermogravimetric analysis (TGA) can be used to determine the amount of coating on the surface of the nanoparticle. TGA experiments run under inert atmosphere can also be used to determine residual metal content present in the sample. In this chapter, the TGA technique and experimental method are described.

  17. Thermogravimetric analysis of anthracite and waste plastics by iso-conversional method

    International Nuclear Information System (INIS)

    Ren, Shan; Zhang, Jianliang

    2013-01-01

    Highlights: • Co-combustion kinetic analysis of solid fuels was made by iso-conversional method. • Thermodynamic and kinetic parameters of combustion for blends were determined. • WP can improve the combustion characteristic of high ash anthracite. • Reasonable utilization the energy of WP is important for industrial production. - Abstract: Combustion mechanisms and kinetics of plastics-coal blends with 0, 10, 20, 40 and 100% waste plastics (WP) are studied separately by thermogravimetric analysis (TGA) from ambient temperature to 900 °C in air atmosphere. These blends are combusted at different heating rates. The results indicate that, with the increase of waste plastics content, the combustion processes of blends could be divided into one stage, two stages, three stages and one stage. Meanwhile, the ignition and final temperatures of them both decrease. The maximum weight loss rate of WP is much higher than that of other samples. The iso-conversional method is used for the kinetic analysis of the non-isothermal thermogravimetric data and results indicate that, when the waste plastics content varied from 0% to 40%, the values of activation energy increase from 113.3 kJ mol −1 to 156.0 kJ mol −1 , and the value of activation energy for pure WP is 278.8 kJ mol −1

  18. Thermogravimetric analysis of the beryllium/steam reaction

    Energy Technology Data Exchange (ETDEWEB)

    Druyts, Frank E-mail: fdruyts@sckcen.be; Iseghem, Pierre van

    2000-11-01

    In view of the safety assessment of new fusion reactor designs, kinetic data are needed on the beryllium/steam reaction. Therefore, thermogravimetric analysis was used to determine the reactivity of beryllium in steam as a function of temperature, irradiation history and porosity of the samples. To this purpose, reference unirradiated S-200 VHP beryllium samples were compared with specimens irradiated in the BR2 reactor up to fast neutron fluences (E>1 MeV) of respectively 1.6x10{sup 21} n cm{sup -2} (resulting in a helium content of 300 appm He and a theoretical density of 99.9%) and 4x10{sup 22} n cm{sup -2} (21000 appm He, 97.2% theoretical density). Kinetics were parabolic for all tested beryllium types at 600 deg. C. At 700 deg. C, kinetics were parabolic for the unirradiated and irradiated 99.9% dense beryllium, and accelerating/linear for the irradiated 97.2% material. At 800 deg. C, all samples showed accelerating/linear behaviour. There was no influence of porosity on the reaction rate of beryllium in steam within the limited investigated density range, except at 700 deg. C, where the measured reaction rate for the irradiated 97.2% dense samples is an order of magnitude higher than for the irradiated 99.9% dense specimens.

  19. Biomass Thermogravimetric Analysis: Uncertainty Determination Methodology and Sampling Maps Generation

    Science.gov (United States)

    Pazó, Jose A.; Granada, Enrique; Saavedra, Ángeles; Eguía, Pablo; Collazo, Joaquín

    2010-01-01

    The objective of this study was to develop a methodology for the determination of the maximum sampling error and confidence intervals of thermal properties obtained from thermogravimetric analysis (TG), including moisture, volatile matter, fixed carbon and ash content. The sampling procedure of the TG analysis was of particular interest and was conducted with care. The results of the present study were compared to those of a prompt analysis, and a correlation between the mean values and maximum sampling errors of the methods were not observed. In general, low and acceptable levels of uncertainty and error were obtained, demonstrating that the properties evaluated by TG analysis were representative of the overall fuel composition. The accurate determination of the thermal properties of biomass with precise confidence intervals is of particular interest in energetic biomass applications. PMID:20717532

  20. Pyrolysis and combustion kinetics of lycopodium particles in thermogravimetric analysis

    Institute of Scientific and Technical Information of China (English)

    Seyed Alireza Mostafavi; Sadjad Salavati; Hossein Beidaghy Dizaji; Mehdi Bidabadi

    2015-01-01

    Biomass is a kind of renewable energy which is used increasingly in different types of combustion systems or in the production of fuels like bio-oil. Lycopodium is a cellulosic particle, with good combustion properties, of which microscopic images show that these particles have spherical shapes with identical diameters of 31 μm. The measured density of these particles is 1.0779 g/cm2. Lycopodium particles contain 64.06% carbon, 25.56% oxygen, 8.55% hydrogen and 1.83% nitrogen, and no sulfur. Thermogravimetric analysis in the nitrogen environment indicates that the maximum of particle mass reduction occurs in the temperature range of 250−550 °C where the maximum mass reduction in the DTG diagrams also occurs in. In the oxygen environment, an additional peak can also be observed in the temperature range of 500−600 °C, which points to solid phase combustion and ignition temperature of lycopodium particles. The kinetics of reactions is determined by curve fitting and minimization of error.

  1. Thermogravimetric analysis of co-combustion between microalgae and textile dyeing sludge.

    Science.gov (United States)

    Peng, Xiaowei; Ma, Xiaoqian; Xu, Zhibin

    2015-03-01

    The synergistic interaction and kinetics of microalgae, textile dyeing sludge and their blends were investigated under combustion condition by thermogravimetric analysis. The textile dyeing sludge was blended with microalgae in the range of 10-90wt.% to investigate their co-combustion behavior. Results showed that the synergistic interaction between microalgae and textile dyeing sludge improved the char catalytic effect and alkali metals melt-induced effect on the decomposition of textile dyeing sludge residue at high temperature of 530-800°C. As the heating rate increasing, the entire combustion process was delayed but the combustion intensity was enhanced. The lowest average activation energy was obtained when the percentage of microalgae was 60%, which was 227.1kJ/mol by OFW and 227.4kJ/mol by KAS, respectively. Copyright © 2015 Elsevier Ltd. All rights reserved.

  2. Investigation of Thermal Behavior for Natural Fibres Reinforced Epoxy using Thermogravimetric and Differential Scanning Calorimetric Analysis

    Directory of Open Access Journals (Sweden)

    Fauzi F.A.

    2016-01-01

    Full Text Available This paper presented the research works on the investigation of the thermal behavior of the natural fibres; i.e. pineapple leaf fibre, kenaf fibre and mengkuang fibres reinforced epoxy. The thermogravimetric analysis and differential scanning calorimetric analysis were used to measure the thermal behavior of the treated and untreated pineapple, kenaf and mengkuang fibres reinforced epoxy. The samples for both analysis were subjected to maximum temperature 600°C at the heating rate of 10°C/min. The results showed that the treated fibres show higher maximum peak temperature as compared to the untreated fibres. Additionally, the glass transition temperature showed a lower value for all treated fibre. It can be concluded that investigation of thermal properties of these natural fibres could improve the utilization of natural fibre composites in various applications i.e. sports applications.

  3. Spectroscopic and thermogravimetric study of nickel sulfaquinoxaline complex

    International Nuclear Information System (INIS)

    Tailor, Sanjay M.; Patel, Urmila H.

    2016-01-01

    The ability of sulfaquinoxaline (4-Amino-N-2-quinoxalinylbenzenesulfonamide) to form metal complexes are investigated. The nickel complex of sulfaquinoxaline is prepared by reflux method and characterized by CHN analysis and IR spectra. The results of IR spectral data suggest that the binding of nickel atom to the sulfonamidic nitrogen are in good agreement. The thermogravimetric analysis (TGA), differential thermal analysis (DTA) and differential thermogravimetric (DTG) analysis of nickel sulfaquinoxaline are carried out from ambient temperature to 750°C in inert nitrogen atmosphere. The activation energy, enthalpy, entropy and Gibbs free energy of nickel sulfaquinoxaline complex is determined from the thermal curves using Broido method. The results are reported in this paper.

  4. Determination of nanoparticle surface coatings and nanoparticle purity using microscale thermogravimetric analysis.

    Science.gov (United States)

    Mansfield, Elisabeth; Tyner, Katherine M; Poling, Christopher M; Blacklock, Jenifer L

    2014-02-04

    The use of nanoparticles in some applications (i.e., nanomedical, nanofiltration, or nanoelectronic) requires small samples with well-known purities and composition. In addition, when nanoparticles are introduced into complex environments (e.g., biological fluids), the particles may become coated with matter, such as proteins or lipid layers. Many of today's analytical techniques are not able to address small-scale samples of nanoparticles to determine purity and the presence of surface coatings. Through the use of an elevated-temperature quartz crystal microbalance (QCM) method we call microscale thermogravimetric analysis, or μ-TGA, the nanoparticle purity, as well as the presence of any surface coatings of nanomaterials, can be measured. Microscale thermogravimetric analysis is used to determine the presence and amount of surface-bound ligand coverage on gold nanoparticles and confirm the presence of a poly(ethylene glycol) coating on SiO2 nanoparticles. Results are compared to traditional analytical techniques to demonstrate reproducibility and validity of μ-TGA for determining the presence of nanoparticle surface coatings. Carbon nanotube samples are also analyzed and compared to conventional TGA. The results demonstrate μ-TGA is a valid method for quantitative determination of the coatings on nanoparticles, and in some cases, can provide purity and compositional data of the nanoparticles themselves.

  5. Uncertainty Determination Methodology, Sampling Maps Generation and Trend Studies with Biomass Thermogravimetric Analysis

    Science.gov (United States)

    Pazó, Jose A.; Granada, Enrique; Saavedra, Ángeles; Eguía, Pablo; Collazo, Joaquín

    2010-01-01

    This paper investigates a method for the determination of the maximum sampling error and confidence intervals of thermal properties obtained from thermogravimetric analysis (TG analysis) for several lignocellulosic materials (ground olive stone, almond shell, pine pellets and oak pellets), completing previous work of the same authors. A comparison has been made between results of TG analysis and prompt analysis. Levels of uncertainty and errors were obtained, demonstrating that properties evaluated by TG analysis were representative of the overall fuel composition, and no correlation between prompt and TG analysis exists. Additionally, a study of trends and time correlations is indicated. These results are particularly interesting for biomass energy applications. PMID:21152292

  6. Thermal decomposition kinetics of sorghum straw via thermogravimetric analysis.

    Science.gov (United States)

    Dhyani, Vaibhav; Kumar, Jitendra; Bhaskar, Thallada

    2017-12-01

    The thermal decomposition of sorghum straw was investigated by non-isothermal thermogravimetric analysis, where the determination of kinetic triplet (activation energy, pre-exponential factor, and reaction model), was the key objective. The activation energy was determined using different isoconversional methods: Friedman, Flynn-Wall-Ozawa (FWO), Kissinger-Akahira-Sunose (KAS), Starink, Iterative method of Chai & Chen, Vyazovkin AIC method, and Li & Tang equation. The pre-exponential factor was calculated using Kissinger's equation; while the reaction model was predicted by comparison of z-master plot obtained from experimental values with the theoretical plots. The values of activation energy obtained from isoconversional methods were further used for evaluation of thermodynamic parameters, enthalpy, entropy and Gibbs free energy. Results showed three zones of pyrolysis having average activation energy values of 151.21kJ/mol, 116.15kJ/mol, and 136.65kJ/mol respectively. The data was well fitting with two-dimension 'Valensi' model for conversion values from 0 to 0.4 with a coefficient of determination (R 2 ) value of 0.988, and with third order reaction model for values from 0.4 to 0.9 with an R 2 value of 0.843. Copyright © 2017 Elsevier Ltd. All rights reserved.

  7. 硫化环氧化天然橡胶的热分析%Thermogravimetric Analysis of ENR Vulcanizate

    Institute of Scientific and Technical Information of China (English)

    张北龙; 陈美; 刘惠伦

    2001-01-01

    The thermogravimetric analysis of ENR(epoxidized natural rubber) has been carried out byTG-DTG methods at temperature rising rate of 5, 10, 15 and 20 ℃ · rmin-1. The results showed thatthe activation energy of the thermoreaction in flowing air during the course of mass loss wasn't alwayskeep rising, but declined at mass loss of 1.0%~10.0%, 20.0%~30.0% and 70. 0%~80. 0%.

  8. Thermogravimetric and kinetic study of methylolmelamine ...

    African Journals Online (AJOL)

    Some salient properties of cotton cellulose which requires it to be treated with additives to improve its versatility were examined taken into consideration, the molecular structure. Thermogravimetric analysis of the cotton fabric and the treated cotton fabric were carried out in an improvised muffled furnace. The result was in ...

  9. Thermogravimetric Analysis of Effects of High-Content Limstone Addition on Combustion Characteristics of Taixi Anthracite

    Institute of Scientific and Technical Information of China (English)

    ZHANG Hong; LI Mei; SUN Min; WEI Xian-yong

    2004-01-01

    Combustion characteristics of Taixi anthracite admixed with high content of limestone addition were investigated with thermogravimetric analysis. The results show that limestone addition has a little promoting effect on the ignition of raw coals as a whole. The addition of limestone is found to significantly accelerate the combustion and burnout of raw coals. The higher the sample mass is, the more significant the effect will be. The results also show that the change of limestone proportion between 45%-80% has little effect on ignition temperatures of coal in the blended samples. Increasing limestone content lowers the temperature corresponding to the maximum weight loss. Although higher maximum mass loss rates are observed with higher limestone content, the effect is found not ascribed to changing limestone addition, but to the decrease of absolute coal mass in the sample. The change of limestone proportion has little effect on its burnout temperature. Mechanism analysis indicates that these phenomena result mainly from improved heat conduction due to limestone addition.

  10. Evaluation of co-pyrolysis petrochemical wastewater sludge with lignite in a thermogravimetric analyzer and a packed-bed reactor: Pyrolysis characteristics, kinetics, and products analysis.

    Science.gov (United States)

    Mu, Lin; Chen, Jianbiao; Yao, Pikai; Zhou, Dapeng; Zhao, Liang; Yin, Hongchao

    2016-12-01

    Co-pyrolysis characteristics of petrochemical wastewater sludge and Huolinhe lignite were investigated using thermogravimetric analyzer and packed-bed reactor coupled with Fourier transform infrared spectrometer and gas chromatography. The pyrolysis characteristics of the blends at various sludge blending ratios were compared with those of the individual materials. Thermogravimetric experiments showed that the interactions between the blends were beneficial to generate more residues. In packed-bed reactor, synergetic effects promoted the release of gas products and left less liquid and solid products than those calculated by additive manner. Fourier transform infrared spectrometer analysis showed that main functional groups in chars gradually disappeared with pyrolysis temperatures increasing, and H 2 O, CH 4 , CO, and CO 2 appeared in volatiles during pyrolysis. Gas compositions analysis indicated that, the yields of H 2 and CO clearly increased as the pyrolysis temperature and sludge blending ratio increasing, while the changes of CH 4 and CO 2 yields were relatively complex. Copyright © 2016 Elsevier Ltd. All rights reserved.

  11. Pyrolysis behaviors and kinetic studies on Eucalyptus residues using thermogravimetric analysis

    International Nuclear Information System (INIS)

    Chen, Zhihua; Zhu, Quanjie; Wang, Xun; Xiao, Bo; Liu, Shiming

    2015-01-01

    Highlights: • The first study on pyrolysis characteristics and kinetic of Eucalyptus residues. • Pyrolysis process can be divided into three stages using differential DTG method. • A new modified discrete DAEM showed better than Gaussian DAEM for kinetic studies. • Variations of activation energy reveal the mechanism change during pyrolysis process. - Abstract: The pyrolysis behaviors and kinetics of Eucalyptus leaves (EL), Eucalyptus bark (EB) and Eucalyptus sawdust (ESD) were investigated by using thermogravimetric analysis (TGA) technique. Three stages for EL, EB and ESD pyrolysis have been divided using differential derivative thermogravimetric (DDTG) method and the second stage is the main pyrolysis process with approximately 86.93% (EL), 88.96% (EB) and 97.84% (ESD) weight loss percentages. Kinetic parameters of Gaussian distributed activation energy model (DAEM) for EL, EB and ESD pyrolysis are: distributed centers (E_0) of 141.15 kJ/mol (EL), 149.21 kJ/mol (EB), 175.79 kJ/mol (ESD), standard deviations (σ) of 18.35 kJ/mol (EL), 18.37 kJ/mol (EB), 14.41 kJ/mol (ESD) and pre-exponential factors (A) of 1.15E+10 s"−"1 (EL), 4.34E+10 s"−"1 (EB), 7.44E+12 s"−"1 (ESD). A new modified discrete DAEM was performed and showed excellent fits to experimental data than Gaussian DAEM. According to the modified discrete DAEM, the activation energies are in ranges of 122.67–308.64 kJ/mol, 118.72–410.80 kJ/mol and 108.39–192.93 kJ/mol for EL, EB and ESD pyrolysis, respectively. The pre-exponential factors of discrete DAEM have wide ranges of 4.84E+13–6.12E+22 s"−"1 (EL), 1.91E+12–4.51E+25 s"−"1 (EB) and 63.43–4.36E+11 s"−"1 (ESD). The variation of activation energy versus conversion reveals the mechanism change during pyrolysis process. The kinetic data would be of immense benefit to model, design and develop suitable thermo-chemical systems for the application of Eucalyptus residues.

  12. Interactions of coal gangue and pine sawdust during combustion of their blends studied using differential thermogravimetric analysis.

    Science.gov (United States)

    Zhang, Yuanyuan; Zhang, Zhezi; Zhu, Mingming; Cheng, Fangqin; Zhang, Dongke

    2016-08-01

    The interactions between coal gangue and pine sawdust during the combustion process were studied using thermogravimetric analysis. The effect of the blending ratio, oxygen concentration and heating rate on the weight loss (TG) and differential thermogravimetric (TGA) profiles was examined. The TG and DTG curves of the blends were not additives of those of the individual materials, suggesting that interactions between coal gangue and pine sawdust had occurred during the combustion, especially in the temperature range of 400-600°C. Kinetic analysis confirmed that the combustion of coal gangue, pine sawdust and their blends was chemical reaction controlled. Further analysis revealed that the interactions between coal gangue and pine sawdust were primarily due to thermal effects rather than structural changes, with the thermal inertia of coal gangue dominating over the behaviour of the blends. The interactions decreased with decreasing the coal gangue ratio in the blend, oxygen concentration and heating rate. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Kinetic Model of LiFePO4 Formation Using Non-Isothermal Thermogravimetric Analysis

    Directory of Open Access Journals (Sweden)

    Abdul Halim

    2014-03-01

    Full Text Available The formation reaction of LiFePO4 from decomposition of precursors LiOH, FeSO4.7H2O and (NH42HPO4 with mol ratio of Li:Fe:P=1:1:1 was investigated. The experiment was carried out by thermogravimetric differential thermal analysis (TG-DTA method using nitrogen as atmosfer at a constant heating rate to obtain kinetic constant parameters. Several heating rates were selected, there are 5, 7, 10, 15, 17.5, 22.5 and 25 °C/min. Activation energy, pre-exponential factor and reaction order were taken using Kissinger method and obtained respectively 56.086 kJ/mol, 6.95×108 min-1, and 1.058. Based on fitting result between reaction model and experiment were obtained that reaction obeyed the three dimension diffusion model. © 2014 BCREC UNDIP. All rights reservedReceived: 19th September 2013; Revised: 9th December 2013; Accepted: 23rd January 2014 [How to Cite: Halim, A., Widiyastuti, W., Setyawan, H., Winardi, S. (2014. Kinetic of LiFePO4 For-mation Using Non-isothermal Thermogravimetric Analysis. Bulletin of Chemical Reaction Engineering & Catalysis, 9 (1: 60-65. (doi:10.9767/bcrec.9.1.5508.60-65][Permalink/DOI: http://dx.doi.org/10.9767/bcrec.9.1.5508.60-65] 

  14. Characteristics of curcumin using cyclic voltammetry, UV–vis, fluorescence and thermogravimetric analysis

    International Nuclear Information System (INIS)

    Masek, Anna; Chrzescijanska, Ewa; Zaborski, Marian

    2013-01-01

    Highlights: • Electrooxidation of curcumin was investigated with cyclic voltammetry. • The curcumin is irreversibly oxidized at the platinum electrode in anhydrous media. • Absorbance, fluorescence and thermogravimetric analysis of curcumin was studied. • The HOMO and Mapped Electron Densities were calculated using HyperChem. • Oxidation mechanism for curcumin proposed. -- Abstract: Curcumin, the yellow, primary bioactive component of turmeric, has recently received attention from chemists due its wide range of potential biological applications as an antioxidant, anti-inflammatory, and anti-carcinogenic agent. The electrochemical behaviour of curcumin at a platinum electrode has been studied by cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The oxidation of curcumin is an irreversible process that proceeds in two steps in 0.1 M (C 4 H 9 ) 4 NClO 4 in acetonitrile. The process of oxidation and its kinetics have been investigated. The rate constant, electron transfer coefficient and diffusion coefficients for the electrochemical oxidation of curcumin were determined. A mechanism for the oxidation of curcumin is proposed. The data obtained are consistent with the current literature and suggest that voltammetric studies on mechanically transferred solids may be a convenient method for elucidating the electrochemical oxidation mechanisms of compounds in anhydrous media. Theoretical calculations regarding the optimization of curcumin, electronic properties like highest occupied molecular orbital (HOMO) and lowest unoccupied molecular orbital (LUMO) were calculated using with HyperChem software by AM1 semi-empirical method. The properties of curcumin in a homogeneous environment were investigated using spectroscopic techniques and thermogravimetric analysis

  15. Thermogravimetric analysis and kinetic study of formation of lithium titanate by solid state route

    International Nuclear Information System (INIS)

    Sonak, Sagar; Jain, Uttam; Sahu, Ashok Kumar; Kumar, Sanjay; Krishnamurthy, Nagaiyar

    2015-01-01

    The kinetics of formation of lithium titanate from the solid state reaction of lithium carbonate and titanium oxide was studied using non-isothermal thermogravimetric technique. Thermogravimetric data for the reaction of lithium carbonate and titanium oxide was obtained at various heating rates. The methods such as Flynn–Wall–Ozawa and Kissinger–Akahira–Sunose were used to estimate the kinetic parameters from the obtained thermogravimetric data. The average activation energy for the formation of lithium titanate by solid state route was found to be 243 kJ/mol K. The reaction mechanism was determined by the method given by Malek. It was found that the three dimensional diffusion model best describes the reaction kinetics. A kinetic equation describing the reaction is proposed and reaction mechanism is discussed

  16. Thermogravimetric Analysis and Kinetic Study on Pyrolysis of Veteri-narian Solid Waste

    Directory of Open Access Journals (Sweden)

    Andrés Felipe Rojas González

    2016-10-01

    Full Text Available Context: Institutional waste from clinical centers can be classified as those coming from health institutions dedicated to human attention and those coming from centers for animal veterinary care. The latter are mainly hazardous wastes, hence their disposal requires incineration. Most of such waste is organic, and it is possible, therefore, to take advantage of their energetic power in combustion or pyrolysis processes. This work is motivated because no literature was found on the pyrolysis kinetics veterinary waste, as this kind of studies are mainly focused on hospital waste of human health care. Method: The kinetics of pyrolysis is characterized and studied by means of thermogravimetric analysis of 6 major veterinary waste (gauze, cotton swabs, cotton, nails, hair, plastic syringes. The characterization is performed by proximate and elemental analysis, and thermogravimetric analysis. Reactivity characteristics and pyrolytic capability of wastes are established. The kinetics study on pyrolysis was carried out by determining the kinetic triplet by isoconversional Starink method. Results: It was established that the pyrolysis index increases with the heating rate and that the thermal degradation depends on the material type of the waste. Similarly, it was found that the temperature (ΔT = Tf - Ti for the thermal decomposition of veterinary waste is: ΔTnails> ΔThair > ΔTcotton swabs > ΔTgauze > ΔTcotton > ΔTplastic syringes; the activation energy is Enails> E hair > Eplastic syringes > Ecotton swabs > E gauze > Ecotton, and the reaction order is: n hair > nnails > ncotton swabs > ncotton > n gauze > n plastic syringes. Conclusions: These results suggest the possibility of using veterinary wastes for power generation, providing an alternative for sustainable energy development to cities in continuous growth, from both, energetic and environmental points of view.

  17. Thermogravimetric and differential thermal analysis of potassium bicarbonate contaminated cellulose

    Science.gov (United States)

    A. Broido

    1966-01-01

    When samples undergo a complicated set of simultaneous and sequential reactions, as cellulose does on heating, results of thermogravimetric and differential thermal analyses are difficult to interpret. Nevertheless, careful comparison of pure and contaminated samples, pyrolyzed under identical conditions, can yield useful information. In these experiments TGA and DTA...

  18. THERMOGRAVIMETRIC INVESTIGATIONS OF VAGINAL SUPPOSITORY WITH THYME OIL

    Directory of Open Access Journals (Sweden)

    N. V. Melnikova

    2015-04-01

    Full Text Available One of the main stages in new medicines creation is the development of their making technology. Technological process of suppository making includes ratherlongthermal treatment during preparation and homogenization of suppository base, active substancesaddition. These factors create danger of chemical and physical transformation of active substances and excipients in suppository up to their destruction and change of pharmacological and physical-chemical properties. Use of thermogravimetric analysis in pharmaceutical technology allows to studythepossibility of chemical interaction in dosage forms over the wide temperature range. The aim of this work is study of thermal treatmenteffects of suppository base with thyme oil over the temperature range of suppository manufacturing. Methods and results. As an object of thermogravimetric study vaginal suppository with thyme oil 0,2 g, suppository-placebo containing propylenglycol, polyethylene glycol 400, proxanol 268, twin 80 and the active ingredient of «Царствоароматов», Ukraine, production were used. Thermogravimetric analysis was carried out on the derivatograph«Shimadzu DTG-60», Japan, with the platinum and platinum-rhodiumthermopair with samples heating in aluminiumcrucibles from 25 to 200ºС. As standard α-Al2O3was used.Heating rate was 10ºСper min.Mass of the samples was 23,45– 39,63 mg. Obtained data were registered by the derivatograph as curves T, DTA, TGA. The T curve on the derivatogramm shows the temperature change and the TGA curve demonstrates the sample mass change during investigation. The DTA curve reflects differentiation of thermal effects and contains information about endothermic and exothermal maximum and is used for qualitative valuation of derivatogramm. According to results of thermogravimetric investigation the thyme oil is thermostable substance which is gradually evaporating during heating. So, at the beginning of study the test sample mass was 23

  19. Thermogravimetric assessment of thermal degradation in asphaltenes

    Energy Technology Data Exchange (ETDEWEB)

    Barneto, Agustín García, E-mail: agustin.garcia@diq.uhu.es [Department of Chemical Engineering, Physical Chemistry and Organic Chemistry, University of Huelva, Huelva (Spain); Carmona, José Ariza [Department of Chemical Engineering, Physical Chemistry and Organic Chemistry, University of Huelva, Huelva (Spain); Garrido, María José Franco [CEPSA, RDI Centre, Madrid (Spain)

    2016-03-20

    Graphical abstract: - Highlights: • Asphaltenes content of visbreaking streams in oil refinery can be measured by using TGA. • Deconvoluting TGA curves allows the thermal-based composition of asphaltenes to be elucidated. • Asphaltenes cracking involves acceleratory stages compatible with autocatalytic kinetic. • Activation energy during asphaltenes pyrolysis increased with increasing temperature. • Activation energy remained almost constant at 200–225 kJ/mol during oxidative cracking. - Abstract: Monitoring asphaltenes is very important with a view to optimizing visbreaking units in oil refineries. Current analyses based on selective dissolution in different solvents are slow, so new, more expeditious methods for measuring asphaltenes are required to facilitate fuel-oil production. In this work, we studied the thermal degradation of asphaltenes as the potential basis for a thermogravimetric method for their monitoring in visbreaking streams. The thermal degradation of asphaltenes occurs largely from 400 to 500 °C; the process is quite smooth in an inert environment but involves several fast mass loss events in the air. Kinetic parameters for characterizing the process were determined by using two model-free methods and the modified Prout–Tompkins kinetic equation to examine asphaltene thermolysis. Both types of methods showed the activation energy to increase during pyrolysis but to remain almost constant during cracking in the presence of oxygen or even diminish during char oxidation. Deconvoluting the thermogravimetric profiles revealed that asphaltene thermolysis in the air cannot be accurately described in terms of an nth order kinetic model because it involves some acceleratory phases. Also, thermogravimetric analyses of visbreaking streams revealed that char production in them is proportional to their asphaltene content. This relationship enables the thermogravimetric measurement of asphaltenes.

  20. Thermogravimetric assessment of thermal degradation in asphaltenes

    International Nuclear Information System (INIS)

    Barneto, Agustín García; Carmona, José Ariza; Garrido, María José Franco

    2016-01-01

    Graphical abstract: - Highlights: • Asphaltenes content of visbreaking streams in oil refinery can be measured by using TGA. • Deconvoluting TGA curves allows the thermal-based composition of asphaltenes to be elucidated. • Asphaltenes cracking involves acceleratory stages compatible with autocatalytic kinetic. • Activation energy during asphaltenes pyrolysis increased with increasing temperature. • Activation energy remained almost constant at 200–225 kJ/mol during oxidative cracking. - Abstract: Monitoring asphaltenes is very important with a view to optimizing visbreaking units in oil refineries. Current analyses based on selective dissolution in different solvents are slow, so new, more expeditious methods for measuring asphaltenes are required to facilitate fuel-oil production. In this work, we studied the thermal degradation of asphaltenes as the potential basis for a thermogravimetric method for their monitoring in visbreaking streams. The thermal degradation of asphaltenes occurs largely from 400 to 500 °C; the process is quite smooth in an inert environment but involves several fast mass loss events in the air. Kinetic parameters for characterizing the process were determined by using two model-free methods and the modified Prout–Tompkins kinetic equation to examine asphaltene thermolysis. Both types of methods showed the activation energy to increase during pyrolysis but to remain almost constant during cracking in the presence of oxygen or even diminish during char oxidation. Deconvoluting the thermogravimetric profiles revealed that asphaltene thermolysis in the air cannot be accurately described in terms of an nth order kinetic model because it involves some acceleratory phases. Also, thermogravimetric analyses of visbreaking streams revealed that char production in them is proportional to their asphaltene content. This relationship enables the thermogravimetric measurement of asphaltenes.

  1. Kinetic analysis on the non-isothermal degradation of plum stone waste by thermogravimetric analysis and integral master-plots method.

    Science.gov (United States)

    Ceylan, Selim

    2015-04-01

    In this study, pyrolysis of plum stone was investigated by thermogravimetric analysis in a nitrogen atmosphere at heating rates of 5, 10, 20 and 40 °C min(-1). Pyrolysis characteristics and the thermal-decomposition rate were significantly affected by variation in the heating rate. However, the heating rate slightly affected the total yield of the volatile matters. Activation energy of the pyrolysis reaction was evaluated by model-free methods, Friedman and Kissingere-Akahirae-Sunose. Results of the Master-Plots method indicated that the most probable reaction model function was the nth order reaction model function as f(x) = (1-x) (3.11), A = 8.02x10(12) under a mean activation energy of 150.61 kJ mol(-1). Proximate and ultimate analysis showed that plum stone can be considered as a favourable source for energy production owing to its low moisture and ash content, and high volatile matter ratio and moderate heating value. © The Author(s) 2015.

  2. Thermogravimetric analysis and kinetic study of bamboo waste treated by Echinodontium taxodii using a modified three-parallel-reactions model.

    Science.gov (United States)

    Yu, Hongbo; Liu, Fang; Ke, Ming; Zhang, Xiaoyu

    2015-06-01

    In this study, the effect of pretreatment with Echinodontium taxodii on thermal decomposition characteristics and kinetics of bamboo wastes was investigated by thermogravimetric analysis. The results showed fungal pretreatment can enhance the thermal degradation of bamboo. The negative effect of extractives in bamboo on the thermal decomposition can be decreased by the pretreatment. A modified three-parallel-reactions model based on isolated lignin was firstly proposed to study pyrolysis kinetics of bamboo lignocellulose. Kinetic analysis showed that with increasing pretreatment time fungal delignification was enhanced to transform the lignin component with high activation energy into that with low activation energy and raise the cellulose content in bamboo, making the thermal decomposition easier. These results demonstrated fungal pretreatment provided a potential way to improve thermal conversion efficiency of bamboo. Copyright © 2015 Elsevier Ltd. All rights reserved.

  3. Thermogravimetric-Mass Spectrometric Study of the Pyrolysis Behavior of PVC

    Institute of Scientific and Technical Information of China (English)

    SUN Qing-lei; SHI Xin-gang; LIN Yun-liang; ZHU He; WANG Xiao; CHENG Chuan-ge; LIU Jian-hua

    2007-01-01

    The pyrolysis characteristics of PVC were systematically investigated using a Netzschne TG thermo-balance coupled to a quadrupole mass spectrometer. The pyrolysis conditions were 0.1 MPa of Ar, a heating rate of 10 ℃/min and a final temperature of 1000 ℃. Both the thermogravimetric properties and the simultaneous evolution of gaseous products during pyrolysis were studied. The TG/DTG results showed that as the pyrolysis temperature increases the weight loss and weight loss rate of PVC increases. Near 412 ℃ the weight loss rate attained its peak value. At higher temperatures the rate of loss gradually decreases. The gases evolved during thermogravimetric analysis were analyzed by a mass spectrometer, monitoring the relative intensity of HCl, C6H6, light hydrocarbon and chlorine-containing gases. The evolution curves showed that HCl, C6H6, light hydrocarbon and chlorine-containing gases all peak at about 416 ℃. This is consistent with the fact that the weight loss curves also peak at about 412 ℃. The extensive HCl evolution is consistent with the high chlorine content of PVC. The formation of these gases can be explained by considering these reactions: dehydrochlorination, intramolecular cyclization and the addition of HCl to unsaturated hydrocarbons.

  4. Combustion characteristics of Malaysian oil palm biomass, sub-bituminous coal and their respective blends via thermogravimetric analysis (TGA).

    Science.gov (United States)

    Idris, Siti Shawalliah; Rahman, Norazah Abd; Ismail, Khudzir

    2012-11-01

    The combustion characteristics of Malaysia oil palm biomass (palm kernel shell (PKS), palm mesocarp fibre (PMF) and empty fruit bunches (EFB)), sub-bituminous coal (Mukah Balingian) and coal/biomass blends via thermogravimetric analysis (TGA) were investigated. Six weight ratios of coal/biomass blends were prepared and oxidised under dynamic conditions from temperature 25 to 1100°C at four heating rates. The thermogravimetric analysis demonstrated that the EFB and PKS evolved additional peak besides drying, devolatilisation and char oxidation steps during combustion. Ignition and burn out temperatures of blends were improved in comparison to coal. No interactions were observed between the coal and biomass during combustion. The apparent activation energy during this process was evaluated using iso-conversional model free kinetics which resulted in highest activation energy during combustion of PKS followed by PMF, EFB and MB coal. Blending oil palm biomass with coal reduces the apparent activation energy value. Copyright © 2012 Elsevier Ltd. All rights reserved.

  5. Thermogravimetric analysis of phase transitions in cement compositions mixed by sodium silicate solution

    Directory of Open Access Journals (Sweden)

    Fedosov Sergey Viktorovich

    2014-01-01

    Full Text Available This paper presents a study of the capability to modify cement by mechanical activation of sodium silicate water solution. Admixtures or blends of binding agents were employed for modifying concrete properties. The liquid glass is applied to protect from chemically or physically unfavorable environmental impacts, such as acidic medium and high temperature. The sodium silicate is a high-capacity setting accelerator. The increasing of the liquid glass proportion in the mix leads to the degradation of the cement paste plasticity and for this reason it is necessary to reduce the amount of liquid glass in the cement paste. The activation of dilute water solution of sodium silicate into rotary pulsating apparatus directly before tempering of the cement paste is an effective way to decrease mass fraction of liquid glass in the cement paste. The results of the combined influence of liquid glass and mechanical activation on physicochemical processes taking place in cement stone are represented in this research. Thermogravimetric analysis was used in order to study cement blends. Thermogravimetric analysis of modified cement stone assays was performed by thermo analyzer SETARAM TGA 92-24. The results of the analysis of phase transition taking place under high-temperature heating of cement stone modified by the mechanical activation of the water solution of the sodium silicate were introduced. Thermograms of cement stone assays were obtained at different hardening age. The comparison of these thermograms allows us to come to a conclusion on the formation and the retention during long time of a more dense structure of the composite matrix mixed by the mechanical activation of sodium silicate water solution. The relation between the concrete composition and its strength properties was stated. Perhaps, the capability of modified concrete to keep calcium ions in sparingly soluble hydrosilicates leads to the increase in its durability and corrosion resistance.

  6. Thermal behavior and kinetics assessment of ethanol/gasoline blends during combustion by thermogravimetric analysis

    International Nuclear Information System (INIS)

    3, CEP 12.516-410 Guaratinguetá, SP (Brazil); U.T.P. – Universidad Tecnológica de Pereira, Faculty of Mechanical Engineering, Pereira, Risaralda (Colombia))" data-affiliation=" (UNESP – Univ Estadual Paulista, Campus of Guaratinguetá, Department of Energy, Laboratory of Combustion and Carbon Capture LC3, CEP 12.516-410 Guaratinguetá, SP (Brazil); U.T.P. – Universidad Tecnológica de Pereira, Faculty of Mechanical Engineering, Pereira, Risaralda (Colombia))" >Rios Quiroga, Luis Carlos; 3, CEP 12.516-410 Guaratinguetá, SP (Brazil))" data-affiliation=" (UNESP – Univ Estadual Paulista, Campus of Guaratinguetá, Department of Energy, Laboratory of Combustion and Carbon Capture LC3, CEP 12.516-410 Guaratinguetá, SP (Brazil))" >Balestieri, José 3, CEP 12.516-410 Guaratinguetá, SP (Brazil))" data-affiliation=" (UNESP – Univ Estadual Paulista, Campus of Guaratinguetá, Department of Energy, Laboratory of Combustion and Carbon Capture LC3, CEP 12.516-410 Guaratinguetá, SP (Brazil))" >Antonio Perrella; 3, CEP 12.516-410 Guaratinguetá, SP (Brazil))" data-affiliation=" (UNESP – Univ Estadual Paulista, Campus of Guaratinguetá, Department of Energy, Laboratory of Combustion and Carbon Capture LC3, CEP 12.516-410 Guaratinguetá, SP (Brazil))" >Ávila, Ivonete

    2017-01-01

    Highlights: • Kinetic parameters of thermal decomposition events were obtained. • Thermal analysis was used as a tool for understanding combustion processes. • Blends would be classified using thermogravimetric analysis technics. • Synergistic effect of ethanol mixed with gasoline was studied and defined. • Relative error and activation energy values were used to analyze the synergy. - Abstract: The use of ethanol as a fuel or as an additive blended with gasoline is very important for most countries, which aim to reduce the heavy dependence on fossil fuels and mitigate greenhouse gases emission. An increased use of ethanol-gasoline blends has placed great relevance on acquiring knowledge about their physical and chemical properties. Thus, knowledge of such properties favors a better understanding of the effect of the percentage of ethanol/gasoline blends on engine performance. Thence, the present study has established a correlation between activation energy and synergetic effects, obtained by a thermal analysis, and ethanol content in gasoline for different blends in order to use this technique as a tool to classify these blends in the process in order to obtain useful energy in spark ignition engines. For such a purpose, a kinetic study has been conducted through a simultaneous thermal analysis system – TGA (thermogravimetry analysis) and DTA (differential thermal analysis) by following the methodology of non-isothermal tests. Thermogravimetric tests were performed and fuel activation energies for gasoline, ethanol, and percentages of 5, 10, 15, 20, 25, 30, 50, and 75% (%v) ethanol mixed with gasoline, which was achieved by the model free kinetics. The analysis results suggest that the theoretical curves characteristics of the thermal decomposition of ethanol-gasoline blends are rather different due to their ethanol content. Furthermore, it was observed significant interactions and synergistic effects, especially regarding those with low ethanol

  7. Oxy-fuel combustion characteristics and kinetics of microalgae Chlorella vulgaris by thermogravimetric analysis.

    Science.gov (United States)

    Chen, Chunxiang; Lu, Ziguang; Ma, Xiaoqian; Long, Jun; Peng, Yuning; Hu, Likun; Lu, Quan

    2013-09-01

    Oxy-fuel or O2/CO2 combustion technology was used to investigate the combustion of Chlorella vulgaris by thermogravimetric analysis (TGA). Oxy-fuel combustion occurs in an O2/CO2 atmosphere instead of an O2/N2 atmosphere and offers an alternative method of C. vulgaris preparation for biofuels processing. Our results show that three stages were observed during C. vulgaris combustion and the main combustion process occurred at the second stage. Compared with a 20%O2/80%N2 atmosphere, the mass loss rate at the DTG peaks (Rp) and the average reaction rate (Rv) in a 20%O2/80%CO2 atmosphere was lower, while the ignition temperature (TI) was higher. As oxygen concentration increases in an O2/CO2 atmosphere, Rp, Rv and the apparent activation energy (E) increases, while TI, the final temperature detected as mass stabilization (Tf) and the residue mass (Mr) decreases; As the heating rate (β) increases, TI, Tf and Rp increase, while Mr decreases. Crown Copyright © 2013. Published by Elsevier Ltd. All rights reserved.

  8. Pyrolysis and oxy-fuel combustion characteristics and kinetics of petrochemical wastewater sludge using thermogravimetric analysis.

    Science.gov (United States)

    Chen, Jianbiao; Mu, Lin; Cai, Jingcheng; Yao, Pikai; Song, Xigeng; Yin, Hongchao; Li, Aimin

    2015-12-01

    The pyrolysis and oxy-fuel combustion characteristics of petrochemical wastewater sludge (PS) were studied in air (O2/N2) and oxy-fuel (O2/CO2) atmospheres using non-isothermal thermogravimetric analysis (TGA). Pyrolysis experiments showed that the weight loss profiles were almost similar up to 1050K in both N2 and CO2 atmospheres, while further weight loss took place in CO2 atmosphere at higher temperatures due to char-CO2 gasification. Compared with 20%O2/80%N2, the drying and devolatilization stage of PS were delayed in 20%O2/80%CO2 due to the differences in properties of the diluting gases. In oxy-fuel combustion experiments, with O2 concentration increasing, characteristic temperatures decreased, while characteristic combustion rates and combustion performance indexes increased. Kinetic analysis of PS decomposition under various atmospheres was performed using Coats-Redfern approach. The results indicated that, with O2 concentration increasing, the activation energies of Step 1 almost kept constant, while the values of subsequent three steps increased. Copyright © 2015 Elsevier Ltd. All rights reserved.

  9. Thermogravimetric analysis of silicon carbide-silicon nitride polycarbosilazane precursor during pyrolysis from ambient to 1000 C

    Science.gov (United States)

    Ledbetter, F. E., III; Daniels, J. G.; Clemons, J. M.; Hundley, N. H.; Penn, B. G.

    1984-01-01

    Thermogravimetric analysis data are presented on the unmeltable polycarbosilazane precursor of silicon carbide-silicon nitride fibers, over the room temperature-1000 C range in a nitrogen atmosphere, in order to establish the weight loss at various temperatures during the precursor's pyrolysis to the fiber material. The fibers obtained by this method are excellent candidates for use in applications where the oxidation of carbon fibers (above 400 C) renders them unsuitable.

  10. Friedel's salt profiles from thermogravimetric analysis and thermodynamic modelling of Portland cement-based mortars exposed to sodium chloride solution

    DEFF Research Database (Denmark)

    Shi, Zhenguo; Geiker, Mette Rica; Lothenbach, Barbara

    2017-01-01

    Thermogravimetric analysis (TGA), powder X-ray diffraction (XRD) and thermodynamic modelling have been used to obtain Friedel's salt profiles for saturated mortar cylinders exposed to a 2.8 M NaCl solution. Comparison of the measured Friedel's salt profiles with the total chloride profiles...

  11. Studies of the thermal properties of horn keratin by dielectric spectroscopy, thermogravimetric analysis and differential thermal analysis

    International Nuclear Information System (INIS)

    Marzec, E.; Piskunowicz, P.; Jaroszyk, F.

    2002-01-01

    The dielectric and thermal properties of horn keratin have been studied bu dielectric spectroscopy in the frequency range 10 1 -10 5 Hz, thermogravimetric analysis (TG) and different thermal analysis (DTA). Measurement of non-irradiated and g amma - irradiated keratin with doses 5, 50 kGy were performed at temperature from 22 to 260 o C. The results revealed the occurrence of phase transitions related to release of loosely bound water and bound water up to 200 o Cand the denaturation of the crystalline structure above this temperature. The influence of γ-irradiation on the thermal behaviour of keratin is significant only in the temperature range of denaturation. The decrease in the temperature of denaturation would suggest that γ-irradiation initiates main-chain degradation. (authors)

  12. Effect of anaerobic digestion on sequential pyrolysis kinetics of organic solid wastes using thermogravimetric analysis and distributed activation energy model.

    Science.gov (United States)

    Li, Xiaowei; Mei, Qingqing; Dai, Xiaohu; Ding, Guoji

    2017-03-01

    Thermogravimetric analysis, Gaussian-fit-peak model (GFPM), and distributed activation energy model (DAEM) were firstly used to explore the effect of anaerobic digestion on sequential pyrolysis kinetic of four organic solid wastes (OSW). Results showed that the OSW weight loss mainly occurred in the second pyrolysis stage relating to organic matter decomposition. Compared with raw substrate, the weight loss of corresponding digestate was lower in the range of 180-550°C, but was higher in 550-900°C. GFPM analysis revealed that organic components volatized at peak temperatures of 188-263, 373-401 and 420-462°C had a faster degradation rate than those at 274-327°C during anaerobic digestion. DAEM analysis showed that anaerobic digestion had discrepant effects on activation energy for four OSW pyrolysis, possibly because of their different organic composition. It requires further investigation for the special organic matter, i.e., protein-like and carbohydrate-like groups, to confirm the assumption. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Thermogravimetric studies on the silicothermic reduction of uranium tetrafluoride under nitrogen

    International Nuclear Information System (INIS)

    Venkataramani, R.; Bhatt, Y.J.; Krishnamurthy, N.; Garg, S.P.

    1986-01-01

    This paper presents details of the experimental procedure and results obtained by thermogravimetric studies on the preparation of uranium nitrides by silicothermic reduction of uranium tetrafluoride under a nitrogen atmosphere. The folowing sequential steps are involved during the reaction: 4UF 4 +Si->4UF 3 +SiF 4 (g), 2UF 3 +Si+N 2 ->2UNF+SiF 4 (g), 4UNF+Si+N 2 ->2U 2 N 3 +SiF 4 (g), the uranium sesquintride U 2 N 3 obtained in the above process then decomposed at 1370 K under a dynamic vacuum of less than 10 -2 Tor to yield uranium mononitride of purity better than 99.9%, according to reaction 2U 2 N 3 ->4UN+N 2 (g). The chemical composition of the intermediate products formed during the sequential steps of the process, assessed by thermogravimetric and differential thermogravimetric studies, were further confirmed by chemical and X-ray analysis

  14. Pyrolysis of tyre powder using microwave thermogravimetric analysis: Effect of microwave power.

    Science.gov (United States)

    Song, Zhanlong; Yang, Yaqing; Zhou, Long; Zhao, Xiqiang; Wang, Wenlong; Mao, Yanpeng; Ma, Chunyuan

    2017-02-01

    The pyrolytic characteristics of tyre powder treated under different microwave powers (300, 500, and 700 W) were studied via microwave thermogravimetric analysis. The product yields at different power levels were studied, along with comparative analysis of microwave pyrolysis and conventional pyrolysis. The feedstock underwent preheating, intense pyrolysis, and final pyrolysis in sequence. The main and secondary weight loss peaks observed during the intense pyrolysis stage were attributed to the decomposition of natural rubbers and synthetic rubbers, respectively. The total mass loss rates, bulk temperatures, and maximum temperatures were distinctively higher at higher powers. However, the maximum mass loss rate (0.005 s -1 ), the highest yields of liquid product (53%), and the minimum yields of residual solid samples (43.83%) were obtained at 500 W. Compared with conventional pyrolysis, microwave pyrolysis exhibited significantly different behaviour with faster reaction rates, which can decrease the decomposition temperatures of both natural and synthetic rubber by approximately 110 °C-140 °C.

  15. Thermogravimetric study of vinpocetine suppository

    Directory of Open Access Journals (Sweden)

    N. А. Nаgоrnaya

    2014-02-01

    Full Text Available Introduction. Development of technology is the one of the main stage in creation of new medications. Technological process of suppository manufacturing includes sufficiently long thermoprocessing during suppository base making, addition of the active substances and homogenisation. This makes risk of chemical and physical transformations of active substances and excipients in suppository which can be destroyed and changed pharmacologicaly. Use of thermogravimetric analyses in pharmaceutical technology allows to study possibility of chemical interactions of components in the wide range of temperature. The aim of this work was to study thermoprocessing effects on suppository base with vinpocetine in temperature range of technological process of suppository manufacturing. Object. Vinpocetine rectal suppository (with 0,5% of surface-active substances, active substance (vinpocetine and excipients (twin 80, cacao oil were used as the objects of thermogravimetric investigation. Thermogravimetric analyses was carried out on the derivatograph «Shimadzu DTG-60» (Japan with the platinum-rhodium thermocouple by heating from 25°C to 200°C in the aluminium crucible. α-Al2O3 was used as standard. Heating speed was 10ºС in minute. Model mass was 14,23 – 34,4 mg. Conclusions. It was established that cacao oil is thermolabile substance with melting temperature 41,32 ºС. Surface-active substance twin 80 displays thermostability from 30 tо 100ºС. Vinpocetine derivatogramme confirmed its thermostability in temperature range from 30 tо 154 ºС. Derivatogramme of vinpocetine rectal suppository 0,01 and suppository base displayed the absence of critical temperature lower 100ºС. Insignificant mass loss (0,21% shows that fact. Investigation of composition over 100ºС wasn’t carried out because these temperatures aren’t used in technological process of suppository manufacturing. Presence of thermal effects on derivatogramme of vinpocetine rectal

  16. The degree of hydration assessment of blended cement pastes by differential thermal and thermogravimetric analysis. Morphological evolution of the solid phases

    International Nuclear Information System (INIS)

    Monteagudo, S.M.; Moragues, A.; Gálvez, J.C.; Casati, M.J.; Reyes, E.

    2014-01-01

    Highlights: • A proposal of hydration degree calculation for blended cement pastes is presented. • The method is based both on the contributions of various authors and on DTA–TG results. • Paste and mortar specimens with BFS, FA and SF mineral admixtures were used. • The evaluation of CH gives information on hydration and pozzolanic reactions. • The assessment of α provides an insight into future strength evolution. - Abstract: The degree of hydration assessment of cement paste from differential thermal and thermogravimetric analysis data has been performed by several authors that have offered a number of proposals for technical application to blended cements. In this paper, two calculation methods are studied in detail. Then, a proposal of the degree of hydration calculation for blended cements, based on the analysis of experimental results of DTA–TG, is presented. The proposed method combines the contributions of the authors and allows straightforward calculation of the degree of hydration from the experimental results. Validation of the methodology was performed by macroscopic and microstructural tests through paste and mortar specimens with blast furnace slag, flying ash and silica fume mineral admixtures bei(g)ng used. Tests of scanning electron microscopy with an energy dispersive analyser on paste specimens, and of mechanical strength on mortar specimens with the same percentages of substitution, were performed. They showed good agreement with the information derived from the differential thermal and thermogravimetric analysis data

  17. Determination of effective moisture diffusivity and drying kinetics for poplar sawdust by thermogravimetric analysis under isothermal condition.

    Science.gov (United States)

    Chen, Dengyu; Zheng, Yan; Zhu, Xifeng

    2012-03-01

    The current study presents a thermogravimetric method to determine the effective moisture diffusivity and drying kinetics of biomass. Drying experiments on poplar sawdust were performed at four temperatures (60, 70, 80, and 90°C) by a thermogravimetric analyzer (TGA). The major assumption in experimentally determining effective diffusivity by Fick's diffusion equation is that drying is mass transfer limited and temperature remains isothermal during drying. The results indicated that TGA could well achieve these determining conditions. The drying process of sawdust mostly took place in the falling rate period. Midilli-Kucuk model showed the best fit for all experimental data. The effective diffusivity values changed from 9.38 × 10(-10)m(2)/s to 1.38 × 10(-9)m(2)/s within the given temperature range, and the activation energy was calculated to be 12.3 kJ/mol. Copyright © 2011 Elsevier Ltd. All rights reserved.

  18. Thermogravimetric, Devolatilization Rate, and Differential Scanning Calorimetry Analyses of Biomass of Tropical Plantation Species of Costa Rica Torrefied at Different Temperatures and Times

    Directory of Open Access Journals (Sweden)

    Johanna Gaitán-Álvarez

    2018-03-01

    Full Text Available We evaluated the thermogravimetric and devolatilization rates of hemicellulose and cellulose, and the calorimetric behavior of the torrefied biomass, of five tropical woody species (Cupressus lusitanica, Dipteryx panamensis, Gmelina arborea, Tectona grandis and Vochysia ferruginea, at three temperatures (TT and three torrefaction times (tT using a thermogravimetric analyzer. Through a multivariate analysis of principal components (MAPC, the most appropriate torrefaction conditions for the different types of woody biomass were identified. The thermogravimetric analysis-derivative thermogravimetry (TGA-DTG analysis showed that a higher percentage of the hemicellulose component of the biomass degrades, followed by cellulose, so that the hemicellulose energy of activation (Ea was less than that of cellulose. With an increase in TT and tT, the Ea for hemicellulose decreased but increased for cellulose. The calorimetric analyses showed that hemicellulose is the least stable component in the torrefied biomass under severe torrefaction conditions, and cellulose is more thermally stable in torrefied biomass. From the MAPC results, the best torrefaction conditions for calorimetric analyses were at 200 and 225 °C after 8, 10, and 12 min, for light and middle torrefaction, respectively, for the five woody species.

  19. Thermogravimetric analysis of the behavior of sub-bituminous coal and cellulosic ethanol residue during co-combustion.

    Science.gov (United States)

    Buratti, C; Barbanera, M; Bartocci, P; Fantozzi, F

    2015-06-01

    The influence of the addition of cellulosic ethanol residue (CER) on the combustion of Indonesian sub-bituminous coal was analyzed by non isothermal thermo-gravimetric analysis (TGA). The effect of blends ratio (5%, 10%, 15% and 20%), interaction mechanism, and heating rate (5°C/min, 10°C/min, 15°C/min, 20°C/min) on the combustion process was studied. The results show that the increase of the blending ratio allows to achieve the increase of the combustibility index from 7.49E-08 to 5.26E-07 at the blending ratio of 20%. Two types of non-isothermal kinetic analysis methods (Ozawa-Flynn-Wall and Vyazovkin) were also applied. Results indicate that the activation energy of the blends decreases with increasing the conversion rate. In particular, the blending ratio of 20% confirms to have the better combustion performance, with the average value of the activation energy equal to 41.10 kJ/mol obtained by Ozawa-Flynn-Wall model and 31.17 kJ/mol obtained by Vyazovkin model. Copyright © 2015 Elsevier Ltd. All rights reserved.

  20. Temperature dependence of the resonance frequency of thermogravimetric devices

    NARCIS (Netherlands)

    Iervolino, E.; Riccio, M.; Van Herwaarden, A.W.; Irace, A.; Breglio, G.; Van der Vlist, W.; Sarro, P.M.

    2010-01-01

    This paper investigates the temperature dependence of the resonance frequency of thermogravimetric (TG) devices for tip heating over the temperature range of View the MathML source 25–600?C. The resonance frequency of a fabricated TG device shows to be temperature independent for tip heating up to

  1. A Thermogravimetric Study of the Behaviour of Biomass Blends During Combustion

    Directory of Open Access Journals (Sweden)

    Ivo Jiříček

    2012-01-01

    Full Text Available The ignition and combustion behavior of biomass and biomass blends under typical heating conditions were investigated. Thermogravimetric analyses were performed on stalk and woody biomass, alone and blended with various additive weight ratios. The combustion process was enhanced by adding oxygen to the primary air. This led to shorter devolatilization/pyrolysis and char burnout stages, which both took place at lower temperatures than in air alone. The results of the ignition study of stalk biomass show a decrease in ignition temperature as the particle size decreases. This indicates homogeneous ignition, where the volatiles burn in the gas phase, preventing oxygen from reaching the particle surface.The behavior of biomass fuels in the burning process was analyzed, and the effects of heat production and additive type were investigated. Mixing with additives is a method for modifying biofuel and obtaining a more continuous heat release process. Differential scanning calorimetric-thermogravimetric (DSC-TGA analysis revealed that when the additive is added to biomass, the volatilization rate is modified, the heat release is affected, and the combustion residue is reduced at the same final combustion temperature.

  2. Thermogravimetric analysis of atomized ferromagnetic composites with multiwalled carbon nanotubes: an unusual behavior of nickel in nanospace.

    Science.gov (United States)

    Chen, Xu; Gupta, S; Santhanam, K S V

    2014-03-01

    A spin polarization of atomized ferromagnetic atoms like cobalt or nickel in nano space results in the modification of the electron configuration in the ferromagnetic atom that changes its oxidative property. We have prepared cobalt and nickel composites with multiwalled carbon nanotubes using atomized cobalt and nickel particles, for investigating their thermal oxidative behavior by thermogravimetric analysis (TGA). The composites showed the absence of a thermal oxidation in the temperature range of ambient to the break down temperature of multiwalled carbon nanotubes at 800 degrees C. At this temperature while Co composite forms cobalt oxide, the Ni composite becomes volatile that results in the divergent behavior of the two ferromagnetic compounds with a weight gain observed in TGA for Co and a loss for Ni. The mechanisms operating in the two cases are discussed in this work.

  3. Thermogravimetric studies of vapour-aerosol interactions

    International Nuclear Information System (INIS)

    Henshaw, J.; Newland, M.S.; Wood, S.J.

    1991-01-01

    Thermogravimetric analysis has been used to study the interaction of iodine vapour with cadmium, silver and manganese monoxide substrates. These studies have demonstrated the importance of time-dependence data on reaction rates. Iodine did not react with manganese monoxide (as expected from thermodynamic considerations); however, extensive reaction did occur with silver and cadmium. Two rate limiting mechanisms were observed: mass transfer of iodine molecules from the gas phase (leading to linear reaction rates) and parabolic kinetics (ie inversely proportional to the extent of reaction) when the rate was limited by a diffusion process through the reaction product. (author)

  4. Thermal degradation of Shredded Oil Palm Empty Fruit Bunches (SOPEFB) embedded with Cobalt catalyst by Thermogravimetric Analysis (TGA)

    Science.gov (United States)

    Alias, R.; Hamid, N. H.; Jaapar, J.; Musa, M.; Alwi, H.; Halim, K. H. Ku

    2018-03-01

    Thermal behavior and decomposition kinetics of shredded oil palm empty fruit bunches (SOPEFB) were investigated in this study by using thermogravimetric analysis (TGA). The SOPEFB were analyzed under conditions of temperature 30 °C to 900 °C with nitrogen gas flow at 50 ml/min. The SOPEFB were embedded with cobalt (II) nitrate solution with concentration 5%, 10%, 15% and 20%. The TG/DTG curves shows the degradation behavior of SOPEFB following with char production for each heating rate and each concentration of cobalt catalyst. Thermal degradation occurred in three phases, water drying phase, decomposition of hemicellulose and cellulose phase, and lignin decomposition phase. The kinetic equation with relevant parameters described the activation energy required for thermal degradation at the temperature regions of 200 °C to 350 °C. Activation energy (E) for different heating rate with SOPEFB embedded with different concentration of cobalt catalyst showing that the lowest E required was at SOPEFB with 20% concentration of cobalt catalyst..

  5. Research on Mechanism of Paper Burning by Thermogravimetric Analysis

    Institute of Scientific and Technical Information of China (English)

    QIN Da; HAN Xingzhou; WANG Xiaoguang; QI Fengliang; WANG Zijie; GUO Zihan; HAO Hongguang

    2015-01-01

    The examination of charred document is a challenge and usually requires a careful application of certain scientific techniques due to its unstable property. To address this issue, the mechanism of paper burning was studied in this paper. Here thermal-gravimetry (TG) was applied to investigate five kinds of paper, along with their TG and derivative thermogravimetric curve (DTG) observed at different atmospheric conditions. The results showed that the shape of curves, albeit similar, varied with the physical and chemical composition of paper. In the burning process, dehydration and de-polymerization are the two main pathways for cellulose, the major ingredient of paper. The heating rate indicated little influence on the curves while the sort of atmosphere worked strongly. The reason is due to the lack of tar oxidation when nitrogen used as the atmospheric environment. At moderate temperature, de-polymerization prevails and the tar can be observed. With temperature increasing, the tar and cellulose are further decomposed, leading to products of high boiling-point. According to the results, the charred document can be classified as one of the dehydrated, tarred, charred and ashed. Except the ashed stage, the other three can be handled and the writing whereon can be deciphered. The results exposed hereof may provide a fundamental for examining and deciphering charred document.

  6. Automation of a McBain-Bakr-type thermogravimetric analyzer using a digital image correlation technique

    International Nuclear Information System (INIS)

    Trexler, M.D.; Sanders, T.H. Jr.; Singh, P.M.

    2006-01-01

    Thermogravimetric analysis was used to obtain corrosion kinetics data for several materials in high-temperature environments. A thermogravimetric analyzer has been developed that uses a McBain-Bakr quartz spring balance in conjunction with a digital image acquisition and analysis package to accurately characterize materials through image correlation. This provides a new method for automatically measuring mass changes continuously with a variable resolution depending on the spring component. The decomposition of calcium oxalate was used to verify the validity of the technique. The results show two reactions, whose reaction temperatures were determined by the intercept method, upon heating to 650 deg. C. The mass loss at the first reaction temperature, 200 deg. C, was 20% and a 30% loss was observed at 500 deg. C. Comparison of the experimentally obtained results with those of other researchers who used commercial instruments suggests that the method of using digital image analysis in conjunction with a spring to monitor mass change is a viable and accurate replacement for automatic electrobalances and cathetometers for thermal analysis of materials. Additional comparison between corrosion tests performed on SA210 steel in H 2 S using both a commercial thermobalance and the developed technique confirmed that high-temperature corrosion can be monitored accurately with the proposed method

  7. Kinetic analysis of thermogravimetric data of thorium-all-cis-1,2,3,4-cyclopentanetetracarboxylic acid complex

    International Nuclear Information System (INIS)

    Ramarao, G.A.; Nair, P.K.R.; Srinivasulu, K.

    1979-01-01

    Thorium (IV) forms 1:1 complex with all-cis-1,2,3,4-cyclopentanetetracarboxylic acid (CPTA). Thermogravimetric analysis indicated that it undergoes primarily a two step decomposition of one corresponding to loss of water and another to the decomposition of the complex. Apparent activation energy, frequency factor and activation entropy were determined. Using the experimental data, the reaction order and activation energy were calculated by Freeman-Carroll method and also by Doyle method as modified by J. Zsako, by calculation of standard deviation instead of curve fitting method. (author)

  8. Miniature quartz crystal-resonator-based thermogravimetric detector.

    Science.gov (United States)

    Sai, N; Tagawa, Y; Sohgawa, M; Abe, T

    2014-09-01

    In this work, a new design for a microheater combined with a quartz crystal microbalance (QCM) array for thermogravimetric analysis is presented. Each QCM consists of two electrodes to excite thickness-shear-mode vibrations and one microheater to increase the temperature on the crystal backside. In addition, all the electrode pads are patterned on the crystal backside, making the design of the QCM compact and user-friendly. Finally, the proposed QCM array was employed to separate ethanol from methanol. This was successfully achieved via thermal desorption spectra calculated by differentiating the frequency changes.

  9. Electrodynamic thermogravimetric analyzer

    International Nuclear Information System (INIS)

    Spjut, R.E.; Bar-Ziv, E.; Sarofim, A.F.; Longwell, J.P.

    1986-01-01

    The design and operation of a new device for studying single-aerosol-particle kinetics at elevated temperatures, the electrodynamic thermogravimetric analyzer (EDTGA), was examined theoretically and experimentally. The completed device consists of an electrodynamic balance modified to permit particle heating by a CO 2 laser, temperature measurement by a three-color infrared-pyrometry system, and continuous weighing by a position-control system. In this paper, the position-control, particle-weight-measurement, heating, and temperature-measurement systems are described and their limitations examined

  10. Rapidly assessing the activation conditions and porosity of metal-organic frameworks using thermogravimetric analysis.

    Science.gov (United States)

    McDonald, Thomas M; Bloch, Eric D; Long, Jeffrey R

    2015-03-25

    A methodology utilizing a thermogravimetric analyzer to monitor propane uptake following incremental increases of the temperature is demonstrated as a means of rapidly identifying porous materials and determining the optimum activation conditions of metal-organic frameworks.

  11. Thermogravimetric investigations of vanadium complexes

    International Nuclear Information System (INIS)

    Bechmann, W.; Uhlemann, E.; Ludwig, W.

    1987-01-01

    Extensive studies on oxovanadium(IV) and (V) complexes with bidentate chelating ligands include thermogravimetric investigations. TG, DTG, and DTA data provide additional facts to redox behaviour and stability of the complexes. These data also allow a critical appreciation of the given melting temperatures. (author)

  12. Synthesis, spectroscopic characterization and thermogravimetric analysis of two series of substituted (metallotetraphenylporphyrins

    Directory of Open Access Journals (Sweden)

    Rasha K. Al-Shewiki

    2017-06-01

    Full Text Available Subsequent treatment of H2TPP(CO2H4 (tetra(p-carboxylic acid phenylporphyrin, 1 with an excess of oxalyl chloride and HNR2 afforded H2TPP(C(ONR24 (R = Me, 2; iPr, 3 with yields exceeding 80%. The porphyrins 2 and 3 could be converted to the corresponding metalloporphyrins MTPP(C(ONR24 (R = Me/iPr for M = Zn (2a, 3a; Cu (2b, 3b; Ni (2c, 3c; Co (2d, 3d by the addition of 3 equiv of anhydrous MCl2 (M = Zn, Cu, Ni, Co to dimethylformamide solutions of 2 and 3 at elevated temperatures. Metalloporphyrins 2a–d and 3a–d were obtained in yields exceeding 60% and have been, as well as 2 and 3, characterized by elemental analysis, electrospray ionization mass spectrometry (ESIMS and IR and UV–vis spectroscopy. Porphyrins 2, 2a–d and 3, 3a–d are not suitable for organic molecular beam deposition (OMBD, which is attributed to their comparatively low thermal stability as determined by thermogravimetric analysis (TG of selected representatives.

  13. Acoustic emission analysis coupled with thermogravimetric experiments dedicated to high temperature corrosion studies on metallic alloys

    International Nuclear Information System (INIS)

    Serris, Eric; Al Haj, Omar; Peres, Veronique; Cournil, Michel; Kittel, Jean; Grosjean, Francois; Ropital, Francois

    2014-01-01

    High temperature corrosion of metallic alloys (like iron, nickel, zirconium alloys) can damage equipment of many industrial fields (refinery, petrochemical, nuclear..). Acoustic emission (AE) is an interesting method owing to its sensitivity and its non-destructive aspect to quantify the level of damage in use of these alloys under various environmental conditions. High temperature corrosive phenomena create stresses in the materials; the relaxation by cracks of these stresses can be recorded and analyzed using the AE system. The goal of our study is to establish an acoustic signals database which assigns the acoustic signals to the specific corrosion phenomena. For this purpose, thermogravimetric analysis (TGA) is coupled with acoustic emission (AE) devices. The oxidation of a zirconium alloy, zircaloy-4, is first studied using thermogravimetric experiment coupled to acoustic emission analysis at 900 C. An inward zirconium oxide scale, preliminary dense, then porous, grow during the isothermal isobaric step. The kinetic rate increases significantly after a kinetic transition (breakaway). This acceleration occurs with an increase of acoustic emission activity. Most of the acoustic emission bursts are recorded after the kinetic transition. Acoustic emission signals are also observed during the cooling of the sample. AE numerical treatments (using wavelet transform) completed by SEM microscopy characterizations allows us to distinguish the different populations of cracks. Metal dusting represents also a severe form of corrosive degradation of metal alloy. Iron metal dusting corrosion is studied by AE coupled with TGA at 650 C under C 4 H 10 + H 2 + He atmosphere. Acoustic emission signals are detected after a significant increase of the sample mass.

  14. A comprehensive evaluation of water uptake on atmospherically relevant mineral surfaces: DRIFT spectroscopy, thermogravimetric analysis and aerosol growth measurements

    Directory of Open Access Journals (Sweden)

    R. J. Gustafsson

    2005-01-01

    Full Text Available The hygroscopicity of mineral aerosol samples has been examined by three independent methods: diffuse reflectance infrared Fourier transform spectroscopy, thermogravimetric analysis and differential mobility analysis. All three methods allow an evaluation of the water coverage of two samples, CaCO3 and Arizona Test dust, as a function of relative humidity. For the first time, a correlation between absolute gravimetric measurements and the other two (indirect methods has been established. Water uptake isotherms were reliably determined for both solids which at 298 K and 80% relative humidity exhibited similar coverages of ~4 monolayers. However, the behaviour at low relative humidity was markedly different in the two cases, with Arizona Test Dust showing a substantially higher affinity for water in the contact layer. This is understandable in terms of the chemical composition of these two materials. The mobility analysis results are in good accord with field observations and with our own spectroscopic and gravimetric measurements. These findings are of value for an understanding of atmospheric chemical processes.

  15. Water desorption of cassava starch granules: A study based on thermogravimetric analysis of aqueous suspensions and humid powders.

    Science.gov (United States)

    Ayala Valencia, Germán; Djabourov, Madeleine; do Amaral Sobral, Paulo José

    2016-08-20

    This work reports on water desorption from cassava starch in relation with the structure and conditioning of granules in suspensions or after equilibration in desiccators. The experimental work is performed by thermogravimetric analysis with isothermal and non-isothermal protocols and interpreted to derive the activation energies and desorption frequencies according to the humidity range with no adjustable parameter. The analysis points out the different types of water interacting with the starch granules and relates the drying coefficients to their microscopic structure. The work helps clarifying contradictory and partial results from the literature. Copyright © 2016 Elsevier Ltd. All rights reserved.

  16. Thermogravimetric investigations of cream with minoxidil

    Directory of Open Access Journals (Sweden)

    I. V. Gnitko

    2016-12-01

    Full Text Available Minoxidil is one of the most effective and modern medications, which is used in modern trichology for hair growth stimulation in case of androgenic and other forms of alopecia. Clinical effect of this substance is caused by the intensification of metabolic processes in the skin due to intensification of microcirculation. For local application domestic dermatology uses imported minoxidil medicines in form of alcohol-water lotions and aerosols. The use of semisolid dosage form with minoxidil for external administration will allow to increase its efficacy and will widen the arsenal of domestic pharmacotherapeutic agents for hair growth stimulation. Rational composition of minoxidil semisolid dosage form for external use with 2% of active substance has been developed at the Department of Medicinal Preparations Technology, Zaporozhye State Medical University as a result of complex physical-chemical, microbiological and biopharmaceutical investigations. The aim of this work is the study of thermal treatment effects of cream-mask with minoxidil for external use over the temperature range, which is used in technological process of this dosage form manufacturing. Materials and methods. Cream with 2% of minoxidil on the emulsion base and its excipients have been used as the object for the thermogravimetric investigations. Thermogravimetric analysis has been carried out on the derivatograph «Shimadzu DTG-60», Japan, with the platinum and platinum-rhodium thermopair with samples’ heating in aluminium crucibles from 25 to 200ºС. Results. According to thermogravimetric experimental data minoxidil is a thermal stable substance from 26 to 240ºС. During experimental process insignificant endothermic effect was determined at 191,72ºС. However the mass of the example to the end of experiment practically didn’t change (decrease on 0,32%. Thermal effects on the derivatogram of minoxidil emulsion cream match with thermal effects of the base components and

  17. Preparation, thermogravimetric study and infrared spectra of rare earth acetates

    International Nuclear Information System (INIS)

    Graehlert, X.; Starke, M.

    1992-01-01

    The anhydrous and the hydrated acetates of Ho, Er, Tm, Yb and Lu have been prepared. The compounds obtained have been investigated by thermogravimetric analysis and infrared spectroscopy. The thermal decomposition of the rare earth acetates may proceed via various steps. It depends on both the number of crystal water molecules in the acetates and the rare earth element's behaviour. (orig.)

  18. Fluid selection and parametric analysis on condensation temperature and plant height for a thermogravimetric heat pump

    International Nuclear Information System (INIS)

    Najafi, Behzad; Obando Vega, Pedro; Guilizzoni, Manfredo; Rinaldi, Fabio; Arosio, Sergio

    2015-01-01

    The Thermogravimetric Heat Pump (TGHP) is a non-conventional system, implementing a reverse cycle, the main difference of which from the usual vapor compression (Rankine) cycle is a quasi-isothermal compression of the working fluid by a high heat capacity carrier fluid. Previous studies showed that employing HFC134a or PF5050 as working fluids may be promising in terms of thermodynamic performance, though the corresponding required plant heights confine its application to tall buildings (from minimum height of 10–12 storeys to skyscrapers). Accordingly, an investigation has been carried out in the present study in order to determine a group of fluids which allow lower heights under the same input conditions. In order to investigate the performance of the system and the required plant height, operation of a 100 kW TGHP has been simulated for 17 different fluids. Accordingly, the corresponding COPs and required heights are determined and based on the achieved COPs, the optimum fluid for each range of building height is selected. The resulting plant heights range from 20 m to nearly 200 m and R245ca is shown to be the most promising fluid for the lowest plant height range. A parametric study is next carried out in order to study the effect of variations in the condensation temperature and the dimensionless plant height on the performance of the system. The obtained results demonstrate that an increase in the former from 313 K to 348 K, for almost all of the analyzed fluids, causes a reduction of around 50% in the COP. It is also shown that, almost independent of the employed fluid, the maximum values of COP are reached for a dimensionless plant height of around 1.8. Moreover, all the analyzed fluids show basically the same COP trend and, at the same operating conditions, the COP values for all fluids are within a 10% range of variation. This leads to the conclusion that the thermophysical properties of the employed fluid mainly influences the required height of

  19. Synthesis, spectroscopic characterization and thermogravimetric analysis of two series of substituted (metallo)tetraphenylporphyrins.

    Science.gov (United States)

    Al-Shewiki, Rasha K; Mende, Carola; Buschbeck, Roy; Siles, Pablo F; Schmidt, Oliver G; Rüffer, Tobias; Lang, Heinrich

    2017-01-01

    Subsequent treatment of H 2 TPP(CO 2 H) 4 (tetra( p -carboxylic acid phenyl)porphyrin, 1 ) with an excess of oxalyl chloride and HNR 2 afforded H 2 TPP(C(O)NR 2 ) 4 (R = Me, 2 ; iPr, 3 ) with yields exceeding 80%. The porphyrins 2 and 3 could be converted to the corresponding metalloporphyrins MTPP(C(O)NR 2 ) 4 (R = Me/iPr for M = Zn ( 2a , 3a ); Cu ( 2b , 3b ); Ni ( 2c , 3c ); Co ( 2d , 3d )) by the addition of 3 equiv of anhydrous MCl 2 (M = Zn, Cu, Ni, Co) to dimethylformamide solutions of 2 and 3 at elevated temperatures. Metalloporphyrins 2a - d and 3a - d were obtained in yields exceeding 60% and have been, as well as 2 and 3 , characterized by elemental analysis, electrospray ionization mass spectrometry (ESIMS) and IR and UV-vis spectroscopy. Porphyrins 2 , 2a - d and 3 , 3a - d are not suitable for organic molecular beam deposition (OMBD), which is attributed to their comparatively low thermal stability as determined by thermogravimetric analysis (TG) of selected representatives.

  20. Pb-H2O Thermogravimetric Plants. The Rankine Cycle

    International Nuclear Information System (INIS)

    Arosio, S.; Carlevaro, R.

    2000-01-01

    An economic evaluation concerning Pb-H 2 O thermogravimetric systems with an electric power in the range 200-1.000 kW has been done. Moreover, plant and running costs for a thermogravimetric and a Rankine cycle, 1 MW power, have been compared. Basically due to the lead charge, the plant cost of the former is higher: nevertheless such amount can be recuperated in less than three years, being higher the running cost of the latter [it

  1. Analysis of Mechanical and Thermogravimetric Properties of Composite Materials Based on PVA/MWCNT and Styrene-Acrylic Copolymer/MWCNT

    Science.gov (United States)

    Volynets, N. I.; Poddubskaya, O. G.; Demidenko, M. I.; Lyubimov, A. G.; Kuzhir, P. P.; Suslyaev, V. I.; Pletnev, M. A.; Zicans, Janis

    2017-08-01

    Mechanical and thermogravimetric properties of polymer composite materials with various concentrations of multiwalled carbon nanotubes effectively shielding radiation in the radio frequency (20 Hz - 1 MHz) and microwave (26-36 GHz) frequency ranges are studied. As a matrix, widely available polymeric materials, such as polyvinyl acetate and styrene-acrylate, were used in the form of dispersions. From the analysis of the obtained experimental data, it was shown that the introduction of carbon nanotubes into the polymer matrix makes it possible to increase mechanical properties and thermal stability of composite materials.

  2. Pyrolysis kinetics investigation of Malaysian based biomass with non-isothermal thermogravimetric analysis (TGA)

    International Nuclear Information System (INIS)

    Seyed Shahabeddin Nehzati; Dayang Radiah Awang Biak; Wan Azlina Wan Abdul Karim Ghani; Mohd Amran Mohd Salleh

    2010-01-01

    Full text: Biomass is currently being used as a sustainable energy source. Otherwise the scarceness of fossil fuel sources and the demand for environmental responsibility force the industries to use biomass as an alternate source of energy. Pyrolysis is the first step of biomass conversion and well understanding of this process can develop the biomass conversion such as gasification, liquefaction, carbonization and combustion .TGA studies of Malaysian based biomass have been carried out. TGA studies provide important insight on the thermochemical behavior of specific solid waste. The results of non-isothermal thermogravimetric analysis of palm kernel shell, coconut shell and bagasse, carried out at heating rates of 10 degree Celsius/ min, 20 degree Celsius/ min and 50 degree Celsius/ min, to ramp the temperature from 30 to 1000 were analysed. The TGA studies were carried out in an inert atmosphere of nitrogen. Arrhenius parameters were estimated by 3 different models namely Kissinger model, three-pseudo component and DEAM model the estimated values and the models were compared. The results show that the three-pseudo component model has a good agreement with the experimental results, indicating that ligno celluloses components in the mixture behave in the same way as they do separately. Also it is seen that the decomposition process shifts to higher temperatures at higher heating rates as a result of the competing effects of heat and mass transfer to the material. (Author)

  3. Thermogravimetric analysis of the co-combustion of paper mill sludge and municipal solid waste

    International Nuclear Information System (INIS)

    Hu, Shanchao; Ma, Xiaoqian; Lin, Yousheng; Yu, Zhaosheng; Fang, Shiwen

    2015-01-01

    Highlights: • Thermogravimetric analysis of paper mill sludge and municipal solid waste were studied. • The combustion of paper mill sludge could be improved by blending municipal solid waste. • There existed significant interaction during co-combustion of the blends. • The OFW and Starink methods were used to obtain the activation energy. • The average activation energy was the lowest by blending 20% municipal solid waste. - Abstract: The thermal characteristics and kinetics of paper mill sludge (PMS), municipal solid waste (MSW) and their blends in the combustion process were investigated in this study. The mass percentages of PMS in the blends were 10%, 30%, 50%, 70% and 90%, respectively. The experiments were carried out at different heating rates (10 °C/min, 20 °C/min and 30 °C/min) and the temperature ranged from room temperature to 1000 °C in a thermogravimetric simultaneous thermal analyzer. The results suggested that the ignition temperature and burnout temperature of MSW were lower than that of PMS, and the mass loss rate of MSW was larger especially at low temperatures. There were only two mass loss peaks in the differential thermogravimetry (DTG) curve, while three mass loss peaks were observed when the blending ratios of PMS were 30%, 50%, 70%. The value of the comprehensive combustion characteristic index of the blends indicated a good combustibility when the percentage of PMS (PPMS) in the blends was less than 30%. There existed certain interaction between the combustion process of PMS and MSW, especially at high temperature stage. Activation energy (E) value obtained by the Ozawa–Flynn–Wall (OFW) method and the Starink method were very consistent. When the mass percentage of PMS in the blends was 80%, the E average value attained the minimum

  4. Biomass pyrolysis and combustion integral and differential reaction heats with temperatures using thermogravimetric analysis/differential scanning calorimetry.

    Science.gov (United States)

    Shen, Jiacheng; Igathinathane, C; Yu, Manlu; Pothula, Anand Kumar

    2015-06-01

    Integral reaction heats of switchgrass, big bluestem, and corn stalks were determined using thermogravimetric analysis/differential scanning calorimetry (TGA/DSC). Iso-conversion differential reaction heats using TGA/DSC pyrolysis and combustion of biomass were not available, despite reports available on heats required and released. A concept of iso-conversion differential reaction heats was used to determine the differential reaction heats of each thermal characteristics segment of these materials. Results showed that the integral reaction heats were endothermic from 30 to 700°C for pyrolysis of switchgrass and big bluestem, but they were exothermic for corn stalks prior to 587°C. However, the integral reaction heats for combustion of the materials followed an endothermic to exothermic transition. The differential reaction heats of switchgrass pyrolysis were predominantly endothermic in the fraction of mass loss (0.0536-0.975), and were exothermic for corn stalks (0.0885-0.850) and big bluestem (0.736-0.919). Study results provided better insight into biomass thermal mechanism. Published by Elsevier Ltd.

  5. Thermogravimetric study of rare earth concentrates

    International Nuclear Information System (INIS)

    Delyagejd, V.V.; Anisimova, V.N.; Eremenko, Z.V.; Kutsev, V.S.

    1974-01-01

    Methods of thermogravimetric, chemical and phase analysis were used in measuring the concentration of rare-earth elements of different origins. At temperatures 400-800 deg C a gradual decomposition of fluorocarbonates takes place leading to the formation of derivatives of corresponding oxides and oxyfluorides. For concentrates containing siderite the process takes place at 550-600 deg C followed by oxidation of bivalent iron into trivalent state. Reaction of rare-earth elements with sodium carbonate and the increase in the concentration of the latter results in a narrowing down of the interval of temperatures at which decomposition takes place. Under these conditions an intense reaction and a fusion take place leading to the formation of eutectic at 500-600 deg C and further synthesis of sodium fluoride and oxyfluoride derivatives of calcium and rare-earth elements

  6. Catalytic thermal decomposition of polyethylene determined by thermogravimetric treatment

    International Nuclear Information System (INIS)

    Nisar, J.; Khan, M.S.; Khan, M.A.

    2014-01-01

    In this study low density polyethylene (LDPE) has been studied by thermogravimetric analysis (TGA) using commercially available oxides as catalysts. TGA experiments were used to evaluate the activity of different catalysts on low density polyethylene (LDPE) degradation and to study the effect in terms of type and amount of catalyst used. All the catalysts used improved the pyrolysis of LDPE. The reaction rates were found to increase with increase in amount of catalyst. Among the catalysts used, alumina acidic active catalyst performed better at all four fractions. Moreover, alumina acidic active reduced weight loss temperature better than others tested catalysts. The effect of alumina neutral catalyst on the pyrolysis of LDPE is less pronounced due to its small surface area and pore size. The effect of these catalysts showed that surface area, number of acidic sites and pore size were found as the key factors for the energy efficient degradation of polymers. (author)

  7. Comparative evaluation of thermal oxidative decomposition for oil-plant residues via thermogravimetric analysis: Thermal conversion characteristics, kinetics, and thermodynamics.

    Science.gov (United States)

    Chen, Jianbiao; Wang, Yanhong; Lang, Xuemei; Ren, Xiu'e; Fan, Shuanshi

    2017-11-01

    Thermal oxidative decomposition characteristics, kinetics, and thermodynamics of rape straw (RS), rapeseed meal (RM), camellia seed shell (CS), and camellia seed meal (CM) were evaluated via thermogravimetric analysis (TGA). TG-DTG-DSC curves demonstrated that the combustion of oil-plant residues proceeded in three stages, including dehydration, release and combustion of organic volatiles, and chars oxidation. As revealed by combustion characteristic parameters, the ignition, burnout, and comprehensive combustion performance of residues were quite distinct from each other, and were improved by increasing heating rate. The kinetic parameters were determined by Coats-Redfern approach. The results showed that the most possible combustion mechanisms were order reaction models. The existence of kinetic compensation effect was clearly observed. The thermodynamic parameters (ΔH, ΔG, ΔS) at peak temperatures were calculated through the activated complex theory. With the combustion proceeding, the variation trends of ΔH, ΔG, and ΔS for RS (RM) similar to those for CS (CM). Copyright © 2017 Elsevier Ltd. All rights reserved.

  8. Thermogravimetric study of the reaction of uranium oxides with fluorine

    International Nuclear Information System (INIS)

    Komura, Motohiro; Sato, Nobuaki; Kirishima, Akira; Tochiyama, Osamu

    2008-01-01

    Thermogravimetric study of the reaction of uranium oxides with fluorine was conducted by TG-DTA method using anti-corrosion type differential thermobalance. When UO 2 was heated from R.T. to 500 deg. C in 5% F 2 /He atmosphere, the weight increase appeared at ca. 250 deg. C with an exothermic peak. Then the weight decreased slightly with a small exothermic peak followed by the complete volatilization with a large exothermic peak at ca. 350 deg. C. At a flow rate of 15, 30, 60 ml min -1 , there seemed to be no significant change for the fluorination of UO 2 . With the different heating rates of 1, 2, 5 and 10 deg. C min -1 , the fluorination peak shifted to higher temperature with increasing heating rates. For the comparison with thermogravimetric results, phase analysis by XRD method was conducted for the products obtained at different temperatures. At 260 deg. C, the product was UO 2 with a small amount of the intermediate compound, UO 2 F. The amount of this compound increased with increasing temperature up to 320 deg. C. Then another phase of UO 2 F 2 appeared at 340 deg. C but it was immediately fluorinated to the volatile fluoride. When U 3 O 8 was used as a starting material, it was found that the steep weight decrease peak appeared at ca. 350 deg. C and the uranium volatilized completely. This result suggests that fluorination of U 3 O 8 occurs at this temperature forming UF 6 . Uranium trioxide showed the similar fluorination behavior to that of U 3 O 8

  9. Thermogravimetric Analysis of Textile Dyeing Sludge (TDS) in N₂/CO₂/O₂ Atmospheres and its Combustion Model with Coal.

    Science.gov (United States)

    Zhuo, Zhongxu; Liu, Jingyong; Sun, Shuiyu; Kuo, Jiahong; Sun, Jian; Chang, Ken-Lin; Fu, Jiewen

    2018-01-01

      The combustion characteristics of textile dyeing sludge (TDS) in N2/O2, CO2/O2, and N2/CO2 atmospheres, and blends of TDS with coal were analyzed using TGA (thermogravimetric analysis). Results showed that the replacement of N2 by CO2 resulted in negative effects on the combustion and pyrolysis of TDS. Comparing N2/O2 and CO2/O2 atmospheres, combustion of TDS was easier in a N2/O2 atmosphere, but the residual mass after TDS pyrolysis in pure CO2 was less than that in N2 by approximately 4.51%. When the proportion of TDS was 30-50% in the blends of coal with TDS, a synergistic interaction clearly occurred, and it significantly promoted combustion. In considering different combustion parameters, the optimal proportion of TDS may be between 20-30%. The activation energy Ea value decreased from 155.6 kJ/mol to 53.35 kJ/mol with an increasing TDS proportion from 0% to 50%, and it rapidly decreased when the TDS proportion was below 20%.

  10. Consequences of poly(vinyl chloride) presence on the thermochemical process of lignocellulosic biomass in CO₂ by thermogravimetric analysis.

    Science.gov (United States)

    He, Yao; Ma, Xiaoqian; Zeng, Guangbo

    2015-02-01

    The thermochemical processes of lignocellulosic biomass and its mixtures with poly(vinyl chloride) (PVC) fractions were investigated by thermogravimetric analysis in CO2 atmosphere. Superposition property was assumed to examine whether and/or to what extent interactions occurred during the mixture decomposition. Results showed that interactions existed, of which the intensities changed with reaction stage, heating rate and PVC quantity, and they actively behaved toward the decomposition in most cases. With PVC presence, lignocellulosic biomass turned from three-stage to four-stage decomposition process where the reactions occurred at lower temperatures with heightened intensity, especially in the first stage. The measured activation energies calculated by Ozawa-Flynn-Wall and Vyazovkin methods were of minor difference <5 kJ/mol, and comparing them between materials in each stage confirmed the results of interaction impact. This work provides a theoretical basis bringing about the possibilities of recycling CO2 into a reaction medium of thermo-treatment of lignocellulosic material with PVC contaminants. Copyright © 2014 Elsevier Ltd. All rights reserved.

  11. Determination of the surface density of polyethylene glycol on gold nanoparticles by use of microscale thermogravimetric analysis.

    Science.gov (United States)

    Sebby, K B; Mansfield, E

    2015-04-01

    The widespread integration of nanoparticle technologies into biomedicine will depend on the ability to repeatedly create particles with well-defined properties and predictable behaviors. For this to happen, fast, reliable, inexpensive, and widely available techniques to characterize nanomaterials are needed. Characterization of the surface molecules is particularly important since the surface, including the surface molecule density, plays a dominant role in determining how nanoparticles interact with their surroundings. Here, 10 and 30 nm gold nanoparticle NIST Standard Reference Materials were functionalized with fluorescently labeled polyethylene glycol (PEG) with either thiolate or lipoic acid anchoring groups to evaluate analytical techniques for determining surface coverage. The coating of the nanoparticles was confirmed with dynamic light scattering, microscale thermogravimetric analysis (μ-TGA), and ultraviolet-visible (UV-vis) spectroscopy. A UV-vis method for determining gold nanoparticle concentrations that takes into account spectral broadening upon functionalization was developed. The amount of bound PEG was quantified with μ-TGA, a technique analogous to thermogravimetric analysis that uses quartz crystal microbalances, and fluorescence spectroscopy of displaced ligands. It is shown that μ-TGA is a convenient technique for the quantification of ligands bound to inorganic particles while sacrificing a minimal amount of sample, and the treatment of the functionalized nanoparticle dispersions with dithiothreitol may be insufficient to achieve complete displacement of the surface ligands for quantification by fluorescence measurements. The μ-TGA and fluorescence results were used to determine ligand footprint sizes-average areas occupied by each ligand on the particles' surface. The lipoic acid bound ligands had footprint sizes of 0.21 and 0.25 nm(2) on 10 and 30 nm particles, respectively while the thiolate ligands had footprint sizes of 0.085 and 0

  12. A novel quantification method of pantaprazole sodium monohydrate in sesquihydrate by thermogravimetric analyzer.

    Science.gov (United States)

    Reddy, V Ranga; Rajmohan, M Anantha; Shilpa, R Laxmi; Raut, Dilip M; Naveenkumar, Kolla; Suryanarayana, M V; Mathad, Vijayavitthal T

    2007-04-11

    To demonstrate the applicability of thermogravimetric analyzer as a tool for the quantification of pantaprazole sodium monohydrate in sesquihydrate, studies have been conducted. Thermal analysis (DSC, TGA) crystallographic (PXRD) and spectroscopic techniques (FT-IR) were used for the characterization of the polymorphs. Thermogravimetric analysis (TGA) analysis was explored by high-resolution dynamic (Hi-Res-dynamic) and high-resolution modulated (Hi-Res-modulated) test procedures to quantify the hydrate polymorphic mixtures. The two polymorphic forms exhibited significant differences and good resolution in the second derivative thermogram generated by Hi-Res-modulated test procedure. Thus, the TGA with Hi-Res-modulated test procedure was considered for the quantification of monohydrate in sesquihydrate. The calibration plot was constructed from the known mixtures of two polymorphs by plotting the peak area of the second derivative thermogram against the weight percent of monohydrate. Using this novel approach, 1 wt% limit of detection (LOD) was achieved. The polymorphic purity results, obtained by TGA in Hi-Res-modulated test procedure were found to be in good agreement with the results predicted by FT-IR and was comparable with the actual values of the known polymorphic mixtures. The Hi-Res-modulated TGA technique is very simple and easy to perform the analysis.

  13. Combustion kinetics of hydrochar produced from hydrothermal carbonisation of Karanj (Pongamia pinnata) fruit hulls via thermogravimetric analysis.

    Science.gov (United States)

    Islam, Md Azharul; Kabir, G; Asif, M; Hameed, B H

    2015-10-01

    This study examined the combustion profile and kinetics of hydrochar produced from hydrothermal carbonisation (HTC) of Karanj fruit hulls (KFH). The HTC-KFH hydrochar combustion kinetics was investigated at 5, 10, and 20°C/min by thermogravimetric analysis. The kinetics model, Kissinger-Akahira-Sunose revealed the combustion kinetics parameters for the extent of conversion from 0.1 to 0.8; the activation energy varies from 114 to 67 kJ/mol respectively. The hydrochar combustion followed multi-steps kinetics; the Coats-Redfern models predicted the activation energies and pre-exponential constants for the hydrochar combustion zones. The diffusion models are the effective mechanism in the second and third zone. Copyright © 2015 Elsevier Ltd. All rights reserved.

  14. Thermogravimetric measurements of liquid vapor pressure

    International Nuclear Information System (INIS)

    Rong Yunhong; Gregson, Christopher M.; Parker, Alan

    2012-01-01

    Highlights: ► Rapid determination of vapor pressure by TGA. ► Demonstration of limitations of currently available approaches in literature. ► New model for vapor pressure assessment of small size samples in TGA. ► New model accounts for vapor diffusion and sample geometry and measures vapor pressure normally within 10%. - Abstract: A method was developed using thermo-gravimetric analysis (TGA) to determine the vapor pressure of volatile liquids. This is achieved by measuring the rate of evaporation (mass loss) of a pure liquid contained within a cylindrical pan. The influence of factors like sample geometry and vapor diffusion on evaporation rate are discussed. The measurement can be performed across a wide range of temperature yielding reasonable results up to 10 kPa. This approach may be useful as a rapid and automatable method for measuring the volatility of flavor and fragrance raw materials.

  15. Thermogravimetric study and kinetic analysis of dried industrial sludge pyrolysis.

    Science.gov (United States)

    Liu, Guangrui; Song, Huijuan; Wu, Jinhu

    2015-07-01

    Thermogravimetric experiments of two different industrial sludge samples were carried out with non-isothermal temperature programs. The results indicated that the pyrolysis process contains three obvious stages and the main decomposition reaction occurred in the range of 200-600°C. The distributed activation energy model (DAEM) was also proposed describing equally well the pyrolysis behavior of the samples. The calculated activation energy was ranged from 170 to 593kJ/mol and 125 to 756kJ/mol for SLYG (sludge sample from chemical fiber factory) and SQD (sludge sample from woody industry), respectively. The reliability of this model not only provided good fit for all experiments, but also allowed accurate extrapolations to relative higher heating rates. Besides, the FTIR measurement was also used to further understand the relationship between pyrolysis behavior and chemical structures for industrial sludge. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Determination of kinetic parameters of Phlomis bovei de Noé using thermogravimetric analysis.

    Science.gov (United States)

    Yahiaoui, Meriem; Hadoun, Hocine; Toumert, Idir; Hassani, Aicha

    2015-11-01

    This paper reports the pyrolysis study of Phlomis bovei biomass by thermogravimetric experiments in order to determine the thermal degradation behavior and kinetic parameters. The weight losses were found to occur in three stages. In the DTG thermograms, an increase of the heating rate tended to delay thermal degradation processes towards higher temperatures. The average values of activation energy and pre-exponential factor calculated from Ozawa-Flynn-Wall, Kissinger-Akahira-Sunose and Kissinger methods are 134.83, 134.06, 223.31kJ/mol and 4.1610(13), 1.1810(10), 2.8110(11)/s, respectively. The three-pseudo-component method shows that the activation energy increases with increasing the heating rate for hemicellulose and cellulose while the activation energy of the lignin decreased with an increase of the heating rate. Predicted results and experimental data exhibit similar tendencies and the three pseudo-components model with n different from unity 1 is recommended as the most suitable for prediction of kinetic behavior of Phlomis bovei de Noé. Copyright © 2015 Elsevier Ltd. All rights reserved.

  17. Pyrolysis kinetics and thermal behavior of waste sawdust biomass using thermogravimetric analysis.

    Science.gov (United States)

    Mishra, Ranjeet Kumar; Mohanty, Kaustubha

    2018-03-01

    The present study reports pyrolysis behavior of three waste biomass using thermogravimetric analysis to determine kinetic parameters at five different heating rates. Physiochemical characterization confirmed that these biomass have the potential for fuel and energy production. Pyrolysis experiments were carried out at five different heating rates (5-25 °C min -1 ). Five model-free methods such as Kissinger-Akahira-Sunose (KAS), Ozawa-Flynn-Wall (OFW), Friedman, Coats-Redfern, and distributed activation energy (DAEM) were used to calculate the kinetic parameters. The activation energy was found to be 171.66 kJ mol -1 , 148.44 kJ mol -1 , and 171.24 kJ mol -1 from KAS model; 179.29 kJ mol -1 , 156.58 kJ mol -1 , and 179.47 kJ mol -1 from OFW model; 168.58 kJ mol -1 , 181.53 kJ mol -1 , and 184.61 kJ mol -1 from Friedman model; and 206.62 kJ mol -1 , 171.63 kJ mol -1 , and 160.45 kJ mol -1 from DAEM model for PW, SW, AN biomass respectively. The calculated kinetic parameters are in good agreement with other reported biomass. Copyright © 2017 Elsevier Ltd. All rights reserved.

  18. Thermal Behaviour of Five Different Date Palm Residues of Algeria by Thermogravimetric Analysis

    Directory of Open Access Journals (Sweden)

    Siham AMIROU

    2013-06-01

    Full Text Available Renewable energy has become moreimportant globally especially with the current fuel andeconomic crisis. Date palm biomasses are highlypotential materials for energy resources. The factthat they are renewable and abundantly availableare amongst the attractive reasons of employingthem as the major source for renewable energy. Thepurpose of this research was to investigate thethermal behavior of date palm biomass in order toevaluate their usefulness for energy production. Inmicroparticular scale, the thermogravimetric analysis(TGA is one of the techniques used to determinethe thermal properties of five different date palmresidues that were studied: (date palm rachis (DPR,date palm trunk (DPT, leaf base (Petiole (LB,fruitstalk prunings (FP and liff (LP. The TGAtechnique consists to record the lost weight duringthe increase in temperature from 20°C until 600°Cwith a 10°C/min heating rate. The thermogramspresented a departure phase of free water (fromroom temperature to 110°C before the degradationprocess of the lignocellulosic constituents. The ligninand hemicellulose play an important role on thedegradation of lignocellulosic materials at thetemperature under 250°C. The degradation ofcellulose begins at 250°C and overlaps to that oflignin until 450°C.

  19. Characteristics and kinetic study on pyrolysis of five lignocellulosic biomass via thermogravimetric analysis.

    Science.gov (United States)

    Chen, Zhihua; Hu, Mian; Zhu, Xiaolei; Guo, Dabin; Liu, Shiming; Hu, Zhiquan; Xiao, Bo; Wang, Jingbo; Laghari, Mahmood

    2015-09-01

    Pyrolysis characteristics and kinetic of five lignocellulosic biomass pine wood sawdust, fern (Dicranopteris linearis) stem, wheat stalk, sugarcane bagasse and jute (Corchorus capsularis) stick were investigated using thermogravimetric analysis. The pyrolysis of five lignocellulosic biomass could be divided into three stages, which correspond to the pyrolysis of hemicellulose, cellulose and lignin, respectively. Single Gaussian activation energy distributions of each stage are 148.50-201.13 kJ/mol with standard deviations of 2.60-13.37 kJ/mol. The kinetic parameters of different stages were used as initial guess values for three-parallel-DAEM model calculation with good fitting quality and fast convergence rate. The mean activation energy ranges of hemicellulose, cellulose and lignin were 148.12-164.56 kJ/mol, 171.04-179.54 kJ/mol and 175.71-201.60 kJ/mol, with standard deviations of 3.91-9.89, 0.29-1.34 and 23.22-27.24 kJ/mol, respectively. The mass fractions of hemicellulose, cellulose and lignin in lignocellulosic biomass were respectively estimated as 0.12-0.22, 0.54-0.65 and 0.17-0.29. Copyright © 2015 Elsevier Ltd. All rights reserved.

  20. Temperature-dependent deliquescence relative humidities and water activities using humidity controlled thermogravimetric analysis with application to malonic acid.

    Science.gov (United States)

    Beyer, Keith D; Schroeder, Jason R; Kissinger, Jared A

    2014-04-03

    We utilize a new experimental technique, humidity-controlled thermogravimetric analysis (HTGA), to determine temperature-dependent deliquescence relative humidities (DRH) and to determine the equilibrium concentration of a solution at a given temperature and relative humidity. To that end, we have investigated the malonic acid/water system determining the DRH and concentration/RH relationship in the temperature range 303-278 K. Excellent agreement is found with literature values for the DRH of malonic acid as a function of temperature and for the concentration/RH relationship at several temperatures. Thus, we extend the DRH and concentration/RH relationship to a broader temperature range and are using the HTGA experiments to investigate other organic acids.

  1. Investigation of co-combustion characteristics of sewage sludge and coffee grounds mixtures using thermogravimetric analysis coupled to artificial neural networks modeling.

    Science.gov (United States)

    Chen, Jiacong; Liu, Jingyong; He, Yao; Huang, Limao; Sun, Shuiyu; Sun, Jian; Chang, KenLin; Kuo, Jiahong; Huang, Shaosong; Ning, Xunan

    2017-02-01

    Artificial neural network (ANN) modeling was applied to thermal data obtained by non-isothermal thermogravimetric analysis (TGA) from room temperature to 1000°C at three different heating rates in air to predict the TG curves of sewage sludge (SS) and coffee grounds (CG) mixtures. A good agreement between experimental and predicted data verified the accuracy of the ANN approach. The results of co-combustion showed that there were interactions between SS and CG, and the impacts were mostly positive. With the addition of CG, the mass loss rate and the reactivity of SS were increased while charring was reduced. Measured activation energies (E a ) determined by the Kissinger-Akahira-Sunose (KAS) and Ozawa-Flynn-Wall (OFW) methods deviated by <5%. The average value of E a (166.8kJ/mol by KAS and 168.8kJ/mol by OFW, respectively) was the lowest when the fraction of CG in the mixture was 40%. Copyright © 2016 Elsevier Ltd. All rights reserved.

  2. Method for Determining the Activation Energy Distribution Function of Complex Reactions by Sieving and Thermogravimetric Measurements.

    Science.gov (United States)

    Bufalo, Gennaro; Ambrosone, Luigi

    2016-01-14

    A method for studying the kinetics of thermal degradation of complex compounds is suggested. Although the method is applicable to any matrix whose grain size can be measured, herein we focus our investigation on thermogravimetric analysis, under a nitrogen atmosphere, of ground soft wheat and ground maize. The thermogravimetric curves reveal that there are two well-distinct jumps of mass loss. They correspond to volatilization, which is in the temperature range 298-433 K, and decomposition regions go from 450 to 1073 K. Thermal degradation is schematized as a reaction in the solid state whose kinetics is analyzed separately in each of the two regions. By means of a sieving analysis different size fractions of the material are separated and studied. A quasi-Newton fitting algorithm is used to obtain the grain size distribution as best fit to experimental data. The individual fractions are thermogravimetrically analyzed for deriving the functional relationship between activation energy of the degradation reactions and the particle size. Such functional relationship turns out to be crucial to evaluate the moments of the activation energy distribution, which is unknown in terms of the distribution calculated by sieve analysis. From the knowledge of moments one can reconstruct the reaction conversion. The method is applied first to the volatilization region, then to the decomposition region. The comparison with the experimental data reveals that the method reproduces the experimental conversion with an accuracy of 5-10% in the volatilization region and of 3-5% in the decomposition region.

  3. Thermogravimetric analysis, PXRD, EDX and XPS study of chrysocolla (Cu,Al)2H2Si2O5(OH)4·nH2O-structural implications

    International Nuclear Information System (INIS)

    Frost, Ray L.; Xi, Yunfei; Wood, Barry J.

    2012-01-01

    Highlights: ► We have undertaken a TG X PS study of the mineral chrysocolla. ► The chemical bonding of Cu, O and Si has been determined. ► It is concluded that chrysocolla is a mineral in its own right. ► It is not a colloidal mixture of spertiniite and amorphous silica. - Abstract: Selected chrysocolla mineral samples from different origins have been studied by using PXRD, SEM, EDX and XPS. The XRD patterns show that the chrysocolla mineral samples are non-diffracting and no other phases are present in the minerals, thus showing the chrysocolla samples are pure. SEM analyses show the chrysocolla surfaces are featureless. EDX analyses enable the formulae of the chrysocolla samples to be calculated. The thermal decomposition of the mineral chrysocolla has been studied using a combination of thermogravimetric analysis and derivative thermogravimetric analysis. Five thermal decomposition mass loss steps are observed for the chrysocolla from Arizona (a) at 125 °C with the loss of water, (b) at 340 °C with the loss of hydroxyl units, (c) at 468.5 °C with a further loss of hydroxyls, (d) at 821 °C with oxygen loss and (e) at 895 °C with a further loss of oxygen. The thermal analysis of the chrysocolla from Congo shows mass losses at 125, 275.3, 805.6 and 877.4 °C and for the Nevada chrysocolla, mass loss steps at 268, 333, 463, 786.0 and 817.7 °C are observed. The thermal analysis of spertiniite is very different from that of chrysocolla and thermally decomposes at around 160 °C. XPS shows that there are two different copper species present, one which is bonded to oxygen and one to a hydroxyl unit. The O 1s is broad and very symmetrical suggesting two O species of equal number. The bond energy of 102.9 eV for the Si 2p suggests that it is in the form of a silicate. The bond energy is much higher for silicas around ∼103.5 eV. The reported value for silica gel has Si 2p at 103.4 eV. The combination of TG, PXRD, EDX and XPS adds to our fundamental

  4. Nonisothermal Thermogravimetric Analysis of Thai Lignite with High CaO Content

    Science.gov (United States)

    Pintana, Pakamon

    2013-01-01

    Thermal behaviors and combustion kinetics of Thai lignite with different SO3-free CaO contents were investigated. Nonisothermal thermogravimetric method was carried out under oxygen environment at heating rates of 10, 30, and 50°C min−1 from ambient up to 1300°C. Flynn-Wall-Ozawa (FWO) and Kissinger-Akahira-Sunose (KAS) methods were adopted to estimate the apparent activation energy (E) for the thermal decomposition of these coals. Different thermal degradation behaviors were observed in lignites with low (14%) and high (42%) CaO content. Activation energy of the lignite combustion was found to vary with the conversion fraction. In comparison with the KAS method, higher E values were obtained by the FWO method for all conversions considered. High CaO lignite was observed to have higher activation energy than the low CaO coal. PMID:24250259

  5. Thermogravimetric and x-ray diffraction analyses of Luna-24 regolith samples

    International Nuclear Information System (INIS)

    Deshpande, V.V.; Dharwadkar, S.R.; Jakkal, V.S.

    1979-01-01

    Two samples of Luna-24 were analysed by X-ray diffraction and thermogravimetric (TG) techniques. The sample 24123.12 shows a weight loss of nearly 0.85 percent between 23O-440deg C and followed by 1.16 percent weight gain from 500 to 800deg C. The sample 23190.13 showed only a weight gain of about 1.5 percent from 5O0deg C to 900deg C. X-ray diffraction analyses show the presence of olivine, plagioclase, pigeonite, enstatite, and native iron in both the virgin samples. The heated samples, however, show that only the native iron got oxidized to iron oxide. The other constituents remain unaltered. (auth.)

  6. Thermogravimetric analysis for rapid assessment of moisture diffusivity in polydisperse powder and thin film matrices.

    Science.gov (United States)

    Thirunathan, Praveena; Arnz, Patrik; Husny, Joeska; Gianfrancesco, Alessandro; Perdana, Jimmy

    2018-03-01

    Accurate description of moisture diffusivity is key to precisely understand and predict moisture transfer behaviour in a matrix. Unfortunately, measuring moisture diffusivity is not trivial, especially at low moisture values and/or elevated temperatures. This paper presents a novel experimental procedure to accurately measure moisture diffusivity based on thermogravimetric approach. The procedure is capable to measure diffusivity even at elevated temperatures (>70°C) and low moisture values (>1%). Diffusivity was extracted from experimental data based on "regular regime approach". The approach was tailored to determine diffusivity from thin film and from poly-dispersed powdered samples. Subsequently, measured diffusivity was validated by comparing to available literature data, showing good agreement. Ability of this approach to accurately measure diffusivity at a wider range of temperatures provides better insight on temperature dependency of diffusivity. Thus, this approach can be crucial to ensure good accuracy of moisture transfer description/prediction especially when involving elevated temperatures. Copyright © 2017 Elsevier Ltd. All rights reserved.

  7. Thermogravimetric studies on alkyl methacrylate polymers and poly(alkyl methacrylate)-grafted polypropylene fibers

    International Nuclear Information System (INIS)

    Hayakawa, Kiyoshi; Taoda, Hiroshi; Kawase, Kaoru; Tazawa, Masato; Yamakita, Hiromi

    1986-01-01

    Thermal behavior of several kinds of poly (alkyl methacrylate) and polypropylene-g-poly (alkyl methacrylate) fibers prepared by γ-irradiation was investigated by thermogravimetric measurements with the intermittent analysis of the gaseous products. The degradation of poly (methyl methacrylate) proceeded according to the deploymerization mechanism reproducing the pristine monomer exclusively. The thermogram in inert atmosphere showed the features of a two-step depolymerization, while in air it showed no such a stepwise decrease with the elevating temperature. The dissolution-precipitation treatment of polymer seemed to affect the decomposition behavior. On other alkyl methacrylate polymers, the thermal decomposition generally proceeded also according to the depolymerization mechanism. But, for instance, at least two kinds of products besides its own monomer were formed from poly (isobutyl methacrylate), and their relative fractions differed with the temperature. Polypropylene-g-poly (alkyl methacrylate) fibers showed lowering of initiation temperature of decomposition with the increase in extent of the grafting, and their initiation temperatures of decomposition in air were lower than those in inert atmosphere. (author)

  8. Pyrolysis characteristics and kinetics of microalgae via thermogravimetric analysis (TGA): A state-of-the-art review.

    Science.gov (United States)

    Bach, Quang-Vu; Chen, Wei-Hsin

    2017-12-01

    Pyrolysis is a promising route for biofuels production from microalgae at moderate temperatures (400-600°C) in an inert atmosphere. Depending on the operating conditions, pyrolysis can produce biochar and/or bio-oil. In practice, knowledge for thermal decomposition characteristics and kinetics of microalgae during pyrolysis is essential for pyrolyzer design and pyrolysis optimization. Recently, the pyrolysis kinetics of microalgae has become a crucial topic and received increasing interest from researchers. Thermogravimetric analysis (TGA) has been employed as a proven technique for studying microalgae pyrolysis in a kinetic control regime. In addition, a number of kinetic models have been applied to process the TGA data for kinetic evaluation and parameters estimation. This paper aims to provide a state-of-the art review on recent research activities in pyrolysis characteristics and kinetics of various microalgae. Common kinetic models predicting the thermal degradation of microalgae are examined and their pros and cons are illustrated. Copyright © 2017 Elsevier Ltd. All rights reserved.

  9. A Combined Raman Spectroscopic and Thermogravimetric Analysis Study on Oxidation of Coal with Different Ranks

    Directory of Open Access Journals (Sweden)

    Weiqing Zhang

    2015-01-01

    Full Text Available Raman spectroscopy and nonisothermal thermogravimetric analysis (TGA measurements have been reported for different rank coals (lignite, bituminous coal, and anthracite and the relationship between the measurements was examined. It was found that the Raman spectra parameters can be used to characterize structure changes in the different rank coals, such as the band area ratios based on the curve-fitted results. Higher ranked coal was found to have higher values of IGR/IAll and IG+GR/IAll but lower values of ID/I(G+GR, IDL/I(G+GR, IS+SL/I(G+GR, and I(GL+GL'/I(G+GR. The oxidation properties of the coal samples were characterized by the reactivity indexes Tig, T20%, and Tmax from TGA data which were found to correlate well with the band area ratios of IGR/IAll, IG+GR/IAll, and IS+SL/I(G+GR. Based on these correlations, the Raman band area ratios were found to correlate with the oxidation activity of coal providing additional structural information which can be used to understand the changes in the TGA measurements.

  10. Pyrolysis kinetics of raw and hydrothermally carbonized Karanj (Pongamia pinnata) fruit hulls via thermogravimetric analysis.

    Science.gov (United States)

    Islam, Md Azharul; Asif, M; Hameed, B H

    2015-03-01

    The pyrolysis of karanj fruit hulls (KFH) and karanj fruit hull hydrothermal carbonization (KFH-HTC) hydrochar was thermogravimetrically investigated under a nitrogen environment at 5 °C/min, 10 °C/min, and 20 °C/min. The pyrolysis decomposition of KFH biomass was faster than that of KFH-HTC hydrochar because of the high volatility and fixed carbon of KFH biomass. Weight loss percentage was also affected by the heating rates. The kinetic data were evaluated with the Kissinger-Akahira-Sunose and Flynn-Wall-Ozawa methods. The activation energy values obtained with these two methods were 61.06 and 68.53 kJ/mol for KFH biomass and 130.49 and 135.87 kJ/mol for KFH-HTC hydrochar, respectively. The analysis of kinetic process mechanisms was verified with the Coats-Redfern method. KFH-HTC hydrochar may play a potential role in transforming biomass to energy-rich feedstock for thermochemical applications because of its high heating value, high fixed carbon, and low ash and sulfur contents. Copyright © 2014 Elsevier Ltd. All rights reserved.

  11. The research of moisture forms in the baking yeast by the thermogravimetric analysis method

    Directory of Open Access Journals (Sweden)

    S. V. Lavrov

    2016-01-01

    Full Text Available The thermogravimetry method is one of the few absolute methods of analysis, that makes it one of the most accurate methods. In this research, thermogravimetric analysis of baking yeast (Saccharomyces cerevisiae was carried out. It allowed to identify temperature zones, which correspond to dripping with various link energy, as well as to predict operating parameters of the process of dehumidification and to choose their most effective dehydration method. The studies were conducted in the laboratory of the collective use center "Control and management of energy efficient projects" of the "Voronezh state university of engineering technologies" on the simultaneous thermal analysis device STA 449 F3 model (NETZSCH, Germany. The device records the change in a substance mass and the difference of the heat flow inside the crucible containing the sample and the crucible containing the standard analyte. The analyzer's working principle is based on continuous recording of the dependence of the material mass on time or temperature and its being heated to the selected temperature program in a specified gas atmosphere. The release or absorption of heat by the sample due to phase transitions or chemical reactions is recorded simultaneously. The study was performed in the following modes: the pressure is atmospheric, the maximum temperature is 588 K, the rate of temperature change is 5 K/min. The experiments were performed in aluminum crucibles with a total weight of 12 mg. The software NETZSCH Proteus was used for processing of the obtained TG and DTG curves. The analysis of the obtained data allowed to identify periods of water dehydration and solids transformation by thermal effect on baking yeast, and to identify temperature zones, which correspond to the release of moisture with different link form and energy.

  12. Determination of kinetic parameters in the pyrolysis operation and thermal behavior of Prosopis juliflora using thermogravimetric analysis.

    Science.gov (United States)

    Chandrasekaran, Arunkumar; Ramachandran, Sethumadhavan; Subbiah, Senthilmurugan

    2017-06-01

    This paper deals with the pyrolysis of Prosopis juliflora fuelwood using thermogravimetric analysis to determine the kinetic parameters at six different heating rates of 2, 5, 10, 15, 20 and 25°C/min. The activation energy of pyrolysis was calculated using different methods, namely Kissinger, Kissinger-Akahira-Sunose, Ozawa-Flynn-Wall and Friedman model and corresponding calculated activation energy were found to be 164.6, 204, 203.2, and 219.3kJ/mol, respectively for each method. The three-pseudo component model was applied to calculate the following three kinetic parameters: activation energy, pre-exponential factor and order of reaction. The experimental results were validated with model prediction for all the six heating rates. The three-pseudo component model is able to predict experimental results much accurately while considering variable order reaction model (n≠1). Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. Determination of activation energy for animal fat and crude glycerol using thermogravimetric analysis

    Energy Technology Data Exchange (ETDEWEB)

    Koch, Crhristoph [University of Hannover, Hannover (Germany); Mortari, Daniela; Avila, Ivonete; Santos, Antonio Moreira dos; Silva, Mario Lucio Cristovam; Crnkovic, Paula Manoel [University of Sao Paulo, Sao Carlos, SP (Brazil)], e-mails: iavila@sc.usp.br, asantos@sc.usp.br, paulam@sc.usp.br

    2010-07-01

    The present study deals with the determination of the activation energy of animal fat and crude glycerol from a biodiesel production plant. The activation energies were investigated by thermogravimetric analysis in the temperature range of {delta}T = 25-600 deg C. The transient experiments were run for every sample (10 mg) at five different heating rates (2.5, 5.0, 10.0, 20.0 and 30.0 deg C/min) in atmosphere of synthetic air. It is possible to establish a direct relation between the activation energy and the ignition delay, which characterizes the combustion quality of a fuel. The activation energy could be determined as a function of the conversion degree and the temperature by the isoconversional model free kinetics. Four distinct phases were found for each sample and one of these phases was identified as low-temperature oxidation (LTO). As this region is responsible for the first vaporization of the fuel, the activation energies were determined for this special region along the whole conversion range (0 - 100 %). The following mean values could be determined: animal fat = 108.87 +- 52.28 kJ/mol, and crude glycerol = 65.37+- 13.17 kJ/mol. From these data, it was possible to conclude that animal fat is the most complex sample between the ones studied in this work (author)

  14. Thermogravimetric analysis and TEM characterization of the oxidation and defect sites of carbon nanotubes synthesized by CVD of methane

    International Nuclear Information System (INIS)

    Li Haipeng; Zhao Naiqin; He Chunnian; Shi Chunsheng; Du Xiwen; Li Jiajun

    2008-01-01

    Changes in the thermogravimetrically determined oxidation behaviors of CVD-grown multi-walled carbon nanotubes (MWNTs) over Ni/Al catalyst with different Ni content were examined. Catalyst type was found to have a measurable impact upon nanotube stability, suggesting differing levels of crystalline perfection in the resulting nanotubes. With increasing the Ni content in the Ni/Al catalyst, the CNTs obtained became less stable during heat treatment in air. Furthermore, high-resolution transmission electron microscopy was employed to investigate the defect sites of as-grown MWNTs. The results provide evidence showing that defect sites along the walls and at the ends of the raw MWNTs facilitate the thermal oxidative destruction of the nanotubes

  15. Modelization of nanospace interaction involving a ferromagnetic atom: a spin polarization effect study by thermogravimetric analysis.

    Science.gov (United States)

    Santhanam, K S V; Chen, Xu; Gupta, S

    2014-04-01

    Ab initio studies of ferromagnetic atom interacting with carbon nanotubes have been reported in the literature that predict when the interaction is strong, a higher hybridization with confinement effect will result in spin polarization in the ferromagnetic atom. The spin polarization effect on the thermal oxidation to form its oxide is modeled here for the ferromagnetic atom and its alloy, as the above studies predict the 4s electrons are polarized in the atom. The four models developed here provide a pathway for distinguishing the type of interaction that exists in the real system. The extent of spin polarization in the ferromagnetic atom has been examined by varying the amount of carbon nanotubes in the composites in the thermogravimetric experiments. In this study we report the experimental results on the CoNi alloy which appears to show selective spin polarization. The products of the thermal oxidation has been analyzed by Fourier Transform Infrared Spectroscopy.

  16. Thermogravimetric studies on electron beam initiated grafting of triallyl cyanurate onto polyethylene

    International Nuclear Information System (INIS)

    Chaki, T.K.; Bhowmik, A.K.; Mukunda, P.G.; Majali, A.B.; Tikku, V.K.

    1993-01-01

    Low density polyethylene (LDPE) containing different levels of triallyl cyanurate (TAC) have been prepared in a Brabender Plasticorder at 120 degC. The moulded samples in the form of rectangular compression sheet were irradiated under electron beam accelerator with different irradiation doses. Thermogravimetric and derivative thermogravimetric analyses of the irradiated samples grafted with TAC have been carried out in order to explore the decomposition behaviour and kinetics of decomposition under nitrogen atmosphere. Initial decomposition temperature (Ti), temperature at which 50% weight loss takes place (T50), final decomposition temperature (Tf) and the kinetic parameters evaluated from TGA traces of samples at different radiation doses (constant TAC level) and at different levels of TAC (constant radiation dose) have been reported. The effect of radiation dose and TAC level on the grafting of TAC onto polyethylene have been explained on the basis of degradation characteristics of irradiated samples. Kinetic studies show that the degradation of the irradiated samples follow first order reaction kinetics. Activation energies of degradation have been determined using McCarty and Green's method. Activation energy of the irradiated samples increases with the increasing radiation dose and also with increasing level of TAC. (author). 3 tabs

  17. Hydrogen Adsorption in Zeolite Studied with Sievert and Thermogravimetric Methods

    International Nuclear Information System (INIS)

    Lesnicenoks, P; Sivars, A; Grinberga, L; Kleperis, J

    2012-01-01

    Natural clinoptilolite (mixture from clinoptilolite, quartz and muscovite) is activated with palladium and tested for hydrogen adsorption capability at temperatures RT - 200°C. Thermogravimetric and volumetric methods showed that zeolite activated with palladium (1.25%wt) shows markedly high hydrogen adsorption capacity - up to 3 wt%. Lower amount of adsorbed hydrogen (∼1.5 wt%) was found for raw zeolite and activated with higher amount of palladium sample. Hypothesis is proposed that the heating of zeolite in argon atmosphere forms and activates the pore structure in zeolite material, where hydrogen encapsulation (trapping) is believed to occur when cooling down to room temperature. An effect of catalyst (Pd) on hydrogen sorption capability is explained by spillover phenomena were less-porous fractions of natural clinoptilolite sample (quartz and muscovite) are involved.

  18. A Combined Raman Spectroscopic and Thermogravimetric Analysis Study on Oxidation of Coal with Different Ranks.

    Science.gov (United States)

    Zhang, Weiqing; Jiang, Shuguang; Hardacre, Christopher; Goodrich, Peter; Wang, Kai; Shao, Hao; Wu, Zhengyan

    2015-01-01

    Raman spectroscopy and nonisothermal thermogravimetric analysis (TGA) measurements have been reported for different rank coals (lignite, bituminous coal, and anthracite) and the relationship between the measurements was examined. It was found that the Raman spectra parameters can be used to characterize structure changes in the different rank coals, such as the band area ratios based on the curve-fitted results. Higher ranked coal was found to have higher values of I GR/I All and I (G + GR)/I All but lower values of I D/I (G+GR), I DL/I (G+GR), I (S + SL)/I (G+GR), and I (GL+GL')/I (G+GR). The oxidation properties of the coal samples were characterized by the reactivity indexes T ig, T 20%, and T max from TGA data which were found to correlate well with the band area ratios of I GR/I All, I (G + GR)/I All, and I (S + SL)/I (G+GR). Based on these correlations, the Raman band area ratios were found to correlate with the oxidation activity of coal providing additional structural information which can be used to understand the changes in the TGA measurements.

  19. Investigation of thermodynamic parameters in the pyrolysis conversion of biomass and manure to biochars using thermogravimetric analysis.

    Science.gov (United States)

    Xu, Yiliang; Chen, Baoliang

    2013-10-01

    The thermodynamic parameters of the conversion of two companion pair materials, i.e., rice straw vs dairy manure, and rice bran vs chicken manure, to biochars were characterized by thermogravimetric analysis. The overall changes of activation energy (Ea) were well described by the Flynn-Wall method. The Ea values increased steeply from about 120 to 180 kJ/mol at the mass conversion (α) at 0.2-0.4, followed by a relatively steady change at 0.40.65. The higher contents of minerals in manures resulted in the larger Ea. The individual conversion of hemicellulose, cellulose and lignin in the feedstocks was identified and their thermodynamic parameters (ΔH°, ΔG° and ΔS°) were calculated. The yields of biochars calculated from TG curve were compared with the determined yields of biochars using muffle pyrolysis. Along with Fourier transform infrared spectra data, the distinct decompositions of biomasses and manures were evaluated. Copyright © 2013 Elsevier Ltd. All rights reserved.

  20. New sample carrier systems for thermogravimetric analysis under forced flow conditions and their influence on microkinetic results.

    Science.gov (United States)

    Seibel, C; Fieback, T M

    2015-09-01

    For thermogravimetric analysis, it has been shown that, depending on the type of sample container, different kinetic results could be obtained despite regarding the same reaction under constant conditions. This is due to limiting macrokinetic effects which are strongly dependant on the type of sample carrying system. This prompted the need for sample containers which deliver results minimally limited by diffusive mass transport. In this way, two container systems were developed, both characterized by a forced flow stream through a solid, porous bed: one from bottom to top (counter-current flow) and one from top to bottom (co-current flow). Optical test measurements were performed, the results indicating that reaction proceedings are almost fully independent of the geometrical shape of the sample containers. The Boudouard reaction was investigated with a standard crucible and the new developed systems; the reaction rates determined differed significantly, up to a factor of 6.2 at 1373 K.

  1. Thermogravimetric Analysis of Modified Hematite by Methane (CH{sub 4}) for Chemical-Looping Combustion: A Global Kinetics Mechanism

    Energy Technology Data Exchange (ETDEWEB)

    Monazam, Esmail R; Breault, Ronald W; Siriwardane, Ranjani; Miller, Duane D

    2013-10-01

    Iron oxide (Fe{sub 2}O{sub 3}) or in its natural form (hematite) is a potential material to capture CO{sub 2} through the chemical-looping combustion (CLC) process. It is known that magnesium (Mg) is an effective methyl cleaving catalyst and as such it has been combined with hematite to assess any possible enhancement to the kinetic rate for the reduction of Fe{sub 2}O{sub 3} with methane. Therefore, in order to evaluate its effectiveness as a hematite additive, the behaviors of Mg-modified hematite samples (hematite –5% Mg(OH){sub 2}) have been analyzed with regard to assessing any enhancement to the kinetic rate process. The Mg-modified hematite was prepared by hydrothermal synthesis. The reactivity experiments were conducted in a thermogravimetric analyzer (TGA) using continuous stream of CH{sub 4} (5, 10, and 20%) at temperatures ranging from 700 to 825 {degrees}C over ten reduction cycles. The mass spectroscopy analysis of product gas indicated the presence of CO{sub 2}, H{sub 2}O, H{sub 2} and CO in the gaseous product. The kinetic data at reduction step obtained by isothermal experiments could be well fitted by two parallel rate equations. The modified hematite samples showed higher reactivity as compared to unmodified hematite samples during reduction at all investigated temperatures.

  2. Pyrolysis of biofuels of the future: Sewage sludge and microalgae – Thermogravimetric analysis and modelling of the pyrolysis under different temperature conditions

    International Nuclear Information System (INIS)

    Soria-Verdugo, Antonio; Goos, Elke; Morato-Godino, Andrés; García-Hernando, Nestor; Riedel, Uwe

    2017-01-01

    Highlights: • Pyrolysis of microalgae and sewage sludge is studied by thermogravimetric analysis. • Accurate values of the kinetic parameters of the pyrolysis reaction are reported. • Pyrolysis is modeled for parabolic and exponential temperature increases. • Estimations of the model are compared with experimental measurements in TGA. • Excellent agreement is reached between the model estimations and the experiments. - Abstract: The pyrolysis process of both microalgae and sewage sludge was investigated separately, by means of non-isothermal thermogravimetric analysis. The Distributed Activation Energy Model (DAEM) was employed to obtain the pyrolysis kinetic parameters of the samples, i.e. the activation energy E_a and the pre-exponential factor k_0. Nine different pyrolysis tests at different constant heating rates were conducted for each sample in a thermogravimetric analyzer (TGA) to obtain accurate values of the pyrolysis kinetic parameters when applying DAEM. The accurate values of the activation energy and the pre-exponential factor that characterize the pyrolysis reaction of Chlorella vulgaris and sewage sludge were reported, together with their associated uncertainties. The activation energy and pre-exponential factor for the C. vulgaris vary between 150–250 kJ/mol and 10"1"0–10"1"5 s"−"1 respectively, whereas values ranging from 200 to 400 kJ/mol were obtained for the sewage sludge activation energy, and from 10"1"5 to 10"2"5 s"−"1 for its pre-exponential factor. These values of E_a and k_0 were employed to estimate the evolution of the reacted fraction with temperature during the pyrolysis of the samples under exponential and parabolic temperature increases, more typical for the pyrolysis reaction of fuel particles in industrial reactors. The estimations of the relation between the reacted fraction and the temperature for exponential and parabolic temperature increases were found to be in good agreement with the experimental values

  3. Effects of additives on the co-pyrolysis of municipal solid waste and paper sludge by using thermogravimetric analysis.

    Science.gov (United States)

    Fang, Shiwen; Yu, Zhaosheng; Lin, Yan; Lin, Yousheng; Fan, Yunlong; Liao, Yanfen; Ma, Xiaoqian

    2016-06-01

    By using thermogravimetric analysis (TGA), the effects of different additives (MgO, Al2O3 and ZnO) on the pyrolysis characteristics and activation energy of municipal solid waste (MSW), paper sludge (PS) and their blends in N2 atmosphere had been investigated in this study. The experiments resulted that these additives were effective in reducing the initial temperature and activation energy. However, not all the additives were beneficial to reduce the residue mass and enhance the index D. For the different ratios of MSW and PS, the same additive even had the different influences. The catalytic effects of additives were not obvious and the pyrolysis became difficult with the increase of the proportion of PS. Based on all the contrast of the pyrolysis characteristics, MgO was the best additive and 70M30P was the best ratio, respectively. Copyright © 2016 Elsevier Ltd. All rights reserved.

  4. Nickel hydroxide electrode. 3: Thermogravimetric investigations of nickel (II) hydroxides

    Science.gov (United States)

    Dennstedt, W.; Loeser, W.

    1982-01-01

    Water contained in Ni hydroxide influences its electrochemical reactivity. The water content of alpha and beta Ni hydroxides is different with respect to the amount and bond strength. Thermogravimetric experiments show that the water of the beta Ni hydroxides exceeding the stoichiometric composition is completely removed at 160 deg. The water contained in the interlayers of the beta hydroxide, however, is removed only at higher temperatures, together with the water originating from the decomposition of the hydroxide. These differences are attributed to the formation of II bonds within the interlayers and between interlayers and adjacent main layers. An attempt is made to explain the relations between water content and the oxidizability of the Ni hydroxides.

  5. A thermogravimetric analysis (TGA) method to determine the catalytic conversion of cellulose from carbon-supported hydrogenolysis process

    International Nuclear Information System (INIS)

    Leal, Glauco F.; Ramos, Luiz A.; Barrett, Dean H.; Curvelo, Antonio Aprígio S.; Rodella, Cristiane B.

    2015-01-01

    Graphical abstract: - Highlights: • A new method to determine the catalytic conversion of cellulose using TGA has been developed. • TGA is able to differentiate between carbon from cellulose and carbon from the catalyst. • Building an analytical curve from TGA results enables the accurate determination of cellulose conversion. - Abstract: The ability to determine the quantity of solid reactant that has been transformed after a catalytic reaction is fundamental in accurately defining the conversion of the catalyst. This quantity is also central when investigating the recyclability of a solid catalyst as well as process control in an industrial catalytic application. However, when using carbon-supported catalysts for the conversion of cellulose this value is difficult to obtain using only a gravimetric method. The difficulty lies in weighing errors caused by loss of the solid mixture (catalyst and non-converted cellulose) after the reaction and/or moisture adsorption by the substrate. These errors are then propagated into the conversion calculation giving erroneous results. Thus, a quantitative method using thermogravimetric analysis (TGA) has been developed to determine the quantity of cellulose after a catalytic reaction by using a tungsten carbide catalyst supported on activated carbon. Stepped separation of TGA curves was used for quantitative analysis where three thermal events were identified: moisture loss, cellulose decomposition and CO/CO 2 formation. An analytical curve was derived and applied to quantify the residual cellulose after catalytic reactions which were performed at various temperatures and reaction times. The catalytic conversion was calculated and compared to the standard gravimetric method. Results showed that catalytic cellulose conversion can be determined using TGA and exhibits lower uncertainty (±2%) when compared to gravimetric determination (±5%). Therefore, it is a simple and relatively inexpensive method to determine catalytic

  6. Computer calculations of activation energy for pyrolysis from thermogravimetric curves

    International Nuclear Information System (INIS)

    Hussain, R.

    1994-01-01

    A BASIC programme to determine energy of activation for the degradation of polymers has been described. The calculations are based on the results of thermogravimetric curves. This method is applicable for those polymers which produce volatile products upon thermal degradation. (author)

  7. Thermogravimetric evaluation of the suitability of precursors for MOCVD

    International Nuclear Information System (INIS)

    Kunte, G V; Shivashankar, S A; Umarji, A M

    2008-01-01

    A method based on the Langmuir equation for the estimation of vapour pressure and enthalpy of sublimation of subliming compounds is described. The variable temperature thermogravimetric/differential thermogravimetric (TG/DTG) curve of benzoic acid is used to arrive at the instrument parameters. Employing these parameters, the vapour pressure–temperature curves are derived for salicylic acid and camphor from their TG/DTG curves. The values match well with vapour pressure data in the literature, obtained by effusion methods. By employing the Clausius–Clapeyron equation, the enthalpy of sublimation could be calculated. Extending the method further, two precursors for metal-organic chemical vapour deposition (MOCVD) of titanium oxide bis-isopropyl bis tert-butyl 2-oxobutanoato titanium, Ti(O i Pr) 2 (tbob) 2 , and bis-oxo-bis-tertbutyl 2-oxobutanoato titanium, [TiO(tbob) 2 ] 2 , have been evaluated. The complex Ti(O i Pr) 2 (tbob) 2 is found to be a more suitable precursor. This approach can be helpful in quickly screening for the suitability of a compound as a CVD precursor

  8. Thermogravimetric analysis and kinetic modeling of low-transition-temperature mixtures pretreated oil palm empty fruit bunch for possible maximum yield of pyrolysis oil.

    Science.gov (United States)

    Yiin, Chung Loong; Yusup, Suzana; Quitain, Armando T; Uemura, Yoshimitsu; Sasaki, Mitsuru; Kida, Tetsuya

    2018-05-01

    The impacts of low-transition-temperature mixtures (LTTMs) pretreatment on thermal decomposition and kinetics of empty fruit bunch (EFB) were investigated by thermogravimetric analysis. EFB was pretreated with the LTTMs under different duration of pretreatment which enabled various degrees of alteration to their structure. The TG-DTG curves showed that LTTMs pretreatment on EFB shifted the temperature and rate of decomposition to higher values. The EFB pretreated with sucrose and choline chloride-based LTTMs had attained the highest mass loss of volatile matter (78.69% and 75.71%) after 18 h of pretreatment. For monosodium glutamate-based LTTMs, the 24 h pretreated EFB had achieved the maximum mass loss (76.1%). Based on the Coats-Redfern integral method, the LTTMs pretreatment led to an increase in activation energy of the thermal decomposition of EFB from 80.00 to 82.82-94.80 kJ/mol. The activation energy was mainly affected by the demineralization and alteration in cellulose crystallinity after LTTMs pretreatment. Copyright © 2018 Elsevier Ltd. All rights reserved.

  9. Thermogravimetric Analysis (TGA) Profile of Modified Sba-15 at Different Amount of Alkoxy silane Group

    International Nuclear Information System (INIS)

    Norhasyimi Rahmat; Nur Fathilah Mohd Yusof; Ezani Hafiza

    2014-01-01

    This study focused on meso porous silica SBA-15 modified with alkoxy silane functional group; phenyltriethoxysilane (PTES) and vinyltriethoxysilane (VTES) using direct synthesis and post-grafting methods. By direct synthesis method, SBA-15 template by triblock copolymer (P123) and functionalized with alkoxy silane groups at different amount of loadings were co-condensed with tetraethyl orthosilicate (TEOS) under acidic conditions. As for post-grafting method, different loadings of alkoxy silane groups were added after co-condensation of TEOS with P123 template. Both synthesis methods used calcination process to remove surfactant template at 550 degree Celsius for 5 hours. The derivatized SBA-15 was characterized by thermogravimetric analysis to evaluate the profile at different loadings of alkoxy silane groups with different synthesis method. At temperature range of 300-800 degree Celsius, post-grafting method displayed the highest weight loss of phenyl and vinyl groups. However, there was no significant difference of weight loss for different amount of organo silane groups. In this study, TGA has shown to be significant characterization means to determine the effects of different method used in synthesizing modified SBA-15. It was shown that different loading of phenyl and vinyl groups did not affect the efficiency of surfactant removal. (author)

  10. Thermogravimetric analysis of rice and wheat straw catalytic combustion in air- and oxygen-enriched atmospheres

    International Nuclear Information System (INIS)

    Yu Zhaosheng; Ma Xiaoqian; Liu Ao

    2009-01-01

    By thermogravimetric analysis (TGA) study, the influences of different catalysts on the ignition and combustion of rice and wheat straw in air- and oxygen-enriched atmospheres have been investigated in this paper. Straw combustion is divided into two stages. One is the emission and combustion of volatiles and the second is the combustion of fixed carbon. The existence of catalysts in the first step enhances the emission of volatiles from the straw. The action of catalysts in the second step of straw combustion may be as a carrier of oxygen to the fixed carbon. Two parameters have been used to compare the characteristics of ignition and combustion of straw under different catalysts and in various oxygen concentrations. One is the temperature when the conversion degree combustible (CDC) of straw is 5%, the other is the CDC when the temperature is 900 deg. C. By comparing the different values of the two parameters, the different influences of the catalysts and oxygen concentration on the ignition and combustion of straw have been studied, the action of these catalysts for straw ignition and combustion in air and oxygen-enriched atmosphere is effective except the oxygen-enriched catalytic combustion of wheat straw fixed carbon

  11. A thermogravimetric analysis (TGA) method developed for estimating the stoichiometric ratio of solid-state {alpha}-cyclodextrin-based inclusion complexes

    Energy Technology Data Exchange (ETDEWEB)

    Bai, Yuxiang; Wang, Jinpeng; Bashari, Mohanad; Hu, Xiuting [The State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122 (China); Feng, Tao [School of Perfume and Aroma Technology, Shanghai Institute of Technology, Shanghai 201418 (China); Xu, Xueming [The State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122 (China); Jin, Zhengyu, E-mail: jinlab2008@yahoo.com [The State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122 (China); Tian, Yaoqi, E-mail: yqtian@jiangnan.edu.cn [The State Key Laboratory of Food Science and Technology, School of Food Science and Technology, Jiangnan University, Wuxi 214122 (China)

    2012-08-10

    Highlights: Black-Right-Pointing-Pointer We develop a TGA method for the measurement of the stoichiometric ratio. Black-Right-Pointing-Pointer A series of formulas are deduced to calculate the stoichiometric ratio. Black-Right-Pointing-Pointer Four {alpha}-CD-based inclusion complexes were successfully prepared. Black-Right-Pointing-Pointer The developed method is applicable. - Abstract: An approach mainly based on thermogravimetric analysis (TGA) was developed to evaluate the stoichiometric ratio (SR, guest to host) of the guest-{alpha}-cyclodextrin (Guest-{alpha}-CD) inclusion complexes (4-cresol-{alpha}-CD, benzyl alcohol-{alpha}-CD, ferrocene-{alpha}-CD and decanoic acid-{alpha}-CD). The present data obtained from Fourier transform-infrared (FT-IR) spectroscopy showed that all the {alpha}-CD-based inclusion complexes were successfully prepared in a solid-state form. The stoichiometric ratios of {alpha}-CD to the relative guests (4-cresol, benzyl alcohol, ferrocene and decanoic acid) determined by the developed method were 1:1, 1:2, 2:1 and 1:2, respectively. These SR data were well demonstrated by the previously reported X-ray diffraction (XRD) method and the NMR confirmatory experiments, except the SR of decanoic acid with a larger size and longer chain was not consistent. It is, therefore, suggested that the TGA-based method is applicable to follow the stoichiometric ratio of the polycrystalline {alpha}-CD-based inclusion complexes with smaller and shorter chain guests.

  12. A thermogravimetric analysis (TGA) method developed for estimating the stoichiometric ratio of solid-state α-cyclodextrin-based inclusion complexes

    International Nuclear Information System (INIS)

    Bai, Yuxiang; Wang, Jinpeng; Bashari, Mohanad; Hu, Xiuting; Feng, Tao; Xu, Xueming; Jin, Zhengyu; Tian, Yaoqi

    2012-01-01

    Highlights: ► We develop a TGA method for the measurement of the stoichiometric ratio. ► A series of formulas are deduced to calculate the stoichiometric ratio. ► Four α-CD-based inclusion complexes were successfully prepared. ► The developed method is applicable. - Abstract: An approach mainly based on thermogravimetric analysis (TGA) was developed to evaluate the stoichiometric ratio (SR, guest to host) of the guest–α-cyclodextrin (Guest-α-CD) inclusion complexes (4-cresol-α-CD, benzyl alcohol-α-CD, ferrocene-α-CD and decanoic acid-α-CD). The present data obtained from Fourier transform-infrared (FT-IR) spectroscopy showed that all the α-CD-based inclusion complexes were successfully prepared in a solid-state form. The stoichiometric ratios of α-CD to the relative guests (4-cresol, benzyl alcohol, ferrocene and decanoic acid) determined by the developed method were 1:1, 1:2, 2:1 and 1:2, respectively. These SR data were well demonstrated by the previously reported X-ray diffraction (XRD) method and the NMR confirmatory experiments, except the SR of decanoic acid with a larger size and longer chain was not consistent. It is, therefore, suggested that the TGA-based method is applicable to follow the stoichiometric ratio of the polycrystalline α-CD-based inclusion complexes with smaller and shorter chain guests.

  13. Thermogravimetric study of γ-irradiated lanthanum oxalate

    International Nuclear Information System (INIS)

    Nayak, H.; Bhatta, D.

    2000-01-01

    Thermogravimetric study of La 2 (C 2 O 4 ) 3 , exposed to different doses (5.0 - 50.0 x 10 -2 MGy) of γ-rays has been carried out. Marginal effect is observed at lower doses which is prominent at higher dose (5.0 x 10 -1 MGy). The radiolytic damaged entities, generated by irradiation favours the reaction by creating new potential nucleation centres in the lattice. The solid product, La 2 O 3 formed by irradiation also acts as a heterogeneous catalyst and brings out changes in the reactivity of the solid. (author)

  14. Thermogravimetric control of intermediate compounds in uranium metallurgy

    International Nuclear Information System (INIS)

    Gasco Sanchez, L.; Fernandez Cellini, R.

    1959-01-01

    The thermal decomposition of some intermediate compounds in the metallurgy of the uranium as uranium peroxide, ammonium uranate, uranium and ammonium penta-fluoride, uranium tetrafluoride and uranous oxide has been study by means of the Chevenard's thermo balance. Some data on pyrolysis of synthetic mixtures of intermediate compounds which may occasionally appear during the industrial process, are given. Thermogravimetric methods of control are suggested, usable in interesting products in the uranium metallurgy. (Author) 20 refs

  15. Quantitative detection of powdered activated carbon in wastewater treatment plant effluent by thermogravimetric analysis (TGA).

    Science.gov (United States)

    Krahnstöver, Therese; Plattner, Julia; Wintgens, Thomas

    2016-09-15

    For the elimination of potentially harmful micropollutants, powdered activated carbon (PAC) adsorption is applied in many wastewater treatment plants (WWTP). This holds the risk of PAC leakage into the WWTP effluent and desorption of contaminants into natural water bodies. In order to assess a potential PAC leakage, PAC concentrations below several mg/L have to be detected in the WWTP effluent. None of the methods that are used for water analysis today are able to differentiate between activated carbon and solid background matrix. Thus, a selective, quantitative and easily applicable method is still needed for the detection of PAC residues in wastewater. In the present study, a method was developed to quantitatively measure the PAC content in wastewater by using filtration and thermogravimetric analysis (TGA), which is a well-established technique for the distinction between different solid materials. For the sample filtration, quartz filters with a temperature stability up to 950 °C were used. This allowed for sensitive and well reproducible measurements, as the TGA was not affected by the presence of the filter. The sample's mass fractions were calculated by integrating the mass decrease rate obtained by TGA in specific, clearly identifiable peak areas. A two-step TGA heating method consisting of N2 and O2 atmospheres led to a good differentiation between PAC and biological background matrix, thanks to the reduction of peak overlapping. A linear correlation was found between a sample's PAC content and the corresponding peak areas under N2 and O2, the sample volume and the solid mass separated by filtration. Based on these findings, various wastewater samples from different WWTPs were then analyzed by TGA with regard to their PAC content. It was found that, compared to alternative techniques such as measurement of turbidity or total suspended solids, the newly developed TGA method allows for a quantitative and selective detection of PAC concentrations down to 0

  16. Preparation and thermogravimetric study of some uranyl phosphates

    International Nuclear Information System (INIS)

    Schaekers, J.M.

    1970-10-01

    The preparation of uranyl ammonium phosphate trihydrate (UAP = UO 2 NH 4 PO 4 .3H 2 O), acid uranyl phosphate tetrahydrate(AUP = UO 2 HPO 4 .4H 2 O) and neutral uranyl phosphate tetrahydrate (NUPT = (UO 2 ) 3 (PO 4 ) 2 .4H 2 O) was investigated during the data from the literature. The thermal decomposition in different atmospheres, such as air, oxygen, nitrogen and argon, was studied in the temperature range 25-1000 0 C. It was found that the pyrophosphate U 2 O 3 P 2 O 7 is a stable decomposition product of UAP as well as of AUP. A mixture of U 3 O 8 and U 2 O 3 P 2 O 7 is obtained when the NUPT is decomposed in an oxygen-free atmosphere. NUPT however is stable in an oxidising atmosphere. Hydrogen and carbon reductions were also carried out, and UO 2 or (UO) 2 P 2 O 7 as well as mixtures of these two products can be obtained, depending on the starting material and the reduction temperature. The different reduction and decomposition reactions were studied by means of thermogravimetric analysis, and activation energies were calculated where possible. I.R. spectral analysis was also used to identify various products with the same composition [af

  17. Thermogravimetric and kinetic analysis of thermal decomposition characteristics of low-lipid microalgae.

    Science.gov (United States)

    Gai, Chao; Zhang, Yuanhui; Chen, Wan-Ting; Zhang, Peng; Dong, Yuping

    2013-12-01

    The thermal decomposition behavior of two microalgae, Chlorella pyrenoidosa (CP) and Spirulina platensis (SP), were investigated on a thermogravimetric analyzer under non-isothermal conditions. Iso-conversional Vyazovkin approach was used to calculate the kinetic parameters, and the universal integral method was applied to evaluate the most probable mechanisms for thermal degradation of the two feedstocks. The differential equations deduced from the models were compared with experimental data. For the range of conversion fraction investigated (20-80%), the thermal decomposition process of CP could be described by the reaction order model (F3), which can be calculated by the integral equation of G(α) = [(1 - α)(-2) - 1]/2. And the apparent activation energy was in the range of 58.85-114.5 kJ/mol. As for SP, it can be described by the reaction order model (F2), which can be calculated by the integral equation of G(α) = (1 - α)(-1) - 1, and the range of apparent activation energy was 74.35-140.1 kJ/mol. Copyright © 2013 Elsevier Ltd. All rights reserved.

  18. Pyrolysis characteristics and kinetics of aquatic biomass using thermogravimetric analyzer.

    Science.gov (United States)

    Wu, Kejing; Liu, Ji; Wu, Yulong; Chen, Yu; Li, Qinghai; Xiao, Xin; Yang, Mingde

    2014-07-01

    The differences in pyrolysis process of three species of aquatic biomass (microalgae, macroalgae and duckweed) were investigated by thermogravimetric analysis (TGA). Three stages were observed during the pyrolysis process and the main decomposition stage could be divided further into three zones. The pyrolysis characteristics of various biomasses were different at each zone, which could be attributed to the differences in their components. A stepwise procedure based on iso-conversional and master-plots methods was used for the kinetic and mechanism analysis of the main decomposition stage. The calculation results based on the kinetic model was in good agreement with the experimental data of weight loss, and each biomass had an increasing activation energy of 118.35-156.13 kJ/mol, 171.85-186.46 kJ/mol and 258.51-268.71 kJ/mol in zone 1, 2 and 3, respectively. This study compares the pyrolysis behavior of various aquatic biomasses and provides basis for further applications of the biomass thermochemical conversion. Copyright © 2014. Published by Elsevier Ltd.

  19. Spectroscopic, thermogravimetric and structural characterization analyses for comparing Municipal Solid Waste composts and vermicomposts stability and maturity.

    Science.gov (United States)

    Soobhany, Nuhaa; Gunasee, Sanjana; Rago, Yogeshwari Pooja; Joyram, Hashita; Raghoo, Pravesh; Mohee, Romeela; Garg, Vinod Kumar

    2017-07-01

    This is the first-ever study of its kind for an extensive assessment and comparison of maturity indexes between compost and vermicompost that have been derived from Municipal Solid Waste (MSW). The spectroscopic (Fourier transform infrared spectroscopy: FT-IR), thermogravimetric analysis (TG), differential scanning calorimetry (DSC) and structural characterization (scanning electron microscope: SEM) were recorded. FT-IR spectra showed an increase in conversion of polysaccharides species and aliphatic methylene groups in vermicompost compared to compost as depicted from the variation of the intensity of the peaks. TG curves of final vermicompost showed a much lower mass loss when compared to compost, indicating higher stability in feedstock. SEM micrographs of the vermicompost reflected strong fragmentation of material than composts which revealed the extent of intra-structural degradation of MSW. These findings elucidate on a clear comparison between composts and vermicomposts in terms of maturity indexes for soil enhancement and in agriculture as organic fertilizer. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Comparative study on pyrolysis of lignocellulosic and algal biomass using a thermogravimetric and a fixed-bed reactor.

    Science.gov (United States)

    Yuan, Ting; Tahmasebi, Arash; Yu, Jianglong

    2015-01-01

    Pyrolysis characteristics of four algal and lignocellulosic biomass samples were studied by using a thermogravimetric analyzer (TGA) and a fixed-bed reactor. The effects of pyrolysis temperature and biomass type on the yield and composition of pyrolysis products were investigated. The average activation energy for pyrolysis of biomass samples by FWO and KAS methods in this study were in the range of 211.09-291.19kJ/mol. CO2 was the main gas component in the early stage of pyrolysis, whereas H2 and CH4 concentrations increased with increasing pyrolysis temperature. Bio-oil from Chlorellavulgaris showed higher content of nitrogen containing compounds compared to lignocellulosic biomass. The concentration of aromatic organic compounds such as phenol and its derivatives were increased with increasing pyrolysis temperature up to 700°C. FTIR analysis results showed that with increasing pyrolysis temperature, the concentration of OH, CH, CO, OCH3, and CO functional groups in char decreased sharply. Copyright © 2014 Elsevier Ltd. All rights reserved.

  1. Thermogravimetric determination of the carbon dioxide reactivity of char from some New Zealand coals and its association with the inorganic geochemistry of the parent coal

    Energy Technology Data Exchange (ETDEWEB)

    Beamish, B.B.; Shaw, K.J.; Rodgers, K.A.; Newman, J. [University of Auckland, Auckland (New Zealand). Dept. of Geology

    1998-02-01

    Thermogravimetrically-determined carbon dioxide reactivities of char formed from New Zealand coals, ranging in rank from lignite to high volatile bituminous, vary from 0.12 to 10.63 mg/h/mg on a dry, ash-free basis. The lowest rank subbituminous coal chars have similar reactivities to the lignite coal chars. Calcium content of the char shows the strongest correlation with reactivity, which increases as the calcium content increases. High calcium per se does not directly imply a high char reactivity. Organically-bound calcium catalyses the conversion of carbon to carbon monoxide in the presence of carbon dioxide, whereas calcium present as discrete minerals in the coal matrix e.g., calcite, fails to significantly affect reactivity. Catalytic effects of magnesium, iron, sodium and phosphorous are not as obvious, but can be recognised for individual chars. The thermogravimetric technique provides a fast, reliable analysis that is able to distinguish char reactivity differences between coals, which may be due to any of the above effects. 27 refs., 6 figs., 4 tabs.

  2. Study of Surface Wettability Change of Unconsolidated Sand Using Diffuse Reflectance Infrared Fourier Transform Spectroscopy and Thermogravimetric Analysis.

    Science.gov (United States)

    Gómora-Herrera, Diana; Navarrete Bolaños, Juan; Lijanova, Irina V; Olivares-Xometl, Octavio; Likhanova, Natalya V

    2018-04-01

    The effects exerted by the adsorption of vapors of a non-polar compound (deuterated benzene) and a polar compound (water) on the surface of Ottawa sand and a sample of reservoir sand (Channel), which was previously impregnated with silicon oil or two kinds of surfactants, (2-hydroxyethyl) trimethylammonium oleate (HETAO) and (2-hydroxyethyl)trimethylammonium azelate (HETAA), were studied by diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) and thermogravimetric analysis (TGA). The surface chemistry of the sandstone rocks was elucidated by X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) with energy dispersive X-ray spectroscopy (EDX). Terminal surface groups such as hydroxyls can strongly adsorb molecules that interact with these surface groups (surfactants), resulting in a wettability change. The wettability change effect suffered by the surface after treating it with surfactants was possible to be detected by the DRIFTS technique, wherein it was observed that the surface became more hydrophobic after being treated with silicon oil and HETAO; the surface became more hydrophilic after treating it with HETAA.

  3. Automation of a thermogravimetric equipment

    International Nuclear Information System (INIS)

    Mussio, L.; Castiglioni, J.; Diano, W.

    1987-01-01

    A low cost automation of some instruments by means of simple electronic circuits and a microcomputer Apple IIe. type is discussed. The electronic circuits described are: a) a position detector including phototransistors connected as differential amplifier; b) a current source that, using the error signal of the position detector, changes the current through the coil of an electromagnetic balance to restore its zero position; c) a proportional temperature controller, zero volt switching to drive a furnace to a desired temperature; d) an interface temperature regulator-microcomputer to control the temperature regulator by software; e) a multiplexer for an analog input of a commercial interface. Those circuits are applied in a thermogravimetric equipment used also for vapours adsorption. A program in block diagram form is included and is able to record change of mass, time, furnace temperature and to drive the temperature regulator in order to have the heating rates or the temperature plateaux needed for the experiment. (author) [pt

  4. Thermogravimetric studies of New Zealand coals

    Energy Technology Data Exchange (ETDEWEB)

    Beamish, B.B.; Rodgers, K.A.; Benfell, K.E.; Shaw, K.J. [University of Auckland, Auckland (New Zealand). Dept. of Geology

    1997-12-31

    The thermal behaviour of New Zealand coals may be reliably characterised by a series of tightly constrained thermogravimetric (TG) procedures of high repeatability developed in the Department of Geology at The University of Auckland. Proximate, combustion and char reactivity analyses can be routinely obtained for run-of-mine samples. Volatile matter determination by TG produces an acceptable reproducible result compared with the ISO method, whereas further refinement of the technique is necessary to achieve the same level of precision for ash content of New Zealand low rank coals. Combining combustion and char reactivity analyses enables the performance of a coal to be assessed under differing operating conditions, and offers the opportunity to elucidate competing effects of major element geochemistry of the coal. 12 refs., 4 figs., 2 tabs.

  5. Dominant thermogravimetric signatures of lignin in cashew shell as compared to cashew shell cake.

    Science.gov (United States)

    Gangil, Sandip

    2014-03-01

    Dominant thermogravimetric signatures related to lignin were observed in cashew shell as compared to these signatures in cashew shell cake. The phenomenon of weakening of lignin from cashew shell to cashew shell cake was explained on the basis of changes in the activation energies. The pertinent temperature regimes responsible for the release of different constituents of both the bio-materials were identified and compared. The activation energies of cashew shell and cashew shell cake were compared using Kissinger-Akahira-Sunose method. Thermogravimetric profiling of cashew shell and cashew shell cake indicated that these were different kinds of bio-materials. Copyright © 2013 Elsevier Ltd. All rights reserved.

  6. Physicotechnical, spectroscopic and thermogravimetric properties of powdered cellulose and microcrystalline cellulose derived from groundnut shells

    Directory of Open Access Journals (Sweden)

    Chukwuemeka P. Azubuike

    2012-09-01

    Full Text Available α-Cellulose and microcrystalline cellulose powders, derived from agricultural waste products, that have for the pharmaceutical industry, desirable physical (flow properties were investigated. α–Cellulose (GCN was extracted from groundnut shell (an agricultural waste product using a non-dissolving method based on inorganic reagents. Modification of this α -cellulose was carried out by partially hydrolysing it with 2N hydrochloric acid under reflux to obtain microcrystalline cellulose (MCGN. The physical, spectroscopic and thermal properties of the derived α-cellulose and microcrystalline cellulose powders were compared with Avicel® PH 101, a commercial brand of microcrystalline cellulose (MCCA, using standard methods. X-ray diffraction and infrared spectroscopy analysis showed that the α-cellulose had lower crystallinity. This suggested that treatment with 2N hydrochloric acid led to an increase in the crystallinity index. Thermogravimetric analysis showed quite similar thermal behavior for all cellulose samples, although the α-cellulose had a somewhat lower stability. A comparison of the physical properties between the microcrystalline celluloses and the α-cellulose suggests that microcrystalline cellulose (MCGN and MCCA might have better flow properties. In almost all cases, MCGN and MCCA had similar characteristics. Since groundnut shells are agricultural waste products, its utilization as a source of microcrystalline cellulose might be a good low-cost alternative to the more expensive commercial brand.

  7. Use of a fluidized bed combustor and thermogravimetric analyzer for the study of coal ignition temperature

    International Nuclear Information System (INIS)

    Ávila, Ivonete; Crnkovic, Paula M.; Luna, Carlos M.R.; Milioli, Fernando E.

    2017-01-01

    Highlights: • Coal ignition tests were conducted in a fluidized bed and thermogravimetric conditions. • The use of two different ignition criteria showed a similar coal ignition temperature. • Coal ignition temperature was obtained by the changes of gas concentrations in FBC. • Ignition temperatures were associated with the activation energy of coal combustion. - Abstract: Ignition experiments with two bituminous coals were carried out in an atmospheric bubbling fluidized bed combustor (FBC) and a thermogravimetric analyzer (TGA). In the FBC tests, the rapid increase in O_2, CO_2, and SO_2 concentrations is an indication of the coal ignition. In the TGA technique, the ignition temperature was determined by the evaluation of the TGA curves in both combustion and pyrolysis processes. Model-Free Kinetics was applied and the coal ignition temperatures were associated with changes in the activation energy values during the combustion process. The results show the coal with the lowest activation energy also showed the lowest ignition temperature, highest values of volatile content and a higher heating value. The application of two different ignition criteria (TGA and FBC) resulted in similar ignition temperatures. The FBC curves indicated the high volatile coal ignites in the freeboard, i.e. during the feeding in the reactor, whereas the low volatile coal ignites in the bed. Finally, the physicochemical characteristics of the investigated coal types were correlated with their reactivities for the prediction of the ignition temperatures behaviors under different operating conditions as those in FBC.

  8. Thermogravimetric and nuclear magnetic resonance study of hydrated Na-β''-alumina

    International Nuclear Information System (INIS)

    Donoso, P.; Panepucci, H.; Gobato, Y.G.; Oliveira, L.N.; Souza, D.P.F. de

    1990-01-01

    This paper reports thermogravimetric and proton spin-lattice relaxation times measurement of hydrated Na-β''-alumina, which yield information about the identification of the sites where the loosely bound water molecules are located in the polycrystalline sample. It examines also the influence of impurities on the motion of the protons. (autor) [pt

  9. Investment casting using multi-jet modelling patterns: the thermogravimetric analysis of visijet® SR200 UV curable acrylate plastic

    International Nuclear Information System (INIS)

    Hafsa, M N; Ibrahim, M; Sharif, S

    2013-01-01

    Rapid Prototyping (RP) technology is actively studied to be implemented in Investment Casting (IC) process. Nowadays RP techniques are studied for their feasibility as IC master patterns, in terms of pattern collapsibility and drainage during burnout. The purpose of the study is to determine the characteristic of Visijet® SR200 acrylate material during burnout process. Traditional IC patterns made from wax have properties that limit their application in precision casting, especially for parts with thin geometries that readily break or deform when handled or dipped in the refractory slurry. Furthermore, it is not economical when producing a small number of parts. Non wax patterns fabricated for IC process, revealed ceramic shell cracking due to excessive thermal expansions, incomplete collapsibility of pattern during burnout, residual ash and poor surface finish. Thermogravimetric analysis (TGA) was used to measured the weight loss of acrylate material as the temperature was increased. TGA measured the change of material's mass as it is heated. It represents the decomposition temperature after being subjected to varying temperatures, as well as the amount of residual ash. In this experiment, the temperature range was from 20°C to 700°C with 5°C increment. Experiment results show the values of material's optimum reaction temperature and decomposing temperature of Visijet® SR200 acrylate. The percentages of remaining materials were also monitored throughout the process to obtain the amount of residual ash. All of the temperature values obtained is a resemblance for the actual burnout process and can be used as references

  10. Investigation on the co-combustion of oil shale and municipal solid waste by using thermogravimetric analysis

    International Nuclear Information System (INIS)

    Fan, Yunlong; Yu, Zhaosheng; Fang, Shiwen; Lin, Yan; Lin, Yousheng; Liao, Yanfen; Ma, Xiaoqian

    2016-01-01

    Highlights: • Co-combustion of oil shale with municipal solid waste created significant changes. • Blending with municipal solid wastes could improve the combustion performance. • 10–30% of oil shale in the blends could be determined as the optimum ratio range. • Activation energy were calculated by the conversion rate and different proportion. - Abstract: The aim of this study is trying to reveal the thermal characteristics and kinetics of oil shale, municipal solid waste and their blends in the combustion process which are needed for efficient utilization. The combustion experiment is carried out in a thermogravimetric simultaneous thermal analyzer, where the temperature ranged from 110 °C to 900 °C at three different heating rates as 10 °C/min, 20 °C/min and 30 °C/min. Their kinetics were studied by Ozawa–Flynn–Wall and Friedmen methods. According to the data analysis, combustion characteristic index increased progressively with the increase of the proportion of municipal solid waste. And it’s suggested that there was certain interaction in the combustion process of oil shale and municipal solid waste. The average activation energy of the blends reached the minimum value, 177.7927 kJ/mol by Ozawa–Flynn–Wall method and 167.4234 kJ/mol by Friedmen method, when the proportion of MSW was 70%.

  11. Combustion studies of coal derived solid fuels by thermogravimetric analysis. III. Correlation between burnout temperature and carbon combustion efficiency

    Science.gov (United States)

    Rostam-Abadi, M.; DeBarr, J.A.; Chen, W.T.

    1990-01-01

    Burning profiles of 35-53 ??m size fractions of an Illinois coal and three partially devolatilized coals prepared from the original coal were obtained using a thermogravimetric analyzer. The burning profile burnout temperatures were higher for lower volatile fuels and correlated well with carbon combustion efficiencies of the fuels when burned in a laboratory-scale laminar flow reactor. Fuels with higher burnout temperatures had lower carbon combustion efficiencies under various time-temperature conditions in the laboratory-scale reactor. ?? 1990.

  12. Thermogravimetric research of hydrogen storage materials

    International Nuclear Information System (INIS)

    Kleperis, J; Grinberga, L; Ergle, M; Chikvaidze, G; Klavins, J

    2007-01-01

    During thermogravimetric research of metal hydrides we noticed mass growth of samples above 200 deg. C even in an argon atmosphere. Further heating is leading to the growth of weight up to 2-7 weight% till 500 0 C. Second run of the same sample without taking out of DTA instrument gave only small mass changes, indicating that noticed mass increase during first run is permanent. Microscope and elemental analyses were made to determine the reason of mass growth. XRD inspection revealed the formation of new phase with bunsenite NiO structure with deformed cubic structure. The new phase is no more active to hydrogen sorption/desorption. Our results demonstrated that the usage of hydrogen storage alloys AB 5 must be taken with care - it is important not to exceed some critical temperature were irreversible structural, compositional and morphological changes will occur

  13. Measurement of the oxidation of spent fuel between 140/degree/ and 225/degree/C by thermogravimetric analysis

    International Nuclear Information System (INIS)

    Woodley, R.E.; Einziger, R.E.; Buchanan, H.C.

    1988-09-01

    A series of PWR spent fuel samples from Turkey Point Unit 3 have been oxidized at temperatures between 140/degree/ and 225/degree/C in air atmospheres with dew points between 14.5/degree/ and /minus/70/degree/C, using a thermogravimetric analysis system (TGA). Tests lasted between 400 and 2100 hours. At the conclusion of a test, the atmosphere was sampled to determine the release of fission gas during testing, and the fuel samples were analyzed for microstructural changes. It appears that the mechanism for oxidation of spent fuel to U/sub 3/O/sub 7/ takes place in two steps that occur somewhat simultaneously. Oxygen migrates along the grain boundaries, which are oxidized and enlarged. The grains oxidize by the inward progression of a layer of U/sub 4/O/sub 9/ saturated with oxygen. A simplified model of the mechanism, which considers oxygen diffusion through the product layer as the rate-controlling step, yields an activation energy of 27 /plus minus/ 4 kcal/mol. Moisture, between dew points of /minus/70/degree/ to +14.5/degree/C, i.e., water vapor partial pressures varying over four orders of magnitude, had no significant effect on the oxidation rate. 34 refs., 12 figs., 6 tabs

  14. Understanding of thermo-gravimetric analysis to calculate number of addends in multifunctional hemi-ortho ester derivatives of fullerenol

    International Nuclear Information System (INIS)

    Singh, Rachana; Goswami, Thakohari

    2011-01-01

    Test results for the applicability of existing thermo-gravimetric analysis (TGA) technique to ascertain average number of exohedral chemical attachment in a new class of fullerene dyads consisting of multiple hemi-ortho esters onto fullerenol is presented. Although the method is nicely applicable for higher fullerenol, but homogeneous phase products calculate lower number of addends, whereas, the hetero phase products indicate higher value. Lower value is attributed to either overlapping of thermal events or substituents effects and higher value is the contribution of tetra butyl ammonium hydroxide (TBAH) impurity used as phase transfer catalyst (PTC) in heterogeneous phase reactions. Presence of TBAH impurity is recognized through thermo-gravimetry mass spectrometry (TG-MS) measurement. Appropriate modification of test method to arrive at accurate and precise values of x (total mass contribution due to addends only) and y (total mass contribution due to fullerene plus char yield) are also reported. Successful use of two more different techniques, viz., electron-spray ionization mass spectrometry (ESI-MS) and X-ray photoelectron spectroscopy (XPS), supplement above results. Influences of fullerene and different substituents on thermal behavior of dyads are assessed.

  15. Kinetic model of the thermal pyrolysis of chrome tanned leather treated with NaOH under different conditions using thermogravimetric analysis.

    Science.gov (United States)

    Bañón, E; Marcilla, A; García, A N; Martínez, P; León, M

    2016-02-01

    The thermal decomposition of chrome tanned leather before and after a soaking treatment with NaOH was studied using thermogravimetric analysis (TGA). The effect of the solution concentration (0.2M and 0.5M) and the soaking time (5min and 15min) was evaluated. TGA experiments at four heating rates (5, 10, 15 and 20°Cmin(-1)) were run in a nitrogen atmosphere for every treatment condition. A kinetic model was developed considering the effect of the three variables studied, i.e.: the NaOH solution concentration, the soaking time and the heating rate. The proposed model for chrome tanned leather pyrolysis involves a set of four reactions, i.e.: three independent nth order reactions, yielding the corresponding products and one of them undergoing a successive cero order reaction. The model was successfully applied simultaneously to all the experimental data obtained. The evaluation of the kinetic parameters obtained (activation energy, pre-exponential factor and reaction order) allowed a better understanding of the effect of the alkali treatment on these wastes. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Thermogravimetric kinetic model of the pyrolysis and combustion of an ethylene-vinyl acetate copolymer refuse

    Energy Technology Data Exchange (ETDEWEB)

    Angela N. Garcia; Rafael Font [Universidad de Alicante, Alicante (Spain). Faculty of Sciences

    2004-06-01

    A kinetic study of the pyrolysis as well as the combustion of EVA copolymer refuse originating from the footwear industry was carried out by thermogravimetric analysis. Different runs were performed at heating rates between 5-20{sup o}C min{sup -1} and atmospheres with different percentages of oxygen: 0, 10 and 20% (v/v). Pyrolysis and combustion processes can be simulated by two series reactions. The results obtained indicate that the second reaction begins when the first one is almost finished which implies that a good correlation is also obtained by simulation of the thermal decomposition of two independent fractions. 32 refs., 4 figs., 3 tabs.

  17. Thermogravimetric studies of the thermo-oxidative stability of irradiated and unirradiated polyethylene

    International Nuclear Information System (INIS)

    Novakovic, L.; Gal, O.; Markovic, V.; Stannett, V.T.

    1985-01-01

    In part one of this series the effects of a phenolic, an amine and a thioester antioxidant on the thermo-oxidative stability of irradiated and unirradiated low-density polyethylene was reported. In this paper the effects of combined phenolic and thioester stabilizers are described. Isothermal thermogravimetric analysis was used to study the systems. Pronounced synergism was observed with the induction periods, the time when the initial weight loss begins and the 5% weight loss. At about 50% of each stabilizer increases greater than twofold were observed both with the unirradiated and irradiated polymers. The rate constants for oxygen uptake were decreased. However, the rates of degradation at 5% weight loss fell between the values of the two pure stabilizers with no pronounced synergism in either case. In the absence of oxygen little effect of either antioxidant or their mixtures was observed. The corresponding activation energies were somewhat higher, however, with the irradiated samples containing antioxidants. Dynamic thermogravimetry was used for this study. A kinetic analysis indicated that there were somewhat different modes of degradation at lower- and higher-temperature ranges. (author)

  18. Thermogravimetric study of the kinetics of lithium titanate reduction by hydrogen

    International Nuclear Information System (INIS)

    Sonak, Sagar; Rakesh, R.; Jain, Uttam; Mukherjee, Abhishek; Kumar, Sanjay; Krishnamurthy, Nagaiyar

    2014-01-01

    Highlights: • Li 2 TiO 3 powder is synthesized by the gel combustion route. • Activation energy of reduction of Li 2 TiO 3 by H 2 found out to be 27.45 kJ/mol H 2 . • Non-stoichiometric phase of Li 2 TiO 3 is formed in hydrogen atmosphere. • One-dimensional diffusion appears to be the most probable mechanism of reduction. - Abstract: The lithium titanate powder was synthesized by gel-combustion route. The mechanism and the kinetics of hydrogen interaction with lithium titanate powder were studied using non-isothermal thermogravimetric technique. Lithium titanate underwent reduction in hydrogen atmosphere which led to the formation of oxygen deficient non-stoichiometric compound in lithium titanate. One-dimensional diffusion appeared to be the most probable reaction mechanism. The activation energy for reduction of lithium titanate under hydrogen atmosphere was found to be 27.4 kJ/mol/K. Structural changes after hydrogen reduction in lithium titanate were observed in X-ray diffraction analysis

  19. Co-combustion characteristics and blending optimization of tobacco stem and high-sulfur bituminous coal based on thermogravimetric and mass spectrometry analyses.

    Science.gov (United States)

    Zhang, Kaihua; Zhang, Kai; Cao, Yan; Pan, Wei-ping

    2013-03-01

    Despite much research on co-combustion of tobacco stem and high-sulfur coal, their blending optimization has not been effectively found. This study investigated the combustion profiles of tobacco stem, high-sulfur bituminous coal and their blends by thermogravimetric analysis. Ignition and burnout performances, heat release performances, and gaseous pollutant emissions were also studied by thermogravimetric and mass spectrometry analyses. The results indicated that combustion of tobacco stem was more complicated than that of high-sulfur bituminous coal, mainly shown as fixed carbon in it was divided into two portions with one early burning and the other delay burning. Ignition and burnout performances, heat release performances, and gaseous pollutant emissions of the blends present variable trends with the increase of tobacco stem content. Taking into account the above three factors, a blending ratio of 0–20% tobacco stem content is conservatively proposed as optimum amount for blending. Copyright © 2012 Elsevier Ltd. All rights reserved.

  20. Thermogravimetric analysis of the co-pyrolysis of paper sludge and municipal solid waste

    International Nuclear Information System (INIS)

    Fang, Shiwen; Yu, Zhaosheng; Lin, Yousheng; Hu, Shanchao; Liao, Yanfen; Ma, Xiaoqian

    2015-01-01

    Highlights: • The co-pyrolysis of municipal solid waste, paper sludge and the blends was studied. • The reactivity of paper sludge could be improved by blending municipal solid waste. • The FWO and KAS methods were used to calculate activation energy. • The average activation energy was the minimum by blending 50% paper sludge. - Abstract: The pyrolysis characteristics of municipal solid waste (MSW), paper sludge (PS) and their blends were studied through a thermogravimetric simultaneous thermal analyzer from room temperature to 1000 °C. Meanwhile their kinetics were studied by Flynn–Wall–Ozawa (FWO) and Kissinger–Akahira–Sunose (KAS) methods. The mass proportions of PS in the blends were 10%, 30%, 50%, 70%, 90%, respectively and the experiments were carried out at different heating rates (30, 40 and 50 °C/min). The initial temperature of MSW was lower than that of PS and the terminated temperature was higher than PS. The comprehensive characteristic index decreased progressively along with the decrease of the MSW proportion. The values of average activation energies calculated by FWO and KAS methods were highly consistent. The average activation energy reached the minimum number, 96.7 kJ/mol by KAS and 11.56 kJ/mol by FWO, with the proportion of PS was 50%

  1. Kinetics of Pyrolysis and Gasification Using Thermogravimetric and Thermovolumetric Analyses

    Directory of Open Access Journals (Sweden)

    Czerski Grzegorz

    2016-03-01

    Full Text Available The carbon dioxide gasification process of Miscanthus giganteus biomass was examined using two methods. First an isothermal thermovolumetric method was applied. The measurement was conducted at 950°C and pressure of 0.1 MPa. Based on the continuous analysis of different kinds of gases formed during the gasification process, the thermovolumetric method allowed the determination of yields and composition of the resulting gas as well as the rate constant of CO formation. Then a non-isothermal thermogravimetric method was applied, during which the loss of weight of a sample as a function of temperature was recorded. In the course of the measurement, the temperature was raised from ambient to 950°C and the pressure was 0.1 MPa. As a result, a change in the carbon conversion degree was obtained. Moreover, TGA methods allow distinguishing various stages of the gasification process such as primary pyrolysis, secondary pyrolysis and gasification, and determining kinetic parameters for each stage. The presented methods differs from each other as they are based either on the analysis of changes in the resulting product or on the analysis of changes in the supplied feedstock, but both can be successfully used to the effective examination of kinetics of the gasification process. In addition, an important advantage of both methods is the possibility to carry out the gasification process for different solid fuels as coal, biomass, or solid waste in the atmosphere of a variety of gasification agents.

  2. Characterization of the Sublimation and Vapor Pressure of 2-(2-Nitrovinyl) Furan (G-0) Using Thermogravimetric Analysis: Effects of Complexation with Cyclodextrins.

    Science.gov (United States)

    Ruz, Vivian; González, Mirtha Mayra; Winant, Danny; Rodríguez, Zenaida; Van den Mooter, Guy

    2015-08-19

    In the present work, the sublimation of crystalline solid 2-(2-nitrovinyl) furan (G-0) in the temperature range of 35 to 60 °C (below the melting point of the drug) was studied using thermogravimetric analysis (TGA). The sublimated product was characterized using Fourier-transformed-infrared spectroscopy (FT-IR) and thin layer chromatography (TLC). The sublimation rate at each temperature was obtained using the slope of the linear regression model and followed apparent zero-order kinetics. The sublimation enthalpy from 35 to 60 °C was obtained from the Eyring equation. The Gückel method was used to estimate the sublimation rate and vapor pressure at 25 °C. Physical mixtures, kneaded and freeze-dried complexes were prepared with 2-hydroxypropyl-β-cyclodextrin (HP-β-CD) and sulfobutyl ether-β-cyclodextrin (SBE-β-CD) and analyzed using isothermal TGA at 50 °C. The complexation contributed to reducing the sublimation process. The best results were achieved using freeze-dried complexes with both cyclodextrins.

  3. Thermogravimetric investigation of the co-combustion between the pyrolysis oil distillation residue and lignite.

    Science.gov (United States)

    Li, Hao; Xia, Shuqian; Ma, Peisheng

    2016-10-01

    Co-combustion of lignite with distillation residue derived from rice straw pyrolysis oil was investigated by non-isothermal thermogravimetric analysis (TGA). The addition of distillation residue improved the reactivity and combustion efficiency of lignite, such as increasing the weight loss rate at peak temperature and decreasing the burnout temperature and the total burnout. With increasing distillation residue content in the blended fuels, the synergistic interactions between distillation residue and lignite firstly increased and then decreased during co-combustion stage. Results of XRF, FTIR, (13)C NMR and SEM analysis indicated that chemical structure, mineral components and morphology of samples have great influence on the synergistic interactions. The combustion mechanisms and kinetic parameters were calculated by the Coats Redfern model, suggesting that the lowest apparent activation energy (120.19kJ/mol) for the blended fuels was obtained by blending 60wt.% distillation residue during main co-combustion stage. Copyright © 2016 Elsevier Ltd. All rights reserved.

  4. A thermogravimetric analyzer for corrosive atmospheres, and its application to the chlorination of ZrO2-C mixtures

    International Nuclear Information System (INIS)

    Pasquevich, Daniel; Caneiro, Alberto

    1990-01-01

    A thermogravimetric analyzer built on the basis of a Cahn 2000 electrobalance, suitable for using with corrosive atmospheres, is reported. The corrections for buoyancy and gas-flow effects, which strongly modify the thermogravimetric curves are discussed. As an application, the kinetics of a reaction between chlorine and a mixture of zirconia and carbon has been studied. It has been able to measure the uptake of chlorine by carbon and the reaction rate within the first 50 seconds. Evidence of a transition to quite a different reaction rate at longer times is presented. (Author)

  5. Thermal and Chemical Characterization of Non-Metallic Materials Using Coupled Thermogravimetric Analysis and Infrared Spectroscopy

    Science.gov (United States)

    Huff, Timothy L.

    2002-01-01

    Thermogravimetric analysis (TGA) is widely employed in the thermal characterization of non-metallic materials, yielding valuable information on decomposition characteristics of a sample over a wide temperature range. However, a potential wealth of chemical information is lost during the process, with the evolving gases generated during thermal decomposition escaping through the exhaust line. Fourier Transform-Infrared spectroscopy (FT-IR) is a powerful analytical technique for determining many chemical constituents while in any material state, in this application, the gas phase. By linking these two techniques, evolving gases generated during the TGA process are directed into an appropriately equipped infrared spectrometer for chemical speciation. Consequently, both thermal decomposition and chemical characterization of a material may be obtained in a single sample run. In practice, a heated transfer line is employed to connect the two instruments while a purge gas stream directs the evolving gases into the FT-IR. The purge gas can be either high purity air or an inert gas such as nitrogen to allow oxidative and pyrolytic processes to be examined, respectively. The FT-IR data is collected realtime, allowing continuous monitoring of chemical compositional changes over the course of thermal decomposition. Using this coupled technique, an array of diverse materials has been examined, including composites, plastics, rubber, fiberglass epoxy resins, polycarbonates, silicones, lubricants and fluorocarbon materials. The benefit of combining these two methodologies is of particular importance in the aerospace community, where newly developing materials have little available data with which to refer. By providing both thermal and chemical data simultaneously, a more definitive and comprehensive characterization of the material is possible. Additionally, this procedure has been found to be a viable screening technique for certain materials, with the generated data useful in

  6. Investigation on the co-combustion of low calorific oil shale and its semi-coke by using thermogravimetric analysis

    International Nuclear Information System (INIS)

    Yang, Yu; Lu, Xiaofeng; Wang, Quanhai

    2017-01-01

    Highlights: • The co-combustion characteristic parameters were studied. • The co-combustion of oil shale and semi-coke could be expressed roughly by the addition of individual components. • Activation energy was calculated by Coats-Redfern, distributed activation energy model and Flynn-Wall-Ozawa methods. - Abstract: In the present work, thermogravimetric analysis was employed to investigate co-combustion behaviors of Fushun low calorific oil shale and its semi-coke. The synergy effect was estimated by using the interaction coefficient and the relative error of mean square root. In addition, activation energy was also calculated by means of Coats-Redfern, distributed activation energy model and Flynn-Wall-Ozawa methods. Results indicated that with the increase of oil shale mass fraction and oxygen concentration, combustion characteristics of the samples were improved. And some little interaction did occur during the co-combustion process, but it was relatively slight. Consequently, the co-combustion of oil shale and semi-coke still could be expressed roughly by the addition of individual components of the mixtures. Furthermore, activation energy of the samples decreased slowly at the initial stage attributed to the minerals’ catalytic effects, and in the final stage, it jumped to a high value, suggesting that the burnout of the samples was difficult. Besides, the mix proportion of oil shale which was added to stabilize the combustion in the circulating fluidized bed was also theoretically calculated.

  7. Thermogravimetric analytical procedures for characterizing New Zealand and eastern Australian coals

    Energy Technology Data Exchange (ETDEWEB)

    Benfell, K.E.; Beamish, B.B.; Rodgers, K.A. [University of Auckland, Auckland (New Zealand). Dept. of Geology

    1996-09-01

    Under tightly constrained experimental conditions (particle size {lt}75 {mu}m, sample mass 5.0 {+-} 0.5 mg), heating rate 15{degree}C min{sup -1}, dry air purge 50 mL min{sup -1}, maximum temperature 900{degree}C a repeatability of {lt} {+-} 2{degree}C, may be achieved for significant temperatures that characterize the differential thermogravimetric burning profiles of typical medium-volatile, bituminous Australian Gondwanan coals and high-volatile, bituminous New Zealand Cretaceous-Tertiary coals.

  8. Thermogravimetric investigation on the degradation properties and combustion performance of bio-oils.

    Science.gov (United States)

    Ren, Xueyong; Meng, Jiajia; Moore, Andrew M; Chang, Jianmin; Gou, Jinsheng; Park, Sunkyu

    2014-01-01

    The degradation properties and combustion performance of raw bio-oil, aged bio-oil, and bio-oil from torrefied wood were investigated through thermogravimetric analysis. A three-stage process was observed for the degradation of bio-oils, including devolatilization of the aqueous fraction and light compounds, transition of the heavy faction to solid, and combustion of carbonaceous residues. Pyrolysis kinetics parameters were calculated via the reaction order model and 3D-diffusion model, and combustion indexes were used to qualitatively evaluate the thermal profiles of tested bio-oils for comparison with commercial oils such as fuel oils. It was found that aged bio-oil was more thermally instable and produced more combustion-detrimental carbonaceous solid. Raw bio-oil and bio-oil from torrefied wood had comparable combustion performance to fuel oils. It was considered that bio-oil has a potential to be mixed with or totally replace the fuel oils in boilers. Copyright © 2013 Elsevier Ltd. All rights reserved.

  9. Pyrolysis of olive residue/low density polyethylene mixture:Part I Thermogravimetric kinetics

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    This paper demonstrates the thermal pyrolysis of olive residue, low density polyethylene (LDPE) and olive residue/LDPE mixture in an inert atmosphere of N2 using thermogravimetric analysis (TGA). Measurements were carried out in the temperature range 300K~973K at heating rates of 2K/min, 10K/min, 20K/min and 50K/min. Based on the results obtained, three temperature regimes were selected for studying the non-isothermal kinetics of olive residue/LDPE mixture. The first two were dominated by the olive residue pyrolysis, while the third was linked to the LDPE pyrolysis, which occurred at much higher temperatures. Discrepancies between the experimental and calculated TG/DTG profiles were considered as a measurement of the extent of interactions occurring on co-pyrolysis. The maximum degradation temperatures of each component in the mixture were higher than those the individual components;thus an increase in thermal stability was expected. The kinetic parameters associated with thermal degradation were determined using Friedman isoconversional method.

  10. Characterization of Synthesized and Commercial Forms of Magnesium Stearate Using Differential Scanning Calorimetry, Thermogravimetric Analysis, Powder X-Ray Diffraction, and Solid-State NMR Spectroscopy.

    Science.gov (United States)

    Delaney, Sean P; Nethercott, Matthew J; Mays, Christopher J; Winquist, Nickolas T; Arthur, Donia; Calahan, Julie L; Sethi, Manish; Pardue, Daniel S; Kim, Junghyun; Amidon, Gregory; Munson, Eric J

    2017-01-01

    Magnesium stearate is the salt of a complex mixture of fatty acids, with the majority being stearate and palmitate. It has multiple crystalline forms and, potentially, an amorphous form. Magnesium stearate is used in the pharmaceutical manufacturing industry as a powder lubricant, and typically is added at low levels (∼1%) during the manufacturing process and blended for a relatively short time (∼5 min). Proper levels and mixing times are needed, as too short a mixing time or too small a quantity will result in improper lubrication, and too much can negatively impact dissolution rates. The complex mixture of multiple fatty acids and crystalline forms in magnesium stearate leads to variability between commercial sources, and switching between sources can impact both the amount of lubricant and mixing time needed for proper lubrication. In order to better understand the complex nature of magnesium stearate, a variety of analytical techniques were used to characterize both synthesized and commercial magnesium stearate samples. The results show that correlation among differential scanning calorimetry, thermogravimetric analysis, solid-state NMR spectroscopy, and other techniques provides a unique insight into the forms of magnesium stearate. Finally, the ability to monitor form changes of magnesium stearate in an intact tablet using solid-state NMR spectroscopy is shown. Copyright © 2016 American Pharmacists Association®. Published by Elsevier Inc. All rights reserved.

  11. Thermogravimetric and Kinetic Analysis of Raw and Torrefied Biomass Combustion

    Directory of Open Access Journals (Sweden)

    Kopczyński Marcin

    2015-06-01

    Full Text Available The use of torrefied biomass as a substitute for untreated biomass may decrease some technological barriers that exist in biomass co-firing technologies e.g. low grindability, high moisture content, low energy density and hydrophilic nature of raw biomass. In this study the TG-MS-FTIR analysis and kinetic analysis of willow (Salix viminalis L. and samples torrefied at 200, 220, 240, 260, 280 and 300 °C (TSWE 200, 220, 240, 260, 280 and 300, were performed. The TG-DTG curves show that in the case of willow and torrefied samples TSWE 200, 220, 240 and 260 there are pyrolysis and combustion stages, while in the case of TSWE 280 and 300 samples the peak associated with the pyrolysis process is negligible, in contrast to the peak associated with the combustion process. Analysis of the TG-MS results shows m/z signals of 18, 28, 29 and 44, which probably represent H2O, CO and CO2. The gaseous products were generated in two distinct ranges of temperature. H2O, CO and CO2 were produced in the 500 K to 650 K range with maximum yields at approximately 600 K. In the second range of temperature, 650 K to 800 K, only CO2 was produced with maximum yields at approximately 710 K as a main product of combustion process. Analysis of the FTIR shows that the main gaseous products of the combustion process were H2O, CO2, CO and some organics including bonds: C=O (acids, aldehydes and ketones, C=C (alkenes, aromatics, C-O-C (ethers and C-OH. Lignin mainly contributes hydrocarbons (3000-2800 cm−1, while cellulose is the dominant origin of aldehydes (2860-2770 cm−1 and carboxylic acids (1790-1650 cm−1. Hydrocarbons, aldehydes, ketones and various acids were also generated from hemicellulose (1790-1650 cm−1. In the kinetic analysis, the two-steps first order model (F1F1 was assumed. Activation energy (Ea values for the first stage (pyrolysis increased with increasing torrefaction temperature from 93 to 133 kJ/mol, while for the second stage (combustion it

  12. Thermogravimetric and Kinetic Analysis of Cassava Starch Based Bioplastic

    Directory of Open Access Journals (Sweden)

    Nanang Eko Wahyuningtyas

    2017-11-01

    Full Text Available Cassava starch based bioplasticfor packaging application has great potency because of the various starch-producing plants in Indonesia.Bioplasticcan contribute to reduce the dependence on fossil fuels andpetroleumthat can solve the environmentalproblem.Thepurpose of this research is to find out the thermal decomposition and the activation energy of cassava starch based bioplastic. The methods weresynthesis bioplastic with cassava starch as main component and glycerol as plasticizer. The thermogravimetry analysis was conducted to obtain the decomposition process mechanism of bioplastic and the heating valueof bioplasticwas measured  using theadiabatic bomb calorimetric.  Data analysis was conducted using  a fitting model approach with an acikalin method to determine the activation energy. The result of thethermogravimetricanalysis showed thatbioplasticisgraduallydecomposedto the moisture, volatilematter, fixed carbon, andash in four stages mechanism. Totally decomposition of bioplastic was 530°C, then all of bioplastic was become the ash. The activation energy in the early and primary thermal decomposition stages are 1.27 kJ/moland 22.62 kJ/mol, respectively and heating valueof bioplastic is 15.16 MJ/kg.

  13. Synthesis, characterization and thermogravimetric study of zinc and cadmium acetates-polyaniline hybrids

    International Nuclear Information System (INIS)

    Fernandes de Farias, Robson

    2004-01-01

    By dissolution of respective acetates and conducting polymer in dimethylformamide, homogeneous zinc acetate and cadmium acetate-polyaniline (PANI) hybrids were synthesized and characterized by infrared spectroscopy, thermogravimetry and SEM microscopy. The infrared spectra suggests that there are interactions between PANI and the metal cations involving both, imine and amine nitrogens in a typical Lewis acid-base reaction. The thermogravimetric degradation profile of the synthesized hybrids resembles those exhibited by PANI samples

  14. Characterization of microalga Chlorella as a fuel and its thermogravimetric behavior

    International Nuclear Information System (INIS)

    Rizzo, Andrea Maria; Prussi, Matteo; Bettucci, Lorenzo; Libelli, Ilaria Marsili; Chiaramonti, David

    2013-01-01

    Highlights: ► Proximate and ultimate analysis of two microalgae (Nannochloropsis and Chlorella spp.). ► TGA of Chlorella spp. and Nannochloropsis investigated at 15 °C/min up to 800 °C. ► 1.2 kg of Chlorella pyrolyzed in a novel batch, intermediate pyrolysis pilot reactor at 450 °C. ► Bio-oil from Chlorella oil analysed and compared to pine chips fast pyrolysis oil. ► Bio-oil from Chlorella exhibited superior properties compared to lignocellulosic pyrolysis oil as intermediate energy carrier. -- Abstract: Microalgae are photosynthetic microorganisms living in marine or freshwater environment. In this study, samples of Chlorella spp. and Nannochloropsis from two different origins were analysed to settle a preliminary characterization of these microorganisms as intermediate energy carriers and their properties compared to a conventional lignocellulosic feedstock (pine chips). Both microalgae samples were characterized in terms of elemental composition (CHONS and P) and thermogravimetric behavior. This was investigated through non-isothermal thermogravimetric analysis in nitrogen atmosphere at heating rate of 15 °C min −1 and temperature up to 800 °C. Solid residues produced at 300 °C and 800 °C from TGA were also analysed to determine the ultimate composition of chars. Activation energy, reaction order and pre-exponential factor were calculated for the single step conversion mechanism of 1 g of Chlorella spp. and compared to literature data on Chlorella protothecoides and Spirulina platensis. Calculated kinetic parameters, given as intervals of several determinations, resulted to be: pre-exponential factor (A) 1.47–1.62E6 min −1 , activation energy (E) 7.13–7.92E4 J mol −1 , reaction order (n) 1.69–2.41. 1.2 kg of Chlorella spp. was then processed in a newly designed batch pyrolysis pilot reactor, capable of converting up to 1.5 kg h −1 of material, and pyrolysis liquid collected, analysed and compared with a sample of fast pyrolysis

  15. Chemometric modeling of thermogravimetric data for the compositional analysis of forest biomass.

    Science.gov (United States)

    Acquah, Gifty E; Via, Brian K; Fasina, Oladiran O; Adhikari, Sushil; Billor, Nedret; Eckhardt, Lori G

    2017-01-01

    The objective of this study was to investigated the use of chemometric modeling of thermogravimetric (TG) data as an alternative approach to estimate the chemical and proximate (i.e. volatile matter, fixed carbon and ash contents) composition of lignocellulosic biomass. Since these properties affect the conversion pathway, processing costs, yield and / or quality of products, a capability to rapidly determine these for biomass feedstock entering the process stream will be useful in the success and efficiency of bioconversion technologies. The 38-minute long methodology developed in this study enabled the simultaneous prediction of both the chemical and proximate properties of forest-derived biomass from the same TG data. Conventionally, two separate experiments had to be conducted to obtain such information. In addition, the chemometric models constructed with normalized TG data outperformed models developed via the traditional deconvolution of TG data. PLS and PCR models were especially robust in predicting the volatile matter (R2-0.92; RPD- 3.58) and lignin (R2-0.82; RPD- 2.40) contents of the biomass. The application of chemometrics to TG data also made it possible to predict some monomeric sugars in this study. Elucidation of PC loadings obtained from chemometric models also provided some insights into the thermal decomposition behavior of the chemical constituents of lignocellulosic biomass. For instance, similar loadings were noted for volatile matter and cellulose, and for fixed carbon and lignin. The findings indicate that common latent variables are shared between these chemical and thermal reactivity properties. Results from this study buttresses literature that have reported that the less thermally stable polysaccharides are responsible for the yield of volatiles whereas the more recalcitrant lignin with its higher percentage of elementary carbon contributes to the yield of fixed carbon.

  16. Chemometric modeling of thermogravimetric data for the compositional analysis of forest biomass.

    Directory of Open Access Journals (Sweden)

    Gifty E Acquah

    Full Text Available The objective of this study was to investigated the use of chemometric modeling of thermogravimetric (TG data as an alternative approach to estimate the chemical and proximate (i.e. volatile matter, fixed carbon and ash contents composition of lignocellulosic biomass. Since these properties affect the conversion pathway, processing costs, yield and / or quality of products, a capability to rapidly determine these for biomass feedstock entering the process stream will be useful in the success and efficiency of bioconversion technologies. The 38-minute long methodology developed in this study enabled the simultaneous prediction of both the chemical and proximate properties of forest-derived biomass from the same TG data. Conventionally, two separate experiments had to be conducted to obtain such information. In addition, the chemometric models constructed with normalized TG data outperformed models developed via the traditional deconvolution of TG data. PLS and PCR models were especially robust in predicting the volatile matter (R2-0.92; RPD- 3.58 and lignin (R2-0.82; RPD- 2.40 contents of the biomass. The application of chemometrics to TG data also made it possible to predict some monomeric sugars in this study. Elucidation of PC loadings obtained from chemometric models also provided some insights into the thermal decomposition behavior of the chemical constituents of lignocellulosic biomass. For instance, similar loadings were noted for volatile matter and cellulose, and for fixed carbon and lignin. The findings indicate that common latent variables are shared between these chemical and thermal reactivity properties. Results from this study buttresses literature that have reported that the less thermally stable polysaccharides are responsible for the yield of volatiles whereas the more recalcitrant lignin with its higher percentage of elementary carbon contributes to the yield of fixed carbon.

  17. Thermal transformation of bioactive caffeic acid on fumed silica seen by UV-Vis spectroscopy, thermogravimetric analysis, temperature programmed desorption mass spectrometry and quantum chemical methods.

    Science.gov (United States)

    Kulik, Tetiana V; Lipkovska, Natalia O; Barvinchenko, Valentyna M; Palyanytsya, Borys B; Kazakova, Olga A; Dudik, Olesia O; Menyhárd, Alfréd; László, Krisztina

    2016-05-15

    Thermochemical studies of hydroxycinnamic acid derivatives and their surface complexes are important for the pharmaceutical industry, medicine and for the development of technologies of heterogeneous biomass pyrolysis. In this study, structural and thermal transformations of caffeic acid complexes on silica surfaces were studied by UV-Vis spectroscopy, thermogravimetric analysis, temperature programmed desorption mass spectrometry (TPD MS) and quantum chemical methods. Two types of caffeic acid surface complexes are found to form through phenolic or carboxyl groups. The kinetic parameters of the chemical reactions of caffeic acid on silica surface are calculated. The mechanisms of thermal transformations of the caffeic chemisorbed surface complexes are proposed. Thermal decomposition of caffeic acid complex chemisorbed through grafted ester group proceeds via three parallel reactions, producing ketene, vinyl and acetylene derivatives of 1,2-dihydroxybenzene. Immobilization of phenolic acids on the silica surface improves greatly their thermal stability. Copyright © 2016 Elsevier Inc. All rights reserved.

  18. Comparative study on the pyrolysis behaviour and kinetics of two macroalgae biomass (Gracilaria changii and Gelidium pusillum) by thermogravimetric analysis

    Science.gov (United States)

    Roslee, A. N.; Munajat, N. F.

    2017-10-01

    Macroalgae are often referred as seaweed and could be significant biomass resource for the production of numerous energy carriers including biofuels. In this study, the chemical composition of Gracilaria changii (G. changii) and Gelidium pusillum (G. pusillum) were determined through proximate and ultimate analysis and the thermal degradation behaviour of G. changii and G. pusillum were investigated via thermogravimetric analysis (TGA) in determining the important main composition to be considered as biomass fuels. It has found the pyrolysis of G. changii and G. pusillum consists of three stages and stage II is the main decomposition stage with major mass loss of around 52.16% and 44.42%, respectively. The TGA data were then used for determination of kinetic parameters of the pyrolysis process using three model-free methods: Kissinger, Kissinger-Akahira-Sunose (KAS) and Flynn-Wall-Ozawa (FWO). The apparent activation energy calculated by using Kissinger method for G. changii was lower than G. Pusillum, i.e.173.12 kJ/mol and 193.22 kJ/mol, respectively. The activation energies calculated from KAS and FWO methods were increased with increasing the pyrolysis conversion with average activation energies of 172.32 kJ/mol and 181.19 kJ/mol for G. changii while for G. pusillum (177.42 kJ/mol and 187.4 kJ/mol). G. pusillum has lower and wider distribution of activation energy and revealed that the pyrolysis process for G. changii was easier than G. pusillum. These data provide information for further application for designing and modelling in thermochemical conversion system of macroalgae biomass.

  19. Study of solid chemical evolution in torrefaction of different biomasses through solid-state "1"3C cross-polarization/magic angle spinning NMR (nuclear magnetic resonance) and TGA (thermogravimetric analysis)

    International Nuclear Information System (INIS)

    Rodriguez Alonso, Elvira; Dupont, Capucine; Heux, Laurent; Da Silva Perez, Denilson; Commandre, Jean-Michel; Gourdon, Christophe

    2016-01-01

    The objective of this work is to compare mass loss and chemical evolution of the solid phase, versus time, during dynamic torrefaction of different types of biomass. For this purpose, two experiments, ThermoGravimetric Analysis and solid-state "1"3C Cross-Polarization/Magic Angle Spinning Nuclear Magnetic Resonance, were run on four representative biomasses. Overall mass loss and chemical evolution of the solid phase were followed, respectively, as a function of temperature and time. Thanks to this coupled information, it was shown that the knowledge of both solid mass loss and chemical evolution is necessary to characterize torrefaction severity. Moreover, biomasses containing higher proportions of xylan lost mass faster than those containing lower proportions. Lignin showed a protecting role towards cellulose, which would lead to a faster degradation of non-woody biomasses in comparison with woody biomasses. Three parameters would have an influence on solid chemical evolution during torrefaction: xylan content in hemicellulose, lignin content in biomass, and cellulose crystallinity. - Highlights: • Torrefaction of four biomasses was studied with TGA and solid-state NMR. • Both solid mass loss and chemical evolution characterize torrefaction severity. • Biomasses containing a higher proportion of xylan lose mass faster. • Lignin shows a stronger protecting role in degradation of woody biomasses. • Xylan, lignin and crystalline cellulose values influence solid chemical evolution.

  20. Investigation of the effects of phase transformations in micro and nano aluminum powders on kinetics of oxidation using thermogravimetric analysis.

    Science.gov (United States)

    Saceleanu, Florin; Atashin, Sanam; Wen, John Z

    2017-07-26

    Aluminum micro and nanoparticles are key ingredients in the synthesis of nano energetic materials. Hence it is important to characterize the kinetics and the rate controlling process of their oxidation. The literature shows that the mass diffusion and phase transformation within the aluminum oxide shell are important. However, the description of physical processes regarding simultaneous oxidation and phase transformation is lacking. In this paper, the controlled thermogravimetric (TGA) oxidation of 40-60 nm and 1 µm Al powders is investigated at constant heating rates and under isothermal conditions, respectively, upon varying the partial pressure of oxygen. It is found that the core-shell model of homogenous oxidation is applicable to explain the TGA results when the shell does not undergo phase transformation, which predicts the apparent activation energy in good agreement with the literature data. On the other hand, the simultaneous oxidation and phase transformation is able to be addressed using the JMAK model which reveals key parameters of the rate controlling processes. Mass diffusion is indeed rate determining during the oxidation of Al micro and nanopowders while the kinetics of the reaction is fast. Unlike the micron powders, the particle size distribution has a significant effect on the shape of the oxidation curves of the nanopowders.

  1. Thermogravimetric kinetic modelling of in-situ catalytic pyrolytic conversion of rice husk to bioenergy using rice hull ash catalyst.

    Science.gov (United States)

    Loy, Adrian Chun Minh; Gan, Darren Kin Wai; Yusup, Suzana; Chin, Bridgid Lai Fui; Lam, Man Kee; Shahbaz, Muhammad; Unrean, Pornkamol; Acda, Menandro N; Rianawati, Elisabeth

    2018-04-07

    The thermal degradation behaviour and kinetic parameter of non-catalytic and catalytic pyrolysis of rice husk (RH) using rice hull ash (RHA) as catalyst were investigated using thermogravimetric analysis at four different heating rates of 10, 20, 50 and 100 K/min. Four different iso conversional kinetic models such as Kissinger, Friedman, Kissinger-Akahira-Sunose (KAS) and Ozawa-Flynn-Wall (OFW) were applied in this study to calculate the activation energy (E A ) and pre-exponential value (A) of the system. The E A of non-catalytic and catalytic pyrolysis was found to be in the range of 152-190 kJ/mol and 146-153 kJ/mol, respectively. The results showed that the catalytic pyrolysis of RH had resulted in a lower E A as compared to non-catalytic pyrolysis of RH and other biomass in literature. Furthermore, the high Gibb's free energy obtained in RH implied that it has the potential to serve as a source of bioenergy production. Copyright © 2018 Elsevier Ltd. All rights reserved.

  2. Thermogravimetric studies of the thermo-oxidative stability of irradiated and unirradiated polyethylene. 2. Combined antioxidants

    Energy Technology Data Exchange (ETDEWEB)

    Novakovic, L; Gal, O; Markovic, V; Stannett, V T

    1985-01-01

    In part one of this series the effects of a phenolic, an amine and a thioester antioxidant on the thermo-oxidative stability of irradiated and unirradiated low-density polyethylene was reported. In this paper the effects of combined phenolic and thioester stabilizers are described. Isothermal thermogravimetric analysis was used to study the systems. Pronounced synergism was observed with the induction periods, the time when the initial weight loss begins and the 5% weight loss. At about 50% of each stabilizer increases greater than twofold were observed both with the unirradiated and irradiated polymers. The rate constants for oxygen uptake were decreased. However, the rates of degradation at 5% weight loss fell between the values of the two pure stabilizers with no pronounced synergism in either case. In the absence of oxygen little effect of either antioxidant or their mixtures was observed. The corresponding activation energies were somewhat higher, however, with the irradiated samples containing antioxidants. Dynamic thermogravimetry was used for this study. A kinetic analysis indicated that there were somewhat different modes of degradation at lower- and higher-temperature ranges. (author).

  3. Study on high-silicon boron-containing zeolite by thermogravimetric and IR-spectroscopy techniques

    International Nuclear Information System (INIS)

    Chukin, G.D.; Nefedov, B.K.; Surin, S.A.; Polinina, E.V.; Khusid, B.L.; Sidel'kovskaya, V.G.

    1985-01-01

    The structure identity of initial Na-forms of boron-containing and aluminosilicate high-silicon zeolites is established by thermogravimetric and IR-spectroscopy methods. The presence of boron in Na-forms of high-silicon zeolites is shown to lead to reduction of structure thermal stability. It is noted that thermal stability of the H-form of both high-silicon boron-containing and boron-free zeolites is practically equal and considerably higher than that of Na-forms

  4. Effect of superfine grinding on the physico-chemical, morphological and thermogravimetric properties of Lentinus edodes mushroom powders.

    Science.gov (United States)

    Ming, Jian; Chen, Long; Hong, Hui; Li, Jinlong

    2015-09-01

    Lentinus edodes is an edible mushroom commonly known as shiitake, which is the second most produced and consumed edible mushroom in the world and is an important nutrient source in the human diet. To fully use L. edodes, the mushrooms are occasionally ground into powder as a flavourful and functional food additive. This study produces powders from the cap and stipe of Lentinus edodes mushrooms through superfine grinding. These powders are composed of sub-micron range particles with various size distributions. The superfine grinding process is then compared with shear pulverisation to determine the different effects on both the cap and stipe powders in terms of particle size and physico-chemical, morphological and thermogravimetric properties. When average particle size was reduced to 0.54 and 0.46 µm, respectively, the moisture and protein content, angles of repose and slide, and water holding capacity of the powders decreased to varied extents. However, soluble dietary fibre, water solubility index, and swelling capacity increased. Scanning electron microscope images suggested that the superfine grinding process effectively changed the original surface structure of the L. edodes powders. The curves of thermogravimetric analysis and those of the derivatives of thermogravimetry indicated that superfine grinding can improve the thermostability of L. edodes powders. Furthermore, superfinely ground L. edodes powders may be used as pharmaceutical or food additives in various fields. The present study suggests that superfinely ground L. edodes powders may be applied in various fields as pharmaceutical or food additives. © 2014 Society of Chemical Industry.

  5. Thermogravimetric-mass spectrometric study on the evolution of nitrogen compounds during coal devolatilisation

    Energy Technology Data Exchange (ETDEWEB)

    Arenillas, A.; Rubiera, F.; Pevida, C.; Pis, J.J. [Department of Energy and Environment, Instituto Nacional del Carbon, CSIC, Apartado 73, 33080 Oviedo (Spain)

    2002-10-01

    Emissions of nitrogen oxides during coal combustion are a major environmental problem. The chemically bound nitrogen in fuel accounts for up to 80% of total NO{sub x} emissions. In this respect, fundamental studies are needed to clarify the mechanisms and to identify the different species that are precursors in the formation of the NO{sub x}. Mass spectrometry (MS) has been used for decades as a successful technique in evolved gas analysis. However, MS is normally used to identify typical volatile compounds formed during coal pyrolysis (i.e. H{sub 2}, CH{sub 4}, CO, CO{sub 2} and H{sub 2}O) but very few works on the detection by MS of nitrogen compounds during coal devolatilisation can be found. In this work, the possibility of detecting different nitrogen compounds by means of thermogravimetric-MS during the temperature-programmed pyrolysis of coal was evaluated. Interferences in the N-compounds MS signals were determined. The use of model compounds provided additional information on the MS response factors of the volatile compounds produced.

  6. Thermogravimetric Studies of Deposited Potash Impregnated for Flame-Retardancy into a Cotton Fabric

    Institute of Scientific and Technical Information of China (English)

    MOSTASHARI, S.M.; NIA, Y.K.; BAIE, S.

    2007-01-01

    The effect of potash as a nondurable finish on the flammability of 100% cotton fabric (plain 180 g/m2) was investigated. The bone-dried weighed fabrics were dipped into suitable concentrations of potash, with a volume of 100 mL at 20-2 ℃. The impregnation was followed by means of squeeze rolls and drying at 110 C. The samples were then reweighed with analytical precision. After conditioning overnight by using our "vertical flame tester" the optimum add-on values to impart flame-retardancy to cotton fabric was determined and expressed by 0.80 g of potash per 100 g fabric to be an efficient addition. Thermogravimetric analysis of pure cotton, treated cotton with potash at its optimum efficiency for donation of flame-retardancy into cotton fabric was fulfilled and the thermograms were compared and commented. The effectiveness of this hydroxide was attributed to the heat dissipation by the remaining consumed material during the combustion. The results obtained are in favor of "Dust or Wall Effect Theory".

  7. Thermogravimetric study of superconducting YBa2Cu3O9-x in hydrogen

    International Nuclear Information System (INIS)

    Swaminathan, K.; Janaki, J.; Rao, G.V.N.; Sreedharan, O.M.; Radhakrishnan, T.S.

    1988-01-01

    The thermogravimetric curve of YBa 2 Cu 3 O 9-x in hydrogen exhibits five steps, the first two corresponding to the reduction of copper oxide to copper by about 683 K (as identified by XRD on quenched samples) followed by three more steps predominantly due to hydration-dehydration behaviour of BaO. The need for blank corrections and the choice of 1223 K as the temperature for the determination of oxygen stoichiometry are discussed. 6 refs.; 2 figs.; 1 table

  8. Thermogravimetric investigation on characteristic of biomass combustion under the effect of organic calcium compounds.

    Science.gov (United States)

    Zhang, Lihui; Duan, Feng; Huang, Yaji

    2015-01-01

    Experiments were conducted in a thermogravimetric analyzer to investigate thermal behavior of different organic calcium compounds (OCCs) and its blended fuels with three kinds of biomass. The effectiveness of synthesized method for OCC was assessed by the pyrolysis test. Effect of the mole ratio of calcium to sulfur on co-combustion characteristics was studied. Results indicated that preparation method of modified calcium acetate (MCA) had high precision and accuracy. Co-combustion characteristic of OCCs blended with biomass was controlled by OCCs' additive amount and the content of volatile matter which is mainly composed of small hydrocarbon molecules. Combustion performance indexes for peanut shell and wheat straw impregnated by OCCs were improved, however, an inverse trend was found for rice husk because of lower additive amount of OCCs. The blended fuel show higher combustion performance indexes compared with combustion of individual biomass, and these indexes decrease with increases of Ca/S ratio. Copyright © 2014 Elsevier Ltd. All rights reserved.

  9. Thermogravimetric Analysis of Rice Husk and Coconut Pulp for Potential Bio fuel Production by Flash Pyrolysis

    International Nuclear Information System (INIS)

    Noorhaza Alias; Norazana Ibrahim; Mohd Kamaruddin Abdul Hamid

    2014-01-01

    The purpose of this paper is to study the characteristics and thermal degradation behavior of rice husk and coconut pulp for bio fuel production via flash pyrolysis technology. The elemental properties of the feedstock were characterized by an elemental analyzer while thermal properties were investigated using thermogravimetric analyzer (TGA). The pyrolysis processes were carried out at room temperature up to 700 degree Celsius in the presence of nitrogen gas flowing at 150 ml/ min. The investigated parameters are particle sizes and heating rates. The particle sizes varied in the range of dp 1 < 0.30 mm and 0.30= dp 2 <0.50 mm. The heating rates applied were 50 degree Celsius/ min and 80 degree Celsius/ min. It was shown smaller particle size produces 2.11-3.59 % less volatile product when pyrolyzed at 50 degree Celsius/ min compared to 80 degree Celsius/ min. Higher heating rates causes biomass degrades in a narrow temperature range by 25 degree Celsius. It also increases the maximum peak rate by 0.01 mg/ s for rice husk at dp 1 and 0.02 mg/ s at dp 2 . In case of coconut pulp, the change is not significant for dp 1 but for dp 2 a 0.02 mg/ s changes was recorded. (author)

  10. Air oxidation of Zr65Cu17.5Ni10Al7.5 in its amorphous and supercooled liquid states, studied by thermogravimetric analysis

    International Nuclear Information System (INIS)

    Dhawan, A.; Sharma, S.K.; Raetzke, K.; Faupel, F.

    2003-01-01

    The oxidation behaviour of the bulk amorphous alloy Zr 65 Cu 17.5 Ni 10 Al 7.5 was studied in air at various temperatures in the temperature range 591-732 K using a thermogravimetric analyser (TGA). The oxidation kinetics of the alloy obeys the parabolic rate law showing two different linear regions (in the plots of mass gain versus square root of oxidation time) which are attributed to the amorphous and the supercooled liquid states of the alloy. The value of the activation energy Q for the amorphous state as calculated from the temperature dependence of the rate constants is found to be 1.80±0.1 eV and the corresponding value obtained for the supercooled liquid state is 1.20±0.1 eV. It is suggested that the rate controlling process during oxidation of the amorphous state is the back-diffusion of Ni, and possibly Cu also, while the oxidation in the supercooled liquid state is dominated by the inward diffusion of oxygen. (copyright 2003 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  11. Thermogravimetric analysis, kinetic study, and pyrolysis-GC/MS analysis of 1,1'-azobis-1,2,3-triazole and 4,4'-azobis-1,2,4-triazole.

    Science.gov (United States)

    Jia, Chenhui; Li, Yuchuan; Zhang, Shujuan; Fei, Teng; Pang, Siping

    2018-03-01

    In general, the greater the number of directly linked nitrogen atoms in a molecule, the better its energetic performance, while the stability will be accordingly lower. But 1,1'-azobis-1,2,3-triazole (1) and 4,4'-azobis-1,2,4-triazole (2) show remarkable properties, such as high enthalpies of formation, high melting points, and relatively high stabilities. In order to rationalize this unexpected behavior of the two compounds, it is necessary to study their thermal decompositions and pyrolyses. Although a great deal of research has been focused on the synthesis and characterization of energetic materials with 1 and 2 as the backbone, a complete report on their fundamental thermodynamic parameters and thermal decomposition properties has not been published. Thermogravimetric-differential scanning calorimetry were used to obtain the thermal decomposition data of the title compounds. Kissinger and Ozawa-Doyle methods, the two selected non-isothermal methods, are presented for analysis of the solid-state kinetic data. Pyrolysis-gas chromatography/mass spectrometry was used to study the pyrolysis process of the title compounds. The DSC curves show that the thermal decompositions of 1 and 2 are at different heating rates involved a single exothermic process. The TG curves provide insight into the total weight losses from the compounds associated with this process. At different pyrolysis temperatures, the compositions and types of the pyrolysis products differ greatly and the pyrolysis reaction at 500 °C is more thorough than 400 °C. Apparent activation energies (E) and pre-exponential factors (lnA/s -1 ) are 291.4 kJ mol -1 and 75.53 for 1; 396.2 kJ mol -1 and 80.98 for 2 (Kissinger). The values of E are 284.5 kJ mol -1 for 1 and 386.1 kJ mol -1 for 2 (Ozawa-Doyle). The critical temperature of thermal explosion (T b ) is evaluated as 187.01 °C for 1 and 282.78 °C for 2. The title compounds were broken into small fragment ions under the pyrolysis conditions

  12. Thermogravimetric kinetics of corn stalk pretreated by oleaginous fungi Cunninghamella echinulata.

    Science.gov (United States)

    Wu, Jianguo; Gao, Shi; Wan, Jilin; Zeng, Yelin; Ma, Fuying; Zhang, Xiaoyu

    2011-04-01

    The thermogravimetric and composition of corn stalk pretreated by oleaginous fungi Cunninghamella echinulata had been studied in this paper. Results indicated that pretreatment by oleaginous fungi C. echinulata could decrease the activation energy and make the pyrolysis more efficient and energy-saving. By bio-pretreatment, the contents of elements agreed with the weight loss, sugar content, and oil contents, especially the sulfur content was greatly decreased, greatly eliminating the inventory of gas contamination such as the emission of SOx and making the pyrolysis more environmentally friendly. Therefore, corn stalk with sugar pretreated by oleaginous fungi C. echinulata should be a good pyrolysis material to obtain high quality bio-oil. Copyright © 2011 Elsevier Ltd. All rights reserved.

  13. Synthesis, thermogravimetric, spectroscopic and theoretical characterization of copper(II) complex with 4-chloro-2-nitrobenzenosulfonamide

    Science.gov (United States)

    Camí, G.; Chacón Villalba, E.; Di Santi, Y.; Colinas, P.; Estiu, G.; Soria, D. B.

    2011-05-01

    4-Chloro-2-nitrobenzenesulfonamide (ClNbsa) was purified and characterized. A new copper(II) complex, [Cu(ClNbsa) 2(NH 3) 2], has been prepared using the sulfonamide as ligand. The thermal behavior of both, the ligand and the Cu(II) complex, was investigated by thermogravimetric analyses (TG) and differential thermal analysis (DT), and the electronic characteristics analyzed by UV-VIS, FTIR, Raman and 1H NMR spectroscopies. The experimental IR, Raman and UV-VIS spectra have been assigned on the basis of DFT calculations at the B3LYP level of theory using the standard (6-31 + G ∗∗) basis set. The geometries have been fully optimized in vacuum and in modeled dimethylsulfoxide (DMSO) solvent, using for the latter a continuum solvation model that reproduced the experimental conditions of the UV-VIS spectroscopy. The theoretical results converged to stable conformations for the free sulfonamide and for the complex, suggesting for the latter a distorted square planar geometry in both environments.

  14. Thermogravimetric characteristics and kinetics of scrap tyre and Juglans regia shell co-pyrolysis.

    Science.gov (United States)

    Uzun, B B; Yaman, E

    2014-10-01

    The degradation kinetics of Juglans regia shell, scrap tyre and their blends were investigated using a thermogravimetric analysis method. Experiments were performed under dynamic conditions and a nitrogen atmosphere in the range 293 to 973 K at different heating rates. During pyrolysis of J. regia shell three mass loss zones were specified as removal of water, decomposition of hemicelluloses and cellulose, and decomposition of lignin. The degradation curves of scrap tyre showed merely one stage which was due to decomposition of styrene butadiene rubber. The kinetic parameters were calculated using both Arrhenius and Coats-Redfern methods. By adopting the Arrhenius method, the average value of activation energies of J. regia shell, scrap tyre and their 1 : 1 blends were found to be 69.22, 71.48 and 47.03 kJ mol(-1), respectively. Additionally, by using the Coats-Redfern method, the average value of activation energies of J. regia shell, scrap tyre and their 1 : 1 blend were determined as 99.85, 78.72 and 63.81 kJ mol(-1), respectively. The addition of J. regia shell to scrap tyre caused a reduction in the activation energies. The difference of weight loss was measured to examine interactions between raw materials. The maximum difference between experimental and theoretical mass loss was 5% at about 648 K with a heating rate of 20 K min(-1). These results indicated a significant synergistic effect was available during co-pyrolysis of J. regia shell and scrap tyre in the high temperature region. © The Author(s) 2014.

  15. Thermogravimetric study of a Phase Change Slurry: Effect of variable conditions

    International Nuclear Information System (INIS)

    Giro-Paloma, J.; Valle-Zermeño, R. del; Fernández, A.I.; Chimenos, J.M.; Formosa, J.

    2016-01-01

    Highlights: • Dry or wet PCS present differences in their thermal behavior. • The optimum conditions of dry PCS were determined by TGA. • Type of atmosphere and heating rate were the variables under consideration. • T peak can be accurately determined at 1 °C·min −1 in N 2. • Fusion/latent heat can be best determined at 10 °C·min −1 . - Abstract: Microcapsules containing Phase Change Materials (MPCM) are widely used for passive systems in energy storage. When MPCM are mixed with a carrier fluid, Phase Change Slurries (PCS) are used for heat transfer fluids in active systems or heat transport systems. The thermal behavior of PCS can be measured as dry or wet basis, resulting in important differences in weight losses. This study explores the optimum conditions for analyzing the thermal behavior of dried PCS by thermogravimetric analysis (TGA) varying the parameter conditions for obtaining peak temperature and heat flow (latent heat). The factors that were taken into account were the atmosphere of study (air and nitrogen) and the heating rate (0.5, 1, 5, and 10 °C·min −1 ). The best conditions to determine peak temperature are at 1 °C·min −1 and in N 2 atmosphere, whereas the decomposition fusion/latent heat of the sample is improved at higher heating velocities towards 10 °C·min −1 .

  16. A Study of the Oxidation Behaviour of Pile Grade A (PGA) Nuclear Graphite Using Thermogravimetric Analysis (TGA), Scanning Electron Microscopy (SEM) and X-Ray Tomography (XRT).

    Science.gov (United States)

    Payne, Liam; Heard, Peter J; Scott, Thomas B

    2015-01-01

    Pile grade A (PGA) graphite was used as a material for moderating and reflecting neutrons in the UK's first generation Magnox nuclear power reactors. As all but one of these reactors are now shut down there is a need to understand the residual state of the material prior to decommissioning of the cores, in particular the location and concentration of key radio-contaminants such as 14C. The oxidation behaviour of unirradiated PGA graphite was studied, in the temperature range 600-1050°C, in air and nitrogen using thermogravimetric analysis, scanning electron microscopy and X-ray tomography to investigate the possibility of using thermal degradation techniques to examine 14C distribution within irradiated material. The thermal decomposition of PGA graphite was observed to follow the three oxidation regimes historically identified by previous workers with limited, uniform oxidation at temperatures below 600°C and substantial, external oxidation at higher temperatures. This work demonstrates that the different oxidation regimes of PGA graphite could be developed into a methodology to characterise the distribution and concentration of 14C in irradiated graphite by thermal treatment.

  17. Determinação da espessura da camada polimérica de fases estacionárias imobilizadas para cromatografia líquida de alta eficiência por termogravimetria Determination of polymeric layer thickness on immobilized stationary phases for high-performance liquid chromatography using thermogravimetric analyses

    Directory of Open Access Journals (Sweden)

    Anizio M. Faria

    2008-01-01

    Full Text Available This paper presents a simple and practical thermogravimetric method for determining the layer thickness of immobilized polymer stationary phases used in reversed-phase high-performance liquid chromatography. In this method, the weight loss of different polysiloxanes immobilized onto chromatographic supports, determined over the temperature range 150-650 ºC, demonstrated excellent agreement with the sum of carbon and hydrogen content obtained by elemental analysis. The results presented here suggest that the thermogravimetric procedure is an accurate and precise method to determine the polymeric material content on polymer-coated stationary phases.

  18. Reaction of LiD with water vapor: thermogravimetric and scanning electron microscopy studies

    International Nuclear Information System (INIS)

    Balooch, M; Dinh, L N; LeMay, J D

    2000-01-01

    The kinetics of hydroxide film growth on LiD have been studied by the thermogravimetric method in nitrogen saturated with water vapor and by scanning electron microscopy (SEM) of samples that have been exposed to air with 50% relative humidity. The reaction probability is estimated to be 4 x 10 -7 for LiD exposed to ambient air with 50% relative humidity, suggesting that the diffusion through the hydroxide film is not the limiting step on the overall process at high moisture levels. The rate of growth is drastically reduced when the temperature is increased to 60 C

  19. DETERMINATION OF SATURATION VAPOR PRESSURE OF LOW VOLATILE SUBSTANCES THROUGH THE STUDY OF EVAPORATION RATE BY THERMOGRAVIMETRIC ANALYSIS

    Directory of Open Access Journals (Sweden)

    R. V. Ralys

    2015-11-01

    Full Text Available Subject of Study.Research of vapor pressure of low volatile substances is a complicated problem due to both direct experimental implementation complexity and, most significantly, the issues faced correctness of the analysis and processing of experimental data. That is why it is usually required engaging the reference substances (with vapor pressures well studied. The latter drastically reduces the effectiveness of the experimental methods used and narrows their applicability. The paper deals with an approach to the evaporation process description (sublimation of low volatile substances based on molecular kinetic description in view of diffusive and convection processes. The proposed approach relies on experimental thermogravimetricfindingsina wide range of temperatures, flow rates ofthe purge gas and time. Method. A new approach is based on the calculation of the vapor pressure and uses the data about the speed of evaporation by thermogravimetric analysis depending on the temperature, the flow rate of the purge gas, and the evaporation time. The basis for calculation is the diffusion-kinetic description of the process of evaporation (mass loss of the substance from the exposed surface. The method is applicable to determine the thermodynamic characteristics for both the evaporation (the equilibrium liquid - vapor and sublimation (the equilibrium solid - vapor. We proposed the appropriate method of the experiment and analysis of its data in order to find the saturated vapor pressure of individual substances of low volatility. Main Results. The method has been tested on substances with insufficiently reliable and complete study of the thermodynamic characteristics but, despite this, are often used (because of the other data limitations as reference ones. The vaporization process (liquid-vapor has been studied for di-n-butyl phthalate C16H22O4 at 323,15–443,15 К, and sublimation for benzoic acid C7H6O2at 303,15–183,15 К. Both processes have

  20. Modified thermogravimetric apparatus to measure magnetic susceptibility on-line during annealing of metastable ferromagnetic materials

    International Nuclear Information System (INIS)

    Luciani, G.; Constantini, A.; Branda, F.; Ausanio, G.; Hison, C.; Iannotti, V.; Luponio, C.; Lanotte, L.

    2004-01-01

    The insertion of proper coils to generate a magnetic field, with controlled gradient, in a standard thermogravimetric apparatus is shown to be a valid solution to measure on-line, upon heat treatment, the magnetic susceptibility in ribbon shaped samples of a metastable ferromagnetic material. The method is very useful to individuate the annealing conditions that optimise soft or hard magnetic properties without using separate apparatuses for heat treatment, control of the structural phase transition and characterization of magnetic susceptibility

  1. Lithium-ion battery electrolyte emissions analyzed by coupled thermogravimetric/Fourier-transform infrared spectroscopy

    Science.gov (United States)

    Bertilsson, Simon; Larsson, Fredrik; Furlani, Maurizio; Albinsson, Ingvar; Mellander, Bengt-Erik

    2017-10-01

    In the last few years the use of Li-ion batteries has increased rapidly, powering small as well as large applications, from electronic devices to power storage facilities. The Li-ion battery has, however, several safety issues regarding occasional overheating and subsequent thermal runaway. During such episodes, gas emissions from the electrolyte are of special concern because of their toxicity, flammability and the risk for gas explosion. In this work, the emissions from heated typical electrolyte components as well as from commonly used electrolytes are characterized using FT-IR spectroscopy and FT-IR coupled with thermogravimetric (TG) analysis, when heating up to 650 °C. The study includes the solvents EC, PC, DEC, DMC and EA in various single, binary and ternary mixtures with and without the LiPF6 salt, a commercially available electrolyte, (LP71), containing EC, DEC, DMC and LiPF6 as well as extracted electrolyte from a commercial 6.8 Ah Li-ion cell. Upon thermal heating, emissions of organic compounds and of the toxic decomposition products hydrogen fluoride (HF) and phosphoryl fluoride (POF3) were detected. The electrolyte and its components have also been extensively analyzed by means of infrared spectroscopy for identification purposes.

  2. Morphological Changes of Limestone Sorbent Particles during Carbonation/Calcination Looping Cycles in a Thermogravimetric Analyzer (TGA) and Reactivation with Steam

    KAUST Repository

    Wu, Y.; Blamey, J.; Anthony, E. J.; Fennell, P. S.

    2010-01-01

    Carbonation and calcination looping cycles were carried out on four limestones in a thermogravimetric analyzer (TGA). The CO2 carrying capacity of a limestone particle decays very quickly in the first 10 cycles, reducing to about 20% of its original

  3. Surface area and pore size characteristics of nanoporous gold subjected to thermal, mechanical, or surface modification studied using gas adsorption isotherms, cyclic voltammetry, thermogravimetric analysis, and scanning electron microscopy

    Science.gov (United States)

    Tan, Yih Horng; Davis, Jason A.; Fujikawa, Kohki; Ganesh, N. Vijaya; Demchenko, Alexei V.

    2012-01-01

    Nitrogen adsorption/desorption isotherms are used to investigate the Brunauer, Emmett, and Teller (BET) surface area and Barrett-Joyner-Halenda (BJH) pore size distribution of physically modified, thermally annealed, and octadecanethiol functionalized np-Au monoliths. We present the full adsorption-desorption isotherms for N2 gas on np-Au, and observe type IV isotherms and type H1 hysteresis loops. The evolution of the np-Au under various thermal annealing treatments was examined using scanning electron microscopy (SEM). The images of both the exterior and interior of the thermally annealed np-Au show that the porosity of all free standing np-Au structures decreases as the heat treatment temperature increases. The modification of the np-Au surface with a self-assembled monolayer (SAM) of C18-SH (coverage of 2.94 × 1014 molecules cm−2 based from the decomposition of the C18-SH using thermogravimetric analysis (TGA)), was found to reduce the strength of the interaction of nitrogen gas with the np-Au surface, as reflected by a decrease in the ‘C’ parameter of the BET equation. From cyclic voltammetry studies, we found that the surface area of the np-Au monoliths annealed at elevated temperatures followed the same trend with annealing temperature as found in the BET surface area study and SEM morphology characterization. The study highlights the ability to control free-standing nanoporous gold monoliths with high surface area, and well-defined, tunable pore morphology. PMID:22822294

  4. Thermogravimetric characteristics of typical municipal solid waste fractions during co-pyrolysis.

    Science.gov (United States)

    Zhou, Hui; Long, YanQiu; Meng, AiHong; Li, QingHai; Zhang, YanGuo

    2015-04-01

    The interactions of nine typical municipal solid waste (MSW) fractions during pyrolysis were investigated using the thermogravimetric analyzer (TGA). To compare the mixture results with the calculation results of superposition of single fractions quantitatively, TG overlap ratio was introduced. There were strong interactions between orange peel and rice (overlap ratio 0.9736), and rice and poplar wood (overlap ratio 0.9774). The interactions of mixture experiments postponed the peak and lowered the peak value. Intense interactions between PVC and rice, poplar wood, tissue paper, wool, terylene, and rubber powder during co-pyrolysis were observed, and the pyrolysis at low temperature was usually promoted. The residue yield was increased when PVC was blended with rice, poplar wood, tissue paper, or rubber powder; while the residue yield was decreased when PVC was blended with wool. Copyright © 2014 Elsevier Ltd. All rights reserved.

  5. A vacuum thermogravimetric method for outgassing evaluations of silicone-coated fiberglass cloth

    Science.gov (United States)

    Jensen, L. B.; Mccauley, G. B.; Honma, M.; Hultquist, A. E.

    1972-01-01

    A method for evaluating outgassing characteristics of space-sensitive materials was devised by modifying a thermogravimetric balance so that a continual weight loss trace is obtained as a function of time at constant temperature and nearly constant pressure. In addition the apparatus is capable of collecting room temperature condensibles during the outgassing run. A series of silicone-coated glass cloth samples were evaluated by this method. The major advantage of the technique is that data presentation is developed in the form of a continuous trace. This data can then be utilized to develop the kinetics of weight loss. The technique has been shown to be a useful and valid one for indicating small differences between materials under vacuum and elevated temperature conditions.

  6. Separation and analysis of low molecular weight plasticizers in poly(vinyl chloride) tubes

    DEFF Research Database (Denmark)

    Wang, Qian; Storm, Birgit Kjærside

    2005-01-01

    ) and thermogravimetric analysis (TGA), as well as by studying the extracted low molecular weight plasticizers by gas chromatography/mass spectroscopy (GC/MS) and GC. It was found that the simple room temperature extraction in chloroform showed the best separation of plasticizers from the PVC matrix. Close results...

  7. Splitting CO2 with a ceria‐based redox cycle in a solar‐driven thermogravimetric analyzer

    Science.gov (United States)

    Takacs, M.; Ackermann, S.; Bonk, A.; Neises‐von Puttkamer, M.; Haueter, Ph.; Scheffe, J. R.; Vogt, U. F.

    2016-01-01

    Thermochemical splitting of CO2 via a ceria‐based redox cycle was performed in a solar‐driven thermogravimetric analyzer. Overall reaction rates, including heat and mass transport, were determined under concentrated irradiation mimicking realistic operation of solar reactors. Reticulated porous ceramic (RPC) structures and fibers made of undoped and Zr4+‐doped CeO2, were endothermally reduced under radiative fluxes of 1280 suns in the temperature range 1200–1950 K and subsequently re‐oxidized with CO2 at 950–1400 K. Rapid and uniform heating was observed for 8 ppi ceria RPC with mm‐sized porosity due to its low optical thickness and volumetric radiative absorption, while ceria fibers with μm‐sized porosity performed poorly due to its opacity to incident irradiation. The 10 ppi RPC exhibited higher fuel yield because of its higher sample density. Zr4+‐doped ceria showed increasing reduction extents with dopant concentration but decreasing specific CO yield due to unfavorable oxidation thermodynamics and slower kinetics. © 2016 American Institute of Chemical Engineers AIChE J, 63: 1263–1271, 2017 PMID:28405030

  8. Splitting CO2 with a ceria-based redox cycle in a solar-driven thermogravimetric analyzer.

    Science.gov (United States)

    Takacs, M; Ackermann, S; Bonk, A; Neises-von Puttkamer, M; Haueter, Ph; Scheffe, J R; Vogt, U F; Steinfeld, A

    2017-04-01

    Thermochemical splitting of CO 2 via a ceria-based redox cycle was performed in a solar-driven thermogravimetric analyzer. Overall reaction rates, including heat and mass transport, were determined under concentrated irradiation mimicking realistic operation of solar reactors. Reticulated porous ceramic (RPC) structures and fibers made of undoped and Zr 4+ -doped CeO 2 , were endothermally reduced under radiative fluxes of 1280 suns in the temperature range 1200-1950 K and subsequently re-oxidized with CO 2 at 950-1400 K. Rapid and uniform heating was observed for 8 ppi ceria RPC with mm-sized porosity due to its low optical thickness and volumetric radiative absorption, while ceria fibers with μm-sized porosity performed poorly due to its opacity to incident irradiation. The 10 ppi RPC exhibited higher fuel yield because of its higher sample density. Zr 4+ -doped ceria showed increasing reduction extents with dopant concentration but decreasing specific CO yield due to unfavorable oxidation thermodynamics and slower kinetics. © 2016 American Institute of Chemical Engineers , 63: 1263-1271, 2017.

  9. Thermogravimetric and Pyrolysis-Capillary Gas Chromatography-Mass Spectrometric Analysis of Pinus Halepensis Mill. Wood

    International Nuclear Information System (INIS)

    Hafsi, S.; Benbouzid, M.; Zimny, T.

    2005-01-01

    The analytical methods TG and Py-capillary-GC-MS were used to study the thermal degradation of Pinus Halepensis Mill. wood. The TG analysis in air and in nitrogen showed that the percentage content of char and ash were, 23.1% and 7.7% respectively. TG and DTG analysis proved that the evolution of organic degradation products occurs mainly between 215C and 380C and has its maximum evolution rate at 360C in nitrogen and 347C in air. Py-capillary-GC-MS analysis of the pyrolysis at 400C identified the presence of valuable chemicals such aliphatic and aromatic hydrocarbons, phenols, aldehydes, esters and saturated and unsaturated long chain fatty acids. (author)

  10. Comparative thermogravimetric analyses of co-combustion of textile dyeing sludge and sugarcane bagasse in carbon dioxide/oxygen and nitrogen/oxygen atmospheres: Thermal conversion characteristics, kinetics, and thermodynamics.

    Science.gov (United States)

    Xie, Wenhao; Wen, Shaoting; Liu, Jingyong; Xie, Wuming; Kuo, Jiahong; Lu, Xingwen; Sun, Shuiyu; Chang, Kenlin; Buyukada, Musa; Evrendilek, Fatih

    2018-05-01

    Thermodynamic and kinetic parameters of co-combustion of textile dyeing sludge (TDS) and sugarcane bagasse (SB) were studied using thermogravimetric analysis in CO 2 /O 2 and N 2 /O 2 atmospheres. Our results showed that the comprehensive combustion characteristic index (CCI) of the blends was improved by 1.71-4.32 times. With the increased O 2 concentration, co-combustion peak temperature decreased from 329.7 to 318.2 °C, with an increase in its maximum weight loss rate from 10.04 to 14.99%/min and its CCI by 1.31 times (β = 20 °C·min -1 ). To evaluate the co-combustion characteristics, thermodynamic and kinetic parameters (entropy, Gibbs free energy and enthalpy changes, and apparent activation energy) were obtained in the five atmospheres. The lowest apparent activation energy of the TB64 blend was obtained in oxy-fuel atmosphere (CO 2 /O 2  = 7/3). Copyright © 2018 Elsevier Ltd. All rights reserved.

  11. Thermogravimetric Characterization of the Microstructui Composition of Polyamide Injection Molded Denture Base Material vs Conventional Compression Molded Heat-cured Denture Base Material.

    Science.gov (United States)

    Al-Dharrab, Ayman; Shinawi, Lana

    2016-02-01

    Thermoplastic resin polymers are widely used in medicine due to their biostability and hypoallergenic properties, making them a possible alternative to poly-methylmethacrylate (PMMA). The current research examined the microstructure of a rapid injection molding system thermoplastic resin for construction of flexible denture compared with that of heat-cured PMMA. A total of 40 disk-shaped specimens (25 mm in diameter and 3 mm in thickness) were prepared and divided into two groups of 20 disks each (group I samples were of thermoplastic acrylic resin while group II was heat-cured PMMA resin). In group I, thermogravimetric analyzer showed that increasing the temperature up to 169°C resulted in about 1.3% of the material loss, and after that the material remains thermally stable up to 200°C. Group 11 showed 2.24% weight loss at 171°C, and further weight loss (12.025%) was observed on heating to 230°C. Fourier transform infrared (FTIR) spectrophotometer analysis in the range of 400-4000 cm(-1) detected the presence of an amine group (N-H) in group I samples and the presence of methylene group attached to inorganic Si as reinforcement filler (Si-CH3). Thermoplastic resin displayed excellent thermal stability and the absence of residual monomer within the polymerized material, suggesting its suitability for the fabrication dentures.

  12. Thermogravimetric study of the pyrolysis of biomass residues from tomato processing industry

    Energy Technology Data Exchange (ETDEWEB)

    Mangut, V.; Sabio, E.; Ganan, J.; Gonzalez, J.F.; Ramiro, A.; Gonzalez, C.M.; Roman, S.; Al-Kassir, A. [Department of Chemical and Energy Engineering, University of Extremadura, Avda. de Elvas s/n, 06071 Badajoz (Spain)

    2006-01-15

    There is an increasing concern with the environmental problems associated with the increasing CO{sub 2}, NO{sub x} and SO{sub x} emissions resulting from the rising use of fossil fuels. Renewable energy, mainly biomass, can contribute to reduce the fossil fuels consumption. Biomass is a renewable resource with a widespread world distribution. Tomato processing industry produces a high amount of biomass residue (peel and seeds) that could be used for thermal energy and electricity. A characterization and thermogravimetric study has been carried out. The residue has a high HHV and volatile content, and a low ash, and S contents. A kinetic model has been developed based on the degradation of hemicellulose, cellulose, lignin and oil that describe the pyrolysis of peel, seeds and peel and seeds residues. (author)

  13. THERMOGRAVIMETRIC INVESTIGATION AND THERMAL CONVERSION KINETICS OF TYPICAL NORTH-AFRICA AND MIDDLE-EAST LIGNOCELLULOSIC WASTES

    Directory of Open Access Journals (Sweden)

    2012-01-01

    Full Text Available The aim of this work was to thermally characterize the renewable lignocellulosic bioresources derived from palm trees in order to highlight their energy potential. Pyrolysis and combustion behaviours of date stones (DS agricultural by-products were tested by thermo-gravimetric analysis, and the main chemical compositions were analyzed. The work has also been conducted to identify their most important physical characteristics. The study of the sizes and heating rate effects constitute the first part of the experimental work. Inert atmosphere and three heating rates: 10, 20, and 50 °C/min, were applied to various particle sizes of DS. In the second part, tests were carried out in an oxidizing atmosphere (21% O2 by varying the size of the DS. The kinetic parameters such as pre-exponential factor and activation energy were determined. Increasing the particle sizes and the heating rates didn’t have an appreciable influence on the global weight losses. However, degradation rates were significant with the porous structure of the DS. Weight losses in inert and oxidizing atmospheres were found to occur in two stages (drying and devolatilization and in three stages (drying, devolatilization, and oxidation of the char.

  14. Sedimentation technique of waste bituminization and thermogravimetric characteristics of the finalproducts

    International Nuclear Information System (INIS)

    Zeger, J.; Knotik, K.

    1976-01-01

    In the research centre of the Oesterreichische Studiengesellschaft fuer Atomenergie GesmbH a semitechnical plant has been installed for waste bituminization, which has been tested inactively since 1973. This plant is using a new technological process for embedding. One of the important features of this new process is that the, normally inactive solution water is distilled off prior to the embedding, resulting in dry and powdery salts. The second important feature is that the mixing of these dry salts with the thin fluid bitumen is done by sedimentation. Expecially there is no mechanical aid used for mixing. Thermogravimetric analysis of samples which simulated the final products of this pilot plant, were carried out to verify the best working parameters and to study the possible chemical damage to the bitumen. Analysis was performed by heating the samples, consisting of various mixtures of bitumen and inorganic salts, in a METTLER-Thermoanalyzer up to 500 0 C using different atmospheres (air, nitrogen). It could be shown that only nitrate and nitrite especially in combination with Fe(III)-ions are of negative influence on the thermostability of bitumen. They lead to a sudden and quick weight loss of the samples between 370 and 410 0 C (above the melting point of both NaNO 2 and NaNO 3 ). The Fe-ions hava a catalytic influence, as it could be shown that 1 1% addiation of Fe(NO 3 ) 3 to NaNO 3 leads to a considerable acceleration of the incineration. This influence of the Fe(III)-ion can be suppressed to some extend by a hydrolysis prior to the embedding. In preparation of further studies concerning the behaviour of radiation damaged bitumen there has been developed a method of measuring the dose rate of an unknown radioactive salt mixture at any point of this mixture. This is done by making two measurements with glass dosimeters. One with a beta-absorber to get a pure gamma-dose and the other without it to get the combined beta and gamma dose. (author)

  15. Thermogravimetric and Magnetic Studies of the Oxidation and Reduction Reaction of SmCoO3 to Nanostructured Sm2O3 and Co

    Science.gov (United States)

    Kelly, Brian; Cichocki, Ronald; Poirier, Gerald; Unruh, Karl

    The SmCoO3 to nanostructured Sm2O3 and Co oxidation and reduction reaction has been studied by thermogravimetric analysis (TGA) measurements in forming gas (FG) and inert N2 atmospheres, x-ray diffraction (XRD) and vibrating sample magnetometry (VSM). The TGA measurements showed two clearly resolvable reduction processes when heating in FG, from the initial SmCoO3 phase through an intermediate nanostructured mixture of Sm2O3 and CoO when heated to 330°C for several minutes, and then the conversion of CoO to metallic Co when heated above 500°C. These phases were confirmed by XRD and VSM. Similar measurements in N2 yielded little mass change below 900°C and coupled reduction processes at higher temperatures. Isoconversional measurements of the CoO to Co reduction reaction in FG yielded activation energies above 2eV/atom in the nanostructured system. This value is several times larger than those reported in the literature or obtained by similar measurements of bulk mixtures of Sm2O3 and CoO, suggesting the nanostructuring was the source of the large increase in activation energy.

  16. Correlation of resistance and thermogravimetric measurements of the Er/sub 1/Ba/sub 2/Cu/sub 3/O/sub 9-δ/ superconductor to sample preparation techniques

    International Nuclear Information System (INIS)

    Lee, S.I.; Golben, J.P.; Song, Y.; Chen, X.D.; McMichael, R.D.; Gaines, J.R.

    1987-01-01

    The resistance dependence and thermogravimetric analysis (TGA) of Er/sub 1/Ba/sub 2/Cu/sub 3/O/sub 9-δ/ has been measured in the temperature range 27 C to 920 CV. The heat treatments and oxygen flow rates simulated actual sintering and annealing processes used in sample preparation. Evidence of a phase transition in Er/sub 1/Ba/sub 2/Cu/sub 3/O/sub 9-δ/ near 680 C is discussed, as well as the implications of the maximum oxygen uptake near 400 C. The impact of sample preparation procedures on sample features is also discussed

  17. Effect of organic calcium compounds on combustion characteristics of rice husk, sewage sludge, and bituminous coal: thermogravimetric investigation.

    Science.gov (United States)

    Zhang, Lihui; Duan, Feng; Huang, Yaji

    2015-04-01

    Experiments were conducted in a thermogravimetric analyzer to assess the enhancement of combustion characteristics of different solid fuels blended with organic calcium compounds (OCCs). Rice husk, sewage sludge, and bituminous coal, and two OCC were used in this study. Effect of different mole ratios of calcium to sulfur (Ca/S ratio) on the combustion characteristics were also investigated. Results indicated that combustion performance indexes for bituminous coal impregnated by OCC were improved, however, an inverse trend was found for sewage sludge because sewage sludge has lower ignition temperature and higher volatile matter content compared to those of OCC. For rice husk, effect of added OCC on the combustion characteristics is not obvious. Different solid fuels show different combustion characteristics with increases of Ca/S ratio. The maximum combustion performance indexes appear at Ca/S ratios of 1:1, 2:1, and 3:1 for OCC blended with Shenhua coal, rice husk, and sewage sludge, respectively. Copyright © 2015 Elsevier Ltd. All rights reserved.

  18. Thermogravimetric control of intermediate compounds in uranium metallurgy; Control termogravimetrico de productos intermedios de la metalurgia del uranio

    Energy Technology Data Exchange (ETDEWEB)

    Gasco Sanchez, L; Fernandez Cellini, R

    1959-07-01

    The thermal decomposition of some intermediate compounds in the metallurgy of the uranium as uranium peroxide, ammonium uranate, uranium and ammonium penta-fluoride, uranium tetrafluoride and uranous oxide has been study by means of the Chevenard's thermo balance. Some data on pyrolysis of synthetic mixtures of intermediate compounds which may occasionally appear during the industrial process, are given. Thermogravimetric methods of control are suggested, usable in interesting products in the uranium metallurgy. (Author) 20 refs.

  19. Thermogravimetric analytical procedures for determining reactivities of chars from New Zealand coals

    Energy Technology Data Exchange (ETDEWEB)

    Shaw, K.J.; Beamish, B.B.; Rodgers, K.A. [University of Auckland, Auckland (New Zealand). Dept. of Geology

    1997-10-22

    This paper describes how tightly constrained thermogravimetric experimental procedures (particle size {lt} 212 {mu}m, sample mass 15.5 mg, CO{sub 2} reactant gas, near isothermal conditions) allow the reactivity of chars from high volatile New Zealand coals to be determined to a repeatability of {+-}0.07 h{sup -1} at 900{degree}C and {+-}0.5 h{sup -1} at 1100{degree}C. The procedure also provides proximate analyses information and affords a quick ({lt} 90 min) comparison between different coal types as well as indicating likely operating conditions and problems associated with a particular coal or blend. A clear difference is evident between reactivities of differing New Zealand coal ranks. Between 900 and 1100{degree}C, bituminous coals increase thirtyfold in reactivity compared with fourfold for subbituminous, with the latter being three to five times greater in reactivity at higher temperature.

  20. Thermogravimetric control of intermediate compounds in uranium metallurgy; Control termogravimetrico de productos intermedios de la metalurgia del uranio

    Energy Technology Data Exchange (ETDEWEB)

    Gasco Sanchez, L.; Fernandez Cellini, R.

    1959-07-01

    The thermal decomposition of some intermediate compounds in the metallurgy of the uranium as uranium peroxide, ammonium uranate, uranium and ammonium penta-fluoride, uranium tetrafluoride and uranous oxide has been study by means of the Chevenard's thermo balance. Some data on pyrolysis of synthetic mixtures of intermediate compounds which may occasionally appear during the industrial process, are given. Thermogravimetric methods of control are suggested, usable in interesting products in the uranium metallurgy. (Author) 20 refs.

  1. INFRARED SPECTRA, THERMOGRAVIMETRIC ANALYSIS AND ...

    African Journals Online (AJOL)

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    2Department of Pesticides Formulation, Central Agricultural Pesticides ... a number of other Fusarium species are able to degrade benzoxazolinone compounds to products which are less inhibitory to fungal growth and also important ...

  2. Thermogravimetric studies of high temperature reactions between potassium salts and chromium

    International Nuclear Information System (INIS)

    Lehmusto, J.; Lindberg, D.; Yrjas, P.; Skrifvars, B.-J.; Hupa, M.

    2012-01-01

    Highlights: ► K 2 CO 3 reacted with Cr 2 O 3 forming K 2 CrO 4 . ► Presence of chlorine did not alone explain the initiation of accelerated oxidation. ► More light was shed to the role of chromates in accelerated oxidation. ► Accelerated oxidation of chromia protected steels occurs in two consecutive stages. ► Both potassium and chloride are required, so that both stages of reaction occur. - Abstract: This study compares the high temperature reactions of potassium chloride (KCl) and potassium carbonate (K 2 CO 3 ), two salts found in fly ashes formed in biomass combustion, with both pure metallic chromium (Cr) and chromium oxide (Cr 2 O 3 ). The reactions were investigated with thermogravimetric measurements and the results discussed based on thermodynamic calculations. In simple terms: potassium chloride reacted with chromium forming potassium chromate (K 2 CrO 4 ) and chromium oxide. Potassium chloride did not react with chromium oxide. Potassium carbonate reacted with chromium oxide, but not with chromium. The presence of potassium is sufficient to initiate accelerated oxidation, but chloride is needed to sustain it.

  3. Thermal decomposition and kinetics of coal and fermented cornstalk using thermogravimetric analysis.

    Science.gov (United States)

    He, Yuyuan; Chang, Chun; Li, Pan; Han, Xiuli; Li, Hongliang; Fang, Shuqi; Chen, Junying; Ma, Xiaojian

    2018-07-01

    The thermal behavior and kinetics of Yiluo coal (YC) and the residues of fermented cornstalk (FC) were investigated in this study. The Kissinger-Akahira-Sunose (KAS) and Flynn-Wall-Ozawa (FWO) methods were used for the kinetic analysis of the pyrolysis process. The results showed that the activation energy (E α ) was increased with the increase of the thermal conversion rate (α), and the average values of E α of YC, FC and the blend (m YC /m FC  = 6/4) were 304.26, 224.94 and 233.46 kJ/mol, respectively. The order reaction model function for the blend was also developed by the master-plots method. By comparing the E a and the enthalpy, it was found that the blend was favored to format activated complex due to the lower potential energy barrier. Meanwhile, the average value of Gibbs free energy of the blend was 169.83 kJ/mol, and the changes of entropies indicated that the pyrolysis process was evolved from ordered-state to disordered-state. Copyright © 2018 Elsevier Ltd. All rights reserved.

  4. Proximate Analysis of Coal

    Science.gov (United States)

    Donahue, Craig J.; Rais, Elizabeth A.

    2009-01-01

    This lab experiment illustrates the use of thermogravimetric analysis (TGA) to perform proximate analysis on a series of coal samples of different rank. Peat and coke are also examined. A total of four exercises are described. These are dry exercises as students interpret previously recorded scans. The weight percent moisture, volatile matter,…

  5. Sedimentation technique of waste bituminization and thermogravimetric characteristics of the final products

    Energy Technology Data Exchange (ETDEWEB)

    Zeger, J; Knotik, K; Jakusch, H

    1976-01-01

    In the research centre of the Oesterreichische Studiengesellschaft fuer Atomenergie GesmbH a semitechnical plant has been installed for waste bituminization, which has been tested inactively since 1973. This plant is using a new technological process for embedding. One of the important features of this new process is that the, normally inactive solution water is distilled off prior to the embedding, resulting in dry and powdery salts. The second important feature is that the mixing of these dry salts with the thin fluid bitumen is done by sedimentation. Expecially there is no mechanical aid used for mixing. Thermogravimetric analysis of samples which simulated the final products of this pilot plant, were carried out to verify the best working parameters and to study the possible chemical damage to the bitumen. Analysis was performed by heating the samples, consisting of various mixtures of bitumen and inorganic salts, in a METTLER-Thermoanalyzer up to 500/sup 0/C using different atmospheres (air, nitrogen). It could be shown that only nitrate and nitrite especially in combination with Fe(III)-ions are of negative influence on the thermostability of bitumen. They lead to a sudden and quick weight loss of the samples between 370 and 410/sup 0/C (above the melting point of both NaNO/sub 2/ and NaNO/sub 3/). The Fe-ions hava a catalytic influence, as it could be shown that 1 1% addiation of Fe(NO/sub 3/)/sub 3/ to NaNO/sub 3/ leads to a considerable acceleration of the incineration. This influence of the Fe(III)-ion can be suppressed to some extend by a hydrolysis prior to the embedding. In preparation of further studies concerning the behaviour of radiation damaged bitumen there has been developed a method of measuring the dose rate of an unknown radioactive salt mixture at any point of this mixture. This is done by making two measurements with glass dosimeters. One with a beta-absorber to get a pure gamma-dose and the other without it to get the combined beta and

  6. Study of Selected Composites Copper Concentrate-Plastic Waste Using Thermal Analysis

    Science.gov (United States)

    Szyszka, Danuta

    2017-12-01

    The paper presents thermal analysis of selected composites (copper concentrate, plastic waste) in two stages. The first stage consisted in thermogravimetric analysis and differential thermal analysis on the applied plastic waste and copper concentrate, and subsequently, a comparative study has been carried out on products obtained, constituting composites of those materials. As a result of analyses, it was found that up to ca. 400 °C composites show high thermal stability, whereas above that temperature, a thermal decomposition of the composite occurs, resulting in emissions of organic compounds, i.e. hydrocarbon compounds and organic oxygenate derivatives.

  7. Differential thermal, Thermogravimetric and X-ray diffraction investigation of hydration phases in cementitious waste form

    International Nuclear Information System (INIS)

    Khalil, M.Y.; Nagy, M.E.; El-Sourougy, M.R.; Zaki, A.A.

    1996-01-01

    Hydration phases of cement determine the final properties of the product. Adding other components to the cement paste may alter the final phases formed and affect properties of the hardened products. In this work ordinary portland cement and/or blast furnace slag cement were hardened with low-or intermediate-level radioactive liquid wastes and different additives. Hydration phases were investigated using differential thermal, thermogravimetric, and X-ray diffraction techniques. Low-and intermediate-level liquid wastes were found not to affect the hydration phases of cement. The addition of inorganic exchangers and latex were found to affect the hydration properties of the cement waste system. This resulted in a reduction of compressive strength. On the contrary, addition of epoxy also affected the hydration causing increase in compressive strength. 10 figs., 2 tabs

  8. Thermogravimetric pyrolysis kinetics of bamboo waste via Asymmetric Double Sigmoidal (Asym2sig) function deconvolution.

    Science.gov (United States)

    Chen, Chuihan; Miao, Wei; Zhou, Cheng; Wu, Hongjuan

    2017-02-01

    Thermogravimetric kinetic of bamboo waste (BW) pyrolysis has been studied using Asymmetric Double Sigmoidal (Asym2sig) function deconvolution. Through deconvolution, BW pyrolytic profiles could be separated into three reactions well, each of which corresponded to pseudo hemicelluloses (P-HC), pseudo cellulose (P-CL), and pseudo lignin (P-LG) decomposition. Based on Friedman method, apparent activation energy of P-HC, P-CL, P-LG was found to be 175.6kJ/mol, 199.7kJ/mol, and 158.4kJ/mol, respectively. Energy compensation effects (lnk 0, z vs. E z ) of pseudo components were in well linearity, from which pre-exponential factors (k 0 ) were determined as 6.22E+11s -1 (P-HC), 4.50E+14s -1 (P-CL) and 1.3E+10s -1 (P-LG). Integral master-plots results showed pyrolytic mechanism of P-HC, P-CL, and P-LG was reaction order of f(α)=(1-α) 2 , f(α)=1-α and f(α)=(1-α) n (n=6-8), respectively. Mechanism of P-HC and P-CL could be further reconstructed to n-th order Avrami-Erofeyev model of f(α)=0.62(1-α)[-ln(1-α)] -0.61 (n=0.62) and f(α)=1.08(1-α)[-ln(1-α)] 0.074 (n=1.08). Two-steps reaction was more suitable for P-LG pyrolysis. Copyright © 2016 Elsevier Ltd. All rights reserved.

  9. ROCKS & MINERALS DETERMINATION AND ANALYSIS

    Institute of Scientific and Technical Information of China (English)

    2015-01-01

    20150204 Abaydulla Alimjan(Department of Chemistry and Environmental Sciences,Kashgar Teachers College,Kashgar 844006,China);Cheng Chunying Non-Metallic Element Composition Analysis of Non-Ferrous Metal Ores from Oytagh Town,Xinjiang(Rock and Mineral Analysis,ISSN0254-5357,CN11-2131/TD,33(1),2014,p.44-50,5illus.,4tables,28refs.)Key words:nonferrous metals ore,nonmetals,chemical analysis,thermogravimetric analysis Anions in non-ferrous ore materials

  10. Kinetics of devolatilisation of forestry wastes from thermogravimetric analysis

    Energy Technology Data Exchange (ETDEWEB)

    Lapuerta, M.; Hernandez, J.J. [Universidad de Castilla-La Mancha, Ciudad real (Spain). Escuela Tecnica Superior de Ingenieros Industriales; Rodriguez, J.J. [Repsol-YPF, Puertollano (Spain). Chemical Department

    2004-10-01

    The great potential of Maritime pine (Pinus pinaster) wastes in the middle regions of Spain has motivated an increasing interest about the energy use of this material, either through combustion or gasification processes. Samples of these biomass wastes have been analysed by thermogravimetry under both inert and oxidant atmospheres, from room temperature up to 1100 K, at different heating rates: 10, 30, 40, 50 and 60 K min{sup -1}. An estimation of the proximate analysis of the samples was made from combination of both resulting weight loss curves. The devolatilisation process of the samples was divided into three non-interacting mass-loss events described as parallel first-order reactions, being the first event identified as the moisture loss process, the second one as the hemicellulose and cellulose decomposition process and the third one as that of lignin decomposition. A fitting algorithm to obtain the kinetic parameters permitted a good agreement with experimental results, as well as a good discrimination of the effect of the heating rate. Due to the non-homogeneous nature of the tested samples, the use of other conventional methods for obtaining the kinetic parameters has been proved to be inadequate. (author)

  11. A preliminary high-pressure thermogravimetric study of combustion reactivity of a Collie coal char

    Energy Technology Data Exchange (ETDEWEB)

    Chan, Yii Leng; Zhang, Zhezi; Zhu, Mingming; Zhang, Dongke [Western Australia Univ., Crawley, WA (Australia). Centre for Energy (M473); Luan, Chao [Western Australia Univ., Crawley, WA (Australia). Centre for Energy (M473); Tsinghua Univ., Beijing (China). Inst. of Thermal Engineering; You, Changfu [Tsinghua Univ., Beijing (China). Inst. of Thermal Engineering

    2013-07-01

    The effect of pressure(up to 20 bar)on the reactivity of a char(150-160 {mu}m) produced from Western Australian Collie coal has been studied using a high-pressure thermogravimetric analyser (HP TGA). The pressure demonstrated a positive effect in enhancing char combustion reactivities.Kinetic parameters have been determined from the experimental data.The apparent reaction order was found to be approximately 0.7 and the apparent activation energies were 91.0 kJ/mol at atmospheric pressure and 1.5 kJ/mol at an elevated pressure(10 bar),indicating a shift in the control regimes of the reaction at elevated pressures.The lumped effect of the sample size, bulk diffusion,interparticle and intraparticle diffusion at the elevated pressures played an important role in reducing the mass transfer during the HP-TGA experimentation.Thus the activation energy calculated at elevated pressures may not represent the intrinsic activation energy of the char particles but the apparent values of the bulk of the samples.

  12. Importance Performance Analysis as a Trade Show Performance Evaluation and Benchmarking Tool

    OpenAIRE

    Tafesse, Wondwesen; Skallerud, Kåre; Korneliussen, Tor

    2010-01-01

    Author's accepted version (post-print). The purpose of this study is to introduce importance performance analysis as a trade show performance evaluation and benchmarking tool. Importance performance analysis considers exhibitors’ performance expectation and perceived performance in unison to evaluate and benchmark trade show performance. The present study uses data obtained from exhibitors of an international trade show to demonstrate how importance performance analysis can be used to eval...

  13. Thermogravimetric analysis of multi-stage hydropyrolysis of different coals

    Energy Technology Data Exchange (ETDEWEB)

    Li, W.; Wang, N.; Li, B [Chinese Academy of Sciences, Taiyuan (China). State Key Lab. of Coal Conversion

    2001-09-01

    Based on the characteristic of hydropyrolysis (HyPy), a multi-stage MHyPy of different coals was investigated using thermogravimetry. The results show that keeping the near peak temperature for some time in HyPy process can obviously increase the conversion rate, which is believed due to the full match between formation rate of free radicals and supply of hydrogen. The fast heating in MHyPy process results in the same conversion rate as that of the slow heating in HyPy process, which leads to the less reaction time and high yield of oil. The effect of MHyPy depends on the coal structure itself and it is notable for the coal with high H/C ratio. This suggests that the external hydrogen promotes the reaction between intrinsic hydrogen and free radicals. The MHyPy improves the removal of sulfur and nitrogen. 5 refs., 7 figs., 2 tabs.

  14. Sedimentation technique of waste bituminization and thermogravimetric characteristics of the final products

    International Nuclear Information System (INIS)

    Zeger, J.; Knotik, K.; Jakusch, H.

    1976-01-01

    In the research centre of the Oesterreichische Studiengesellschaft fuer Atomenergie GmbH a semi-technical plant has been installed for waste bituminization, which has been tested inactively since 1973. This plant uses a new technological process for embedding. One of the important features of this new process is that the solution water, which is normally inactive, is distilled off before embedding, resulting in dry and powdery salts. The second important feature is that these dry salts are mixed with the thin fluid bitumen by sedimentation. A special feature is that there is no mechanical aid used for mixing. Thermogravimetric analysis of samples which simulated the final products of this pilot plant was carried out to verify the best working parameters and to study the possible chemical damage to the bitumen. It was shown that only nitrate and nitrite, especially in combination with Fe(III)-ions, are of negative influence on the thermostability of bitumen. They lead to a sudden and quick weight loss of the samples between 370 and 410 0 C (above the melting point of both NaNO 2 and NaNO 3 ). The Fe-ions have a catalytic influence, as it could be shown that a 1% addition of Fe(NO 3 ) 3 to NaNO 3 leads to a considerable acceleration of the incineration. This influence of the Fe(III)-ion can be suppressed to some extent by a hydrolysis before the embedding. There is, however, no danger to the embedding process from these effects since the process temperature of maximum 200 0 C is well below the ignition temperatures. A method of measuring the dose rate of an unknown radioactive salt mixture at any point of this mixture has been developed. This is done by making two measurements with glass dose-meters, one with a beta-absorber to get a pure gamma dose and the other without it to get the combined beta and gamma dose. During the first measurement the dose-meters were protected against contamination by a thin layer of rubber

  15. An Integrated Approach to Thermal Analysis of Pharmaceutical Solids

    Science.gov (United States)

    Riley, Shelley R. Rabel

    2015-01-01

    A three-tiered experiment for undergraduate Instrumental Analysis students is presented in which students characterize the solid-state thermal behavior of an active pharmaceutical ingredient (acetaminophen) and excipient (a-lactose hydrate) using differential scanning calorimetry, thermogravimetric analysis, and thermal microscopy. Students are…

  16. Molten salt corrosion behavior of structural materials in LiCl-KCl-UCl3 by thermogravimetric study

    Science.gov (United States)

    Rao, Ch Jagadeeswara; Ningshen, S.; Mallika, C.; Mudali, U. Kamachi

    2018-04-01

    The corrosion resistance of structural materials has been recognized as a key issue in the various unit operations such as salt purification, electrorefining, cathode processing and injection casting in the pyrochemical reprocessing of spent metallic nuclear fuels. In the present work, the corrosion behavior of the candidate materials of stainless steel (SS) 410, 2.25Cr-1Mo and 9Cr-1Mo steels was investigated in molten LiCl-KCl-UCl3 salt by thermogravimetric analysis under inert and reactive atmospheres at 500 and 600 °C, for 6 h duration. Insignificant weight gain (less than 1 mg/cm2) in the inert atmosphere and marginal weight gain (maximum 5 mg/cm2) in the reactive atmosphere were observed at both the temperatures. Chromium depletion rates and formation of Cr-rich corrosion products increased with increasing temperature of exposure in both inert and reactive atmospheres as evidenced by SEM and EDS analysis. The corrosion attack by LiCl-KCl-UCl3 molten salt, under reactive atmosphere for 6 h duration was more in the case of SS410 than 9Cr-1Mo steel followed by 2.25Cr-1Mo steel at 500 °C and the corrosion attack at 600 °C followed the order: 9Cr-1Mo steel >2.25Cr-1Mo steel > SS410. Outward diffusion of the minor alloying element, Mo was observed in 9Cr-1Mo and 2.25Cr-1Mo steels at both temperatures under reactive atmosphere. Laser Raman spectral analysis of the molten salt corrosion tested alloys under a reactive atmosphere at 500 and 600 °C for 6 h revealed the formation of unprotected Fe3O4 and α-as well as γ-Fe2O3. The results of the present study facilitate the selection of structural materials for applications in the corrosive molten salt environment at high temperatures.

  17. Thermogravimetric analysis of combustible waste components

    DEFF Research Database (Denmark)

    Munther, Anette; Wu, Hao; Glarborg, Peter

    In order to gain fundamental knowledge about the co-combustion of coal and waste derived fuels, the pyrolytic behaviors of coal, four typical waste components and their mixtures have been studied by a simultaneous thermal analyzer (STA). The investigated waste components were wood, paper, polypro......In order to gain fundamental knowledge about the co-combustion of coal and waste derived fuels, the pyrolytic behaviors of coal, four typical waste components and their mixtures have been studied by a simultaneous thermal analyzer (STA). The investigated waste components were wood, paper...

  18. Thermal analysis of RFETS SS and C

    International Nuclear Information System (INIS)

    Korinko, P.S.

    2000-01-01

    In support of the gas generation test program (GGTP) for the 9975 shipping container, thermogravimetric analysis (TGA) was conducted. The objective of this activity was to determine the moisture content as an input to the gas generation model

  19. Thermogravimetric, Calorimetric, and Structural Studies of the Co3 O4 /CoO Oxidation/Reduction Reaction

    Science.gov (United States)

    Unruh, Karl; Cichocki, Ronald; Kelly, Brian; Poirier, Gerald

    2015-03-01

    To better assess the potential of cobalt oxide for thermal energy storage (TES), the Co3O4/CoO oxidation/reduction reaction has been studied by thermogravimetric (TGA), calorimetric (DSC), and x-ray diffraction (XRD) measurements in N2 and atmospheric air environments. TGA measurements showed an abrupt mass loss of about 6.6% in both N2 and air, consistent with the stoichiometric reduction of Co3O4 to CoO and structural measurements. The onset temperature of the reduction of Co3O4 in air was only weakly dependent on the sample heating rate and occurred at about 910 °C. The onset temperature for the oxidation of CoO varied between about 850 and 875 °C for cooling rates between 1 and 20 °C/min, but complete re-conversion to Co3O4 could only be achieved at the slowest cooling rates. Due to the dependence of the rate constant on the oxygen partial pressure, the oxidation of Co3O4 in a N2 environment occurred at temperatures between about 775 and 825 °C for heating rates between 1 and 20 °C/min and no subsequent re-oxidation of the reduced Co3O4 was observed on cooling to room temperature. In conjunction with a measured transition heat of about 600 J/g of Co3O4, these measurements indicate that cobalt oxide is a viable TES material.

  20. Thermal analysis of kieselguhr sludge

    Directory of Open Access Journals (Sweden)

    S. T. Antipov

    2013-01-01

    Full Text Available It’s currently necessary to clarify the mechanisms of thermodynamic and mass transfer processes in capillary porous media. In this paper we obtain the thermogravimetric curves of evaporation drying kieselguhr sludge. It is also an analysis of the curves, allowing to choose the optimum conditions of drying.

  1. Offgas Analysis and Pyrolysis Mechanism of Activated Carbon from Bamboo Sawdust by Chemical Activation With KOH

    Institute of Scientific and Technical Information of China (English)

    TIAN Yong; LIU Ping; WANG Xiufang; ZHONG Guoying; CHEN Guanke

    2011-01-01

    Bamboo sawdust was used as the precursor for the multipurpose use of waste.Offgases released during the activation process of bamboo by KOH were investigated quantitatively and qualitatively by a gas analyzer. TG/DTG curves during the pyrolysis process with different impregnation weight ratios (KOH to bamboo) were obtained by a thermogravimetric analyzer. Pyrolysis mechanism of bamboo was proposed. The results showed that the offgases were composed of CO, NO,SO2 and hydrocarbon with the concentration of 1 372, 37, 86, 215 mg/L, respectively. Thermogravimetric analysis indicated that the pyrolytic process mainly experienced two steps. The first was the low temperature activation step (lower than 300 ℃), which was the pre-activation and induction period.The second was the high temperature activation step(higher than 550 ℃), which was a radial activation followed by pore production. The second process was the key to control the pore distribution of the final product.

  2. Biological CO2 fixation using Chlorella vulgaris and its thermal characteristics through thermogravimetric analysis.

    Science.gov (United States)

    Razzak, Shaikh A; Ali, Saad Aldin M; Hossain, Mohammad M; Mouanda, Alexis Nzila

    2016-11-01

    The present research is focused on cultivation of microalgae strain Chlorella vulgaris for bio-fixation of CO2 coupled with biomass production. In this regard, a single semi-batch vertical tubular photobioreactor and four similar photobioreactors in series have been employed. The concentration of CO2 in the feed stream was varied from 2 to 12 % (v/v) by adjusting CO2 to air ratio. The amount of CO2 capture and algae growth were monitored by measuring decrease of CO2 concentration in the gas phase, microalgal cell density, and algal biomass production rate. The results show that 4 % CO2 gives maximum amount of biomass (0.9 g L(-1)) and productivity (0.118 g L(-1) day(-1)) of C. vulgaris in a single reactor. In series reactors, average productivity per reactor found to be 0.078 g L(-1) day(-1). The maximum CO2 uptake for single reactor also found with 4 % CO2, and it is around 0.2 g L(-1) day(-1). In series reactors, average CO2 uptake is 0.13 g L(-1) day(-1) per reactor. TOC analysis shows that the carbon content of the produced biomass is around 40.67 % of total weight. The thermochemical characteristics of the cultivated C. vulgaris samples were analyzed in the presence of air. All samples burn above 200 °C and the combustion rate become faster at around 600 °C. Almost 98 wt% of the produced biomass is combustible in this range.

  3. Thermogravimetric method of estimation of uranyl cation state in melts of alkali metal chlorides and their mixtures

    International Nuclear Information System (INIS)

    Vorobej, M.P.; Desyatnik, V.N.

    1979-01-01

    The thermogravimetric method was used to study the chloridizing of uranium oxides in molten media. The study of the uranium oxide chloridizing served as a basis for evaluating comparatively, using the DTA method, the uranyl-cation state in a melt. Using the alkali metals as example, it was shown that the decomposition of the frozen uranium oxychlorides proceeds with the formation of intermediate chlorouranates. The final product of the thermolysis are uranates Me 2 U 2 O 7 (Me-Li, Na, K, Rb, Cs). The time and the conditions of the change of uranium oxides to the oxyanion [UO 2 Cl 4 ] 2- were determined as a function of the chloridizing agent. The method can be employed for evaluating uranyl-ions in molten media where they are used as electrolytes in the extraction of uranium dioxide

  4. Thermal analysis of physical and chemical changes occuring during regeneration of activated carbon

    Directory of Open Access Journals (Sweden)

    Radić Dejan B.

    2017-01-01

    Full Text Available High-temperature thermal process is a commercial way of regeneration of spent granular activated carbon. The paper presents results of thermal analysis conducted in order to examine high-temperature regeneration of spent activated carbon, produced from coconut shells, previously used in drinking water treatment. Results of performed thermogravimetric analysis, derivative thermogravimetric analysis, and differential thermal analysis, enabled a number of hypotheses to be made about different phases of activated carbon regeneration, values of characteristic parameters during particular process phases, as well as catalytic impact of inorganic materials on development of regeneration process. Samples of activated carbon were heated up to 1000°C in thermogravimetric analyser while maintaining adequate oxidizing or reducing conditions. Based on diagrams of thermal analysis for samples of spent activated carbon, temperature intervals of the first intense mass change phase (180-215°C, maximum of exothermic processes (400-450°C, beginning of the second intense mass change phase (635-700°C, and maximum endothermic processes (800-815°C were deter-mined. Analysing and comparing the diagrams of thermal analysis for new, previously regenerated and spent activated carbon, hypothesis about physical and chemical transformations of organic and inorganic adsorbate in spent activated carbon are given. Transformation of an organic adsorbate in the pores of activated carbon, results in loss of mass and an exothermic reaction with oxygen in the vapour phase. The reactions of inorganic adsorbate also result the loss of mass of activated carbon during its heating and endothermic reactions of their degradation at high temperatures.

  5. The oxygen potential of near- and non-stoichiometric urania-25 mol% plutonia solid solutions: a comparison of thermogravimetric and galavanic cell measurements

    International Nuclear Information System (INIS)

    Woodley, R.E.; Adamson, M.G.

    1979-01-01

    To resolve discrepancies between the existing low temperature ΔGsub(0 2 )(mean) data for solid solution mixed (U, Pu)-oxide nuclear fuel material, additional measurements have been performed on Usub(0.75)Pusub(0.25) employing a combined thermogravimetric (TGA) and solid-electrolyte galvanic cell technique. These measurements, which were performed at temperatures between 800 and 1000 0 C, and for O:M ratios in the range 1.940 to 2.028, are reasonably self-consistent and show good agreement with the results of previous TGA measurements. However, they do not corroborate the earlier EMF cell measurements of Markin and McIver. (1967). Possible explanations for errors in these earlier EMF cell results are examined. The new results indicate that the ΔGsub(O 2 )(mean) of stoichiometric mixed oxide at typical outer surface fuel temperature is close to -100 kcal/mol 0 2 (-419 kJ/mol O 2 ). Attempts have been made to fit the new ΔGsub(O 2 )(mean) data to two equations derived from recent defect models, and it is shown that neither equation accurately represents the experimental psub(O 2 ) - x data over more than a short range of x. (Auth.)

  6. Combustion of Sewage Sludge as Alternative Fuel for Cement Industry

    Institute of Scientific and Technical Information of China (English)

    LI Fuzhou; ZHANG Wei

    2011-01-01

    The combustion of sewage sludge and coal was studied by thermogravimetric analysis.Both differential scanning calorimetric analysis and derivative thermogravimetric profiles showed differences between combustion of sewage sludge and coal, and non-isothermal kinetics analysis method was applied to evaluate the combustion process. Based on Coats-Redfem integral method, some reaction models were tested,the mechanism and kinetics of the combustion reaction were discussed. The results show that the combustion of sewage sludge is mainly in the Iow temperature stage, meanwhile the ignition temperature and Arrhenius activation energy are lower than that of coal. The combustion of sewage sludge has the advantage over coal in some aspects, thus sewage sludge can partly replace coal used as cement industry fuel.

  7. Vaporization enthalpies of imidazolium based ionic liquids. A thermogravimetric study of the alkyl chain length dependence

    International Nuclear Information System (INIS)

    Verevkin, Sergey P.; Zaitsau, Dzmitry H.; Emel’yanenko, Vladimir N.; Ralys, Ricardas V.; Yermalayeu, Andrei V.; Schick, Christoph

    2012-01-01

    Highlights: ► Enthalpies of vaporization of ionic liquids were measured with thermogravimetry. ► We studied 1-alkyl-3-methyl-imidazolium bis(trifluoromethanesulfonyl)imide. ► The linear alkyl chain length was 4, 6, 8, 10, 12, 14, 16, and 18 C-atoms. ► A linear dependence on the chain length of the alkyl-imidazolium cation was found. - Abstract: Vaporization enthalpies for a series of ten ionic liquids (ILs) 1-alkyl-3-methyl-imidazolium bis(trifluoromethanesulfonyl)imide [C n mim][NTf 2 ], with the alkyl chain length n = 4, 6, 8, 10, 12, 14, 16, and 18 were determined using the thermogravimetric method. An internally consistent set of experimental data and vaporization enthalpies at 540 K was obtained. Vaporization enthalpies at 540 K have shown a linear dependence on the chain length of the alkyl-imidazolium cation in agreement with the experimental results measured previously with a quartz crystal microbalance. Ambiguity of Δ l g C pm o -values required for the extrapolation of experimental vaporization enthalpies to the reference temperature 298 K has been discussed.

  8. Effect of biopretreatment on thermogravimetric and chemical characteristics of corn stover by different white-rot fungi.

    Science.gov (United States)

    Yang, Xuewei; Zeng, Yelin; Ma, Fuying; Zhang, Xiaoyu; Yu, Hongbo

    2010-07-01

    The thermogravimetric and chemical characterization of corn stover biopretreated by three different species of white-rot fungi have been studied in this research. Results indicated that biopretreatment can optimize the thermal decomposition, decrease the reaction temperature and reduce the gas contamination (SO(x)), making the biomass pyrolysis more efficient and environmentally friendly. Biopretreatment can decrease the activation energy and reacting temperature of the hemicellulose and cellulose pyrolysis (up to 36 degrees C), shorten the temperature range of the active pyrolysis (up to 14 degrees C), and increase the thermal decomposition rate, greatly promoting the reaction and making the biomass pyrolysis easier to start and carry on. On the other hand, by biopretreatment, the sulphur content can decrease up to 46.15%, which can considerably reduce the inventory of SO(x) emission. Moreover, the mechanism of the biopretreatment was also explored that the deconstruction and depolymerization of the recalcitrant linkages of lignin and cellulose by biopretreatment can make the structure of biomass incompact and easier to be pyrolyzed. Copyright (c) 2010 Elsevier Ltd. All rights reserved.

  9. Effect of biodegradation on thermogravimetric and chemical characteristics of hardwood and softwood by brown-rot fungus.

    Science.gov (United States)

    Gao, Zhenzhong; Fan, Qi; He, Zesen; Wang, Zhinan; Wang, Xiaobo; Sun, Jin

    2016-07-01

    The thermogravimetric and chemical characterization of hardwood Eucalyptus urophylla (Ep) and softwood Pinus massoniana (Mp) pretreated by brown-rot fungus Gloeophyllum trabeum were investigated. The results indicated that the brown-rot fungus pretreatment can optimize the thermal decomposition and decrease the initiation temperatures (8-11°C lower) of both the Ep and Mp pyrolysis. The mean activation energy values of the bio-treated samples were 29.7kJ/mol (for Ep) and 42.3kJ/mol (for Mp) lower than that of the un-treated samples at the conversion rate from 0.1 to 0.7 based on Flynn-Wall-Ozawa (FWO) method. After the bio-pretreatment, the required temperatures were lower (4-7°C) for the pyrolysis rates of hemicellulose and cellulose in Mp reaching maximum and termination. However, the situation was just the opposite for Ep. The variations in chemical properties of hydrogen bonding, as well as the relative changes in lignin/carbohydrate composition of both wood species were also examined. Copyright © 2016 Elsevier Ltd. All rights reserved.

  10. Análise termogravimétrica do óleo essencial de pimenta longa (Piper hispidinervium C. DC Thermogravimetric analysis of long pepper (Piper hispidinervium C.DC. essential oil

    Directory of Open Access Journals (Sweden)

    Marco Aurelio Cremasco

    2011-01-01

    Full Text Available A pimenta longa (Piper hispidinervium C. DC. é um arbusto originário da região amazônica, cujo óleo essencial é rico em safrol. O óleo essencial da pimenta longa é comercializado in natura, o que faz o processamento para a obtenção do safrol elemento fundamental de investigação científica e tecnológica. Uma importante etapa para a obtenção do safrol é a definição da estratégia da sua separação do óleo essencial a partir, por exemplo, da destilação. Neste caso, torna-se essencial o conhecimento de parâmetros termodinâmicos, tais como energia de ativação e calor latente de vaporização. Neste trabalho é utilizada a técnica termogravimétrica para a obtenção dos valores da energia de ativação e calor latente de vaporização do óleo essencial de P. hispidinervium. O processo de evaporação do óleo essencial obedece à cinética de ordem zero, resultando para a energia de ativação e calor latente de vaporização os valores 42,11 kJ.mol-1 e 43,73 kJ.mol-1, respectivamente.Long pepper (Piper hispidinervium C. DC. is a shrub found in the Amazon region, which supplies an essential oil rich in safrole. Normally, long pepper essential oil is commercialized in natura, which makes its processing a fundamental step in scientific and technological investigation. An important step of safrole commercialization is the separation of essential oil by, for example, a distillation process. In such a case it is important to know some thermodynamics parameters, such as energy of activation and enthalpy of vaporization. The present study was aimed at applying the kinetic of zero order evaporation process for the essential oil of P. hispidinervum by thermogravimetric analysis. The thermal analysis data were utilized to determine the energy of activation and enthalpy of vaporization, which resulted in the values 41.11 kJ.mol-1 and 43.73 kJ.mol-1, respectively.

  11. Synthesis and Characterization of Magnesium Substituted Aluminophosphate Molecular Sieves with AEL Structure

    Institute of Scientific and Technical Information of China (English)

    Benjing Xu; Ling Qian; Xinmei Liu; Chunmin Song; Zifeng Yan

    2004-01-01

    MAPO-11 molecular sieves were synthesized by hydrothermal methods. The influence of precursor of magnesium, Mg/Al ratio, synthesis temperature, synthesis time and the type of template on the formation and properties of MAPO-11 molecular sieves was examined. The samples were characterized by the techniques of X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric/differential thermogravimetric analysis (TG-DGA), etc. The results show that the shape and size of crystal were influenced by the precursor of Mg, the Mg/Al ratio and the type of template, and the TG-DGA analysis shows that MAPO-11 molecular sieves as-synthesized have poor thermal stability.

  12. Development and in house validation of a new thermogravimetric method for water content analysis in soft brown sugar.

    Science.gov (United States)

    Ducat, Giseli; Felsner, Maria L; da Costa Neto, Pedro R; Quináia, Sueli P

    2015-06-15

    Recently the use of brown sugar has increased due to its nutritional characteristics, thus requiring a more rigid quality control. The development of a method for water content analysis in soft brown sugar is carried out for the first time by TG/DTA with application of different statistical tests. The results of the optimization study suggest that heating rates of 5°C min(-1) and an alumina sample holder improve the efficiency of the drying process. The validation study showed that thermo gravimetry presents good accuracy and precision for water content analysis in soft brown sugar samples. This technique offers advantages over other analytical methods as it does not use toxic and costly reagents or solvents, it does not need any sample preparation, and it allows the identification of the temperature at which water is completely eliminated in relation to other volatile degradation products. This is an important advantage over the official method (loss on drying). Copyright © 2015 Elsevier Ltd. All rights reserved.

  13. Thermogravimetric measurement of hydrogen storage in carbon-based materials: promise and pitfalls

    International Nuclear Information System (INIS)

    Pinkerton, F.E.; Wicke, B.G.; Olk, C.H.; Tibbetts, G.G.; Meisner, G.P.; Meyer, M.S.; Herbst, J.F.

    2000-01-01

    We have used a thermogravimetric analyzer (TGA) to measure the hydrogen absorption capacity of a variety of carbon-based storage materials, including Li- and K-intercalated graphite and Li-doped multi-wall nanotubes. The TGA uses weight gain/loss as a function of time and temperature to monitor hydrogen absorption/desorption in flowing hydrogen gas. Creating and maintaining a contaminant-free atmosphere is critical to the accurate TGA measurement of hydrogen absorption in carbon-based materials; even low concentrations of impurity gases such as O 2 or H 2 O are sufficient to masquerade as hydrogen absorption. We will discuss examples of this effect relevant to recent reports of hydrogen storage appearing in the literature. The precautions required are non-trivial. In our TGA, for instance, about 16% of the original atmosphere remains after a two-hour purge; at least 15 hours is required to fully purge the apparatus. Furthermore, we cover the TGA with a protective atmosphere enclosure during sample loading to minimize the introduction of impurity gases. With these precautions it is possible to unambiguously measure hydrogen storage. For example, we have determined the hydrogen absorption capacity of our K-intercalated graphite samples to be 1.3 wt% total hydrogen absorption above 50 o C, of which 0.2 wt% can be reproducibly recovered with temperature cycling. With due care, TGA measurements provide complementary information to that obtained from standard pressure techniques for measuring hydrogen sorption, which rely on measuring the loss of gas pressure in a known volume. Taken together, TGA and pressure measurements provide a powerful combination for determining verifiable hydrogen storage capacity. (author)

  14. Synthesis of lithium-manganese-oxide spinels: A study by thermal analysis

    CSIR Research Space (South Africa)

    Thackeray, MM

    1994-12-01

    Full Text Available The synthesis of lithium-manganese-oxide spinels by reaction of Li2CO3 and MnCO3 in air and under nitrogen to T(max) = 600°C has been investigated by thermogravimetric analysis and differential scanning calorimetry. When the reaction is conducted...

  15. A Combined Variable-Temperature Neutron Diffraction and Thermogravimetric Analysis Study on a Promising Oxygen Electrode, SrCo0.9Nb0.1O3-δ, for Reversible Solid Oxide Fuel Cells.

    Science.gov (United States)

    Yang, Tianrang; Wang, Jie; Chen, Yan; An, Ke; Ma, Dong; Vogt, Thomas; Huang, Kevin

    2017-10-11

    The present study investigates the temperature-structure-stoichiometry relationship of a promising oxygen electrode SrCo 0.9 Nb 0.1 O 3-δ over a temperature (T) range from room temperature (RT) to 900 °C. The techniques employed are variable-temperature neutron diffraction (VTND) and thermogravimetric analysis (TGA). At T < 75 °C, VTND reveals a tetragonal (P4/mmm) structure with a G-type magnetic ordering. Above 75 °C, the nucleus structure remains the same, while the magnetic ordering disappears. A phase transition from tetragonal (P4/mmm) to cubic (Pm3̅m) is observed at 412 °C, where the two Co sites and three O sites in the P4/mmm phase converge to one equivalent site, respectively. The phase transition temperature coincides with the peak temperature of oxygen uptake obtained by TGA. It is also observed that the Nb dopant has no preferred Co site to occupy. The oxygen vacancies are mostly located at the O3 site surrounding the Co2 site in the P4/mmm structure. The intermediate-spin state of Co 3+ at the Co2 site is responsible for the observed distortions of CoO 6 octahedra, i.e., elongation of Co2O 6 octahedra and shortening of Co1O 6 octahedra along the c-axis, which is a phenomenon known as Jahn-Teller distortion. At high temperatures, large thermal displacement factor for O 2- is observed with high concentration of oxygen vacancies, providing a structural environment favorable to high O 2- conductivity in Nb-doped SrCoO 3 -based oxygen electrode materials.

  16. Fat stigmatization in television shows and movies: a content analysis.

    Science.gov (United States)

    Himes, Susan M; Thompson, J Kevin

    2007-03-01

    To examine the phenomenon of fat stigmatization messages presented in television shows and movies, a content analysis was used to quantify and categorize fat-specific commentary and humor. Fat stigmatization vignettes were identified using a targeted sampling procedure, and 135 scenes were excised from movies and television shows. The material was coded by trained raters. Reliability indices were uniformly high for the seven categories (percentage agreement ranged from 0.90 to 0.98; kappas ranged from 0.66 to 0.94). Results indicated that fat stigmatization commentary and fat humor were often verbal, directed toward another person, and often presented directly in the presence of the overweight target. Results also indicated that male characters were three times more likely to engage in fat stigmatization commentary or fat humor than female characters. To our knowledge, these findings provide the first information regarding the specific gender, age, and types of fat stigmatization that occur frequently in movies and television shows. The stimuli should prove useful in future research examining the role of individual difference factors (e.g., BMI) in the reaction to viewing such vignettes.

  17. Effect of humidity on the hydration behaviour of prazosin hydrochloride polyhydrate: Thermal, sorption and crystallographic study

    International Nuclear Information System (INIS)

    Kumar, Lokesh; Bansal, Arvind K.

    2011-01-01

    Highlights: → Utility of TGA to differentiate between unbound and bound water was demonstrated. → Nature of the lattice arrangement in prazosin hydrochloride polyhydrate was confirmed to be expanded (non-stoichiometric) type hydrate. → Correlation of the DSC, TGA, PXRD and DVS for dehydration of prazosin hydrochloride polyhydrate was delineated. - Abstract: In this study, hydration behaviour of prazosin hydrochloride polyhydrate was assessed using differential scanning calorimetry, thermogravimetric analysis, powder X-ray diffraction and dynamic vapour sorption techniques. Differential scanning calorimetry and thermogravimetric analysis at faster heating rate (20 o C/min) showed single step water loss, attributed to both dihydrate and unbound water. In contrast, thermogravimetric analysis at slower heating rate (1 o C/min) showed unbound and dihydrate lattice water separately, with unbound water being lost initially, followed by loss of dihydrate water. Variable vacuum and variable humidity PXRD study revealed shift in diffraction peaks to higher values on removal of unbound water. Initial PXRD patterns were regained when kept again at ambient conditions. Dynamic vapour sorption depicted type I sorption isotherm with interstitial water, indicating that polyhydrate form show reversible behaviour with change in humidity. Correlation between thermal, sorption and crystallographic data established hydration behaviour to be characteristic of expanded channel type (non-stoichiometric) hydrate.

  18. Preparation of self-supporting molecularly imprinted films via transition layer construction and RAFT polymerization, and their use in HPLC

    International Nuclear Information System (INIS)

    Ding, Peng; Tang, Shengfu; Shi, Liyi; Li, Zongzhou; Song, Na

    2013-01-01

    Molecularly imprinted films with self-supporting property (SS-MIFs) have been prepared by using the strategy of transition layer construction followed by reversible addition-fragmentation chain transfer (RAFT) polymerization. The structure, composition and selectivity of the SS-MIFs as well as the mechanism of mass transfer were characterized by scanning electron microscopy, X-ray diffraction, Fourier transform IR spectrometry, specific surface area analysis, thermogravimetric analysis, and HPLC. Surface area analysis showed the samples possessed specific surface areas as high as 80.5 m 2 .g −1 . This is almost 9 times more than that of the original porous anodic aluminum oxide substrate. Thermogravimetric analysis also showed the samples to be thermally stable up to 350 °C. The separating power was investigated by HPLC and revealed a selective separation effect for the target molecules theobromine. The separation factor is 5.37. (author)

  19. Purification of bentonite clays from the district of Cubati, PB, for other uses

    International Nuclear Information System (INIS)

    Costa, M.R.; Araujo, J.P.; Silva, I.A.; Cardoso, M.A.; Silva, C.D.; Neves, G.A.; Ferreira, H.C.

    2012-01-01

    The state of Paraiba is responsible for the increased production of crude bentonite in the country, coming from one of the largest mines of Brazil, located in Boa Vista, PB. Recently, in the regions of Cubati and Pedra Lavrada, PB, found new deposits of bentonite that could expand the state reserves. The paper aims at the characterization and development of clay purified using the techniques of screening and hydrocycloning, from bentonite clay recently discovered in the city of Cubati, PB, for various uses. The sample characterization was performed through techniques: granulometric analysis by laser diffraction, X-ray diffraction and chemical analysis by X-ray fluorescence and thermogravimetric and differential thermogravimetric analysis. The results showed that the samples are typical of bentonite clay, and that the purification process using only the hydrocycloning shows better results. (author)

  20. Synthesis of a Biglucoside and Its Application as Montmorillonite Hydration Inhibitor

    Directory of Open Access Journals (Sweden)

    Xin-chun Zhang

    2014-01-01

    Full Text Available A biglucoside (BG was synthesized with glucose and epichlorohydrin as raw materials. The inhibition of BG against montmorillonite swelling was investigated by various methods including montmorillonite linear expansion test, mud ball immersing test, thermogravimetric analysis, and scanning electron microscopy. The results show that the BG has good inhibition ability to the hydration swelling and dispersion of montmorillonite. Under the same condition, the linear expansion ratio of montmorillonite in BG solution is much lower than that of MEG. The particle distribution measurement, thermogravimetric analysis, FT-IR, and scanning electron microscopy results all prove the efficient inhibition of BG.

  1. Analysis Of The Reactivity Of Radpro Solution With Cotton Rags

    International Nuclear Information System (INIS)

    Marusich, R.M.

    2009-01-01

    Rags containing RadPro(reg s ign) solution will be generated during the decontamination of the Plutonium Finishing Plant (PFP). Under normal conditions, the rags will be neutralized with sodium carbonate prior to placing in the drums. The concern with RadPro solutions and cotton rags is that some of the RadPro solutions contain nitric acid. Under the right conditions, nitric acid and cotton rags exothermically react. The concern is, will RadPro solutions react with cotton rags exothermically? The potential for a runaway reaction for any of the RadPro solutions used was studied in Section 5.2 of PNNL-15410, Thermal Stability Studies of Candidate Decontamination Agents for Hanford's Plutonium Finishing Plant Plutonium-Contaminated Gloveboxes. This report shows the thermal behavior of cotton rags having been saturated in one of the various neutralized and non-neutralized RadPro solutions. The thermal analysis was performed using thermogravimetric Analysis (TGA), Differential Thermal Analysis (DTA) and Accelerating Rate Calorimetry (ARC).

  2. Thermal analysis and structural characterization of chitinous exoskeleton from two marine invertebrates

    International Nuclear Information System (INIS)

    Juárez-de la Rosa, B.A.; May-Crespo, J.; Quintana-Owen, P.; Gónzalez-Gómez, W.S.; Yañez-Limón, J.M.; Alvarado-Gil, J.J.

    2015-01-01

    Highlights: • Thermal analysis of exoskeletons: Antipathes caribbeana and Limulus polyphemus. • DMTA revealed Limulus has a stronger structure with a stepper glass transition. • DSC measurements exhibited a much larger water holding capacity in Antipathes. • X-ray diffraction analysis shows a higher crystallinity index in Limulus • FTIR showed α-chitin structures and high temperature C–N groups prevalence. - ABSTRACT: Thermomechanical and structural properties of two marine species exoskeletons, Antipathes caribbeana (black coral) and Limulus polyphemus (xiphosure), were studied using dynamic mechanical thermal analysis (DMTA), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). DMTA curves indicate the viscoelastic behavior and glass transition around 255 °C, black coral presented a second transition (175 °C) associated to the acetamide group attached to the α-chitin chain. DSC measurements showed a endothermic peak around 100 °C, with enthalpies of 4.02 and 118.04 J/g, indicating strong differences between exoskeletons respect to their water holding capacity and strength water–polymer interaction. A comparative analysis involving DSC and X-ray diffraction showed that lower values ΔH in xiphosure correspond to a material with a higher crystallinity (30), in contrast black coral exhibits higher values ΔH and a lower crystallinity (19). FTIR confirmed α-chitin based structure, at higher temperature diminishes the amide bands and a new one appears, related to C–N groups

  3. Thermal analysis and structural characterization of chitinous exoskeleton from two marine invertebrates

    Energy Technology Data Exchange (ETDEWEB)

    Juárez-de la Rosa, B.A., E-mail: balej05@yahoo.com.mx [Laboratory of Natural Polymers, CIAD – Coordinación Guaymas, Carretera al Varadero Nacional km. 6.6, Col. Las Playitas, 85480 Guaymas, Sonora (Mexico); Applied Physics Department, CINVESTAV-IPN Unidad Mérida, Carretera antigua a Progreso, km. 6. Apdo, Postal 73, Cordemex, 97310 Mérida, Yucatan (Mexico); May-Crespo, J.; Quintana-Owen, P.; Gónzalez-Gómez, W.S. [Applied Physics Department, CINVESTAV-IPN Unidad Mérida, Carretera antigua a Progreso, km. 6. Apdo, Postal 73, Cordemex, 97310 Mérida, Yucatan (Mexico); Yañez-Limón, J.M. [Materials and Engineering Science, CINVESTAV-IPN, Unidad Querétaro, Libramiento Norponiente No. 2000, Fracc. Real de Juriquilla, 76230 Santiago de Querétaro, Querétaro (Mexico); Alvarado-Gil, J.J., E-mail: jjag@mda.cinvestav.mx [Applied Physics Department, CINVESTAV-IPN Unidad Mérida, Carretera antigua a Progreso, km. 6. Apdo, Postal 73, Cordemex, 97310 Mérida, Yucatan (Mexico)

    2015-06-20

    Highlights: • Thermal analysis of exoskeletons: Antipathes caribbeana and Limulus polyphemus. • DMTA revealed Limulus has a stronger structure with a stepper glass transition. • DSC measurements exhibited a much larger water holding capacity in Antipathes. • X-ray diffraction analysis shows a higher crystallinity index in Limulus • FTIR showed α-chitin structures and high temperature C–N groups prevalence. - ABSTRACT: Thermomechanical and structural properties of two marine species exoskeletons, Antipathes caribbeana (black coral) and Limulus polyphemus (xiphosure), were studied using dynamic mechanical thermal analysis (DMTA), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). DMTA curves indicate the viscoelastic behavior and glass transition around 255 °C, black coral presented a second transition (175 °C) associated to the acetamide group attached to the α-chitin chain. DSC measurements showed a endothermic peak around 100 °C, with enthalpies of 4.02 and 118.04 J/g, indicating strong differences between exoskeletons respect to their water holding capacity and strength water–polymer interaction. A comparative analysis involving DSC and X-ray diffraction showed that lower values ΔH in xiphosure correspond to a material with a higher crystallinity (30), in contrast black coral exhibits higher values ΔH and a lower crystallinity (19). FTIR confirmed α-chitin based structure, at higher temperature diminishes the amide bands and a new one appears, related to C–N groups.

  4. Molecular structure, vibrational, HOMO-LUMO, MEP and NBO analysis of hafnium selenite

    Science.gov (United States)

    Yankova, Rumyana; Genieva, Svetlana; Dimitrova, Ginka

    2017-08-01

    In hydrothermal condition hafnium selenite with estimated chemical composition Hf(SeO3)2·n(H2O) was obtained and characterized by powder X-Ray diffraction, IR spectroscopy and thermogravimetrical analysis. The composition of the obtained crystalline phase was established as dihydrate of tetraaqua complex of the hafnium selenite [Hf(SeO3)2(H2O)4]·2H2O. The results of the thermogravimetrical analysis are shown that the two hydrated water molecules are released in the temperature interval 80-110°C, while the four coordinated water molecules - at 210-300°C. By DFT method, with Becke's three parameter exchange-functional combined with gradient-corrected correlation functional of Lee, Yang and Parr and 6-31G(d), 6-311 + G(d,p) basis sets and LANL2DZ for Hf atom were calculated the molecular structure, vibrational frequencies and thermodynamic properties of the structure. The UV-Vis spectra and electronic properties are presented. The energy and oscillator strength calculated by time-dependent density functional theory corresponds well with the experimental ones. Molecular electrostatic potential (MEP) was performed. Mulliken population analysis on atomic charges was also calculated. The stability and intramolecular interactions are interpreted by NBO analysis.

  5. Mechanical, Rheological and Thermal Properties of Polystyrene/1-Octadecanol Modified Carbon Nanotubes Nanocomposites

    KAUST Repository

    Amr, Issam Thaher

    2014-09-04

    The results of the studies on the functionalization of multi-walled carbon nanotubes (MWCNT) with 1-octadecanol and its usage as reinforcing filler in the bulk polymerization of styrene are reported in this article. Both unmodified and modified CNTs were utilized in different loadings, however, without any initiator. The resulting composites were characterized by using mechanical testing, differential scanning calorimetry, thermogravimetric analysis and melt rheology. The tensile tests show the addition of 0.5wt% of CNT-C18 results in 19.5% increment of Young\\'s modulus. The DSC study shows a decrease in T-g values of prepared PS/CNT nanocomposite. The rheological study was conducted at 190 degrees C and shows that addition of pure CNT increased the viscoelastic behavior of the PS matrices, while the CNT-C18 act as plasticizer. Thermogravimetric analysis shows that the incorporation of CNT into PS enhanced the thermal properties significantly.

  6. Properties of nonvolatile and antibacterial bioboard produced from bamboo macromolecules by hot pressing

    Directory of Open Access Journals (Sweden)

    Shengbo Ge

    2018-03-01

    Full Text Available Employing the antibacterial property of industrial bamboo vinegar (IBV and the photocatalytic degradation of TiO2, bamboo macromolecules were pretreated and processed into nonvolatile and antibacterial bio board (NVABB. The NVABB was then analyzed by conducting Fourier-transform infrared spectroscopy, thermogravimetric analysis and differential thermal analysis. Results show that NVABB samples had average density of 0.96 g/cm3, which is appropriate for application. In terms of physical and mechanical properties, the best NVABB sample obtained from IBV, TiO2 and bamboo had an IBV pretreatment time of 10 min, 2% TiO2 and 1% bamboo charcoal. Fourier-transform infrared spectroscopy demonstrated that optimum conditions for hot pressing were a temperature of 170 °C, duration of 15 min and the addition of IBV and TiO2. Thermogravimetric analysis/differential thermal analysis curves suggest that the thermal degradation of NVABB was less than that of bamboo and that hot pressing obviously increased the thermal stability of HDBB samples. Analysis of the antimicrobial effect revealed that IBV pretreatment improves the antibacterial property of NVABB. Keywords: Industrial bamboo vinegar, Nonvolatile and antibacterial bio board, Bamboo macromolecules, Fourier-transform infrared spectroscopy, Thermogravimetric analysis/differential thermal analysis

  7. Synthesis and physicochemical analysis of Sm (II, III) acetylacetone chelate complexes

    International Nuclear Information System (INIS)

    Kostyuk, N.N.; Dik, T.A.; Trebnikov, A.G.

    2004-01-01

    Sm (II, III) acetylacetone chelate complexes were synthesized by electrochemical method. It was shown that anode dissolution of the metal samarium over acetylacetone leads to formation of the Sm (II, III) chelate complexes: xSm(acac)2 · ySm(acac)3 · zH(acac). Factors x, y and z depend on quantity of the electricity, which flew through the electrolysis cell. The compositions of the obtained substances were confirmed by the physicochemical analysis (ultimate analysis, IR-, mass spectroscopy and thermal analysis (thermogravimetric, isothermal warming-up and differential scanning colorimetry). (Authors)

  8. Optimization of lead (ii) ions adsorption on to chemically activated ...

    African Journals Online (AJOL)

    The derivative thermal analysis (DTA) and thermogravimetric analysis (TGA) profile of the activated carbon were employed in the proximate analysis. The BET surface area shows a high microporous surface area and micropore volume of 840.38 m2/g and 0.30 cc/g respectively which aids sorption efficiency. The adsorption ...

  9. Synergetic effect of sewage sludge and biomass co-pyrolysis: A combined study in thermogravimetric analyzer and a fixed bed reactor

    International Nuclear Information System (INIS)

    Wang, Xuebin; Deng, Shuanghui; Tan, Houzhang; Adeosun, Adewale; Vujanović, Milan; Yang, Fuxin; Duić, Neven

    2016-01-01

    Highlights: • The synergetic effect of sewage sludge and wheat straw co-pyrolysis was studied. • The mass balance measurement of gas, tar, and char was performed. • The synergetic effect shows strongest under a certain biomass addition ratio around 60%. • The required heat of co-pyrolysis is significantly reduced. - Abstract: Much attention has been given to the valuable products from the pyrolysis of sewage sludge. In this study, the pyrolysis of sewage sludge, biomass (wheat straw) and their mixtures in different proportions were carried out in a thermogravimetric analyzer (TGA) and fixed-bed reactor. The effects of pyrolysis temperature and percentage of wheat straw in wheat straw–sewage sludge mixtures on product distributions in terms of gas, liquid and char and the gas composition were investigated. Results indicate that there is a significantly synergetic effect during the co-pyrolysis processes of sewage sludge and wheat straw, accelerating the pyrolysis reactions. The synergetic effect resulted in an increase in gas and liquid yields but a decrease in char yield. The gas composition and the synergetic effect degree are strongly affected by the wheat straw proportions, and the strongest synergetic effect of sewage sludge and wheat straw co-pyrolysis appears at the biomass proportion of 60 wt.%. With an increase of temperature, the gas yield from the pyrolysis of sewage sludge increased but the liquid and char yields decreased. Moreover, the required heat of co-pyrolysis is significantly reduced compared with the pyrolysis of sewage sludge and wheat straw pyrolysis alone, because of the exothermic reactions between the ash components in two fuel samples.

  10. Effect of acid treated carbon nanotubes on mechanical, rheological and thermal properties of polystyrene nanocomposites

    KAUST Repository

    Amr, Issam Thaher

    2011-09-01

    In this work, multiwall carbon nanotubes (CNT) were functionalized by acid treatment and characterized using Fourier Transform Infrared Spectroscopy (FTIR) and thermogravimetric analysis (TGA). Polystyrene/CNT composites of both the untreated and acid treated carbon nanotubes were prepared by thermal bulk polymerization without any initiator at different loadings of CNT. The tensile tests showed that the addition of 0.5 wt.% of acid treated CNT results in 22% increase in Young\\'s modulus. The DSC measurements showed a decrease in glass transition temperature (Tg) of PS in the composites. The rheological studies at 190 °C showed that the addition of untreated CNT increases the viscoelastic behavior of the PS matrix, while the acid treated CNT acts as plasticizer. Thermogravimetric analysis indicated that the incorporation of CNT into PS enhanced the thermal properties of the matrix polymer. © 2011 Elsevier Ltd. All rights reserved.

  11. Preparation and characterization of polyurethane microcapsules containing functional oil

    Energy Technology Data Exchange (ETDEWEB)

    Kim, I.H.; Seo, J.B.; Kim, Y.J. [Sungkyunkwan University, Suwon (Korea)

    2002-05-01

    Polyurethane microcapsules containing functional oil (citronella oil) were successfully prepared by conventional interfacial polymerization of tolulene 2,4-diisocyanate (TDI) and ethylene glycol (EG) and characterized by Fourier transform (FT-IR) spectroscopy, Ultraviolet spectroscopy, particle size analysis, thermogravimetric analysis (TGA), and scanning electron microscopy (SEM). The effects of polymerization variables such as surfactant concentration and agitation speed, on the particle size and particle size distribution were investigated. FT-IR spectroscopic data showed that citronella oil was successfully encapsulated in the microcapsule. Thermogravimetric analysis data showed that the microcapsule was thermally stable up to 220 deg. C. The controlled release of the citronella oil present in the microcapsule core in a methanol medium was demonstrated by ultraviolet spectroscopy, showing that the amount of released citronella oil was increased with increasing time. It was observed that the amount of released citronella oil was increased with increasing stirring speed and emulsifier concentration in the microcapsule preparation step. Polyurethane microcapsules containing citronella oil showed excellent anti-moth property. (author). 28 refs., 1 tab., 12 figs.

  12. Thermal analysis and kinetics of coal during oxy-fuel combustion

    Science.gov (United States)

    Kosowska-Golachowska, Monika

    2017-08-01

    The pyrolysis and oxy-fuel combustion characteristics of Polish bituminous coal were studied using non-isothermal thermogravimetric analysis. Pyrolysis tests showed that the mass loss profiles were almost similar up to 870°C in both N2 and CO2 atmospheres, while further mass loss occurred in CO2 atmosphere at higher temperatures due to char-CO2 gasification. Replacement of N2 in the combustion environment by CO2 delayed the combustion of bituminous coal. At elevated oxygen levels, TG/DTG profiles shifted through lower temperature zone, ignition and burnout temperatures decreased and mass loss rate significantly increased and complete combustion was achieved at lower temperatures and shorter times. Kinetic analysis for the tested coal was performed using Kissinger-Akahira-Sunose (KAS) method. The activation energies of bituminous coal combustion at the similar oxygen content in oxy-fuel with that of air were higher than that in air atmosphere. The results indicated that, with O2 concentration increasing, the activation energies decreased.

  13. Kinetic Parameters of Non-Isothermal Thermogravimetric Non-Catalytic and Catalytic Pyrolysis of Empty Fruit Bunch with Alumina by Kissinger and Ozawa Methods

    Science.gov (United States)

    Rahayu Mohamed, Alina; Li, Nurfahani; Sohaimi, Khairunissa Syairah Ahmad; Izzati Iberahim, Nur; Munirah Rohaizad, Nor; Hamzah, Rosniza

    2018-03-01

    The non-isothermal thermogravimetric non-catalytic and catalytic empty fruit bunch (EFB) pyrolysis with alumina were performed at different heating rates of 10, 15, 20, 25, 30 and 40 K/min under nitrogen atmosphere at a flow rate of 100 ml/min under dynamic conditions from 301 K to 1273 K. The activation energy were calculated based on Kissinger and Ozawa methods. Both reactions followed first order reactions. By Kissinger method, the activation energy and Ln A values for non-catalytic and catalytic EFB pyrolysis with alumina were 188.69 kJ mol-1 and 201.67 kJ/mol respectively. By Ozawa method, the activation energy values for non-catalytic and catalytic EFB pyrolysis with alumina were 189.13 kJ/mol and 201.44 kJ/mol respectively. The presence of catalyst increased the activation energy values for EFB pyrolysis as calculated by Kissinger and Ozawa methods.

  14. Characterization​ and ​analysis of ​m​otion ​m​echanism​ of electroactive​ chitosan-based actuator.

    Science.gov (United States)

    Altınkaya, Emine; Seki, Yoldaş; Çetin, Levent; Gürses, Barış Oğuz; Özdemir, Okan; Sever, Kutlay; Sarıkanat, Mehmet

    2018-02-01

    In order to analyze the bending mechanism of the electroactive​ chitosan-based actuator, different amounts of poly(diallyldimethylammonium chloride) (PDAD) were incorporated in chitosan solution. The effects of PDAD concentration on electromechanical performance of chitosan actuator were investigated under various excitation voltages. With the incorporation of PDAD into chitosan solution, crosslinked chitosan film acts as an actuator showing a considerable displacement behavior. However it can be noted that higher incorporation of PDAD into chitosan solution decreased the performance of the actuators. Thermal, viscoelastic, and crystallographic properties of the chitosan films were examined by thermogravimetric analysis, dynamic mechanical analysis, and X-ray diffraction analysis, respectively. The effect of incorporation of PDAD in chitosan-based film on morphological properties of chitosan film was determined by scanning electron microscopy. It was observed that the films involving PDAD have larger pore size than the PDAD free film. Copyright © 2017 Elsevier Ltd. All rights reserved.

  15. IN SITU AND POST REACTION COBALT-INCORPORATION INTO ...

    African Journals Online (AJOL)

    Thermogravimetric analysis and Raman spectroscopy show that the surfactant is removed by solvent extraction. Cobalt ion incorporation is confirmed by Raman spectroscopy and UV-vis diffuse reflectance spectroscopy. KEY WORDS: Bifunctional periodic mesoporous organosilica, 1,2-bistrimethoxysilylethane, ...

  16. High temperature impedance spectroscopy of barium stannate

    Indian Academy of Sciences (India)

    ... differential thermal analysis, thermogravimetric analysis and Fourier transform infrared techniques. Electrical properties were studied using a.c. impedance spectroscopy technique in the temperature range of 50–650 °C and frequency range of 10 Hz–13 MHz. The complex impedance plots at temperature ≥ 300 °C show ...

  17. Analysis of Structural Units and Their Influence on Thermal Degradation of Alkali Lignins

    Directory of Open Access Journals (Sweden)

    Wen Hua

    2016-01-01

    Full Text Available The chemical structures of four alkali lignins isolated from poplar, fir, straw, and bagasse were investigated. To explore the relationship between the structural units and the thermal decomposition behavior, the system was tested by elemental analysis, Fourier transform infrared spectrometry, thermogravimetric analysis (TGA, and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS. The results indicated that the carbon content of poplar lignin (PL was higher than that of others. Fir lignin (FL exhibited the highest guaiacol units, while the other three lignins were abundant in syringol units. The thermal decomposition characteristics and pyrolysis products of the four lignins were influenced by the material structural and composition. The DTG curves showed that the initial temperatures and major degradation temperatures of woody lignins(FL and PL) with complex inherent structures were shifted to the high temperature zoom compared with that of non-woody (BL and SL)lignins. Py-GC/MS analysis showed that guaiacol-type phenolic compounds were predominant pyrolysis products derived from the four lignins. The yield of guaiacol-type phenols could reach 82.87%. Moreover, the BL had selectively on phenol-type compounds with yield of 27.89%.

  18. Pyrolysis kinetics and thermodynamic parameters of castor (Ricinus communis) residue using thermogravimetric analysis.

    Science.gov (United States)

    Kaur, Ravneet; Gera, Poonam; Jha, Mithilesh Kumar; Bhaskar, Thallada

    2018-02-01

    Castor plant is a fast-growing, perennial shrub from Euphorbiaceae family. More than 50% of the residue is generated from its stems and leaves. The main aim of this work is to study the pyrolytic characteristics, kinetics and thermodynamic properties of castor residue. The TGA experiments were carried out from room temperature to 900 °C under an inert atmosphere at different heating rates of 5, 10, 15, 20, 30 and 40 °C/min. The kinetic analysis was carried using different models namely Kissinger, Flynn-Wall-Ozawa (FWO) and Kissinger-Akahira-Sunose (KAS). The average E ɑ calculated by FWO and KAS methods were 167.10 and 165.86 kJ/mole respectively. Gibbs free energy varied from 150.62-154.33 to 150.59-154.65 kJ/mol for FWO and KAS respectively. The HHV of castor residue was 14.43 MJ/kg, considered as potential feedstock for bio-energy production. Kinetic and thermodynamic results will be useful input for the design of pyrolytic process using castor residue as feedstock. Copyright © 2017 Elsevier Ltd. All rights reserved.

  19. Large-scale fabrication and utilization of novel hexagonal/turbostratic composite boron nitride nanosheets

    KAUST Repository

    Zhong, Bo; Zhang, Xiaodong; Xia, Long; Yu, Yuanlie; Wen, Guangwu

    2017-01-01

    mechanism of h/t-BNNSs is also discussed based on the thermogravimetric analysis of AB which clearly shows two step weight loss. The h/t-BNNSs are further used for making thermoconductive h/t-BNNSs/epoxy resin composites. The thermal conductivity

  20. Combustion behaviour of Sydney and Bowen Basin coals determined by thermogravimetry

    Energy Technology Data Exchange (ETDEWEB)

    Benfell, K.E.; Beamish, B.B.; Rodgers, K.A.; Crosdale, P.J. [University of Auckland, Auckland (New Zealand). Department of Geology

    1996-08-01

    Assesses the suitability of thermogravimetric (TG) and derivative thermogravimetric (DTG) analysis techniques to characterise the combustion behaviour of Sydney and Bowen basin coals. Results indicate that the thermogravimetric technique is suitable for characterising the effects of rank, maceral, sub-maceral and seam variations on the combustion behaviour of these coals. 6 refs., 6 figs., 2 tabs.

  1. Analysis of annealed thin polymer films prepared from dichloro(methyl)phenylsilane by plasma polymerization

    Czech Academy of Sciences Publication Activity Database

    Cech, V.; Horvath, P.; Trchová, M.; Zemek, Josef; Matějková, Jiřina

    2001-01-01

    Roč. 82, - (2001), s. 2106-2112 ISSN 0021-8995 R&D Projects: GA ČR GV106/98/K013; GA ČR GA104/00/0708 Institutional research plan: CEZ:AV0Z1010914 Keywords : plasma polymerization * thin films * thermogravimetric analysis ( TSA ) * FTIR * ESCA/XPS Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 0.992, year: 2001

  2. Synthesis and characterization of chromium doped boehmite nanofibres

    International Nuclear Information System (INIS)

    Yang Jing; Frost, Ray L.; Yuan Yong

    2009-01-01

    Thermogravimetric and differential thermogravimetric analysis has been used to study synthesised chromium doped boehmite. The dehydroxylation temperature increases significantly from 0 to 5% doping, after which the dehydroxylation temperature shows a small steady increase up to the 20% doping level. The temperature of dehydroxylation increases with time of hydrothermal treatment. Chromium doped boehmite nanofibres were also characterised by X-ray diffraction and transmission electron microscopy. Hydrothermal treatment of doped boehmite with chromium resulted in the formation of nanofibres over a wide dopant range. Nanofibres up to 500 nm in length and between 4 and 6 nm in width were produced

  3. Thermogravimetric study of thermal decontamination of soils polluted by hexachlorobenzene, 4-chlorobiphenyl, naphthalene, or n-decane.

    Science.gov (United States)

    Risoul, V; Pichon, C; Trouvé, G; Peters, W A; Gilot, P; Prado, G

    1999-02-15

    To determine decontamination behavior as affected by temperature, shallow beds of a clay-rich, a calcerous, and a sedimentary soil, artificially polluted with hexachlorobenzene, 4-chlorobiphenyl, naphthalene, or n-decane, were separately heated at 5 degrees C min-1 in a thermogravimetric analyzer. Temperatures for deep cleaning of the calcerous and the sedimentary soil increased with increasing boiling point (bp) of the aromatic contaminants, but removal efficiencies still approached 100% well below the bp. Decontamination rates were therefore modelled according to a pollutant evaporation-diffusion transport model. For the calcerous and sedimentary soils, this model reasonably correlated removal of roughly the first 2/3 of the naphthalene, but gave only fair predictions for hexachlorobenzene and 4-chlorobiphenyl. It was necessary to heat the clay soil above the aromatics bp to achieve high decontamination efficiencies. Weight loss data imply that for temperatures from near ambient to as much as 150 degrees C, interactions of each aromatic with the clay soil, or its decomposition products, result in lower net volatilization of the contaminated vs. neat clay. A similar effect was observed in heating calcerous soil polluted with hexachlorobenzene from near ambient to about 140 degrees C. Decontamination mechanisms remain to be established, although the higher temperatures needed to remove aromatics from the clay may reflect a more prominent role for surface desorption than evaporation. This would be consistent with our estimates that the clay can accommodate all of the initial pollutant loadings within a single surface monolayer, whereas the calcerous and sedimentary soils cannot.

  4. Preparation of Tetramethylguanidine-Functionalized Mesoporous ...

    African Journals Online (AJOL)

    The catalyst was characterized by various techniques including Diffuse Reflectance FTIR, 13C NMR, elemental analysis and simultaneous thermogravimetric and differential scanning calorimetry analyses. It was then screened in the epoxidation of electron deficient alkenes. The results obtained show that indeed the ...

  5. Synthesis, Spectroscopy, Thermal Analysis, Magnetic Properties and Biological Activity Studies of Cu(II and Co(II Complexes with Schiff Base Dye Ligands

    Directory of Open Access Journals (Sweden)

    Saeid Amani

    2012-05-01

    Full Text Available Three azo group-containing Schiff base ligands, namely 1-{3-[(3-hydroxy-propyliminomethyl]-4-hydroxyphenylazo}-4-nitrobenzene (2a, 1-{3-[(3-hydroxypropyl-iminomethyl]-4-hydroxyphenylazo}-2-chloro-4-nitrobenzene (2b and 1-{3-[(3-hydroxy-propyliminomethyl]-4-hydroxyphenylazo}-4-chloro-3-nitrobenzene (2c were prepared. The ligands were characterized by elemental analysis, FTIR spectroscopy, UV-Vis spectroscopy, 13C- and 1H-NMR spectroscopy and thermogravimetric analysis. Next the corresponding copper(II and cobalt(II metal complexes were synthesized and characterized by the physicochemical and spectroscopic methods of elemental analysis, FTIR spectroscopy, UV-Vis spectroscopy, magnetic moment measurements, and thermogravimetric analysis (TGA and (DSC. The room temperature effective magnetic moments of complexes are 1.45, 1.56, 1.62, 2.16, 2.26 and 2.80 B.M. for complexes 3a, 3b, 3c, 4a 4b, and 4c, respectively, indicating that the complexes are paramagnetic with considerable electronic communication between the two metal centers.

  6. Morphological Changes of Limestone Sorbent Particles during Carbonation/Calcination Looping Cycles in a Thermogravimetric Analyzer (TGA) and Reactivation with Steam

    KAUST Repository

    Wu, Y.

    2010-04-15

    Carbonation and calcination looping cycles were carried out on four limestones in a thermogravimetric analyzer (TGA). The CO2 carrying capacity of a limestone particle decays very quickly in the first 10 cycles, reducing to about 20% of its original uptake capacity after 10 cycles for the four limestones studied in this work, and it decreases further to 6-12% after 50 cycles. A new steam reactivation method was applied on the spent sorbent to recover the loss of reactivity. The steam reactivation of multi-cycled samples was conducted at atmospheric pressure. Steam reactivation for 5 min at 130 °C of particles that had undergone 10 cycles resulted in an immediate increase (by 45-60% points) in carrying capacity. The morphological changes of limestone particles during the cycling and steam reactivation were studied using both an optical microscope and scanning electron microscopy (SEM). The diameters of limestone particles shrank by about 2-7% after 10 carbonation/calcination cycles, and the particle diameters swelled significantly (12-22% increase) after steam reactivation. These size changes are important for studies of attrition and mathematical modeling of carbonation. © 2010 American Chemical Society.

  7. Consequences of sludge composition on combustion performance derived from thermogravimetry analysis

    Energy Technology Data Exchange (ETDEWEB)

    Li, Meiyan; Xiao, Benyi; Wang, Xu; Liu, Junxin, E-mail: jxliu@rcees.ac.cn

    2015-01-15

    Highlights: • Volatiles, particularly proteins, play a key role in sludge combustion. • Sludge combustion performance varies with different sludge organic concentrations. • Carbohydrates significantly affect the combustion rate in the second stage. • Combustion performance of digested sludge is more negative compared with others. - Abstract: Wastewater treatment plants produce millions of tons of sewage sludge. Sewage sludge is recognized as a promising feedstock for power generation via combustion and can be used for energy crisis adaption. We aimed to investigate the quantitative effects of various sludge characteristics on the overall sludge combustion process performance. Different types of sewage sludge were derived from numerous wastewater treatment plants in Beijing for further thermogravimetric analysis. Thermogravimetric–differential thermogravimetric curves were used to compare the performance of the studied samples. Proximate analytical data, organic compositions, elementary composition, and calorific value of the samples were determined. The relationship between combustion performance and sludge composition was also investigated. Results showed that the performance of sludge combustion was significantly affected by the concentration of protein, which is the main component of volatiles. Carbohydrates and lipids were not correlated with combustion performance, unlike protein. Overall, combustion performance varied with different sludge organic composition. The combustion rate of carbohydrates was higher than those of protein and lipid, and carbohydrate weight loss mainly occurred during the second stage (175–300 °C). Carbohydrates have a substantial effect on the rate of system combustion during the second stage considering the specific combustion feature. Additionally, the combustion performance of digested sewage sludge is more negative than the others.

  8. Consequences of sludge composition on combustion performance derived from thermogravimetry analysis

    International Nuclear Information System (INIS)

    Li, Meiyan; Xiao, Benyi; Wang, Xu; Liu, Junxin

    2015-01-01

    Highlights: • Volatiles, particularly proteins, play a key role in sludge combustion. • Sludge combustion performance varies with different sludge organic concentrations. • Carbohydrates significantly affect the combustion rate in the second stage. • Combustion performance of digested sludge is more negative compared with others. - Abstract: Wastewater treatment plants produce millions of tons of sewage sludge. Sewage sludge is recognized as a promising feedstock for power generation via combustion and can be used for energy crisis adaption. We aimed to investigate the quantitative effects of various sludge characteristics on the overall sludge combustion process performance. Different types of sewage sludge were derived from numerous wastewater treatment plants in Beijing for further thermogravimetric analysis. Thermogravimetric–differential thermogravimetric curves were used to compare the performance of the studied samples. Proximate analytical data, organic compositions, elementary composition, and calorific value of the samples were determined. The relationship between combustion performance and sludge composition was also investigated. Results showed that the performance of sludge combustion was significantly affected by the concentration of protein, which is the main component of volatiles. Carbohydrates and lipids were not correlated with combustion performance, unlike protein. Overall, combustion performance varied with different sludge organic composition. The combustion rate of carbohydrates was higher than those of protein and lipid, and carbohydrate weight loss mainly occurred during the second stage (175–300 °C). Carbohydrates have a substantial effect on the rate of system combustion during the second stage considering the specific combustion feature. Additionally, the combustion performance of digested sewage sludge is more negative than the others

  9. Influence of alkali catalyst on product yield and properties via hydrothermal liquefaction of barley straw

    DEFF Research Database (Denmark)

    Zhu, Z.; Toor, Saqib; Rosendahl, Lasse

    2015-01-01

    (thermogravimetric analysis) and GC-MS. The addition of K2CO3 increased the bio-crude yield to 34.85 wt%, and inhibited solid residue formation. Moreover, the bio-crude produced in the presence of a catalyst had better properties, in terms of higher heating value and lower O/C. GC-MS analysis showed that the major...

  10. Layered Metal Hydroxides Containing Calcium and Their Structural Analysis

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Tae Hyun; Heo, Il; Lee, Sung Han; Oh, Jae Min [College of Science and Technology, Yonsei University, Wonju (Korea, Republic of); Paek, Seung Min [Kyungpook National University, Daegu (Korea, Republic of); Park, Chung Berm; Choi, Ae Jin [National Institute of Horticultural and Herbal Science of R and D Eumseong (Korea, Republic of); Choy, Jin Ho [Ewha Womans University, Seoul (Korea, Republic of)

    2012-06-15

    Layered metal hydroxides (LMHs) containing calcium were synthesized by coprecipitation in solution having two different trivalent metal ions, iron and aluminum. Two mixed metal solutions (Ca{sup 2+}/Al{sup 3+} and Ca{sup 2+}/Fe{sup 3+} = 2/1) were added to sodium hydroxide solution and the final pH was adjusted to {approx}11.5 and {approx}13 for CaAl-and CaFe-LMHs. Powder X-ray diffraction (XRD) for the two LMH samples showed well developed (00l) diffractions indicating 2-dimensional crystal structure of the synthesized LMHs. Rietveld refinement of the X-ray diffraction pattern, the local structure analysis through X-ray absorption spectroscopy, and thermal analysis also confirmed that the synthesized precipitates show typical structure of LMHs. The chemical formulae, Ca{sub 2.04}Al{sub 1}(OH){sub 6}(NO{sub 3}){center_dot}5.25H{sub 2}O and Ca{sub 2.01}Fe{sub 1}(OH){sub 6}(NO{sub 3}){center_dot}4.75H{sub 2}O were determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Particle morphology and thermal behavior for the synthesized LMHs were examined by field emission scanning electron microscopy and thermogravimetric differential scanning calorimetry

  11. Molecularly imprinted membrane extraction combined with high-performance liquid chromatography for selective analysis of cloxacillin from shrimp samples.

    Science.gov (United States)

    Du, Wei; Sun, Min; Guo, Pengqi; Chang, Chun; Fu, Qiang

    2018-09-01

    Nowadays, the abuse of antibiotics in aquaculture has generated considerable problems for food safety. Therefore, it is imperative to develop a simple and selective method for monitoring illegal use of antibiotics in aquatic products. In this study, a method combined molecularly imprinted membranes (MIMs) extraction and liquid chromatography was developed for the selective analysis of cloxacillin from shrimp samples. The MIMs was synthesized by UV photopolymerization, and characterized by scanning electron microscope, Fourier transform infrared spectra, thermo-gravimetric analysis and swelling test. The results showed that the MIMs exhibited excellent permselectivity, high adsorption capacity and fast adsorption rate for cloxacillin. Finally, the method was utilized to determine cloxacillin from shrimp samples, with good accuracies and acceptable relative standard deviation values for precision. The proposed method was a promising alternative for selective analysis of cloxacillin in shrimp samples, due to the easy-operation and excellent selectivity. Copyright © 2018. Published by Elsevier Ltd.

  12. The influence of cellulose nanocrystal additions on the performance of cement paste

    Science.gov (United States)

    Yizheng Cao; Pablo Zavaterri; Jeff Youngblood; Robert Moon; Jason Weiss

    2015-01-01

    The influence of cellulose nanocrystals (CNCs) addition on the performance of cement paste was investigated. Our mechanical tests show an increase in the flexural strength of approximately 30% with only 0.2% volume of CNCs with respect to cement. Isothermal calorimetry (IC) and thermogravimetric analysis (TGA) show that the degree of hydration (DOH) of the cement paste...

  13. Water Transport in MgSO4·7H2O during Dehydration in View of Thermal Storage

    NARCIS (Netherlands)

    Donkers, P.A.J.; Beckert, S.; Pel, L.; Stallmach, F.; Steiger, M.; Adan, O.C.G.

    2015-01-01

    The water phases in a MgSO4·7H2O crystal during heating were studied with the help of NMR. The thermogravimetric analysis (TGA) data showed that the heating rate has a strong effect on the dehydration process. NMR experiments showed that pore water, i.e., an aqueous solution of MgSO4, was produced

  14. Interpretation of Quasi-Isothermal Thermogravimetric Weight Curves

    DEFF Research Database (Denmark)

    Sørensen, Ole Toft

    1979-01-01

    Quasi-isothermal analysis (QIA) is a very useful technique. Compared to conventional non-isothermal thermogravimetry, close-lying reactions can easily be separated by use of this method and kinetic data can be obtained for each intermediate reaction in a single run. This paper discusses the shape...

  15. Synthesis, Spectral, Thermogravimetric, XRD, Molecular Modelling and Potential Antibacterial Studies of Dimeric Complexes with Bis Bidentate ON–NO Donor Azo Dye Ligands

    Directory of Open Access Journals (Sweden)

    Bipin Bihari Mahapatra

    2013-01-01

    Full Text Available The dimeric complexes of Co(II, Ni(II, Cu(II, Zn(II, Cd(II, and Hg(II with two new symmetrical ON–NO donor bis bidentate (tetradentate azo dye ligands, LH2 = 4,4′-bis(4′-hydroxyquinolinolinylazodiphenylsulphone, and L′H2 = 4,4′-bis(acetoacetanilideazodiphenylsulphone have been synthesized. The metal complexes have been characterised by elemental analytical, conductance, magnetic susceptibility, IR, electronic spectra, ESR, NMR, thermogravimetry, X-ray diffraction (powder pattern spectra, and molecular modelling studies. The Co(II and Ni(II complexes are found to be octahedral, Cu(II complexes are distorted octahedral, and a tetrahedral stereochemistry has been assigned to Zn(II, Cd(II, and Hg(II complexes. The thermogravimetric study indicates that compounds are quite stable. The energy optimized structures are proposed using the semiempirical ZINDO/1 quantum mechanical calculations. The potential antibacterial study of the ligands and some metal complexes has been made with one gram positive bacteria Staphylococcus aureus and one gram negative bacteria E. coli which gives encouraging results. Both the Co(II complexes are found to possess monoclinic crystal system.

  16. Polymethyl methacrylate and polystyrene with layered double hydroxide nano composites: In situ synthesis, morphology and thermal properties; Nanocompositos de polimetacrilato de metila e poliestireno com hidroxido duplo lamelar: sintese in situ, morfologia e propriedades termicas

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2011-07-01

    Over the past decade, polymer nanocomposites have attracted interest, both in industry and in academia, because they often exhibit remarkable improvement in their properties when compared with pure polymer or conventional micro and macro-composites using low levels of reinforcements. In this work polymethyl methacrylate and polystyrene reinforced with layered double hydroxide, which was intercalated with sodium dodecyl sulfate were synthesized by in situ bulk polymerization. The nanocomposites were characterized and compared by X-ray diffraction, thermogravimetric analysis and flammability test. The X-ray diffraction demonstrated that synthesized nanocomposites showed a high global dispersion of layered double hydroxide, suggesting exfoliated morphology. The result of thermogravimetric analysis and flammability test for synthesized polystyrene/ layered double hydroxide nanocomposite presented a significant improvement in thermal stability and flammability property when compared with pure polymer. (author)

  17. An effective approach to synthesis of poly(methyl methacrylate)/silica nanocomposites

    International Nuclear Information System (INIS)

    Ding Xuefeng; Wang Zichen; Han Dongxue; Zhang Yuanjian; Shen Yanfei; Wang Zhijuan; Niu Li

    2006-01-01

    A novel synthetic route for nearly monodispersed poly(methyl methacrylate)/SiO 2 composite particles (PMSCP) is reported. Silica nanoparticles modified with oleic acid were used as 'seeds'. Methyl methacrylate (MMA) monomer was copolymerized with oleic acid via in situ emulsion polymerization, in the presence of an initiator; it resulted finally in the formation of composites with core-shell morphology. The composite particles were examined by transmission electron microscopy (TEM), scanning electron microscopy (SEM), x-ray photoelectron spectroscopy (XPS) and thermogravimetric analysis (TGA). The number of silica particles inside the composite particles increases with an increase in the silica concentration. The effect of grafted silica concentration on the morphology of PMSCP is also reported in detail. It was found by thermogravimetric analysis that PMSCP show a potential application for fire retardance

  18. Polymethyl methacrylate and polystyrene with layered double hydroxide nano composites: In situ synthesis, morphology and thermal properties

    International Nuclear Information System (INIS)

    Botan, Rodrigo; Nogueira, Telma R.; Lona, Liliane M.F.; Wypych, Fernando

    2011-01-01

    Over the past decade, polymer nanocomposites have attracted interest, both in industry and in academia, because they often exhibit remarkable improvement in their properties when compared with pure polymer or conventional micro and macro-composites using low levels of reinforcements. In this work polymethyl methacrylate and polystyrene reinforced with layered double hydroxide, which was intercalated with sodium dodecyl sulfate were synthesized by in situ bulk polymerization. The nanocomposites were characterized and compared by X-ray diffraction, thermogravimetric analysis and flammability test. The X-ray diffraction demonstrated that synthesized nanocomposites showed a high global dispersion of layered double hydroxide, suggesting exfoliated morphology. The result of thermogravimetric analysis and flammability test for synthesized polystyrene/ layered double hydroxide nanocomposite presented a significant improvement in thermal stability and flammability property when compared with pure polymer. (author)

  19. Self-standing paper based anodes prepared from siliconcarbonitride-MoS2 composite for Li-ion battery applications

    Science.gov (United States)

    David, Lamuel; Singh, Gurpreet

    2013-03-01

    We study synthesis of free-standing polymer derived SiCN/ MoS2 composite paper anode for Li-ion battery application. This was achieved following a two-step approach: First, polysilazane was interfaced with exfoliated MoS2 nanosheets which upon pyrolysis resulted in SiCN/MoS2 composite. Second, dispersion of SiCN/MoS2 in isopropanol was vacuum filtered resulting in formation of a self-standing composite paper. Physical and chemical characterization of the composite was carried out by use of electron microscopy, Fourier transform infrared spectroscopy (FT-IR) and Thermo-gravimetric analysis (TGA). FT-IR data indicated complete conversion of polysilazane precursor to SiCN ceramic, while electron microscopy confirmed layered structure of the paper. Thermo-gravimetric analysis showed enhanced thermodynamic stability of the composite paper up to 800 °C. Electrochemical analysis of SiCN/MoS2 composite paper anodes showed that Li-ion can reversible intercalate in the voltage range of 0-2.5 V with a first cycle discharge capacity of 770 mAh/g at a current density of 100 mA/g.

  20. TG-FTIR analysis of biomass pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Bassilakis, R.; Carangelo, R.M.; Wojtowicz, M.A. [Advanced Fuel Research Inc., Hartford, CT (United States)

    2001-10-09

    A great need exists for comprehensive biomass-pyrolysis models that could predict yields and evolution patterns of selected volatile products as a function of feedstock characteristics and process conditions. A thermogravimetric analyzer coupled with Fourier transform infrared analysis of evolving products (TG-FTIR) can provide useful input to such models in the form of kinetic information obtained under low heating rate conditions. In this work, robust TG-FTIR quantification routes were developed for infrared analysis of volatile products relevant to biomass pyrolysis. The analysis was applied to wheat straw, three types of tobacco (Burley, Oriental, and Bright) and three biomass model compounds (xylan, chlorogenic acid, and D-glucose). Product yields were compared with literature data, and species potentially quantifiable by FT-IR are reviewed. Product-evolution patterns are reported for all seven biomass samples. 41 refs., 7 figs., 2 tabs.

  1. Proteome Analysis of the Plant Pathogenic Fungus Monilinia laxa Showing Host Specificity

    Directory of Open Access Journals (Sweden)

    Olja Bregar

    2012-01-01

    Full Text Available Brown rot fungus Monilinia laxa (Aderh. & Ruhl. Honey is an important plant pathogen in stone and pome fruits in Europe. We applied a proteomic approach in a study of M. laxa isolates obtained from apples and apricots in order to show the host specifity of the isolates and to analyse differentially expressed proteins in terms of host specifity, fungal pathogenicity and identification of candidate proteins for diagnostic marker development. Extracted mycelium proteins were separated by 2-D electrophoresis (2-DE and visualized by Coomassie staining in a non-linear pH range of 3–11 and Mr of 14–116 kDa. We set up a 2-DE reference map of M. laxa, resolving up to 800 protein spots, and used it for image analysis. The average technical coefficient of variance (13 % demonstrated a high reproducibility of protein extraction and 2-D polyacrylamide gel electrophoresis (2-DE PAGE, and the average biological coefficient of variance (23 % enabled differential proteomic analysis of the isolates. Multivariate statistical analysis (principal component analysis discriminated isolates from two different hosts, providing new data that support the existence of a M. laxa specialized form f. sp. mali, which infects only apples. A total of 50 differentially expressed proteins were further analyzed by LC-MS/MS, yielding 41 positive identifications. The identified mycelial proteins were functionally classified into 6 groups: amino acid and protein metabolism, energy production, carbohydrate metabolism, stress response, fatty acid metabolism and other proteins. Some proteins expressed only in apple isolates have been described as virulence factors in other fungi. The acetolactate synthase was almost 11-fold more abundant in apple-specific isolates than in apricot isolates and it might be implicated in M. laxa host specificity. Ten proteins identified only in apple isolates are potential candidates for the development of M. laxa host-specific diagnostic markers.

  2. Characterization and evaluation of employment of nanostructured spinel MA on oxidation resistance of graffiti; Caracterizacao e avaliacao do emprego de espinelio MA nanoestruturado na resistencia a oxidacao de grafites

    Energy Technology Data Exchange (ETDEWEB)

    Vitor, P.A.M.; Guaglianoni, W.C.; Braganca, S.R.; Bergmann, C.P., E-mail: pedroaugusto89@hotmail.com [Universidade Federal do Rio Grande do Sul (LACER/UFRS), Porto Alegre, RS (Brazil). Laboratorio de Materiais Ceramicos

    2016-07-01

    This study aimed to investigate the obtaining of nanostructured powders of spinel MA (MgAl2O4) via synthesis of combustion in solution (SCS), and the influence of its incorporation in oxidation resistance in natural graphites. The crystalline phase only was obtained after a heat treatment at 900 ° C of the powder as-synthesized. The powders were characterized by differential thermal analysis (DTA) and thermogravimetric (ATG) and crystallographic analysis by X-ray diffraction (XRD) and Raman spectroscopy. The results, using thermogravimetric dynamic and isothermal analysis showed a relationship between embedded content of spinel (as-synthesized and calcined) and the raising of the temperature to start the oxidation process (onset temperature) of the samples. The rate of oxidation is reduced at temperatures from 700 ° C, retarding the oxidation of graphite with increasing level of spinel, but this effect ceases at temperatures above 1000 ° C. (author)

  3. Research on pyrolysis characteristics and kinetics of super fine and conventional pulverized coal

    International Nuclear Information System (INIS)

    Zhang Chaoqun; Jiang Xiumin; Wei Lihong; Wang Hui

    2007-01-01

    Based on isothermal thermogravimetric analysis (TGA) and kinetic equations, the optimization toolbox of MATLAB was applied to study the effects of particle size and heating rate on the pyrolysis characteristics and kinetics and to obtain the mechanism function and kinetic parameters of Yuanbaoshan coal at four different particle sizes and heating rates. The pyrolysis characteristics of the samples were analyzed using thermogravimetric (TG) curves and differential thermogravimetric (DTG) curves. The results show that the coal pyrolysis process is strongly affected by heating rate and particle size. As the heating rate increases, the temperature of volatile matter initiation increases, the total volatile matter evolved decreases and the DTG peak shifts toward higher temperature. As the particle size decreases, the temperature of volatile matter initiation of the coal sample decreases and the maximum rate of mass loss increases. In the pyrolysis of coal, the activation energies of the samples were found to increase with growing particle size and decreasing heating rate for both of the devolatilization temperature stages. In the lower temperature stage, the coal samples show a great difference in mechanism function at different particle sizes and heating rates

  4. ANALYSIS OF BIODEGRABILITY OF DEGRADABLE/BIODEGRADABLE PLASTIC MATERIAL IN CONTROLLED COMPOSTING ENVIRONMENT

    Directory of Open Access Journals (Sweden)

    Dana Adamcová

    2016-09-01

    Full Text Available We have obtained eight degradable/biodegradable materials based on starch (certified compostable, sample 4–7, HDPE mixed with totally degradable plastic additive (TDPA, sample 2 and polyethylene with the addition of pro-oxidant additive (d2w, sample 1. Composition of sample 3 has not been reported. The materials have been tested as to the rate and character of their degradability/biodegradability in controlled composting conditions. Experiment explored also the effect of degradation/biodegradation of plastic bags on compost quality. The material of the original samples was subjected to assessment using the Nicolet 6700 FT-IR spectrometer, the outcome thereof was obtaining infrared spectra of the samples. For further specification the original samples were tested using the thermogravimetrical analysis. The texture of the foils at different stages of degradation is presented in the Scanning Electron Microscope (SEM photographs. Plastic bags certified as compostable have degraded in laboratory conditions and their degradation had no impact on the quality and features of compost. Selected samples (4, 6 showed significant erosion on surface when subjected to the SEM analysis. Samples labeled (by their producers as 100% degradable (samples 1, 2, 3 did not show any visual signs of degradation and the process of degradation had no impact on the quality and features of compost. Only one of the samples (sample 1 showed certain erosion of surface when submitted for the SEM analysis.

  5. Analysis of briquetting process of sewage sludge with coal to combustion process

    Directory of Open Access Journals (Sweden)

    Kosturkiewicz Bogdan

    2016-01-01

    Full Text Available Energy recovery from sewage sludge can be achieved by several thermal technologies, but before those processes sewage sludge requires special pretreatment. The paper presents the investigation of the sewage sludge with coal briquettes as a fuel for combustion process. Research is conducted at Department of Manufacturing Systems and Department of Thermal Engineering and Environmental Protection, AGH University of Science and Technology to develop a technology of briquette preparation. The obtained results showed possibility of briquetting of municipal sewage sludge with coal in roll presses, equipped with asymmetric thickening gravity feed system. The following properties were determined for the obtained briquettes: density, drop strength and compressive strength. Based on physical and chemical analysis of prepared briquettes it was confirmed that briquettes have good fuel properties to combustion process. Thermal behaviour of studied sewage sludge and prepared mixture was investigated by thermogravimetric analysis (TG. For the thermo gravimetric analysis (TG the samples were heated in an alumina crucible from an ambient temperature up to 1000 °C at a constant rates: 10 °C/min, 40 °C/min and 100 °C/min in a 40 ml/min flow of air.

  6. Carbon elimination from silicon kerf: Thermogravimetric analysis and mechanistic considerations.

    Science.gov (United States)

    Vazquez-Pufleau, Miguel; Chadha, Tandeep S; Yablonsky, Gregory; Biswas, Pratim

    2017-01-18

    40% of ultrapure silicon is lost as kerf during slicing to produce wafers. Kerf is currently not being recycled due to engineering challenges and costs associated with removing its abundant impurities. Carbon left behind from the lubricant remains as one of the most difficult contaminants to remove in kerf without significant silicon oxidation. The present work enables to better understand the mechanism of carbon elimination in kerf which can aid the design of better processes for kef recycling and low cost photovoltaics. In this paper, we studied the kinetics of carbon elimination from silicon kerf in two atmospheres: air and N 2, under a regime of no-diffusion-limitation. We report the apparent activation energy in both atmospheres using three methods: Kissinger, and two isoconversional approaches. In both atmospheres, a bimodal apparent activation energy is observed, suggesting a two stage process. A reaction mechanism is proposed in which (a) C-C and C-O bond cleavage reactions occur in parallel with polymer formation; (b) at higher temperatures, this polymer fully degrades in air but leaves a tarry residue in N 2 that accounts for about 12% of the initial total carbon.

  7. SYNTHESIS AND CHARACTERIZATION OF NEW HEAT ...

    African Journals Online (AJOL)

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    The thermal properties of the polymers 6a-c were investigated by thermogravimetric analysis (TGA). Polymer 6c due to presence of SO2 group as a polar group shows better thermal properties compare with polymer 6a and 6b. KEY WORDS: Polycondensation, Polyamide, Ether group, Thermal properties. INTRODUCTION.

  8. Polypropylene-modified kaolinite composites: Effect of chemical ...

    African Journals Online (AJOL)

    PP/kaolinite compounds were prepared by the melt intercalation method. The effects of modified clay on properties of the prepared composites were studied. The XRD results showed that the treatment with the ammonium salt caused the return to the initial state of the clay. The thermogravimetric analysis thermograms (TGA) ...

  9. 阻燃共聚酯的热降解动力学研究——Ⅰ.含磷共聚PET和PET的比较%STUDY ON KINETIC OF THERMAL DEGRADATION OF FLAME RETARDANT COPOLYESTERS——Ⅰ.THE COMPARISION BETWEEN PHOSPHORUS-CONTAINING COPOLYESTER AND PET

    Institute of Scientific and Technical Information of China (English)

    吴博; 王玉忠

    2001-01-01

    The thermal degradation of poly (ethylene terephthalate)(PET) and phosphorus-containing copolyester,obtained from the polycondensation of terephthalate acid,ethylene glycol and 2-carboxyethyl (phenyl phosphinic) acid in air were studied by thermogravimetric analysis(TG) in order to determine the activation energy of phosphorus-containing copolyester and PET.The activation energy was determined using Kissinger method and Flynn-Wall-Ozawa method,withaut the knowledge of the reaction mechanism(RM),giving the values 219.18~229.65kJ/mol and 217.61~238.85kJ/mol respectively.The results show that there is little difference between the values of thermogravimetric activation energy of phosphorus-containing copolyester and PET,both of the reaction mechanism are same.

  10. Thermogravimetric and calorimetric characteristics during co-pyrolysis of municipal solid waste components.

    Science.gov (United States)

    Ansah, Emmanuel; Wang, Lijun; Shahbazi, Abolghasem

    2016-10-01

    The thermogravimetric and calorimetric characteristics during pyrolysis of wood, paper, textile and polyethylene terephthalate (PET) plastic in municipal solid wastes (MSW), and co-pyrolysis of biomass-derived and plastic components with and without torrefaction were investigated. The active pyrolysis of the PET plastic occurred at a much higher temperature range between 360°C and 480°C than 220-380°C for the biomass derived components. The plastic pyrolyzed at a heating rate of 10°C/min had the highest maximum weight loss rate of 18.5wt%/min occurred at 420°C, followed by 10.8wt%/min at 340°C for both paper and textile, and 9.9wt%/min at 360°C for wood. At the end of the active pyrolysis stage, the final mass of paper, wood, textile and PET was 28.77%, 26.78%, 21.62% and 18.31%, respectively. During pyrolysis of individual MSW components at 500°C, the wood required the least amount of heat at 665.2J/g, compared to 2483.2J/g for textile, 2059.4J/g for paper and 2256.1J/g for PET plastic. The PET plastic had much higher activation energy of 181.86kJ/mol, compared to 41.47kJ/mol for wood, 50.01kJ/mol for paper and 36.65kJ/mol for textile during pyrolysis at a heating rate of 10°C/min. H2O and H2 peaks were observed on the MS curves for the pyrolysis of three biomass-derived materials but there was no obvious H2O and H2 peaks on the MS curves of PET plastic. There was a significant interaction between biomass and PET plastic during co-pyrolysis if the biomass fraction was dominant. The amount of heat required for the co-pyrolysis of the biomass and plastic mixture increased with the increase of plastic mass fraction in the mixture. Torrefaction at a proper temperature and time could improve the grindability of PET plastic. The increase of torrefaction temperature and time did not affect the temperature where the maximum pyrolytic rates occurred for both biomass and plastic but decreased the maximum pyrolysis rate of biomass and increased the maximum pyrolysis

  11. Chemical phase analysis of seed mediated synthesized anisotropic silver nanoparticles

    International Nuclear Information System (INIS)

    Bharti, Amardeep; Goyal, Navdeep; Singh, Suman; Singla, M. L.

    2015-01-01

    Noble-metal nanoparticles are of great interest because of its broad applications almost in every stream (i.e. biology, chemistry and engineering) due to their unique size/shape dependant properties. In this paper, chemical phase of seed mediated synthesized anisotropic silver nanoparticle (AgNPs) has been investigated via fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA). These nanaoparticles were synthesized by seed-growth method controlled by urea and dextrose results to highly stable 12-20 nm particle size revealed by zeta potential and transmission electron microscopy (TEM)

  12. The comparative kinetic analysis of Acetocell and Lignoboost® lignin pyrolysis: the estimation of the distributed reactivity models.

    Science.gov (United States)

    Janković, Bojan

    2011-10-01

    The non-isothermal pyrolysis kinetics of Acetocell (the organosolv) and Lignoboost® (kraft) lignins, in an inert atmosphere, have been studied by thermogravimetric analysis. Using isoconversional analysis, it was concluded that the apparent activation energy for all lignins strongly depends on conversion, showing that the pyrolysis of lignins is not a single chemical process. It was identified that the pyrolysis process of Acetocell and Lignoboost® lignin takes place over three reaction steps, which was confirmed by appearance of the corresponding isokinetic relationships (IKR). It was found that major pyrolysis stage of both lignins is characterized by stilbene pyrolysis reactions, which were subsequently followed by decomposition reactions of products derived from the stilbene pyrolytic process. It was concluded that non-isothermal pyrolysis of Acetocell and Lignoboost® lignins can be best described by n-th (n>1) reaction order kinetics, using the Weibull mixture model (as distributed reactivity model) with alternating shape parameters. Copyright © 2011 Elsevier Ltd. All rights reserved.

  13. Modeling of biomass pyrolysis

    International Nuclear Information System (INIS)

    Samo, S.R.; Memon, A.S.; Akhund, M.A.

    1995-01-01

    The fuels used in industry and power sector for the last two decades have become expensive. As a result renewable energy source have been emerging increasingly important, of these, biomass appears to be the most applicable in the near future. The pyrolysis of biomass plays a key role amongst the three major and important process generally encountered in a gas producer, namely, pyrolysis, combustion and reduction of combustion products. Each biomass has its own pyrolysis characteristics and this important parameters must be known for the proper design and efficient operation of a gasification system. Thermogravimetric analysis has been widely used to study the devolatilization of solid fuels, such as biomass. It provides the weight loss history of a sample heated at a predetermined rate as a function of time and temperature. This paper presents the experimental results of modelling the weight loss curves of the main biomass components i.e. cellulose, hemicellulose and lignin. Thermogravimetric analysis of main components of biomass showed that pyrolysis is first order reaction. Furthermore pyrolysis of cellulose and hemicelluloe can be regarded as taking place in two stages, for while lignin pyrolysis is a single stage process. This paper also describes the Thermogravimetric Analysis (TGA) technique to predict the weight retained during pyrolysis at any temperature, for number of biomass species, such as cotton stalk, bagasse ad graoundnut shell. (author)

  14. Carboxyl-terminated butadiene-acrylonitrile-toughened epoxy/carboxyl-modified carbon nanotube nanocomposites: Thermal and mechanical properties

    Directory of Open Access Journals (Sweden)

    H. F. Xie

    2012-09-01

    Full Text Available Carboxyl-modified multi-walled carbon nanotubes (MWCNT–COOHs as nanofillers were incorporated into diglycidyl ether of bisphenol A (DGEBA toughened with carboxyl-terminated butadiene-acrylonitrile (CTBN. The carboxyl functional carbon nanotubes were characterized by Fourier-transform infrared spectroscopy and thermogravimetric analysis. Furthermore, cure kinetics, glass transition temperature (Tg, mechanical properties, thermal stability and morphology of DGEBA/CTBN/MWCNT–COOHs nanocomposites were investigated by differential scanning calorimetry (DSC, dynamic mechanical analysis (DMA, universal test machine, thermogravimetric analysis and scanning electron microscopy (SEM. DSC kinetic studies showed that the addition of MWCNT–COOHs accelerated the curing reaction of the rubber-toughened epoxy resin. DMA results revealed that Tg of rubber-toughened epoxy nanocomposites lowered with MWCNT–COOH contents. The tensile strength, elongation at break, flexural strength and flexural modulus of DGEBA/CTBN/MWCNT-COOHs nanocomposites were increased at lower MWCNT-COOH concentration. A homogenous dispersion of nanocomposites at lower MWCNT–COOH concentration was observed by SEM.

  15. Effect of Chemical Treatment on Physical, Mechanical and Thermal Properties of Ladies Finger Natural Fiber

    Directory of Open Access Journals (Sweden)

    S. I. Hossain

    2013-01-01

    Full Text Available In present research, natural fiber obtained from ladies finger plant was chemically treated separately using alkali (2% NaOH, chromium sulfate (4% , and chromium sulfate and sodium bicarbonate (4% . Both raw and chemically treated fibers were subsequently characterized using mechanical (tensile, structural (Fourier transform infrared spectroscopy and scanning electron microscopy, and thermal (thermogravimetric analysis. Fourier analysis showed the presence of (−OH group in the ladies plant fiber. Scanning electron micrographs revealed rougher surface in case of alkali treated fiber, while thin coating layer was formed on the fiber surface during other two treatments. Tensile test on ladies finger single fiber was carried out by varying span length. The tensile strength and Young's modulus values were found to be increased after chemical treatment. For both raw and chemically treated fibers, Young's modulus increased and tensile strength decreased with increase in span length. Thermogravimetric analysis indicated the same level of thermal stability for both raw and treated ladies finger fibers.

  16. Synthesis and characterization of new heat resistance and ...

    African Journals Online (AJOL)

    The thermal properties of the polymers 6a-c were investigated by thermogravimetric analysis (TGA). Polymer 6c due to presence of SO2 group as a polar group shows better thermal properties compare with polymer 6a and 6b. KEY WORDS: Polycondensation, Polyamide, Ether group, Thermal properties. Bull. Chem. Soc.

  17. Kinetic study and thermal decomposition behavior of viscoelastic memory foam

    International Nuclear Information System (INIS)

    Garrido, María A.; Font, Rafael; Conesa, Juan A.

    2016-01-01

    Highlights: • The thermal degradation has been studied under three different atmospheres. • Pyrolysis and combustion kinetic models have been proposed. • Evolved products under different atmospheres have been analyzed by TG-FTIR and TG-MS. - Abstract: A systematic investigation of the thermal decomposition of viscoelastic memory foam (VMF) was performed using thermogravimetric analysis (TGA) to obtain the kinetic parameters, and thermogravimetric analysis coupled to Fourier Transformed Infrared Spectrometry (TGA-FTIR) and thermogravimetric analysis coupled to Mass Spectrometry (TGA-MS) to obtain detailed information of evolved products on pyrolysis and oxidative degradations. Two consecutive nth-order reactions were employed to correlate the experimental data from dynamic and isothermal runs performed at three different heating rates (5, 10 and 20 K/min) under an inert atmosphere. On the other hand, for the kinetic study of the oxidative decomposition, the data from combustion (synthetic air) and poor oxygen combustion (N_2:O_2 = 9:1) runs, at three heating rates and under dynamic and isothermal conditions, were correlated simultaneously. A kinetic model consisting of three consecutive reactions presented a really good correlation in all runs. TGA-FTIR analysis showed that the main gases released during the pyrolysis of VMF were determined as ether and aliphatic hydrocarbons, whereas in combustion apart from the previous gases, aldehydes, amines and CO_2 have also been detected as the main gases. These results were confirmed by the TGA-MS.

  18. Analysis of the elements sputtered during the lanthanum implantation in stainless steels

    International Nuclear Information System (INIS)

    Ager, F.J.; Respaldiza, M.A.; Silva, M.F. da; Redondo, L.M.; Soares, J.C.

    1998-01-01

    The evidence of the modification of the surface structure of the AISI-304 stainless steel during the implantation of lanthanum makes the analysis of the sputtered elements very interesting. Those sputtered elements are deposited on a carbon sheet placed in front of the steel being implanted, and studied by means of RBS and PIXE, together with the implanted specimens. Besides, the protective effect of the implanted ions during the high temperature oxidation is also studied by those techniques together with XRD and thermogravimetric methods. (orig.)

  19. Theoretical (in B3LYP/6-3111++G** level), spectroscopic (FT-IR, FT-Raman) and thermogravimetric studies of gentisic acid and sodium, copper(II) and cadmium(II) gentisates.

    Science.gov (United States)

    Regulska, E; Kalinowska, M; Wojtulewski, S; Korczak, A; Sienkiewicz-Gromiuk, J; Rzączyńska, Z; Swisłocka, R; Lewandowski, W

    2014-11-11

    The DFT calculations (B3LYP method with 6-311++G(d,p) mixed with LanL2DZ for transition metals basis sets) for different conformers of 2,5-dihydroxybenzoic acid (gentisic acid), sodium 2,5-dihydroxybenzoate (gentisate) and copper(II) and cadmium(II) gentisates were done. The proposed hydrated structures of transition metal complexes were based on the results of experimental findings. The theoretical geometrical parameters and atomic charge distribution were discussed. Moreover Na, Cu(II) and Cd(II) gentisates were synthesized and the composition of obtained compounds was revealed by means of elemental and thermogravimetric analyses. The FT-IR and FT-Raman spectra of gentisic acid and gentisates were registered and the effect of metals on the electronic charge distribution of ligand was discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

  20. Thermal Analysis of Braille Formed by Using Screen Printing and Inks with Thermo Powder

    Directory of Open Access Journals (Sweden)

    Svіtlana HAVENKO

    2015-03-01

    Full Text Available In order to improve the integration of blind people into society, suitable conditions should be provided for them. The expansion of Braille (BR use could serve the purpose. Depending on the materials used for Braille, it can be formed or printed in different ways: embossing, screen printing, thermoforming, digital printing. The aim of this research is to determine the effect of thermal properties of screen printing inks and inks with thermo-powder on the qualitative parameters of Braille. Screen printing inks and inks with thermo-powder were chosen for the research. Carrying out the qualitative analysis of printouts with Braille, the thermal stability was evaluated by analyzing the thermograms obtained with derivatograph Q-1500. This paper presents the findings of the thermogravimetric (TG, differential thermogravimetric (DTG and differential thermal analysis (DTA of printouts printed on paperboard Plike and using traditional screen printing inks and screen printing inks with thermo-powder. Based on the testing findings it is determined that thermal stability of printouts printed with thermo-powder ink is higher than printed with screen printing inks. It is determined that the appropriate temperature range of screen printing inks with thermo-powder drying is 98 ºC – 198 ºC because in this case better relief of Braille dots is obtained.DOI: http://dx.doi.org/10.5755/j01.ms.21.1.5702

  1. Preparation, Investigation and the Study of the Effect of Mn(II Complex of Catechol and 2-Aminopyridine on Seed Germination

    Directory of Open Access Journals (Sweden)

    F. I. El-Moshaty

    2011-01-01

    Full Text Available The formation of mixed ligand complex of Mn(II with catechol (L1 and 2-aminopyridine (L2 was determined by elemental analyses (C, H and N, molar conductance measurement, thermogravimetric analysis, infrared, electronic and electron paramagnetic resonance spectroscopies. The elemental analysis data show the formation of 1:1:1 [M: L1: L2] complex. The molar conductance measurement shows a non-electrolyte nature. The thermogravimetric analysis data of the complex display the existence of hydrated and coordinated water molecules. The infrared spectral data exhibit the coordination sites that are through -OH,-C=N and –NH2 groups. The electronic spectral data display the electronic transitions of the ligands and suggest an octahedral structure for the complex. The electron paramagnetic resonance spectrum of the complex reveals the existence of paramagnetic phenomena and supports its geometrical structure. Seed germination and root length of grass were also assayed under the effect of MnCl2.4H2O, catechol, 2-aminopyridine and its complex. Mn(II salt was the most effective on germination than its complex which possess the high test effect on root length, while the ligands are the least active of all.

  2. Thermal gravimetric analysis of the CsCuCl3, Cs2CuCl4 and Cs2CuCl4x2H2O crystals

    International Nuclear Information System (INIS)

    Soboleva, L.V.; Vasil'eva, M.G.

    1977-01-01

    The thermal characteristics of crystals of Cs 2 CuCl 4 , Cs 2 CuCl 4 x2H 2 O, and CsCuCl 3 were investigated thermogravimetrically. The derivatogram of the Cs 2 CuCl 4 crystal is characterized by the presence of a single endothermal effect at 505 deg C. The derivatogram of the Cs 2 CuCl 4 x2H 2 O crystal contains three endothermal effects: at 40, 135, and 480 deg C. The derivatogram of the CsCuCl 3 crystal shows the presence of two endothermal effects at 142 and 455 deg C. The thermogravimetric data on Cs 2 CuCl 4 and CsCuCl 3 crystals reveal crystal decomposition on melting; hence, these crystals cannot be grown from melts

  3. Synthesis, crystal structure and properties of [Co(L2](ClO42 (L=1,3-bis(1H-benzimidazol-2-yl-2-oxapropane

    Directory of Open Access Journals (Sweden)

    Tavman Aydin

    2015-01-01

    Full Text Available The reaction of 1,3-bis(1H-benzimidazol-2-yl-2-oxapropane (L with Co(ClO42•6H2O in absolute ethanol produces di[1,3-bis(1H-benzimidazol-2-yl-2-oxapropane-k2N,N’]cobalt(IIdiperchlorate chelate complex ([Co(L2](ClO42, 1. The complex 1 was characterized by elemental analysis, magnetic moment, molar conductivity, thermogravimetric analysis, FT-IR, UV-visible, mass spectrometry, and its solid state structure was determined by single crystal X-ray diffraction. According to the thermogravimetric analysis data, there is no any water coordinated or uncoordinated in 1 as well as elemental analysis. The complex 1 has 1:2 M:L ionic characteristic according to the molar conductivity. In the complex, the distances between the cobalt and the ethereal oxygen atoms (Co1-O2: 2.805(3; Co2-O1: 2.752(2 Å show the semi-coordination bonding and the Co(II ion is six-coordinated with a N4O2 ligand set, resulting in a distorted octahedron.

  4. Thermal degradation and isothermal crystalline behavior of poly(trimethylene terephthalate)

    Institute of Scientific and Technical Information of China (English)

    Jian Liu; Shu Guang Bian; Min Xiao; Shuan Jin Wang; Yue Zhong Meng

    2009-01-01

    Poly(trimethylene terephthalate)(PTT)is an excellent fiber material.Its thermal degradation and isothermal crystalline behaviors were in this study investigated using thermogravimetric analysis(TGA),thermogravimetric analysis-Fourier transform infrared spectroscopy(TGA-FTIR)analysis,differential scanning calorimetry(DSC)and X-ray diffraction(XRD).The thermal degradation mechanism of PTT follows Mclafferty rearrangement principle.The PTT with intrinsicviscosity(IV)of 0.74 dL/g has a maximum crystallinity of about 55%at 190℃,as demonstrated by DSC and XRD measurements consistently.

  5. Synthesis and Characterization of Benzimidazolium Salts as Novel Ionic Liquids and their Catalytic Behavior in the Reaction of Alkylation

    Institute of Scientific and Technical Information of China (English)

    Wei Guo HUANG; Bo CHEN; Yuan Yuan WANG; Li Yi DAI; Yong Kui SHAN

    2005-01-01

    A new series of ionic liquids have been prepared containing benzimidazolium cation (abbreviated as Bim). These salts were characterized by DSC, NMR, elemental analysis and thermogravimetric analysis. They showed different properties compared to imidazolium cation due to the introduction of benzene ring. The alkylation of benzene/diphenyl ether with 1-dodecene was carried in C4eBimBr-AlCl3 ionic liquids showing high catalytic activity when the mole ratio of C4eBimB:AlCl3 was 1:2.

  6. Analysis of the structural stability of the smectite submitted to high pressures and temperatures

    International Nuclear Information System (INIS)

    Alabarse, Frederico Gil

    2009-10-01

    The thermal stability of bentonite is of particular interest for containment barrier in nuclear waste disposal facilities. However, very little is known about the stability of smectite (principal component of bentonite) under high-pressure and high-temperature conditions (HPHT). The objective of this work was to investigate the stability of the smectite structure under HP-HT conditions. The HP-HT experiments were performed on toroidal chambers (TC) with pressure up 7.7 GPa and temperatures of 1000 deg C. The samples were characterized by X-ray diffraction after the HP-HT processing. Furthermore, one sample from the original material was analyzed using Fourier transformed infra-red (FTIR) in situ measurements on a diamond anvil cell (DAC) in experiments up to 12 GPa. The original sample of bentonite, calcium dioctahedral montmorillonite with small fraction of quartz, was characterized by FTIR, XRD, X-ray fluorescence (XRF), scanning electron microscopy (SEM), surface area, thermogravimetric analysis (TGA) and differential thermal analysis (DTA). In the experiment performed using the DAC up to 12 GPa, the FTIR in situ measurements analysis showed that the smectite structure is stable with a reversible deformation in the Si-O bond and that the smectite did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 250 deg C of temperature, during 3.5 h showed, after analysis by XRD and FTIR, that the smectite structure is stable and did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 1000 deg C of temperature, during 3.5 h showed, after analysis by XRD and SEM, the transformation of bentonite to the mineral assemblage: Coesite, Quartz, Kyanite and Pyrope. (author)

  7. Effect of electron beam irradiation on the thermal properties of polycarbonate / polyester blend

    International Nuclear Information System (INIS)

    Zarie, K.A.

    2007-01-01

    The effect of electron beam irradiation on the thermal properties of Bayfol (polycarbonate/polyester blend) solid state nuclear track detector (SSNTD) was investigated. Non-isothermal studies were carried out using thermogravimetric analysis (TGA) and differential thermogravimetric (DTG) to obtain the activation energy of thermal decomposition for Bayfol detector. The thermogravimetric analysis (TGA) indicated that the Bayfol samples were decomposed in one main break down stage. Samples of 250 μm thickness sheets were exposed to electron beam irradiations in the dose range 20-600 KGy. The variation of melting temperatures with the electron dose was determined using differential thermal analysis (DTA). The results indicated that the electron irradiation in the dose range 200-600 KGy decreases the melting temperature of the Bayfol samples and this is most suitable for applications requiring the molding of this polymer at lower temperatures

  8. Characterization behavior of some polymeric composite ion exchangers

    International Nuclear Information System (INIS)

    El-Zahhar, A.A; Ahdel-Aziz, H.M.; Siyam, T.

    2005-01-01

    Polymeric composite resins were prepared by template polymerization process in aqueous solution. Thermogravimetric analysis (TGA), differential thermal analysis (DTA) and The X-ray diffraction patterns (XRD) were performed to evaluate the physico chemical properties of the different polymeric composite resins. The TGA and DTA clarify high thermal stability of prepared polymeric composite resins. XRD of prepared polymeric composite shows that there is crystalline structure of some resins while other are amorphous one

  9. Using thermal analysis techniques for identifying the flash point temperatures of some lubricant and base oils

    Directory of Open Access Journals (Sweden)

    Aksam Abdelkhalik

    2018-03-01

    Full Text Available The flash point (FP temperatures of some lubricant and base oils were measured according to ASTM D92 and ASTM D93. In addition, the thermal stability of the oils was studied using differential scanning calorimeter (DSC and thermogravimetric analysis (TGA under nitrogen atmosphere. The DSC results showed that the FP temperatures, for each oil, were found during the first decomposition step and the temperature at the peak of the first decomposition step was usually higher than FP temperatures. The TGA results indicated that the temperature at which 17.5% weigh loss take placed (T17.5% was nearly identical with the FP temperature (±10 °C that was measured according to ASTM D92. The deviation percentage between FP and T17.5% was in the range from −0.8% to 3.6%. Keywords: Flash point, TGA, DSC

  10. Thermogravimetric Study and Modeling of Direct Sulfation of Limestone by Sulfur Dioxide%二氧化硫对石灰石的直接硫酸盐化作用的热重分析的研究与建模

    Institute of Scientific and Technical Information of China (English)

    R. Hallaj; M. Nikazar; B. Dabir

    2004-01-01

    The direct sulfation of limestone from different sources in Iran was studied in a thermogravimetric analyzer under atmospheric pressure. All limestone samples tested have higher than 97% CaCO3. Experimental conditions were as follows: particle size levels ranging from 1.6μm to 7.8μm, four level reaction temperatures (700°C,750°C, 800°C and 850°C), and two SO2 concentrations (2.4 × 10-3 and 3.2 × 10-3 mol.mol-i). The particle size and temperature showed dominant influences on the rate and level of conversion while the effect of SO2 concentration was weak. The shrinking core model can be used to describe the behavior of the sulfation process. The reaction kinetics and diffusion mechanism are both important in controlling the rate of the process. The two key parameters of the model, chemical rate constant Ks and effective diffusion coefficient Deff were obtained. Model predictions are in good agreement with the experimental data.

  11. Structure–property relationships of synthetic organophosphorus flame retardant oligomers by thermal analysis

    International Nuclear Information System (INIS)

    Bai, Zhiman; Wang, Xin; Tang, Gang; Song, Lei; Hu, Yuan; Yuen, Richard K.K.

    2013-01-01

    Highlights: • Oligomers with different chemical components in molecular chains were synthesized. • FP-3 containing three IFR components possessed high thermal stability. • FP-3 possessed lowest flammability. • FP-3 exhibited a synergistic interaction between gas and condensed phase. - Abstract: A series of flame retardant oligomers with different chemical components in molecular chains, designated as FP-1, FP-2 and FP-3, respectively, were successfully synthesized using solution polycondensation and well characterized. The thermal properties and flammability of these oligomers were investigated by thermogravimetric analysis (TGA) and microscale combustion calorimeter (MCC). The results demonstrated that FP-3 had the lowest flammability in terms of the lowest maximum mass loss rate, and FP-1 possessed the highest thermal stability and char yield, due to its higher stable hexatomic ring structure of piperazine compared with the linear alkane chain structure of neopentyl glycol. The gases evolved during decomposition were analyzed using Fourier transform infrared coupled with the thermogravimetric analyzer (TG–IR) technique. The char residues of the flame retardant oligomers were investigated by scanning electron microscopy (SEM) and Raman spectroscopy. The results demonstrated that FP-3 exhibited a synergistic interaction between the gas phase and condensation phase, increasing its flame retardancy

  12. Micromechanical thermogravimetry

    Science.gov (United States)

    Berger, R.; Lang, H. P.; Gerber, Ch.; Gimzewski, J. K.; Fabian, J. H.; Scandella, L.; Meyer, E.; Güntherodt, H.-J.

    1998-09-01

    We demonstrate a new method for thermal analysis of nanogram quantities of material using a micromechanical thermogravimetric technique. The cantilever-type device uses an integrated piezoresistor to sense bending and simultaneously to ramp the temperature and control temperature cycles. It has a mass resolution in the picogram range. A quantitative analysis of the dehydration of copper-sulfate-pentahydrate (CuSO 4·5H 2O) is presented. The technique outperforms current thermogravimetric approaches by five orders of magnitude.

  13. Effect of Residence Time on Hydrothermal Carbonization of Corn Cob Residual

    Directory of Open Access Journals (Sweden)

    Lei Zhang

    2015-05-01

    Full Text Available Hydrothermal carbonization is a promising technique for conversion of industrial waste into valuable products. Producing hydrochar from corn cob residual (CCR in a cost-effective way is key, from an economic standpoint. For this purpose, the effect of residence time in the range of 0.5 to 6 h was studied under the optimal temperature of 250 °C. Results showed that the higher heating value (HHV of hydrochar increased approximately 40% in comparison to that of the raw material; however, prolonging the residence time beyond 0.5 h had a negligible effect on the HHV increase. Chemical compositions and H/C and O/C ratios of hydrochars revealed a minimal effect of longer residence time. Furthermore, thermogravimetric and derivative thermogravimetric analysis (TG/DTG, Fourier transform infrared spectroscopy (FTIR, and X-ray diffraction (XRD analysis of hydrochars also verified that the pyrolysis behavior and chemical structure of hydrochars with various residence times were similar.

  14. Phase transformation behavior of titanium during carbothermic reduction of titanomagnetite ironsand

    Institute of Scientific and Technical Information of China (English)

    Yi-ran Liu; Jian-liang Zhang; Zheng-jian Liu; Xiang-dong Xing

    2016-01-01

    The reduction of titanomagnetite (TTM) ironsand, which contains 11.41wt% TiO2 and 55.63wt% total Fe, by graphite was per-formed using a thermogravimetric analysis system under an argon gas atmosphere at 1423–1623 K. The behavior and effects of titanium in TTM ironsand during the reduction process were investigated by means of thermogravimetric analysis, X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy. During the reduction procedure, the titanium concentrated in the slag phase, where the phase transformation followed this sequence: FeO + FeTiO3→ Fe2TiO4→ FeTiO3→ FeTi2O5→ TiO2. The calculated results for the reduction kinetics showed that the carbothermic reduction was controlled by the diffusion of ions through the product layer. Furthermore, the apparent activation energy was 170.35 kJ·mol−1.

  15. Flame retardancy and thermal properties of epoxy acrylate resin/alpha-zirconium phosphate nanocomposites used for UV-curing flame retardant films

    International Nuclear Information System (INIS)

    Xing Weiyi; Jie Ganxin; Song Lei; Wang Xin; Lv Xiaoqi; Hu Yuan

    2011-01-01

    This paper reported the UV-curing flame retardant film, which consisted of epoxy acrylate resin (EA) used as an oligomer, tri(acryloyloxyethyl) phosphate (TAEP) and triglycidyl isocyanurate acrylate (TGICA) used as flame retardant (FR). The flame retardancy and thermal properties of films were reinforced by using alpha-zirconium phosphate (α-Zr (HPO 4 ) 2 H 2 O, α-ZrP). The morphology of nanocomposite film was characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results showed that the organophilic α-ZrP (OZrP) layers were dispersed well in epoxy acrylate resin. Microscale Combustion Calorimeter (MCC), thermogravimetric analysis (TGA) and thermogravimetric analysis/infrared spectrometry (TGA-IR) were used to characterize the flame retardant property and thermal stability. It was found that the incorporation of TAEP and TGICA can reduce the flammability of EA. Moreover, further reductions were observed due to the addition of OZrP. The char residue for systems with or without OZrP was also explored by scanning electron microscopy (SEM).

  16. Discernment of synergism in pyrolysis of biomass blends using thermogravimetric analysis.

    Science.gov (United States)

    Mallick, Debarshi; Poddar, Maneesh Kumar; Mahanta, Pinakeswar; Moholkar, Vijayanand S

    2018-04-12

    This study reports pyrolysis kinetics of biomass blends using isoconversional methods, viz. Friedman, FWO and KAS. Blends of three biomasses, viz. saw dust, bamboo dust and rice husk, were used. Extractives and volatiles in biomass and minerals in ash had marked influence on enhancement of reaction kinetics during co-pyrolysis, as indicated by reduction in activation energy and increase in decomposition intensity. Pyrolysis kinetics of saw dust and rice husk accelerated (positive synergy), while that of bamboo dust decelerated after blending (negative synergy). Predominant reaction mechanism of all biomass blends was 3-D diffusion in lower conversion range (α ≤ 0.5), while for α ≥ 0.5 pyrolysis followed random nucleation (or nucleation and growth mechanism). Higher reaction order for pyrolysis of blends of rice husk with saw dust and bamboo dust was attributed to catalytic effect of minerals in ash. Positive ΔH and ΔG was obtained for pyrolysis of all biomass blends. Copyright © 2018 Elsevier Ltd. All rights reserved.

  17. Preparation and Characterization of Starch-g-PVA/Nano-hydroxyapatite Complex Hydrogel

    Institute of Scientific and Technical Information of China (English)

    2005-01-01

    Starch-g-PVA/hydroxyapatite complex hydrogel was prepared with two-repeated freezing/ thawing circles. SEM observation results exhibits that hydroxyapatite is dispersed in starch-g-PVA in nanoscale. Thermogravimetric analysis curves show that the remained fraction keeps the same at the temperatures higher than 490℃ . It was found the dried starch-g- PVA/ hydroxyapatite films could reswell within 12 minutes.

  18. Defect structure, nonstoichiometry, and phase stability of Ca-doped YCrO3

    International Nuclear Information System (INIS)

    Carini, G.F. II; Anderson, H.U.; Nasrallah, M.M.; Sparlin, D.M.

    1991-01-01

    The dependence of the defect structure of Ca-doped YCrO 3 on oxygen activity and temperature was investigated by high temperature thermogravimetric measurements. Defect models developed from electrical conductivity data obtained in a previous study were used to interpret the thermogravimetric data. A correlation was found between the electrical conductivity and the thermogravimetric data which suggested that these data were concomitantly dependent on the acceptor dopant and oxygen vacancy dependence of the thermodynamic parameters. Kroeger-Vink type diagrams showing the regions of stability with respect to oxygen activity and temperature were constructed. The TGA data show that Ca-doped YCrO 3 is even more stable toward reduction than doped LaCrO 3

  19. Infrared and Raman spectroscopic characterization of the silicate mineral olmiite CaMn2+[SiO3(OH)](OH) - implications for the molecular structure

    Science.gov (United States)

    Frost, Ray L.; Scholz, Ricardo; López, Andrés; Xi, Yunfei; Granja, Amanda; Žigovečki Gobac, Željka; Lima, Rosa Malena Fernandes

    2013-12-01

    We have studied the mineral olmiite CaMn[SiO3(OH)](OH) which forms a series with its calcium analogue poldervaartite CaCa[SiO3(OH)](OH) using a range of techniques including scanning electron microscopy, thermogravimetric analysis, Raman and infrared spectroscopy. Chemical analysis shows the mineral is pure and contains only calcium and manganese in the formula. Thermogravimetric analysis proves the mineral decomposes at 502 °C with a mass loss of 8.8% compared with the theoretical mass loss of 8.737%. A strong Raman band at 853 cm-1 is assigned to the SiO stretching vibration of the SiO3(OH) units. Two Raman bands at 914 and 953 cm-1 are attributed to the antisymmetric vibrations. Two intense Raman bands observed at 3511 and 3550 cm-1 are assigned to the OH stretching vibration of the SiO3(OH) units. The observation of multiple OH bands supports the concept of the non-equivalence of the OH units. Vibrational spectroscopy enables a detailed assessment of the molecular structure of olmiite.

  20. A real time analysis of the self-assembly process using thermal analysis inside the differential scanning calorimeter instrument.

    Science.gov (United States)

    Roy, Debmalya; Shastri, Babita; Mukhopadhyay, K

    2012-07-12

    The supramolecular assembly of the regioregular poly-3-hexylthiophene (rr-P3HT) in solution has been investigated thoroughly in the past. In the current study, our focus is on the enthalpy of nanofiber formation using thermal analysis techniques by performing the self-assembly process inside the differential scanning calorimetry (DSC) instrument. Thermogravimetric analysis (TGA) was carried out to check the concentration of the solvent during the self-assembly process of P3HT in p-xylene. Ultraviolet visible (UV-vis) spectophotometric technique, small-angle X-ray scattering (SAXS) experiment, atomic force microscopic (AFM), and scanning electron microscopic (SEM) images were used to characterize the different experimental yields generated by cooling the reaction mixture at desired temperatures. Comparison of the morphologies of self-assembled products at different fiber formation temperatures gives us an idea about the possible crystallization parameters which could affect the P3HT nanofiber morphology.

  1. Fluoride substitution in LiBH4; destabilization and decomposition

    DEFF Research Database (Denmark)

    Richter, Bo; Ravnsbaek, Dorthe B.; Sharma, Manish

    2017-01-01

    Fluoride substitution in LiBH4 is studied by investigation of LiBH4-LiBF4 mixtures (9:1 and 3:1). Decomposition was followed by in situ synchrotron radiation X-ray diffraction (in situ SR-PXD), thermogravimetric analysis and differential scanning calorimetry with gas analysis (TGA/DSC-MS) and in ......Fluoride substitution in LiBH4 is studied by investigation of LiBH4-LiBF4 mixtures (9:1 and 3:1). Decomposition was followed by in situ synchrotron radiation X-ray diffraction (in situ SR-PXD), thermogravimetric analysis and differential scanning calorimetry with gas analysis (TGA...

  2. Analysis of glass fibre sizing

    DEFF Research Database (Denmark)

    Petersen, Helga Nørgaard; Kusano, Yukihiro; Brøndsted, Povl

    2014-01-01

    Glass fibre reinforced polymer composites are widely used for industrial and engineering applications which include construction, aerospace, automotive and wind energy industry. During the manufacturing glass fibres, they are surface-treated with an aqueous solution. This process and the treated...... surfaces are called sizing. The sizing influences the properties of the interface between fibres and a matrix, and subsequently affects mechanical properties of composites. In this work the sizing of commercially available glass fibres was analysed so as to study the composition and chemical structures....... Soxhlet extraction was used to extract components of the sizing from the glass fibres. The glass fibres, their extracts and coated glass plates were analysed by Thermo-Gravimetric Analysis combined with a mass spectrometer (TGA-MS), and Attenuated Total Reflectance Fourier Transform Infrared (ATR...

  3. Proteomic Analysis Shows Constitutive Secretion of MIF and p53-associated Activity of COX-2−/− Lung Fibroblasts

    Directory of Open Access Journals (Sweden)

    Mandar Dave

    2017-12-01

    Full Text Available The differential expression of two closelyassociated cyclooxygenase isozymes, COX-1 and COX-2, exhibited functions beyond eicosanoid metabolism. We hypothesized that COX-1 or COX-2 knockout lung fibroblasts may display altered protein profiles which may allow us to further differentiate the functional roles of these isozymes at the molecular level. Proteomic analysis shows constitutive production of macrophage migration inhibitory factor (MIF in lung fibroblasts derived from COX-2−/− but not wild-type (WT or COX-1−/− mice. MIF was spontaneously released in high levels into the extracellular milieu of COX2−/− fibroblasts seemingly from the preformed intracellular stores, with no change in the basal gene expression of MIF. The secretion and regulation of MIF in COX-2−/− was “prostaglandin-independent.” GO analysis showed that concurrent with upregulation of MIF, there is a significant surge in expression of genes related to fibroblast growth, FK506 binding proteins, and isomerase activity in COX-2−/− cells. Furthermore, COX-2−/− fibroblasts also exhibit a significant increase in transcriptional activity of various regulators, antagonists, and co-modulators of p53, as well as in the expression of oncogenes and related transcripts. Integrative Oncogenomics Cancer Browser (IntroGen analysis shows downregulation of COX-2 and amplification of MIF and/or p53 activity during development of glioblastomas, ependymoma, and colon adenomas. These data indicate the functional role of the MIF-COX-p53 axis in inflammation and cancer at the genomic and proteomic levels in COX-2-ablated cells. This systematic analysis not only shows the proinflammatory state but also unveils a molecular signature of a pro-oncogenic state of COX-1 in COX-2 ablated cells.

  4. Thermal analysis and infrared emission spectroscopic study of halloysite-potassium acetate intercalation compound

    Energy Technology Data Exchange (ETDEWEB)

    Cheng, Hongfei [School of Geoscience and Surveying Engineering, China University of Mining and Technology, Beijing 100083 China (China); School of Mining Engineering, Inner Mongolia University of Science and Technology, Baotou 014010 (China); Chemistry Discipline, Faculty of Science and Technology, Queensland University of Technology, 2 George Street, GPO Box 2434, Brisbane, Queensland 4001 (Australia); Liu, Qinfu [School of Geoscience and Surveying Engineering, China University of Mining and Technology, Beijing 100083 China (China); Yang, Jing [Chemistry Discipline, Faculty of Science and Technology, Queensland University of Technology, 2 George Street, GPO Box 2434, Brisbane, Queensland 4001 (Australia); Zhang, Jinshan [School of Mining Engineering, Inner Mongolia University of Science and Technology, Baotou 014010 (China); Frost, Ray L., E-mail: r.frost@qut.edu.au [Chemistry Discipline, Faculty of Science and Technology, Queensland University of Technology, 2 George Street, GPO Box 2434, Brisbane, Queensland 4001 (Australia)

    2010-11-20

    The thermal decomposition of halloysite-potassium acetate intercalation compound was investigated by thermogravimetric analysis and infrared emission spectroscopy. The X-ray diffraction patterns indicated that intercalation of potassium acetate into halloysite caused an increase of the basal spacing from 1.00 to 1.41 nm. The thermogravimetry results show that the mass losses of intercalation the compound occur in main three main steps, which correspond to (a) the loss of adsorbed water, (b) the loss of coordination water and (c) the loss of potassium acetate and dehydroxylation. The temperature of dehydroxylation and dehydration of halloysite is decreased about 100 {sup o}C. The infrared emission spectra clearly show the decomposition and dehydroxylation of the halloysite intercalation compound when the temperature is raised. The dehydration of the intercalation compound is followed by the loss of intensity of the stretching vibration bands at region 3600-3200 cm{sup -1}. Dehydroxylation is followed by the decrease in intensity in the bands between 3695 and 3620 cm{sup -1}. Dehydration was completed by 300 {sup o}C and partial dehydroxylation by 350 {sup o}C. The inner hydroxyl group remained until around 500 {sup o}C.

  5. High Efficiency Photovoltaic Devices Fabricated from Self-Assemble Block Insulating-Conducting Copolymer Containing Semiconducting Nanoparticles

    Science.gov (United States)

    2005-12-14

    71.3° TESDT ɝ° 45.3° 59.5° 67.2° 75.0° The amount of D-A linkers anchored on TiO2 nanoparticles was determined by thermogravimetric analysis ...e.g. lamellae, cylinders and spheres of copolymers were fabricated. Semiconducting nanoparticles of cadmium sulfide ( CdS ) was incorporated into PPP...water contact angle measurement, thermogravimetric analysis , and XPS spectra, we can presume that compact SAMs were formed on the surface of TiO2

  6. Surface adsorption in strontium chloride ammines

    DEFF Research Database (Denmark)

    Ammitzbøll, Andreas L.; Lysgaard, Steen; Klukowska, Agata

    2013-01-01

    An adsorbed state and its implications on the ab- and desorption kinetics of ammonia in strontium chloride ammine is identified using a combination of ammonia absorption measurements, thermogravimetric analysis, and density functional theory calculations. During thermogravimetric analysis, ammonia...... desorption originating from the adsorbed state is directly observed below the bulk desorption temperature, as confirmed by density functional theory calculations. The desorption enthalpy of the adsorbed state of strontium chloride octa-ammine is determined with both techniques to be around 37-39 k...

  7. Kinetic analysis of the termal decomposition of colombian vacuum residua by termogravimetry

    Directory of Open Access Journals (Sweden)

    Fabian Andrey Diaz Mateus

    2015-09-01

    Full Text Available Five different Colombian vacuum residues were thermally decomposed in a thermogravimetric analyzer. Three heating rates were employed to heat the sample up to 650°C. The kinetic analysis was performed by the Coats-Redfern method to describe the non-isothermal pyrolysis of the residua, a reaction model where the reaction order gradually increases from first to second order is proposed and an excellent agreement of the experimental with the calculated data is presented. The results also indicate that the pyrolysis of a vacuum residue cannot be modeled by a single reaction mechanism.

  8. Thermal analysis of formation of nano-crystalline BaTiO3 using Ba(NO32 and TiO2

    Directory of Open Access Journals (Sweden)

    Md. Jawed Ansaree

    2015-12-01

    Full Text Available The reaction of Ba(NO32 with TiO2 was studied by thermogravimetric (TG and differential scanning calorimetric (DSC techniques up to 1000 °C and in nitrogen atmosphere. It was found that the formation of BaTiO3 takes place above 600 °C and that precursor mixing time and heating rate have no effect on the reaction temperature. BaTiO3 powder was prepared by calcination of Ba(NO32 and TiO2 precursor mixture at 800 °C for 8 h. X-ray diffraction analysis of the synthesized BaTiO3 confirmed the formation of tetragonal phase with lattice parameters a = 3.9950±0.0003 Å and c = 4.0318±0.0004 Å. Thermal analysis of the synthesized BaTiO3 powder showed weight loss within temperature range 40–1000 °C of only 0.40%. This small amount of weight loss was connected with some impurity phase, and identified as BaCO3 using Fourier transform infrared (FTIR technique.

  9. Essential work of fracture analysis for starch filled poly(propylene carbonate) composites

    International Nuclear Information System (INIS)

    Wang, X.L.; Li, R.K.Y.; Cao, Y.X.; Meng, Y.Z.

    2007-01-01

    Starch filled poly(propylene carbonate) composites are environmental friendly materials. In this study, the fracture toughness of composites under mode I loading was determined by the essential work of fracture concept. The specific essential fracture work of the poly(propylene carbonate)/starch composites decreases with increasing the starch content, while the non-essential work term, βw p increases with increasing the starch content. In addition, the morphologies, thermal properties, thermo-mechanical properties were studied by scanning electron microscope, thermogravimetric analysis, dynamic mechanical analysis, and differential scanning calorimetry, respectively. The thermal and thermo-mechanical measurements revealed that increasing starch content led to an increase in glass transition temperature and thermal stability. Morphology observation indicates that poly(propylene carbonate) and starch have weak interfacial adhesion

  10. Intumescent coatings with improved properties for high-rise construction

    Science.gov (United States)

    Ustinov, Andrey; Zybina, Olga; Tanklevsky, Leonid; Lebedev, Vasily; Andreev, Andrey

    2018-03-01

    The paper overviews the way of creating intumescent fire-protective compositions with improved properties by adding nano-and micro-sized supplements into them. Intumescent paints are inert at low temperatures, and at higher temperatures they expand and degrade to provide a charred layer of low conductivity materials. The modified intumescent paints are able to form a more stable charred layer than the classical paints. The stability of a charred layer is crucial if the fire safety in high-rise construction must be secured, because a weak charred layer will not provide a required fire endurance for steel bearing structures and they will break down in case of fire. The fire-protective properties of modified intumescent paints were estimated using an electrical furnace. Also the way of thermal decomposition of the paints was studied with thermogravimetric analysis. Results show that modified intumescent paints form a charred layer with improved fire-protective properties; it can serve as a thermal barrier for a longer period of time. Thermogravimetric analysis confirms this fact showing that the temperatures of full thermal decay in case of modified paints are higher than those of non-modified paints.

  11. Preparation, melting behavior and thermal stability of poly(lactic acid)/poly(propylene carbonate) blends processed by vane extruder

    Energy Technology Data Exchange (ETDEWEB)

    Zou, Wei, E-mail: zw55624@163.com; Chen, Rongyuan; Zhang, Haichen; Qu, Jinping, E-mail: jpqu@scut.edu.cn [National Engineering Research Center of Novel Equipment for Polymer Processing, South China University of Technology, Guangzhou 510640 (China)

    2016-03-09

    Poly (lactic acid) (PLA)/Poly (propylene carbonate) (PPC) blends were prepared by vane extruder which is a type of novel polymer processing extruder based on elongation force field. Scanning electron microscope (SEM), differential scanning calorimetry (DSC) and thermogravimetric (TG) were used respectively to analyze the compatibility, the melting behavior and thermal stability properties of PLA/PPC blends affected by the different content of PPC. The results showed that with the increase of the PPC content, the glass transition temperature of PLA was reduced, and the glass transition temperature of PPC was increased, which indicated that PLA and PPC had partial compatibility. The cold crystallization temperature of PLA increased with the increase of the PPC content, which showed that PPC hindered the cold crystallization process of PLA. The addition of PPC had little impact on the melting process of PLA, and the melting temperature of PLA was almost kept the same value. Thermogravimetric analysis showed that the thermal stability of PPC was worse than that of PLA, the addition of PPC reduced the thermal stability of PLA.

  12. Thermal Analysis: A Complementary Method to Study the Shurijeh Clay Minerals

    Directory of Open Access Journals (Sweden)

    Golnaz Jozanikohan

    2015-06-01

    Full Text Available Clay minerals are considered the most important components of clastic reservoir rock evaluation studies. The Shurijeh gas reservoir Formation, represented by shaly sandstones of the Late Jurassic-Early Cretaceous age, is the main reservoir rock in the Eastern Kopet-Dagh sedimentary Basin, NE Iran. In this study, X-ray diffraction (XRD, X-ray fluorescence (XRF, scanning electron microscopic (SEM studies, and thermal analysis including differential thermal analysis (DTA, and thermogravimetric analysis (TGA techniques were utilized in the characterization of the Shurijeh clay minerals in ten representative samples. The XRF studies showed that silica and aluminum oxides are present quantities. The XRD test was then used to determine the mineralogical composition of bulk components, as well as the clay fraction. The XRD patterns indicated the presence of dominant amount of quartz and plagioclase, with moderate to minor amounts of alkali feldspar, anhydrite, carbonates (calcite and dolomite, hematite and clay minerals. The most common clays in the Shurijeh Formation were illite, chlorite, and kaolinite. However, in very few samples, glauconite, smectite, and mixed layer clay minerals of both illite-smectite and chlorite-smectite types were also recognized. The XRD results were quantified, using the elemental information from the XRF test, showing that each Shurijeh exhibited low to moderate amounts of clay minerals, typically up to 21%. The amount of illite, the most dominant clay mineral, reached maximum of 13.5%, while the other clay types were significantly smaller. Based on the use of SEM and thermal data, the results of the identification of clay minerals, corresponded with the powder X-ray diffraction analysis, which can be taken into account as an evidence of the effectiveness of the thermal analysis technique in clay typing, as a complementary method besides the XRD.

  13. Ionic liquid thermal stabilities: decomposition mechanisms and analysis tools.

    Science.gov (United States)

    Maton, Cedric; De Vos, Nils; Stevens, Christian V

    2013-07-07

    The increasing amount of papers published on ionic liquids generates an extensive quantity of data. The thermal stability data of divergent ionic liquids are collected in this paper with attention to the experimental set-up. The influence and importance of the latter parameters are broadly addressed. Both ramped temperature and isothermal thermogravimetric analysis are discussed, along with state-of-the-art methods, such as TGA-MS and pyrolysis-GC. The strengths and weaknesses of the different methodologies known to date demonstrate that analysis methods should be in line with the application. The combination of data from advanced analysis methods allows us to obtain in-depth information on the degradation processes. Aided with computational methods, the kinetics and thermodynamics of thermal degradation are revealed piece by piece. The better understanding of the behaviour of ionic liquids at high temperature allows selective and application driven design, as well as mathematical prediction for engineering purposes.

  14. ZnS, CdS and HgS Nanoparticles via Alkyl-Phenyl Dithiocarbamate Complexes as Single Source Precursors

    OpenAIRE

    Onwudiwe, Damian C.; Ajibade, Peter A.

    2011-01-01

    The synthesis of II-VI semiconductor nanoparticles obtained by the thermolysis of certain group 12 metal complexes as precursors is reported. Thermogravimetric analysis of the single source precursors showed sharp decomposition leading to their respective metal sulfides. The structural and optical properties of the prepared nanoparticles were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) UV-Vis and photoluminescen...

  15. Advertising Discourse Analysis of FES stores: Killing Love, Cowards Show

    Directory of Open Access Journals (Sweden)

    Cristian Venegas Ahumada

    2013-08-01

    Full Text Available The objective is to analyze the structural and photographic discourse of the Autumn-Winter campaign 2008 of FES stores for young people. This was done by a semiotic theory and a critical-structural methodology of discourse. An analysis of 4 advertising photographs was done, and at once an analysis of the discourse “FES says no to violence against Women”, which explains the campaign’s target. The result is: The discourse was subjected to production condition (society of control and makes advertising a way to homogenize subjectivity of masses to consume. Recognition conditions demonstrate that this advertising discourse of symbolic violence means a type of violation of Men and Women Rights. An action like this requires commitment of Psychology in order to promote the social humanizing change, by means of university teaching and professional tasks.

  16. In situ preparation of magnetic nanocomposites of goethite in a styrene-maleimide copolymer template

    International Nuclear Information System (INIS)

    Sepulveda-Guzman, S.; Perez-Camacho, O.; Rodriguez-Fernandez, O.; Garcia-Zamora, M.

    2005-01-01

    Magnetic composites were prepared by in situ precipitation of α-FeOOH (goethite) using a new styrene-co-N-4 carboxybutylmaleimide cross-linked copolymer as template. Thermogravimetric analysis showed iron oxide content in the composites up to 45%. The iron oxide phase was identified as goethite by X-ray diffraction analysis. Transmission electron microscopy revealed that the crosslinking extent of polymeric templates affected both the shape and dimension of the goethite particles, and consequently, the magnetic behavior of the polymer/iron oxide composites

  17. New fillers in the synthesis of polypropylene nano composites with Ziegler-Natta catalysts; Novas cargas na sintese de nanocompositos de polipropileno com catalisadores Ziegler-Natta

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    2011-07-01

    In this study, Ziegler-Natta catalysts bi-supported on MgCl{sub 2} and natural clays were prepared in order to synthesize polypropylene nanocomposites. The employed clays were bentonite, as reference, as well as halloysite, vermiculite and mica. Propylene polymerizations were carried out using those catalysts and the properties of the obtained materials were analyzed using techniques of thermogravimetric analysis X-ray diffraction, dynamic mechanical thermal analysis e scanning electronic microscopy. Results showed the production of nanocomposites with higher thermal degradation temperature. (author)

  18. New fillers in the synthesis of polypropylene nano composites with Ziegler-Natta catalysts

    International Nuclear Information System (INIS)

    Rosa, Jeferson L.S.; Silva, Marcelo C.V.; Marques, Maria F.V.

    2011-01-01

    In this study, Ziegler-Natta catalysts bi-supported on MgCl 2 and natural clays were prepared in order to synthesize polypropylene nanocomposites. The employed clays were bentonite, as reference, as well as halloysite, vermiculite and mica. Propylene polymerizations were carried out using those catalysts and the properties of the obtained materials were analyzed using techniques of thermogravimetric analysis X-ray diffraction, dynamic mechanical thermal analysis e scanning electronic microscopy. Results showed the production of nanocomposites with higher thermal degradation temperature. (author)

  19. Thermal Degradation Mechanism of a Thermostable Polyester Stabilized with an Open-Cage Oligomeric Silsesquioxane

    Directory of Open Access Journals (Sweden)

    Yolanda Bautista

    2017-12-01

    Full Text Available A polyester composite was prepared through the polymerization of an unsaturated ester resin with styrene and an open-cage oligomeric silsesquioxane with methacrylate groups. The effect of the open-cage oligomeric silsesquioxane on the thermal stability of the thermostable polyester was studied using both thermogravimetric analysis and differential thermal analysis. The results showed that the methacryl oligomeric silsesquioxane improved the thermal stability of the polyester. The decomposition mechanism of the polyester/oligomer silsesquioxane composite was proposed by Fourier transform infrared spectroscopy (FTIR analysis of the volatiles.

  20. Synthesis and Thermal Properties of a Novel Nitrogen-containing Epoxy Resin

    Institute of Scientific and Technical Information of China (English)

    Xing Hong ZHANG; Hong Mei WAN; Yu Qin MIN; Zuo FANG; Guo Rong QI

    2005-01-01

    A new nitrogen-containing epoxy resin (XT resin) was synthesized from chain extension of xylenephenolformaldehyde resin (XPF) and triglycidyl isocyanurate (TGIC) in the presence of base catalyst. FT-IR and 1H-NMR analysis confirmed the chemical structure of XT resin. It was cured with dicyandiamide (DICY) and diaminodiphenyl sulfone (DDS). Dynamic mechanical analysis (DMA) results showed that the introduction of triazine ring provides epoxy polymer with good thermal stability. Furthermore, high char yields at 800℃ in thermogravimetric (TGA)analysis indicated that XT resin had potential flame retardance.

  1. Co-combustion of anthracite coal and wood pellets: Thermodynamic analysis, combustion efficiency, pollutant emissions and ash slagging.

    Science.gov (United States)

    Guo, Feihong; Zhong, Zhaoping

    2018-08-01

    This work presents studies on the co-combustion of anthracite coal and wood pellets in fluidized bed. Prior to the fluidized bed combustion, thermogravimetric analysis are performed to investigate the thermodynamic behavior of coal and wood pellets. The results show that the thermal decomposition of blends is divided into four stages. The co-firing of coal and wood pellets can promote the combustion reaction and reduce the emission of gaseous pollutants, such as SO 2 and NO. It is important to choose the proportion of wood pellets during co-combustion due to the low combustion efficiency caused by large pellets with poor fluidization. Wood pellets can inhibit the volatilization of trace elements, especially for Cr, Ni and V. In addition, the slagging ratio of wood pellets ash is reduced by co-firing with coal. The research on combustion of coal and wood pellets is of great significance in engineering. Copyright © 2018 Elsevier Ltd. All rights reserved.

  2. Polyurethane foam impregnated with lignin as a filler for the removal of crude oil from contaminated water

    Energy Technology Data Exchange (ETDEWEB)

    Santos, O.S.H. [Departamento de Química, Instituto de Ciências Exatas, Universidade Federal de Minas Gerais, Belo Horizonte, Minas Gerais, CEP: 31.270-901 (Brazil); Coelho da Silva, Mercês [Engenharia de Materiais, Universidade Federal de Itajubá—UNIFEI, Campus Universitário de Itabira. Itabira, Minas Gerais, CEP: 35.903-087 (Brazil); Silva, V.R.; Mussel, W.N. [Departamento de Química, Instituto de Ciências Exatas, Universidade Federal de Minas Gerais, Belo Horizonte, Minas Gerais, CEP: 31.270-901 (Brazil); Yoshida, M.I., E-mail: mirene@ufmg.br [Departamento de Química, Instituto de Ciências Exatas, Universidade Federal de Minas Gerais, Belo Horizonte, Minas Gerais, CEP: 31.270-901 (Brazil)

    2017-02-15

    Highlights: • The presence of lignin in polyurethane foams increased oil sorption capacity. • The presence of lignin resulted in a decrease in the hydrophobicity of the foams. • Langmuir isotherm predicted a maximum oil adsorption of 28.9 g g{sup −1} by the PUF-10. • ΔG° (−4.4 kJ mol{sup −1}) indicated that adsorption process by PUF-10 was spontaneous. • The recyclability of the foam showed efficiency greater than 95% after five cycles. - Abstract: The present study describes the influence of the concentration of lignin when used as a filler in polyurethane foam for crude oil sorption. The foams (lignin 0–20 wt%) were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), thermogravimetric analysis, contact angle and density. The FTIR analysis confirmed urethane linkage formation, showing that the chemical structure of the polymer was preserved, despite the addition of different lignin concentrations. Thermogravimetric analysis showed that the presence of lignin has altered the onset temperature (T{sub onset}) of the foams, decreasing as the concentration of lignin is increased. The contact angle analysis showed a decrease in the hydrophobicity of the foams with increasing lignin concentration. All modified foams showed an improvement in the oil sorption capacity in a PUF/oil/water system, and the PUF-10 showed an improvement of about 35.5% compared to the PUF-blank. The Langmuir isotherm showed a better fit to the data and predicted a maximum oil adsorption of 28.9 g g{sup −1} by the PUF-10. The ΔG° value of −4.4 kJ mol{sup −1} indicated that crude oil adsorption process by PUF-10 was spontaneous. The results of reuse of the PUF-10 showed that oil removal efficiency remained greater than 95% after five consecutive cycles.

  3. Palladium nanoparticles supported on layered hydroxide salts and their use in carbon-carbon coupling organic reactions

    OpenAIRE

    Martínez,Maby; Ocampo,Rogelio; Rios,Luz Amalia; Ramírez,Alfonso; Giraldo,Oscar

    2011-01-01

    Palladium nanoparticles supported on zinc hydroxide salts were prepared by intercalation of [PdCl6]2- and its further reduction with ethanol under reflux. All the materials were completely characterized by atomic absorption spectroscopy (AAS), X-ray diffraction (XRD), thermogravimetric/derivative thermogravimetric (TG/DTG) analyses, scanning electron microscopy (SEM), UV-Visible spectrometry and transmission electron microscopy (TEM). TEM analysis confirmed that the palladium nanoparticles we...

  4. Quantitative study of Portland cement hydration by X-ray diffraction/Rietveld analysis and independent methods

    International Nuclear Information System (INIS)

    Scrivener, K.L.; Fuellmann, T.; Gallucci, E.; Walenta, G.; Bermejo, E.

    2004-01-01

    X-ray diffraction (XRD) is a powerful technique for the study of crystalline materials. The technique of Rietveld refinement now enables the amounts of different phases in anhydrous cementitious materials to be determined to a good degree of precision. This paper describes the extension of this technique to a pilot study of the hydration of a typical Portland cement. To validate this XRD-Rietveld analysis technique, its results were compared with independent measures of the same materials by the analysis of backscattered electron images (BSE/IA) and thermogravimetric analysis (TGA). In addition, the internal consistency of the measurements was studied by comparing the XRD estimates of the amounts of hydrates formed with the amounts expected to form from the XRD estimates of the amounts of anhydrous materials reacted

  5. #13ReasonsWhy Health Professionals and Educators are Tweeting: A Systematic Analysis of Uses and Perceptions of Show Content and Learning Outcomes.

    Science.gov (United States)

    Walker, Kimberly K; Burns, Kelli

    2018-04-27

    This study is a content analysis of health professionals' and educators' tweets about a popular Netflix show that depicts teen suicide: 13 Reasons Why. A content analysis of 740 tweets was conducted to determine the main themes associated with professionals' and educators' tweets about the show, as well as the valence of the tweets. Additionally, a thematic analysis of linked content in tweets (n = 178) was conducted to explore additional content shared about the show and modeling outcomes. Results indicated the largest percentage of tweets was related to social learning, particularly about outcomes that could occur from viewing the show. The valence of the tweets about outcomes was more positive than negative. However, linked materials commonly circulated in tweets signified greater concern with unintended learning outcomes. Some of the linked content included media guidelines for reporting on suicide with recommendations that entertainment producers follow the guidelines. This study emphasizes the importance of including social learning objectives in future typologies of Twitter uses and demonstrates the importance of examining linked content in Twitter studies.

  6. Thermodynamic Studies of the Phase Relationships of Nonstoichiometric Cerium Oxides at Higher Temperatures

    DEFF Research Database (Denmark)

    Sørensen, Ole Toft

    1976-01-01

    Partial molar thermodynamic quantities for oxygen in nonstoichiometric cerium oxides were determined by thermogravimetric analysis in CO/CO2 mixtures in the temperature range 900–1400°C. Under these conditions compositions within the range 2.00 greater-or-equal, slanted O/M greater-or-equal, slan......Partial molar thermodynamic quantities for oxygen in nonstoichiometric cerium oxides were determined by thermogravimetric analysis in CO/CO2 mixtures in the temperature range 900–1400°C. Under these conditions compositions within the range 2.00 greater-or-equal, slanted O/M greater...

  7. Genomic analysis of codon usage shows influence of mutation pressure, natural selection, and host features on Marburg virus evolution.

    Science.gov (United States)

    Nasrullah, Izza; Butt, Azeem M; Tahir, Shifa; Idrees, Muhammad; Tong, Yigang

    2015-08-26

    The Marburg virus (MARV) has a negative-sense single-stranded RNA genome, belongs to the family Filoviridae, and is responsible for several outbreaks of highly fatal hemorrhagic fever. Codon usage patterns of viruses reflect a series of evolutionary changes that enable viruses to shape their survival rates and fitness toward the external environment and, most importantly, their hosts. To understand the evolution of MARV at the codon level, we report a comprehensive analysis of synonymous codon usage patterns in MARV genomes. Multiple codon analysis approaches and statistical methods were performed to determine overall codon usage patterns, biases in codon usage, and influence of various factors, including mutation pressure, natural selection, and its two hosts, Homo sapiens and Rousettus aegyptiacus. Nucleotide composition and relative synonymous codon usage (RSCU) analysis revealed that MARV shows mutation bias and prefers U- and A-ended codons to code amino acids. Effective number of codons analysis indicated that overall codon usage among MARV genomes is slightly biased. The Parity Rule 2 plot analysis showed that GC and AU nucleotides were not used proportionally which accounts for the presence of natural selection. Codon usage patterns of MARV were also found to be influenced by its hosts. This indicates that MARV have evolved codon usage patterns that are specific to both of its hosts. Moreover, selection pressure from R. aegyptiacus on the MARV RSCU patterns was found to be dominant compared with that from H. sapiens. Overall, mutation pressure was found to be the most important and dominant force that shapes codon usage patterns in MARV. To our knowledge, this is the first detailed codon usage analysis of MARV and extends our understanding of the mechanisms that contribute to codon usage and evolution of MARV.

  8. Synthesis and characterization of ZSM-12 type zeolytic catalysts by using different aluminium sources in the petroleum industry; Sintese e caracterizacao de catalisadores zeoliticos do tipo ZSM-12 utilizando diferentes fontes de aluminio na industria do petroleo

    Energy Technology Data Exchange (ETDEWEB)

    Moraes, Marilia R.F.S.; Jesus, Daniela B.; Souza, Marcelo J.B. [Universidade Federal de Sergipe (UFS), Sao Cristovao, SE (Brazil). Dept. de Engenharia Quimica; Santos, Consuelo D.; Machado, Sanny W.M.; Pedrosa, Anne M. Garrido [Universidade Federal de Sergipe (UFS), Sao Cristovao, SE (Brazil). Dept. de Quimica

    2010-12-15

    The main objective was to synthesize and characterize ZSM-12 zeolites from different sources of aluminium, using hydrothermal method and characterize the catalysts synthesized by X-ray diffractions, thermal analysis and infrared absorption spectroscopy. The X-ray diffractogram showed the formation of zeolites of the family pantasil crystalline. Thermogravimetric curves and FTIR spectra were utilized by monitoring the removal of template and by monitoring the maintenance of zeolite structure. (author)

  9. The influence of expanded graphite on thermal properties for paraffin/high density polyethylene/chlorinated paraffin/antimony trioxide as a flame retardant phase change material

    International Nuclear Information System (INIS)

    Zhang Ping; Song Lei; Lu Hongdian; Wang Jian; Hu Yuan

    2010-01-01

    The influences of expanded graphite (EG) on the thermal properties of chlorinated paraffin (CP) and antimony trioxide (AT) on phase change material which bases on paraffin/high density polyethylene (HDPE) are studied. Differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), thermogravimetric analysis-Fourier transform infrared spectrometry (TGA-FTIR), microscale combustion calorimeter (MCC) and cone calorimeter (CONE) were used to evaluate the influence of EG on paraffin/HDPE/CP/AT system. The DSC results indicated that the latent heat value of PCM could be increased when the mass fraction of HDPE was decreased in the PCM, and EG could confine the molecular heat movement of paraffin. EG could improve the thermal stability and increase the char residue at high temperature for paraffin/HDPE/CP/AT hybrid. The volatilized products formed on thermal degradation of paraffin/HDPE/CP/AT with EG showed the release of CO 2 gas was hastened and increased, and the amount of combustible gases were decreased by TGA-FTIR analysis. The MCC and CONE results presented that the flame retardant efficiency of CP/AT could be improved by adding EG in paraffin/HDPE/CP/AT system.

  10. Vibrational spectroscopic study of poldervaartite CaCa[SiO3(OH)(OH)

    Science.gov (United States)

    Frost, Ray L.; López, Andrés; Scholz, Ricardo; Lima, Rosa Malena Fernandes

    2015-02-01

    We have studied the mineral poldervaartite CaCa[SiO3(OH)(OH)] which forms a series with its manganese analogue olmiite CaMn[SiO3(OH)](OH) using a range of techniques including scanning electron microscopy, thermogravimetric analysis, Raman and infrared spectroscopy. Chemical analysis shows the mineral is reasonably pure and contains only calcium and manganese with low amounts of Al and F. Thermogravimetric analysis proves the mineral decomposes at 485 °C with a mass loss of 7.6% compared with the theoretical mass loss of 7.7%. A strong Raman band at 852 cm-1 is assigned to the SiO stretching vibration of the SiO3(OH) units. Two Raman bands at 914 and 953 cm-1 are attributed to the antisymmetric vibrations. Intense prominent peaks observed at 3487, 3502, 3509, 3521 and 3547 cm-1 are assigned to the OH stretching vibration of the SiO3(OH) units. The observation of multiple OH bands supports the concept of the non-equivalence of the OH units. Vibrational spectroscopy enables a detailed assessment of the molecular structure of poldervaartite.

  11. Factor analysis shows association between family activity environment and children's health behaviour.

    Science.gov (United States)

    Hendrie, Gilly A; Coveney, John; Cox, David N

    2011-12-01

    To characterise the family activity environment in a questionnaire format, assess the questionnaire's reliability and describe its predictive ability by examining the relationships between the family activity environment and children's health behaviours - physical activity, screen time and fruit and vegetable intake. This paper describes the creation of a tool, based on previously validated scales, adapted from the food domain. Data are from 106 children and their parents (Adelaide, South Australia). Factor analysis was used to characterise factors within the family activity environment. Pearson-Product Moment correlations between the family environment and child outcomes, controlling for demographic variation, were examined. Three factors described the family activity environment - parental activity involvement, opportunity for role modelling and parental support for physical activity - and explained 37.6% of the variance. Controlling for demographic factors, the scale was significantly correlated with children's health behaviour - physical activity (r=0.27), screen time (r=-0.24) and fruit and vegetable intake (r=0.34). The family activity environment questionnaire shows high internal consistency and moderate predictive ability. This study has built on previous research by taking a more comprehensive approach to measuring the family activity environment. This research suggests the family activity environment should be considered in family-based health promotion interventions. © 2011 The Authors. ANZJPH © 2011 Public Health Association of Australia.

  12. Synthesis, Thermal, Electrical and Catalytic Studies of Some Transition Metal Polychelates of Bis-bidentate Schiff Base

    Institute of Scientific and Technical Information of China (English)

    BANSOD Ashish; ASWAR Anand

    2007-01-01

    Polychelates of Mn(Ⅱ),Fe(Ⅱ),Co(Ⅱ), Ni(Ⅱ),Cu(Ⅱ),Zn(Ⅱ) and Cd(Ⅱ) with the bis salen-type ligand derivedfrom 4,4'-bis[(salicylaldehyde-5)azo]biphenyl and 1,4-diaminobutane have been synthesized.All the polychelates have been characterized by elemental analysis,magnetic susceptibility measurements,IR,electronic spectra and thermogravimetric studies.All the complexes isolated in solid state are dark coloured and insoluble in water and common organic solvents.The ligand behaves as a bis-bidentate molecule coordinating through the phenolic oxygen and azomethine nitrogen atoms.The thermal decomposition of these metal complexes was investigated by thermogravimetric analysis and data have been analyzed for kinetic parameters using Broido equation.The solid-state electrical conductivity of the ligand and its polychelates in the form of compressed pellet was studied in the temperature range from 313 to 413 K.All the polychelates were found to show semiconducting nature.The Mn(Ⅱ),Fe(Ⅱ),Co(Ⅱ) and Ni(Ⅱ) polychelates have been assessed for the catalytic epoxidation of styrene.

  13. Characterising the combustion behaviour of New Zealand coals by thermogravimetry

    Energy Technology Data Exchange (ETDEWEB)

    Benfell, K.E.; Beamish, B.B.; Rodgers, K.A. [University of Auckland, Auckland (New Zealand). Dept. of Geology

    1995-12-31

    Thirty-three New Zealand coals were subjected to thermogravimetric analysis (TG) and derivative thermogravimetric analysis (DTG) to evaluate the techniques` applicability to New Zealand coals. Generally, New Zealand sub-bituminous coals have lower burnout temperatures than bituminous coals. However, local and regional differences occur, where some sub-bituminous coals show both higher and lower char burnout temperatures than may be otherwise expected from their rank and T{sub 6} values (the peak temperature where the rate of weight loss of the sample is the greatest). There is a sizeable variations in the char burnout temperature (T{sub 8}) (465 to 636{degree}C) in coals with volatile matter contents above 40%, whereas coals with lower volatile contents have T{sub 8} values around 646{degree}C. The temperature of char burnout gives a better indication of combustion efficiency than rank or volatile matter content alone. Industrial operators could use this technique to provide an indication of burnout performance before a coal is purchased, assisting evaluation of the coal`s suitability for a particular usage. 10 refs., 4 figs., 3 tabs.

  14. Radiographic analysis of odontogenic cysts showing displacement of the mandibular canal

    International Nuclear Information System (INIS)

    Cho, Bong Hae

    2003-01-01

    To assess the radiographic findings of odontogenic cysts showing displacement of the mandibular canal using computed tomographic (CT) and panoramic images. CT and panoramic images of 63 odontogenic cysts (27 dentigerous, 16 odontogenic keratocysts, and 20 radicular cysts) were analyzed to evaluate the following parameters: the dimension and shape of the cysts, and the effect of the cysts on the mandibular canal and cortical plates. Of the 63 cysts examined in the study, 35 (55.6%) showed inferior displacement of the mandibular canal and 46 (73.0%) showed perforation of the canal. There were statistically significant differenced between CT and panoramic images in depicting displacement and perforation of the mandibular canal. Cortical expansion was seen in 46 cases (73.0%) and cortical perforation in 23 cases (36.5%). The radicular cysts showed cortical expansion and perforation less frequently than the other cyst groups. Large cysts of mandible should be evaluated by multiplanar CT images in order to detect the mandibular canal and cortical bone involvement.

  15. Eucalyptus kraft pulp production: Thermogravimetry monitoring

    International Nuclear Information System (INIS)

    Barneto, Agustin G.; Vila, Carlos; Ariza, Jose

    2011-01-01

    Highlights: → Thermogravimetric analysis can be used to monitor the pulping process in a pulp mill. → ECF bleaching process affects the crystalline cellulose volatilization. → The fibre size has an influence on composition and thermal behavior of pulp. - Abstract: Under oxidative environment the thermal degradation of lignocellulosic materials like wood or pulp is sensitive to slight composition changes. For this, in order to complement the chemical and X-ray diffraction results, thermogravimetric analyses (TGA) were used to monitor pulp production in a modern pulp mill. Runs were carried out on crude, oxygen delignified and bleached pulps from three eucalyptus woods from different species and geographical origins. Moreover, with the modeling of thermogravimetric data, it was possible to obtain an approximate composition of samples which includes crystalline and amorphous cellulose. TGA results show that pulping has an intensive effect on bulk lignin and hemicellulose, but it has limited influence on the removal of these substances when they are linked to cellulose microfibril. The stages of oxygen delignification and bleaching, based in chlorine dioxide and hydrogen peroxide, increase the crystalline cellulose volatilization rate. These changes are compatible with a more crystalline microfibril. The influence of the fibre size on pulp composition, crystallinity and thermal degradation behavior was observed.

  16. Kinetics of the Thermal Degradation of Granulated Scrap Tyres: a Model-free Analysis

    Directory of Open Access Journals (Sweden)

    Félix A. LÓPEZ

    2013-12-01

    Full Text Available Pyrolysis is a technology with a promising future in the recycling of scrap tyres. This paper determines the thermal decomposition behaviour and kinetics of granulated scrap tyres (GST by examining the thermogravimetric/derivative thermogravimetric (TGA/DTG data obtained during their pyrolysis in an inert atmosphere at different heating rates. The model-free methods of Friedman, Flynn-Wall-Ozawa and Coats-Redfern were used to determine the reaction kinetics from the DTG data. The apparent activation energy and pre-exponential factor for the degradation of GST were calculated. A comparison with the results obtained by other authors was made.DOI: http://dx.doi.org/10.5755/j01.ms.19.4.2947

  17. From root to fruit: RNA-Seq analysis shows that arbuscular mycorrhizal symbiosis may affect tomato fruit metabolism.

    Science.gov (United States)

    Zouari, Inès; Salvioli, Alessandra; Chialva, Matteo; Novero, Mara; Miozzi, Laura; Tenore, Gian Carlo; Bagnaresi, Paolo; Bonfante, Paola

    2014-03-21

    Tomato (Solanum lycopersicum) establishes a beneficial symbiosis with arbuscular mycorrhizal (AM) fungi. The formation of the mycorrhizal association in the roots leads to plant-wide modulation of gene expression. To understand the systemic effect of the fungal symbiosis on the tomato fruit, we used RNA-Seq to perform global transcriptome profiling on Moneymaker tomato fruits at the turning ripening stage. Fruits were collected at 55 days after flowering, from plants colonized with Funneliformis mosseae and from control plants, which were fertilized to avoid responses related to nutrient deficiency. Transcriptome analysis identified 712 genes that are differentially expressed in fruits from mycorrhizal and control plants. Gene Ontology (GO) enrichment analysis of these genes showed 81 overrepresented functional GO classes. Up-regulated GO classes include photosynthesis, stress response, transport, amino acid synthesis and carbohydrate metabolism functions, suggesting a general impact of fungal symbiosis on primary metabolisms and, particularly, on mineral nutrition. Down-regulated GO classes include cell wall, metabolism and ethylene response pathways. Quantitative RT-PCR validated the RNA-Seq results for 12 genes out of 14 when tested at three fruit ripening stages, mature green, breaker and turning. Quantification of fruit nutraceutical and mineral contents produced values consistent with the expression changes observed by RNA-Seq analysis. This RNA-Seq profiling produced a novel data set that explores the intersection of mycorrhization and fruit development. We found that the fruits of mycorrhizal plants show two transcriptomic "signatures": genes characteristic of a climacteric fleshy fruit, and genes characteristic of mycorrhizal status, like phosphate and sulphate transporters. Moreover, mycorrhizal plants under low nutrient conditions produce fruits with a nutrient content similar to those from non-mycorrhizal plants under high nutrient conditions

  18. Biodegradable green composites reinforced by the fiber recycling from disposable chopsticks

    International Nuclear Information System (INIS)

    Shih, Yeng-Fong; Huang, Chien-Chung; Chen, Po-Wei

    2010-01-01

    The use of disposable chopsticks is very popular in chopsticks-using countries, such as Taiwan, China and Japan, and is one of the major sources of waste in these countries. In this study, the fiber recycling from disposable chopsticks was chemically modified by coupling agents. Furthermore, the modified fiber was added to the biodegradable polymer (polylactic acid, PLA), to form novel fiber-reinforced green composites. These composites prepared by melt-mixing method, were examined by scanning electron microscopy, differential scanning calorimetry, thermogravimetric analysis, and mechanical tests. The results indicated that the T g of PLA was increased by the addition of fiber, which may improve the heat resistance of PLA. The thermogravimetric analysis of the composites showed that the degradation process of fiber-filled systems started earlier than that of plain PLA, but possessed a higher char yield. Mechanical tests showed that the tensile strength of the composites markedly increased with the fiber content, reaching 115 MPa in the case of being reinforced with 40 phr fiber, which is about 3 times higher as compared to the pristine PLA. Furthermore, this type of reinforced PLA would be more environmental friendly than the artificial additive-reinforced one, and could effectively reduce and reuse the waste of disposable chopsticks.

  19. Tomato Fruits Show Wide Phenomic Diversity but Fruit Developmental Genes Show Low Genomic Diversity.

    Directory of Open Access Journals (Sweden)

    Vijee Mohan

    Full Text Available Domestication of tomato has resulted in large diversity in fruit phenotypes. An intensive phenotyping of 127 tomato accessions from 20 countries revealed extensive morphological diversity in fruit traits. The diversity in fruit traits clustered the accessions into nine classes and identified certain promising lines having desirable traits pertaining to total soluble salts (TSS, carotenoids, ripening index, weight and shape. Factor analysis of the morphometric data from Tomato Analyzer showed that the fruit shape is a complex trait shared by several factors. The 100% variance between round and flat fruit shapes was explained by one discriminant function having a canonical correlation of 0.874 by stepwise discriminant analysis. A set of 10 genes (ACS2, COP1, CYC-B, RIN, MSH2, NAC-NOR, PHOT1, PHYA, PHYB and PSY1 involved in various plant developmental processes were screened for SNP polymorphism by EcoTILLING. The genetic diversity in these genes revealed a total of 36 non-synonymous and 18 synonymous changes leading to the identification of 28 haplotypes. The average frequency of polymorphism across the genes was 0.038/Kb. Significant negative Tajima'D statistic in two of the genes, ACS2 and PHOT1 indicated the presence of rare alleles in low frequency. Our study indicates that while there is low polymorphic diversity in the genes regulating plant development, the population shows wider phenotype diversity. Nonetheless, morphological and genetic diversity of the present collection can be further exploited as potential resources in future.

  20. Recruitment Methods and Show Rates to a Prostate Cancer Early Detection Program for High-Risk Men: A Comprehensive Analysis

    Science.gov (United States)

    Giri, Veda N.; Coups, Elliot J.; Ruth, Karen; Goplerud, Julia; Raysor, Susan; Kim, Taylor Y.; Bagden, Loretta; Mastalski, Kathleen; Zakrzewski, Debra; Leimkuhler, Suzanne; Watkins-Bruner, Deborah

    2009-01-01

    Purpose Men with a family history (FH) of prostate cancer (PCA) and African American (AA) men are at higher risk for PCA. Recruitment and retention of these high-risk men into early detection programs has been challenging. We report a comprehensive analysis on recruitment methods, show rates, and participant factors from the Prostate Cancer Risk Assessment Program (PRAP), which is a prospective, longitudinal PCA screening study. Materials and Methods Men 35–69 years are eligible if they have a FH of PCA, are AA, or have a BRCA1/2 mutation. Recruitment methods were analyzed with respect to participant demographics and show to the first PRAP appointment using standard statistical methods Results Out of 707 men recruited, 64.9% showed to the initial PRAP appointment. More individuals were recruited via radio than from referral or other methods (χ2 = 298.13, p < .0001). Men recruited via radio were more likely to be AA (p<0.001), less educated (p=0.003), not married or partnered (p=0.007), and have no FH of PCA (p<0.001). Men recruited via referrals had higher incomes (p=0.007). Men recruited via referral were more likely to attend their initial PRAP visit than those recruited by radio or other methods (χ2 = 27.08, p < .0001). Conclusions This comprehensive analysis finds that radio leads to higher recruitment of AA men with lower socioeconomic status. However, these are the high-risk men that have lower show rates for PCA screening. Targeted motivational measures need to be studied to improve show rates for PCA risk assessment for these high-risk men. PMID:19758657

  1. Thermogravimetric experiments with titanium

    International Nuclear Information System (INIS)

    Porter, L.J.; Longhurst, G.R.

    1991-02-01

    In the process of preparing for pyrophoricity experiments involving uranium, we conducted hydriding and air-exposure experiments on titanium. In these experiments the hydriding reactions and response to air-exposure was generally within the range expected based on work reported by others. One aberrant behavior was a sudden weight gain followed by a significant weight loss. We speculate that loss may be due to hydrogen evolution from the TiH 2 resulting from local heating by oxidation reactions. We verified that titanium is not pyrophoric at temperatures less than 750 degree C. 18 refs. 1 fig

  2. Interpretation of biomass gasification yields regarding temperature intervals under nitrogen-steam atmosphere

    Energy Technology Data Exchange (ETDEWEB)

    Haykiri-Acma, H.; Yaman, S. [Istanbul Technical University, Chemical and Metallurgical Engineering Faculty, Chemical Engineering Department, 34469 Maslak, Istanbul (Turkey)

    2007-04-15

    Gasification of some agricultural waste biomass samples (sunflower shell, pine cone, cotton refuse, and olive refuse) and colza seed was performed using a thermogravimetric analyzer at temperatures up to 1273 K with a constant heating rate of 20 K/min under a dynamic nitrogen-steam atmosphere. Derivative thermogravimetric analysis profiles of the samples were derived from the non-isothermal thermogravimetric analysis data. Gasification yields of the biomass samples at temperature intervals of 473-553 K, 553-653 K, 653-773 K, 773-973 K, and 973-1173 K were investigated considering the successive stages of ''evolution of carbon oxides'', ''start of hydrocarbon evolution'', ''evolution of hydrocarbons'', ''dissociation'', and ''evolution of hydrogen'', respectively. Although, there were some interactions between these stages, some evident relations were observed between the gasification yields in a given stage and the chemical properties of the parent biomass materials. (author)

  3. Study of thermal stability and degradation of fire resistant candidate polymers for aircraft interiors

    Science.gov (United States)

    Hsu, M. T. S.

    1976-01-01

    The thermochemistry of bismaleimide resins and phenolphthalein polycarbonate was studied. Both materials are fire-resistant polymers and may be suitable for aircraft interiors. The chemical composition of the polymers has been determined by nuclear magnetic resonance and infrared spectroscopy and by elemental analysis. Thermal properties of these polymers have been characterized by thermogravimetric analyses. Qualitative evaluation of the volatile products formed in pyrolysis under oxidative and non-oxidative conditions has been made using infrared spectrometry. The residues after pyrolysis were analyzed by elemental analysis. The thermal stability of composite panel and thermoplastic materials for aircraft interiors was studied by thermogravimetric analyses.

  4. Examination of the Thermo-mechanical Properties of E-Glass/Carbon Composites

    Directory of Open Access Journals (Sweden)

    Hande Sezgin

    2017-12-01

    Full Text Available Eight-ply E-glass, carbon and E-glass/carbon fabric-reinforced polyester based hybrid composites were manufactured in this study. A vacuum infusion system was used as the production method. Dynamic mechanical analysis, thermogravimetric analysis and differential scanning calorimetry analysis were conducted to examine the thermo-mechanical properties of composite samples. The effect of reinforcement type and different stacking sequences of fabric plies on the thermo-mechanical properties of composite samples were also investigated. Results showed that the type and alignment of reinforcement material has a signifi cant effect on the dynamic mechanical properties of composite samples.

  5. Characterization and stability analysis of zinc oxide nanoencapsulated conjugated linoleic acid.

    Science.gov (United States)

    Choy, Jin-Ho; Shin, Jiwon; Lim, Seung-Yong; Oh, Jae-Min; Oh, Mi-Hwa; Oh, Sangsuk

    2010-08-01

    Nanoencapsulation technology has a diverse range of applications, including drug-delivery systems (DDS) and cosmetic and chemical carriers, because it can deliver various bio- and organic-molecules and improve their stabilities. Conjugated linoleic acid (CLA) has health benefits, including being an anticancer agent, but it decreases flavor due to volatiles from oxidation. To improve the stability of CLA for food applications, nanoencapsulated CLA was synthesized for use in zinc basic salt (ZBS) and characterized by powder X-ray diffractometry, thermogravimetric analysis (TGA), elemental CHN analysis, inductively coupled plasma (ICP) analysis, UV/VIS spectroscopy, and FTIR spectroscopy. The thermal stability of nanoencapsulated CLA at 180 degrees C, a temperature similar to that used in cooking, was analyzed by gas chromatography. The gallery height of nanoencapsulated CLA was determined to be approximately 26 A through powder X-ray diffractometry; therefore, the CLA molecules were closely packed with zig-zag form between the intracrystalline spaces of nano particles. Elemental CHN analysis and ICP data determined the chemical composition of nanoencapsulated CLA to be Zn(4.86)(OH)(8.78)(CLA)(0.94). By TGA, it was determined about 45% (wt/wt) of weight loss corresponded to CLA, which is good agreement with the 42.13% (wt/wt) determined from high-performance liquid chromatography (HPLC) and elemental CHN analysis. UV/VIS spectroscopy and Fourier-transformed infrared (FTIR) spectroscopy showed encapsulated CLA maintained a conjugated diene structure, supporting the presence of CLA. Nanoencapsulation improved the thermal stability of CLA by about 25%, compared to pristine CLA. Practical Application: This system can be used for protection of encapsulated negatively-charged food ingredients from thermal processing.

  6. Fast Pyrolysis of Four Lignins from Different Isolation Processes Using Py-GC/MS

    OpenAIRE

    Lin, Xiaona; Sui, Shujuan; Tan, Shun; Pittman, Charles; Sun, Jianping; Zhang, Zhijun

    2015-01-01

    Pyrolysis is a promising approach that is being investigated to convert lignin into higher value products including biofuels and phenolic chemicals. In this study, fast pyrolysis of four types of lignin, including milled Amur linden wood lignin (MWL), enzymatic hydrolysis corn stover lignin (EHL), wheat straw alkali lignin (AL) and wheat straw sulfonate lignin (SL), were performed using pyrolysis gas-chromatography/mass spectrometry (Py-GC/MS). Thermogravimetric analysis (TGA) showed that the...

  7. Synthesis and characterization of poly(glycerol citrate/sebacate)

    International Nuclear Information System (INIS)

    Brioude, Michel M.; Guimaraes, Danilo H.; Fiuza, Raigenis P.; Boaventura, Jaime S.; Jose, Nadia M.

    2011-01-01

    In this work were prepared and characterized the poly(glycerol citrate/sebacate) in three different ratios between acids. The polymers were prepared by a polycondensation reaction between glycerol and citric/sebacic acids and characterized by X-ray diffraction (XRD), infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), scanning differential calorimetry (DSC), scanning electron microscopy (SEM). The results showed that the polymers are polyesters and its crystallinity, thermal and morphological properties were modified by sebacic acid adding. (author)

  8. Synthesis and characterization of poly(glycerol citrate/sebacate); Preparacao de caracterizacao do poli(glicerol citrato/sebacato)

    Energy Technology Data Exchange (ETDEWEB)

    Brioude, Michel M.; Guimaraes, Danilo H.; Fiuza, Raigenis P.; Boaventura, Jaime S.; Jose, Nadia M., E-mail: mbrioude@gmail.com [Universidade Federal da Bahia - UFBA, Instituto de Quimica, Salvador, BA (Brazil)

    2011-07-01

    In this work were prepared and characterized the poly(glycerol citrate/sebacate) in three different ratios between acids. The polymers were prepared by a polycondensation reaction between glycerol and citric/sebacic acids and characterized by X-ray diffraction (XRD), infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), scanning differential calorimetry (DSC), scanning electron microscopy (SEM). The results showed that the polymers are polyesters and its crystallinity, thermal and morphological properties were modified by sebacic acid adding. (author)

  9. Preparation and characterization of gelatin/cerium(Ⅲ) film

    Institute of Scientific and Technical Information of China (English)

    黄崇军; 黄雅钦; 田娜; 童元建; 殷瑞贤

    2010-01-01

    A novel gelatin film with antibacterial activity was prepared by electrostatic crosslinking using cerium (Ⅲ) nitrate hexahydrate as the crosslinking agent. The structure and properties of the films were investigated by Fourier transform infrared spectra, tensile tests, thermogravimetric analysis, static drop contact angle and disc diffusion method. The results showed that cross-linking could not only improve the thermal and mechanical properties and lower the hydrophilic property of the films, but also make...

  10. HIV-1 phylogenetic analysis shows HIV-1 transits through the meninges to brain and peripheral tissues.

    Science.gov (United States)

    Lamers, Susanna L; Gray, Rebecca R; Salemi, Marco; Huysentruyt, Leanne C; McGrath, Michael S

    2011-01-01

    Brain infection by the human immunodeficiency virus type 1 (HIV-1) has been investigated in many reports with a variety of conclusions concerning the time of entry and degree of viral compartmentalization. To address these diverse findings, we sequenced HIV-1 gp120 clones from a wide range of brain, peripheral and meningeal tissues from five patients who died from several HIV-1 associated disease pathologies. High-resolution phylogenetic analysis confirmed previous studies that showed a significant degree of compartmentalization in brain and peripheral tissue subpopulations. Some intermixing between the HIV-1 subpopulations was evident, especially in patients that died from pathologies other than HIV-associated dementia. Interestingly, the major tissue harboring virus from both the brain and peripheral tissues was the meninges. These results show that (1) HIV-1 is clearly capable of migrating out of the brain, (2) the meninges are the most likely primary transport tissues, and (3) infected brain macrophages comprise an important HIV reservoir during highly active antiretroviral therapy. Copyright © 2010 Elsevier B.V. All rights reserved.

  11. Dioscorea alata tuber proteome analysis shows over thirty dioscorin isoforms and novel tuber proteins.

    Science.gov (United States)

    Sharma, Shruti; Gupta, Ravi; Deswal, Renu

    2017-05-01

    In Dioscorea, dioscorin (31 kDa) is the major storage protein constituting 85% of the total tuber proteins. An integrated proteomic and biochemical approach was used to understand the physiological role of dioscorin in the two contrasting growth stages (germinating and mature tuber). HPLC analysis showed 3 fold reduction in mannitol and 12.88 and 1.24 fold increase in sucrose and maltose in the germinating tuber. A 1.8 and 3 fold increase in sucrose phosphate synthase and mannitol dehydrogenase activity respectively was observed in the germinating tuber while a 2 fold higher invertase probably lowers the sucrose accumulation in the mature tuber. SDS-PAGE and 2-D maps of the mature and germinating tubers confirmed depletion (more than 50%) of dioscorin on germination. Dioscorin was purified using ion exchange and gel filtration chromatography with 43.32 fold purification and 38.16 yield. Out of a trail of 35 spots at 31 kDa only 12 spots (identified as dioscorin isoforms) were present in the 2D gel of the purified fraction. To search for other tuber proteins besides dioscorin, the unbound fractions of DEAE column were analysed by 2DGE. DREB 1A, caffeic acid 3-O-methyltransferase and Rab-1 small GTP binding protein were identified perhaps for the first time in the Dioscorea proteome. The interactome analysis revealed these to be involved in oxidative stress, carotenoid synthesis and vesicular transport. This is perhaps the first attempt to identify tuber proteome (although limited) and to understand the physiological significance of these proteins. Copyright © 2017 Elsevier Masson SAS. All rights reserved.

  12. Potassium and soot interaction in fast biomass pyrolysis at high temperatures

    DEFF Research Database (Denmark)

    Trubetskaya, Anna; Hofmann Larsen, Flemming; Shchukarev, Andrey

    2018-01-01

    2 reactivity was studied by thermogravimetric analysis. The XPS results showed that potassium incorporation with oxygen-containing surface groups in the soot matrix did not occur during high temperature pyrolysis. The potassium was mostly found as water-soluble salts such as KCl, KOH, KHCO3 and K2CO...... potassium amount was incorporated in the soot matrix during pyrolysis. Raman spectroscopy results showed that the carbon chemistry of biomass soot also affected the CO2 reactivity. The less reactive pinewood soot was more graphitic than herbaceous biomass soot samples with the disordered carbon structure...

  13. Fulltext PDF

    Indian Academy of Sciences (India)

    differential thermal analysis (TG–DTA). ... −2 was observed. Keywords. Ceramics; fuel cells; solid state reactions; electromotive force; ionic conduction. 1. ... thermal analysing balance based on the thermogravimetric/ differential thermal analysis ...

  14. Analysis of the structural stability of the smectite submitted to high pressures and temperatures; Analise da estabilidade estrutural da esmectita sob altas pressoes e altas temperaturas

    Energy Technology Data Exchange (ETDEWEB)

    Alabarse, Frederico Gil

    2009-10-15

    The thermal stability of bentonite is of particular interest for containment barrier in nuclear waste disposal facilities. However, very little is known about the stability of smectite (principal component of bentonite) under high-pressure and high-temperature conditions (HPHT). The objective of this work was to investigate the stability of the smectite structure under HP-HT conditions. The HP-HT experiments were performed on toroidal chambers (TC) with pressure up 7.7 GPa and temperatures of 1000 deg C. The samples were characterized by X-ray diffraction after the HP-HT processing. Furthermore, one sample from the original material was analyzed using Fourier transformed infra-red (FTIR) in situ measurements on a diamond anvil cell (DAC) in experiments up to 12 GPa. The original sample of bentonite, calcium dioctahedral montmorillonite with small fraction of quartz, was characterized by FTIR, XRD, X-ray fluorescence (XRF), scanning electron microscopy (SEM), surface area, thermogravimetric analysis (TGA) and differential thermal analysis (DTA). In the experiment performed using the DAC up to 12 GPa, the FTIR in situ measurements analysis showed that the smectite structure is stable with a reversible deformation in the Si-O bond and that the smectite did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 250 deg C of temperature, during 3.5 h showed, after analysis by XRD and FTIR, that the smectite structure is stable and did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 1000 deg C of temperature, during 3.5 h showed, after analysis by XRD and SEM, the transformation of bentonite to the mineral assemblage: Coesite, Quartz, Kyanite and Pyrope. (author)

  15. Kenaf fiber-reinforced copolyester biocomposites

    CSIR Research Space (South Africa)

    Mokhothu, Thabang H

    2011-12-01

    Full Text Available scanning calorimetry (DSC), thermogravimetric analysis (TGA), dynamic mechanical analysis (DMA), tensile properties, environmental scanning electron microscopy (ESEM), and biodegradability. The extent of silane initiated grafting was followed by gel content...

  16. Genome-wide analysis of adolescent psychotic-like experiences shows genetic overlap with psychiatric disorders.

    Science.gov (United States)

    Pain, Oliver; Dudbridge, Frank; Cardno, Alastair G; Freeman, Daniel; Lu, Yi; Lundstrom, Sebastian; Lichtenstein, Paul; Ronald, Angelica

    2018-03-31

    This study aimed to test for overlap in genetic influences between psychotic-like experience traits shown by adolescents in the community, and clinically-recognized psychiatric disorders in adulthood, specifically schizophrenia, bipolar disorder, and major depression. The full spectra of psychotic-like experience domains, both in terms of their severity and type (positive, cognitive, and negative), were assessed using self- and parent-ratings in three European community samples aged 15-19 years (Final N incl. siblings = 6,297-10,098). A mega-genome-wide association study (mega-GWAS) for each psychotic-like experience domain was performed. Single nucleotide polymorphism (SNP)-heritability of each psychotic-like experience domain was estimated using genomic-relatedness-based restricted maximum-likelihood (GREML) and linkage disequilibrium- (LD-) score regression. Genetic overlap between specific psychotic-like experience domains and schizophrenia, bipolar disorder, and major depression was assessed using polygenic risk score (PRS) and LD-score regression. GREML returned SNP-heritability estimates of 3-9% for psychotic-like experience trait domains, with higher estimates for less skewed traits (Anhedonia, Cognitive Disorganization) than for more skewed traits (Paranoia and Hallucinations, Parent-rated Negative Symptoms). Mega-GWAS analysis identified one genome-wide significant association for Anhedonia within IDO2 but which did not replicate in an independent sample. PRS analysis revealed that the schizophrenia PRS significantly predicted all adolescent psychotic-like experience trait domains (Paranoia and Hallucinations only in non-zero scorers). The major depression PRS significantly predicted Anhedonia and Parent-rated Negative Symptoms in adolescence. Psychotic-like experiences during adolescence in the community show additive genetic effects and partly share genetic influences with clinically-recognized psychiatric disorders, specifically schizophrenia and

  17. Spectroscopic Analysis of a Theropod Dinosaur (Reptilia, Archosauria from the Ipubi Formation, Araripe Basin, Northeastern Brazil

    Directory of Open Access Journals (Sweden)

    João Hermínio da Silva

    2013-01-01

    Full Text Available The Araripe Sedimentary Basin is known by the excellence of its fossils, regarding the preservation, diversity, and quantity. Here, we present a spectroscopic analysis using several experimental techniques (X-ray energy dispersion spectroscopy, Fourier-transform infrared spectroscopy as well as X-ray diffraction and thermogravimetric analysis applied in small fragments of bones from the posterior members of a theropod dinosaur. The results agree regarding the different composition of the stone matrix and the fossilized bone, indicating a partial substitution of the material by elements present in the depositional environment. However, differently from what is believed to occur, there is evidence that pyritization is not the only mechanism of fossilization for a specimen of Ipubi formation, but calcification, additionally, plays an important role in the fossil production of this Formation.

  18. Production of Synthetic Phosphoanhydrite and Its Use as a Binder in Self-Leveling Underlayments (SLU)

    OpenAIRE

    Schaefer, Cec?lia Ogliari; Cheriaf, Malik; Rocha, Jana?de Cavalcante

    2017-01-01

    An experimental study was conducted to investigate the potential use of phosphogypsum (PG) to produce self-leveling underlayments. The study was designed in two stages. Initially a phosphoanhydrite (PA) was produced by heating phosphogypsum at temperatures of 350 ?C, 450 ?C, 550 ?C, and 650 ?C. Two periods of heating were applied (2 and 4 h). The formation of anhydrite was determined by thermogravimetric analysis (DTA-TG) and confirmed by X-ray diffraction (XRD). The results show that anhydri...

  19. Synthesis, spectral and thermal studies of pyridyl adducts of Zn(II) and Cd(II) dithiocarbamates, and their use as single source precursors for ZnS and CdS nanoparticles

    OpenAIRE

    Onwudiwe, Damian C.; Strydom, Christien A.; Jordaan, Anine; Oluwafemi, Oluwatobi S.; Hosten, Eric

    2014-01-01

    The synthesis, spectroscopic characterisation, and thermal studies of pyridyl adducts of Zn(II) and Cd(II) complexes of N-ethyl-N-phenyl dithiocarbamate, represented as [ZnL2py] and [CdL2py2], are reported. Single-crystal X-ray structural analysis of the Zn compound showed that it is five-coordinate with four sulphurs from dithiocarbamate and one nitrogen from pyridine in a distorted square pyramidal geometry. The thermogravimetric studies indicate that the zinc and cadmium compou...

  20. Synthesis, spectral characterization thermal stability, antimicrobial studies and biodegradation of starch–thiourea based biodegradable polymeric ligand and its coordination complexes with [Mn(II), Co(II), Ni(II), Cu(II), and Zn(II)] metals

    OpenAIRE

    Nahid Nishat; Ashraf Malik

    2016-01-01

    A biodegradable polymer was synthesized by the modification reaction of polymeric starch with thiourea which is further modified by transition metals, Mn(II), Co(II), Ni(II), Cu(II) and Zn(II). All the polymeric compounds were characterized by (FT-IR) spectroscopy, 1H NMR spectroscopy, 13C NMR spectroscopy, UV–visible spectra, magnetic moment measurements, thermogravimetric analysis (TGA) and antibacterial activities. Polymer complexes of Mn(II), Co(II) and Ni(II) show octahedral geometry, wh...

  1. Dielectric, thermal and mechanical properties of ADP doped PVA composites

    Science.gov (United States)

    Naik, Jagadish; Bhajantri, R. F.; Ravindrachary, V.; Rathod, Sunil G.; Sheela, T.; Naik, Ishwar

    2015-06-01

    Polymer composites of poly(vinyl alcohol) (PVA), doped with different concentrations of ammonium dihydrogen phosphate (ADP) has been prepared by solution casting. The formation of complexation between ADP and PVA was confirmed with the help of Fourier transforms infrared (FTIR) spectroscopy. Thermogravimetric analysis (TGA) shows thermal stability of the prepared composites. Impedance analyzer study revealed the increase in dielectric constant and loss with increase the ADP concentration and the strain rate of the prepared composites decreases with ADP concentration.

  2. Production and characterization of amorphous and crystalline zirconium phosphate for using as ion exchanger

    International Nuclear Information System (INIS)

    Medeiros, F.F.P.; Serafim, M.J.S.

    1996-01-01

    This work presents and discusses the results obtained from the development of sintered zirconium phosphates in their amorphous and crystalline structures aimed to be used as ionic exchanger. Such materials, prepared with suitable stoichiometric formula, were obtained from zirconila chloride originated from brazilian zirconite. We have used chemical analysis along with thermogravimetric, differential thermogravimetric, and X-ray diffraction techniques to determine the synthesis parameters obtained from on techniques to determine the synthesis parameters obtained from the suitable powders. The physical characteristics of the samples were available from the analysis of surface area, size and shape of the particles and agglomerates and also from the porosity of the powders. (author)

  3. Polyaniline on surface modification of diatomite: a novel way to obtain conducting diatomite fillers

    International Nuclear Information System (INIS)

    Li Xingwei; Bian Chaoqing; Chen Wei; He Jinbo; Wang Zhaoquen; Xu Ning; Xue Gi

    2003-01-01

    A conducting diatomite was obtained by polyaniline on surface modification of diatomite, and was characterized via Fourier-transform Raman spectra, UV-Vis absorption spectra, thermogravimetric analysis and scanning electron microscope, as well as conductivity. The results of spectroanalysis illustrate that polyaniline is not simply blended with diatomite. An interaction exists at the interface of diatomite and polyaniline, which may associate with hydrogen bond formed between the surface of diatomite with electronegativity and N-H bond in polyaniline macromolecule. The results of thermogravimetric analysis suggest that the conducting diatomite only contains 8% polyaniline by mass, but its conductivity has reached 2.8x10 -2 S cm -1 at 20 deg. C

  4. Thermal Dehydration Kinetics of Gypsum and Borogypsum under Non-isothermal Conditions

    Institute of Scientific and Technical Information of China (English)

    I.Y.Elbeyli; S.Piskin

    2004-01-01

    Thermal dehydration of gypsum and borogypsum was investigated under nonisothermal conditions in air by using simultaneous thermogravimetric-differential thermal analyzer. Nonisothermal experiments were carried out at various linear heating rates. Kinetics of dehydration in the temperature range of 373-503 K were evaluated from the DTA (differential thermal analysis)-TGA (thermogravimetric analysis) data by means of Coats-Redfern,Kissinger and Doyle Equations. Values of the activation energy and the pre-exponential factor of the dehydration were calculated. The results of thermal experiments and kinetic parameters indicated that borogypsum is similar to gypsum from dehydration mechanism point of view although it consists of boron and small amount of alkali metal oxides.

  5. PREPARATION AND PROPERTIES OF MMA/1-PROPYLMETHACRYLATE-POSS COPOLYMER WITH ATOM TRANSFER RADICAL POLYMERIZATION

    Institute of Scientific and Technical Information of China (English)

    He-xin Zhang; Ho-young Lee; Young-jun Shin; Dong-ho Lee; Seok Kyun Noh

    2008-01-01

    The methyl methacrylate(MMA)/1-propylmethacrylate-polyhedral oligomeric silsesquioxane(PM-POSS) copolymers were synthesized via atom transfer radical polymerization with CuBr as catalyst.The unreacted PM-POSS monomer could be removed completely by washing the copolymerization product with n-hexane.The copolymers were characterized with 1H-NMR,X-ray diffraction,difierential scanning calorimetry,thermogravimetric analysis and gel permeatlon chromatography.With increasing PM-POSS feed ratio.the total conversion increased while the glass transition temperatures of copolymer decreased.The thermogravimetric analysis demonstrated that the thermal stability of copolymer improved slightly with PM-POSS addition.The molecular weight of copolymers increased with incorporation of PM-POSS.

  6. Thermal Dehydration Kinetics of Gypsum and Borogypsum under Non-isothermal Conditions%在非等温条件下石膏和硼石膏的加热脱水动力学研究

    Institute of Scientific and Technical Information of China (English)

    ī.Y.Elbeyli; S.Piskin

    2004-01-01

    Thermal dehydration of gypsum and borogypsum was investigated under nonisothermal conditions in air by using simultaneous thermogravimetric-differential thermal analyzer. Nonisothermal experiments were carried out at various linear heating rates. Kinetics of dehydration in the temperature range of 373-503 K were evaluated from the DTA (differential thermal analysis)-TGA (thermogravimetric analysis) data by means of Coats-Redfern,Kissinger and Doyle Equations. Values of the activation energy and the pre-exponential factor of the dehydration were calculated. The results of thermal experiments and kinetic parameters indicated that borogypsum is similar to gypsum from dehydration mechanism point of view although it consists of boron and small amount of alkali metal oxides.

  7. Bulletin of Materials Science | News

    Indian Academy of Sciences (India)

    ray diffraction (XRD), thermogravimetric analysis (TGA) and Fourier transmission ... Investigation of electroluminescence properties of CdTe@CdS core-shell ... Analysis of Li-related defects in ZnO thin films influenced by annealing ambient.

  8. Synthesis, characterization and field evaluation of a new calcium-based CO2 absorbent for radial diffusive sampler

    Science.gov (United States)

    Cucciniello, Raffaele; Proto, Antonio; Alfano, Davide; Motta, Oriana

    2012-12-01

    In this paper the use of passive sampling as a powerful approach to monitor atmospheric CO2 is assessed. Suitable substrate based on calcium-aluminium oxide was synthetized according to a process which permits to control the particle size of the CaO/Al based sorbent. The study shows that hydration of substrate is an essential part of the process of CO2 absorption and subsequent conversion to carbonate. X-ray diffraction, thermogravimetric analysis, environmental scanning electron microscopic analysis were used in order to characterize the substrate and to establish the best performances both in terms of particle size and CO2 absorption capacity. Passive samplers for CO2 monitoring were prepared and then tested at laboratory level and in the atmospheric environment. Validation was performed by comparison with an infrared continuous detector. Thermogravimetric analysis results, carried out to evaluate the absorbing capability of this new passive device, were in accordance with data collected at the same time by the active continuous analyser. The diffusive sampling rate and the diffusion coefficient of CO2 respect to this new passive device were also evaluated resulting equal to 47 ± 3 ml min-1 and 0.0509 ± 0.005 cm2 s-1, respectively.

  9. Systems level analysis of systemic sclerosis shows a network of immune and profibrotic pathways connected with genetic polymorphisms.

    Directory of Open Access Journals (Sweden)

    J Matthew Mahoney

    2015-01-01

    Full Text Available Systemic sclerosis (SSc is a rare systemic autoimmune disease characterized by skin and organ fibrosis. The pathogenesis of SSc and its progression are poorly understood. The SSc intrinsic gene expression subsets (inflammatory, fibroproliferative, normal-like, and limited are observed in multiple clinical cohorts of patients with SSc. Analysis of longitudinal skin biopsies suggests that a patient's subset assignment is stable over 6-12 months. Genetically, SSc is multi-factorial with many genetic risk loci for SSc generally and for specific clinical manifestations. Here we identify the genes consistently associated with the intrinsic subsets across three independent cohorts, show the relationship between these genes using a gene-gene interaction network, and place the genetic risk loci in the context of the intrinsic subsets. To identify gene expression modules common to three independent datasets from three different clinical centers, we developed a consensus clustering procedure based on mutual information of partitions, an information theory concept, and performed a meta-analysis of these genome-wide gene expression datasets. We created a gene-gene interaction network of the conserved molecular features across the intrinsic subsets and analyzed their connections with SSc-associated genetic polymorphisms. The network is composed of distinct, but interconnected, components related to interferon activation, M2 macrophages, adaptive immunity, extracellular matrix remodeling, and cell proliferation. The network shows extensive connections between the inflammatory- and fibroproliferative-specific genes. The network also shows connections between these subset-specific genes and 30 SSc-associated polymorphic genes including STAT4, BLK, IRF7, NOTCH4, PLAUR, CSK, IRAK1, and several human leukocyte antigen (HLA genes. Our analyses suggest that the gene expression changes underlying the SSc subsets may be long-lived, but mechanistically interconnected

  10. Urine proteome analysis in Dent's disease shows high selective changes potentially involved in chronic renal damage.

    Science.gov (United States)

    Santucci, Laura; Candiano, Giovanni; Anglani, Franca; Bruschi, Maurizio; Tosetto, Enrica; Cremasco, Daniela; Murer, Luisa; D'Ambrosio, Chiara; Scaloni, Andrea; Petretto, Andrea; Caridi, Gianluca; Rossi, Roberta; Bonanni, Alice; Ghiggeri, Gian Marco

    2016-01-01

    Definition of the urinary protein composition would represent a potential tool for diagnosis in many clinical conditions. The use of new proteomic technologies allows detection of genetic and post-trasductional variants that increase sensitivity of the approach but complicates comparison within a heterogeneous patient population. Overall, this limits research of urinary biomarkers. Studying monogenic diseases are useful models to address this issue since genetic variability is reduced among first- and second-degree relatives of the same family. We applied this concept to Dent's disease, a monogenic condition characterised by low-molecular-weight proteinuria that is inherited following an X-linked trait. Results are presented here on a combined proteomic approach (LC-mass spectrometry, Western blot and zymograms for proteases and inhibitors) to characterise urine proteins in a large family (18 members, 6 hemizygous patients, 6 carrier females, and 6 normals) with Dent's diseases due to the 1070G>T mutation of the CLCN5. Gene ontology analysis on more than 1000 proteins showed that several clusters of proteins characterised urine of affected patients compared to carrier females and normal subjects: proteins involved in extracellular matrix remodelling were the major group. Specific analysis on metalloproteases and their inhibitors underscored unexpected mechanisms potentially involved in renal fibrosis. Studying with new-generation techniques for proteomic analysis of the members of a large family with Dent's disease sharing the same molecular defect allowed highly repetitive results that justify conclusions. Identification in urine of proteins actively involved in interstitial matrix remodelling poses the question of active anti-fibrotic drugs in Dent's patients. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Fulltext PDF

    Indian Academy of Sciences (India)

    Administrator

    of X-ray line profile analysis. 43. Backscattering ... nanoparticles before and after transfer from liquid phase to polystyrene ..... Nanocrystals. Swift heavy ion irradiation effect on Cu-doped CdS nano- ..... Thermogravimetric analysis. Studies on ...

  12. Show-Bix &

    DEFF Research Database (Denmark)

    2014-01-01

    The anti-reenactment 'Show-Bix &' consists of 5 dias projectors, a dial phone, quintophonic sound, and interactive elements. A responsive interface will enable the Dias projectors to show copies of original dias slides from the Show-Bix piece ”March på Stedet”, 265 images in total. The copies are...

  13. Influent of Borax Decahydrate Composition as Additional Flux into Stoneware Bodies

    Science.gov (United States)

    Bakil, Siti Natrah Abd; Hussin, Rosniza; Bakar Aramjat, Abu

    2017-08-01

    Stoneware is vitrified, has less porosity and requires high sintering temperature. The influent of borax decahydrate composition at sintering temperature 1050°C and 1150°C on the thermal analysis, fracture surface, linear shrinkage, water absorption and modular of rapture (MOR) were investigated. Rectangular sample were produced by uniaxially pressing at 40MPa. The thermal behavior was determined by thermogravimetric and different thermal analysis (TGA-DTA). The Scanning electron microscopy (SEM) was used for fracture surface analysis. The water absorption (%) of the sample were determined using Archimedes’ method. The experimental result showed that content of borax decahydrate have influent the properties of stoneware bodies.

  14. Effect of ethylene glycol on the orientation and magnetic properties of barium ferrite thin films derived by chemical solution deposition

    KAUST Repository

    Meng, Siqin

    2014-03-01

    Tb-doped BiFeO3 multiferroics nanoparticles fabricated via micro-emulsion route were characterized by thermogravimetric analysis (TGA), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The fully characterized TbxBi1-xFeO3 nanoparticles were then subjected to magnetic behavior evaluation for various technological applications. The thermogravimetric analysis (TGA) conducted in the range 25-1000 degrees C predicted the temperature (similar to 960 degrees C) for phase formation. XRD estimated the crystallite size 30-47 nm, while the particles size estimated by SEM was found (80-120 nm). The XRD data confirmed the rhombohedral (space group R3c) phase with average cell volume 182.66 angstrom(3) (for BiFeO3). Various other physical parameters like bulk density, X-ray density and porosity were also determined from the XRD data and found in agreement with theoretical predictions. The magnetic studies showed that as Bi3+ was substituted by Tb3+, all magnetic parameters were altered. The maximum saturation magnetization (M-s) (0.6691 emug(-1)) was exhibited by Tb0.02Bi0.98FeO3 while the Tb0.00Bi1.00Fe1.00O3 showed the maximum (549 Oe) coercivity. The evaluated magnetic behavior categorized these materials as soft magnetic materials that may be useful for fabricating advanced technological applications. (C) 2013 Elsevier B.V. All rights reserved.

  15. Syntheses and electrochromic and fluorescence properties of three double dithienylpyrroles derivatives

    International Nuclear Information System (INIS)

    Wang Gang; Fu Xiangkai; Huang Jing; Wu Chuanlong; Wu Liu; Deng Jun; Du Qiuliang; Zou Xiaochuan

    2011-01-01

    Highlights: → Three kinds of double dithienylpyrroles derivatives have been successfully prepared by the Knorr-Paal condensation between 1,4-di(thiophen-2-yl) butane-1,4-dione and aromatic diamines. → Their polymer films were successfully synthesized via electropolymerization. → The polymer films had stable and well-defined reversible redox process, low optical band gap and multicolor electrochromic behavior. → All the monomers and polymers exhibited different intensity emission bands at different wavelengths. - Abstract: Three double dithienylpyrroles derivatives have been successfully prepared by performing a Knorr-Paal condensation between 1,4-di(thiophen-2-yl) butane-1,4-dione and various aromatic diamines. Additionally, their corresponding polymer films were synthesized via electropolymerization. Their electrochemical, spectroelectrochemical and electrochromic behaviors were further investigated by thermogravimetric analysis, scanning electron microscopy, cyclic voltammetry, UV-vis absorption and fluorescence emission spectra. Scanning electron microscopy and thermogravimetric analysis demonstrated that the polymer films possessed homogeneous, compact and smooth layer structures and thermal stabilities (up to nearly 180 deg. C). Cyclic voltammograms and UV-vis absorption spectra studies showed that the polymer films have stable, well-defined, reversible redox processes, low optical band gaps (E g < 2.2 eV) and multicolor electrochromic behaviors. Additionally, the fluorescence spectra study showed that all of the monomers and polymers exhibited different intensity emission bands at different wavelengths.

  16. TbxBi1-xFeO3 nanoparticulate multiferroics fabricated by micro-emulsion technique: Structural elucidation and magnetic behavior evaluation

    KAUST Repository

    Anwar, Zobia

    2014-04-01

    Tb-doped BiFeO3 multiferroics nanoparticles fabricated via micro-emulsion route were characterized by thermogravimetric analysis (TGA), X-ray diffraction (XRD) and scanning electron microscopy (SEM). The fully characterized TbxBi1-xFeO3 nanoparticles were then subjected to magnetic behavior evaluation for various technological applications. The thermogravimetric analysis (TGA) conducted in the range 25-1000 C predicted the temperature (~960 C) for phase formation. XRD estimated the crystallite size 30-47 nm, while the particles size estimated by SEM was found (80-120 nm). The XRD data confirmed the rhombohedral (space group R3c) phase with average cell volume 182.66 Å3 (for BiFeO 3). Various other physical parameters like bulk density, X-ray density and porosity were also determined from the XRD data and found in agreement with theoretical predictions. The magnetic studies showed that as Bi3+ was substituted by Tb3+, all magnetic parameters were altered. The maximum saturation magnetization (Ms) (0.6691 emug -1) was exhibited by Tb0.02Bi0.98FeO 3 while the Tb0.00Bi1.00Fe1.00O 3 showed the maximum (549 Oe) coercivity. The evaluated magnetic behavior categorized these materials as soft magnetic materials that may be useful for fabricating advanced technological applications. © 2013 Elsevier B.V.

  17. Heavy fuel oil pyrolysis and combustion: kinetics and evolved gases investigated by TGA-FTIR

    KAUST Repository

    Abdul Jameel, Abdul Gani; Han, Yunqing; Brignoli, Omar; Telalovic, Selvedin; Elbaz, Ayman M.; Im, Hong G.; Roberts, William L.; Sarathy, Mani

    2017-01-01

    investigated using non-isothermal thermo-gravimetric analysis (TGA) coupled with a Fourier-transform infrared (FTIR) spectrometer. TG and DTG (differential thermo-gravimetry) were used for the kinetic analysis and to study the mass loss characteristics due

  18. Thermal Oxidation Resistance of Rare Earth-Containing Composite Elastomer

    Institute of Scientific and Technical Information of China (English)

    邱关明; 张明; 周兰香; 中北里志; 井上真一; 冈本弘

    2001-01-01

    The rare earth-containing composite elastomer was obtained by the reaction of vinyl pyridine-SBR (PSBR) latex with rare earth alkoxides, and its thermal oxidation resistance was studied. After aging test, it is found that its retention rate of mechanical properties is far higher than that of the control sample. The results of thermogravimetric analysis show that its thermal-decomposing temperature rises largely. The analysis of oxidation mechanisms indicates that the main reasons for thermal oxidation resistance are that rare earth elements are of the utility to discontinue autoxidation chain reaction and that the formed complex structure has steric hindrance effect on oxidation.

  19. Phase equilibria in the system Nd(PO3)3 - KPO3

    International Nuclear Information System (INIS)

    Znamierowska, T.; Mizer, D.

    2002-01-01

    The system Nd(PO 3 ) 3 - KPO 3 has been investigated by differential thermal analysis (during heating), thermogravimetric analysis, mass spectrometry, Raman spectroscopy and X-ray powder diffraction and its phase diagram was proposed. It was discovered that initial metaphosphates react at a 1:1 molar ratio forming intermediate compound KNd(PO 3 ) 4 . It was found that it melts incongruently at 854 o C giving Nd(po)3) 3 and a liquid rich in KPO 3 . Phosphate KNd(PO 3 ) 4 is stable down to room temperature and does not show any polymorphic transitions. (author)

  20. Characterization of ceramic bodies to produce bricks from Campos Goytacazes, Brazil

    International Nuclear Information System (INIS)

    Almeida, L.L.P. de; Maia, F.S.; Petrucci, L.J.T.; Pessanha, E.M.; Paixao, L.P.

    2010-01-01

    This work has for objective to study comparatively the characteristics and technological properties of four typical ceramic bodies from the region of Campos dos Goytacazes-RJ used to fabricate red ceramics. The characterization techniques used were: X-ray fluorescence, X-ray diffraction, differential thermal analysis (DTA), thermogravimetric analysis (TGA) and dilatometry. Specimens were molded by extrusion and then fired at 750, 850 and 950 deg C. The evaluated firing properties were: linear shrinkage and water absorption. The results showed that the investigated ceramic bodies have similar chemical and mineralogical composition. It is also concluded that the bodies are adequate to produce bricks. (author)

  1. Preparation and Flame Retardant and Smoke Suppression Properties of Bamboo-Wood Hybrid Scrimber Filled with Calcium and Magnesium Nanoparticles

    Directory of Open Access Journals (Sweden)

    Bin Fu

    2014-01-01

    Full Text Available The physical and mechanical properties of bamboo-wood hybrid scrimber filled with different loadings of nanoparticles were studied. The effects of nanoparticles on flame retardant and smoke suppression properties of bamboo-wood hybrid scrimber were studied by means of thermogravimetric analysis (TGA, cone calorimeter (CONE, and scanning electron microscope (SEM. The results showed that the physical and mechanical properties of bamboo-wood hybrid scrimber were improved by adding a moderate loading of nanoparticles; the optimal loading of nanoparticles was 10%. The heat transfer in bamboo-wood hybrid scrimber was prevented and the escaping channel of combustible gas was blocked by the uniformly filling effect of nanoparticles. The gas concentration was diluted by the noncombustible gas produced by pyrolysis of nanoparticles; the combustion chain reaction was suppressed by highly reactive free radicals produced by pyrolysis of nanoparticles. The residual mass of bamboo-wood hybrid scrimber filled with nanoparticles in thermogravimetric (TG curve at 900 s and burned by method of cone calorimeter (CONE at 600 s was increased compared to that of untreated one, which showed that inorganic mineral powder has the effect of catalytic charring.

  2. Synthesis, Crystal Structure, and Luminescence Properties of a New Calcium(II Coordination Polymer Based on L-Malic Acid

    Directory of Open Access Journals (Sweden)

    Duraisamy Senthil Raja

    2013-01-01

    Full Text Available A new calcium coordination polymer [Ca(HL-MA]n (H3L-MA = L-malic acid has been solvothermally synthesized. The structure of the newly synthesized complex has been determined by single-crystal X-ray diffraction analysis and further characterized by elemental analysis, reflectance UV-Vis & IR spectra, powder X-ray diffraction (PXRD, and thermogravimetric analysis (TGA. The single crystal structure analysis showed that the complex forms three-dimensional framework. The new Ca(II complex has displayed very high thermal stability which was inferred from TGA and PXRD results. As far as the optical property of the new complex is concerned, the complex emitted its own characteristic sensitized luminescence.

  3. Comportamento agressivo em shows musicais: analisando notícias de jornal impresso

    Directory of Open Access Journals (Sweden)

    Carlos Eduardo Pimentel

    2011-08-01

    Full Text Available This paper reports a content analysis of the newspaper articles dealing with aggressive behavior in music shows. This analysis permits an understanding of the characteristics of these situations, the aggressive behaviors in shows, and the way in which the print media treat the subject. Despite of the newspapers’ influence on public opinion formation, that is, the transmission of attitudes and behavior repertoires, this kind of analysis is rarely reported in Brazilian social psychological literature. Some 31 newspaper articles were content analyzed as to aggressive behavior during music shows. Results indicate that aggressive behaviors occur in shows of most varied musical styles. Results are discussed on the basis of social cognitive theory.

  4. Retrospective Analysis of Patient Presentations at the Sydney (Australia) Royal Easter Show from 2012 to 2014.

    Science.gov (United States)

    Crabtree, Nathan; Mo, Shirley; Ong, Leon; Jegathees, Thuvarahan; Wei, Daniel; Fahey, David; Liu, Jia Jenny

    2017-04-01

    Introduction Comprehensive studies on the relationship between patient demographics and subsequent treatment and disposition at a single mass-gathering event are lacking. The Sydney Royal Easter Show (SRES; Sydney Olympic Park, New South Wales, Australia) is an annual, 14-day, agricultural mass-gathering event occurring around the Easter weekend, attracting more than 800,000 patrons per year. In this study, patient records from the SRES were analyzed to examine relationships between weather, crowd size, day of week, and demographics on treatment and disposition. This information would help to predict factors affecting patient treatment and disposition to guide ongoing training of first responders and to evaluate the appropriateness of staffing skills mix at future events. Hypothesis Patient demographics, environmental factors, and attendance would influence the nature and severity of presentations at the SRES, which would influence staffing requirements. A retrospective analysis of 4,141 patient record forms was performed for patients who presented to St John Ambulance (Australian Capital Territory, Australia) at the SRES between 2012 and 2014 inclusive. Presentation type was classified using a previously published minimum data set. Data on weather and crowd size were obtained from the Australian Bureau of Meteorology (Melbourne, Victoria, Australia) and the SRES, respectively. Statistical analyses were performed using SPSS v22 (IBM; Armonk, New York USA). Between 2012 to 2014, over 2.5 million people attended the SRES with 4,141 patients treated onsite. As expected, the majority of presentations were injuries (49%) and illnesses (46%). Although patient demographics and presentation types did not change over time, the duration of treatment increased. A higher proportion of patients were discharged to hospital or home compared to the proportion of patients discharged back to the event. Patients from rural/regional locations (accounting for 15% of all patients) were

  5. Thermogravimetric and microscopic analysis of SiC/SiC materials with advanced interfaces

    Energy Technology Data Exchange (ETDEWEB)

    Windisch, C.F. Jr.; Jones, R.H. [Pacific Northwest National Lab., Richland, WA (United States); Snead, L.L. [Oak Ridge National Lab., TN (United States)

    1997-04-01

    The chemical stability of SiC/SiC composites with fiber/matrix interfaces consisting of multilayers of SiC/SiC and porous SiC have been evaluated using a thermal gravimetric analyzer (TGA). Previous evaluations of SiC/SiC composites with carbon interfacial layers demonstrated the layers are not chemically stable at goal use temperatures of 800-1100{degrees}C and O{sub 2} concentrations greater than about 1 ppm. No measureable mass change was observed for multilayer and porous SiC interfaces at 800-1100{degrees}C and O{sub 2} concentrations of 100 ppm to air; however, the total amount of oxidizable carbon is on the order of the sensitivity of the TGA. Further studies are in progress to evaluate the stability of these materials.

  6. Methyl methacrylate oligomerically-modified clay and its poly(methyl methacrylate) nanocomposites

    International Nuclear Information System (INIS)

    Zheng Xiaoxia; Jiang, David D.; Wilkie, Charles A.

    2005-01-01

    A methyl methacrylate oligomerically-modified clay was used to prepare poly(methyl methacrylate) clay nanocomposites by melt blending and the effect of the clay loading level on the modified clay and corresponding nanocomposite was studied. These nanocomposites were characterized by X-ray diffraction, transmission electron microscopy, thermogravimetric analysis and cone calorimetry. The results show a mixed intercalated/delaminated morphology with good nanodispersion. The compatibility between the methylacrylate-subsituted clay and poly(methyl methacrylate) (PMMA) are greatly improved compared to other oligomerically-modified clays

  7. Experimental investigation of pyrolysis process of corn straw

    OpenAIRE

    Lei Wang; Shengqiang Shen; Shuhua Yang; Xinguang Shi

    2010-01-01

    The present paper was performed to analyze the pyrolysis process of corn straw. Based on the thermogravimetric analysis, the component of pyrolysis gas of corn straw was tested using the gas chromatograph analyzer. Experimental results showed that, as the reaction temperature increases, the component of H 2 and CH 4 increases, whereas the component of CO and CO 2 decreases. Finally, the mechanism of pyrolysis process of corn straw was revealed from the point of view of the molecular structure...

  8. Dynamic mechanical thermal analysis of composite resins with CQ and PPD as photo-initiators photoactivated by QTH and LED units.

    Science.gov (United States)

    Brandt, William Cunha; Silva, Cristina Gomes; Frollini, Elisabete; Souza-Junior, Eduardo Jose Carvalho; Sinhoreti, Mário Alexandre Coelho

    2013-08-01

    The aim of this study was to evaluate the thermal and mechanical properties of the composite resins containing the photo-initiators camphorquinone (CQ) and/or phenyl-propanodione (PPD) when photoactivated with halogen lamp (XL2500/3M-ESPE), monowave (UltraBlueIS/DMC) and polywave (UltraLume5/Ultradent) LED units. A blend of BisGMA, UDMA, BisEMA and TEGDMA was prepared with the same wt% of photo-initiators CQ and/or PPD and 65wt% of silaneted filler particles. Compression strength (CS), diametral tensile strength (DTS) and diametral modulus (DM) were tested. Thermogravimetric analysis (TGA) was made and the lost residual monomer were verified. Dynamic mechanical thermal analysis (DMTA) was used for to analyze the glass transition temperature (Tg) and the storage modulus in 37°C. Degree of conversion (DC) was accomplished in the same samples of DMA using middle-infrared spectroscopy (mid-IR). CQ, CQ/PPD and PPD obtained the same results for all mechanical properties (CS, DTS and DM), lost residual monomer and storage modulus in 37°C, regardless LCU used. The results of Tg showed that the combination PPD-UltraLume5 produced the highest values. DC showed that the combination CQ-UltraLume5 resulted in the highest values and PPD-XL2500 in the lowest DC values. The study shows that PPD is not only effective photosensitizers, but also photocrosslinking agents for dental composite resins with a similar efficiency to CQ. Copyright © 2013 Elsevier Ltd. All rights reserved.

  9. Co-gasification of biosolids with biomass: Thermogravimetric analysis and pilot scale study in a bubbling fluidized bed reactor.

    Science.gov (United States)

    Yu, Ming Ming; Masnadi, Mohammad S; Grace, John R; Bi, Xiaotao T; Lim, C Jim; Li, Yonghua

    2015-01-01

    This work studied the feasibility of co-gasification of biosolids with biomass as a means of disposal with energy recovery. The kinetics study at 800°C showed that biomass, such as switchgrass, could catalyze the reactions because switchgrass ash contained a high proportion of potassium, an excellent catalyst for gasification. However, biosolids could also inhibit gasification due to interaction between biomass alkali/alkaline earth metals and biosolids clay minerals. In the pilot scale experiments, increasing the proportion of biosolids in the feedstock affected gasification performance negatively. Syngas yield and char conversion decreased from 1.38 to 0.47m(3)/kg and 82-36% respectively as the biosolids proportion in the fuel increased from 0% to 100%. Over the same range, the tar content increased from 10.3 to 200g/m(3), while the ammonia concentration increased from 1660 to 19,200ppmv. No more than 25% biosolids in the fuel feed is recommended to maintain a reasonable gasification. Copyright © 2014 Elsevier Ltd. All rights reserved.

  10. Synthesis and biodegradation studies of optically active poly (amide–imide) s based on N, N′-(pyromellitoyl)-bis-l-amino acid

    DEFF Research Database (Denmark)

    Wu, Qiuxiang; Yang, Zhizhou; Yao, Jinshui

    2015-01-01

    (FTIR) and proton nuclear magnetic resonance spectroscopy, elemental analysis, inherent viscosity measurement, solubility tests, specific rotation, and thermogravimetric analysis (TGA). The biodegradation studies of the PAIs were performed in soil and in phosphate buffer solution. The surface morphology...

  11. A Thermomechanical and Adhesion Analysis of Epoxy/Al2O3 Nanocomposites

    Directory of Open Access Journals (Sweden)

    Juliana Primo Basílio de Souza

    2015-06-01

    Full Text Available The thermomechanial properties of polymeric nanocom‐ posites are related to the quality of the adhesion between matrix and nanoparticle. Since the adhesion is related to the nature of the materials and the surface available for chemical, electrostatic and mechanical interactions among these materials, weak bonding forces between alumina (inorganic and polymer matrices (organic were expected. Furthermore, using nanoparticles with greater diameters means that the specific surface area reduction will have an adverse impact on the adhesive process. For epoxy matrices reinforced with alumina nanoparticles, different volume fractions and sizes were observed by differential scanning calorimetry (DSC: a relation between the glass transition temperature (Tg and the nanoparticle size. This observa‐ tion was tested by dynamic mechanical analysis (DMA and the cross-link density was calculated. In addition, the thermal stability enhanced by alumina addition to organic resins and the quality of the adhesion was observed by thermogravimetric analysis (TGA.

  12. An in situ FTIR spectroscopic and thermogravimetric analysis study of the dehydration and dihydroxylation of SnO2: the contribution of the (100), (110) and (111) facets.

    Science.gov (United States)

    Christensen, P A; Attidekou, P S; Egdell, R G; Maneelok, S; Manning, D A C

    2016-08-17

    Nanoparticulate SnO2 produced by a hydrothermal method was characterised by BET, XRD, TGA-MS and in situ variable temperature diffuse reflectance infra red spectroscopy (DRIFTS) to determine the surface behaviour of water. For the (100) facets, hydrogen bonding does not occur, and water adsorption is less strong than for the (111) and (110) facets where hydrogen bonding does occur. Reversible uptake of oxygen was observed. These findings have implications for other surface-gas reactions in which Ni and Sb co-doped SnO2 (NATO) anodes are used for ozone generation. BET showed the relatively high surface area and nanometer scale of the SnO2 particles, whilst XRD confirmed the nano dimension of the crystallites and showed only the cassiterite phase. TGA analysis indicated four temperature regions over which mass loss was observed. These and the in situ DRIFTS studies revealed the existence of various forms of water associated with specific crystal facets of the SnO2, as well as the existence of isolated O-H groups and adsorbed oxygen species. Electronic absorptions were also observed and the data rationalised in terms of the existence of both free electron absorptions, and absorptions from oxygen vacancy states. The role of adsorbed molecular oxygen in electrochemical ozone generation at Ni and Sb co-doped SnO2 (NATO) anodes was strongly suggested by this work.

  13. Synthesis and characterization particles of Ba{sub 0,50}Sr{sub 0,50}Co{sub 0,80}Fe{sub 0,20}O{sub 3} obtained by the citrate-EDTA technique; Sintese e caracterizacao de particulados de Ba{sub 0,50}Sr{sub 0,50}Co{sub 0,80}Fe{sub 0,20}O{sub 3} obtidos pela tecnica dos citratos-EDTA

    Energy Technology Data Exchange (ETDEWEB)

    Bonturim, E; Vargas, R A; Andreoli, M; Seo, E S.M., [Instituto de Pesquisas Energeticas e Nucleares (CCTM/IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Ciencia e Tecnologia de Materiais

    2010-07-01

    The Ba{sub (1-x)}Sr{sub (x)}Co{sub (1-y)}Fe{sub (y)}O{sub (3)} (BSCF) has been studied as a cathode material for Intermediate Temperature Solid Oxide Fuel Cell, due to its better ion and electron conduction. This work aims to study the synthesis of the compound obtained from the citrate-EDTA technique. Thermogravimetric analysis indicated the formation of the compound above 800 deg C. The materials calcined at temperatures of 700, 800 and 900 deg C for 5 h showed cubic pseudo-perovskite structure, according to the literature. By analysis of X-ray fluorescence were obtained powders with nominal chemical composition in the temperature range studied. The micrographs obtained by SEM and particle size distribution analysis showed the formation of particle with diameters below 1 micron. (author)

  14. Online Italian fandoms of American TV shows

    Directory of Open Access Journals (Sweden)

    Eleonora Benecchi

    2015-06-01

    Full Text Available The Internet has changed media fandom in two main ways: it helps fans connect with each other despite physical distance, leading to the formation of international fan communities; and it helps fans connect with the creators of the TV show, deepening the relationship between TV producers and international fandoms. To assess whether Italian fan communities active online are indeed part of transnational online communities and whether the Internet has actually altered their relationship with the creators of the original text they are devoted to, qualitative analysis and narrative interviews of 26 Italian fans of American TV shows were conducted to explore the fan-producer relationship. Results indicated that the online Italian fans surveyed preferred to stay local, rather than using geography-leveling online tools. Further, the sampled Italian fans' relationships with the show runners were mediated or even absent.

  15. Vibrational, DFT, and thermal analysis of 2,4,6-triamino-1,3,5-triazin-1-ium 3-(prop-2-enoyloxy) propanoate acrylic acid monosolvate monohydrate

    Science.gov (United States)

    Sangeetha, V.; Govindarajan, M.; Kanagathara, N.; Marchewka, M. K.; Drozd, M.; Anbalagan, G.

    2013-12-01

    New organic crystals of 2,4,6-triamino-1,3,5-triazin-1-ium 3-(prop-2-enoyloxy) propanoate acrylic acid monosolvate monohydrate (MAC) have been obtained from aqueous solution by the slow solvent evaporation method at room temperature. Single crystal X-ray diffraction analysis reveals that the compound crystallises in the triclinic system with centrosymmetric space group P-1. FT-IR and FT-Raman spectra of MAC have been recorded and analyzed. The molecular geometry and vibrational frequencies and intensity of the vibrational bands are interpreted with the aid of structure optimization based on density functional theory (DFT) B3LYP method with 6-31G(d,p) basis set. The results of the optimized molecular structure are presented and compared with the experimental X-ray diffraction data. The theoretical results show that the optimized geometry can well reproduce the crystal structure, and the calculated vibrational frequency values show good agreement with experimental values. A study of the electronic properties, such as HOMO and LUMO energies and Molecular electrostatic potential (MEP) were performed. Mulliken charges and NBO charges of the title molecule were also calculated and interpreted. Thermogravimetric analysis has been done to study the thermal behaviour of MAC. The 13C and 1H nuclear magnetic resonance (NMR) chemical shifts of the molecule are calculated by the gauge independent atomic orbital (GIAO) method and compared with experimental results.

  16. Moessbauer investigations of palygorskite from Xuyi, China

    International Nuclear Information System (INIS)

    Huang Yanjun; Li Zhen; Li Shuzhen; Shi Ziliang; Yin Lin; Hsia Yuanfu

    2007-01-01

    The original palygorskite clay mineral has been collected from Longwangshan, Xuyi, Jiangsu Province, China. XRF analysis was performed to study its chemical compositions. Thermogravimetric analysis and differential thermogravimetric analysis (TGA/DTA) were used to study the weight loss due to dehydration and dehydroxylation. Then eight samples were prepared by heating at various temperatures. X-ray diffraction (XRD) patterns and Moessbauer spectra were measured to study the crystal evolvement and the occupation of iron cations. It revealed that the iron ions occupied the M1 and M2 with the ratio closed to 3:1. Hematite has been observed when heated at 650 deg. C, which indicated that iron cations mainly occupy M1 sites. An unknown silicate was identified when heated at 750 deg. C and dominated at 850 deg. C

  17. Thermal analysis and temperature dependent dielectric responses of Co doped anatase TiO2 nanoparticles

    International Nuclear Information System (INIS)

    Alamgir; Khan, Wasi; Ahammed, Nashiruddin; Naqvi, A. H.; Ahmad, Shabbir

    2015-01-01

    Nanoparticles (NPs) of pure and 5 mol % cobalt doped TiO 2 synthesized through acid modified sol-gel method were characterized to understand their thermal, structural, morphological, and temperature dependent dielectric properties. Thermogravimetric analysis (TGA) has been used for thermal studies and indicates the weight loss in two steps due to the removal of residual organics. X-ray diffraction study was employed to confirm the formation of single anatase phase with tetragonal symmetry for both pure and 5 mol % Co doped TiO 2 NPs. The average crystallite size of both samples was calculated from the Scherrer’s formula and was found in the range from 9-11 nm. TEM micrographs of these NPs reflect their shape and distribution. The dielectric constant (ε′), dielectric loss (tanδ) and ac conductivity (σ ac ) were also studied as a function of temperature at different frequencies. Electrical responses of the synthesized NPs have been analyzed carefully in the framework of relevant models. It is also noticed that the dielectric constant (ε′) of the samples found to decrease with increasing frequency but increases with increasing temperature up to a particular value and then sharply decreases. Temperature variation of dielectric constant exhibits step like escalation and shows relaxation behavior. Study of dielectric properties shows dominant dependence on the grain size as well as Co ion incorporation in TiO 2

  18. ANALYSIS OF THERMAL AND AQUEOUS SUSPENSION STABILITIES OF CHITOSAN BASED NANOENCAPSULATED VITAMINS

    Directory of Open Access Journals (Sweden)

    Douglas de Britto

    Full Text Available The food nutritional content is reduced as result of vitamins degradation. In order to minimize such losses, the encapsulation technique into polymeric nanoparticles (NPs could offer an additional protection, extending the stability. The crosslinking formed by the ionic gelation process of chitosan and tripolyphosphate (Chi-TPP has been widely used as an encapsulating matrix for several chemical compounds. In this way, Chi-TPP was used for encapsulation of C, B9 and B12 vitamins. The stability of the vitamins in NPs was evaluated in aqueous suspension by UV-Visible spectroscopy under different conditions: stored in dark, light exposure and effect of oxygen bubbling. The results indicated that encapsulation had a positive effect in preserving the vitamins, mainly vitamin C. The encapsulation preserved 47% of the initial concentration of vitamin C by the tenth day and around 28% after 17 days. Conversely, in non-encapsulated controls (neutral and acidic medium the losses were higher, reaching 13% by the tenth day and almost 3% after 17 days of storage in both medium. When exposed to light and O2 the protection provided by the encapsulation was even greater. By thermogravimetric analysis, the pure and the encapsulated vitamins showed distinct thermal behavior confirming Chi-TPP as a potential encapsulation material.

  19. Mineralogical study of Brazilian fly ashes; origin, characteristics and quality

    International Nuclear Information System (INIS)

    Kihara, Y.

    1984-01-01

    Thirty-one fly ash samples from the five main Brazilian coal-powered thermoelectric plants were subjected to gravimetric chemical analysis, complexometry, flame photometry, X-ray diffractometry, thermodifferential and thermogravimetric analysis, transmitted and reflected light microscopy, electron microprobe analysis and transmited and scanning electron microscopy. (Author) [pt

  20. Bulletin of Materials Science | News

    Indian Academy of Sciences (India)

    Synthesis and characterization of fluorophore attached silver nanoparticles ... by X-ray diffraction, differential thermal analysis, thermogravimetric analysis, Fourier ..... Infrared spectra, Raman laser, XRD, DSC/TGA and SEM investigations on the ..... composite materials based on polyaniline–polyethylene glycol–CdS system.

  1. SYNTHESIS, STRUCTURAL AND ANTIBACTERIAL STUDY OF ...

    African Journals Online (AJOL)

    diffraction, thermogravimetric analysis, scanning electron microscopy, atomic ... possess interesting biological properties like antibacterial properties [4-7]. ... compounds used for treating mental illness, epilepsy, and nicotine addiction [9, 10].

  2. Improved covalent functionalization of multi-walled carbon ...

    Indian Academy of Sciences (India)

    MWCNTs). The structures of the functionalized MWCNTs were characterized with Fourier-transform infrared spectroscopy. Thermogravimetric analysis results also demonstrated the presence of organic portions of the functionalized MWCNTs.

  3. Characterization of polyurethane based on polyol synthesized from glycerol and hexamethylene diisocyanate

    International Nuclear Information System (INIS)

    Carvalho, Sabrina M.; Weber, Vanessa; Silva, Tailu N.; Barreto, Pedro L.M.

    2009-01-01

    A new polyol based on glycerol was synthesized and used in the production of polyurethane by reaction with hexamethylene diisocyanate. The polyol was characterized by nuclear magnetic resonance spectroscopy (NMR) and Fourier transform-infrared spectroscopy (FTIR). The polyurethane produced was characterized by FTIR, thermogravimetry (TG), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). The polyol was shown to be reactive with hexamethylene diisocyanate, as the FTIR spectrum showed no free isocyanate groups and identified the presence of group -C=O of urethane groups. Analysis by DSC showed that the sample of polyurethane has a glass transition temperature around -8.53 deg C and SEM micrographs showed fracture and surface continuous and not broken. The thermogravimetric analysis showed that the polyurethane produced has a high thermal stability with a temperature of maximum degradation around 430 deg C. (author)

  4. The Last Gender Picture Show to Closure Buffy the Vampire Slayer

    Directory of Open Access Journals (Sweden)

    Sven Grampp

    2016-03-01

    Full Text Available This work presents in (and especially on one detail what it means to practice gender analysis as formal image analysis in the context of television shows. The chosen example for that is the closing scene of “Buffy the Vampire Slayer” (USA 1997-2003. This television show engages in a highly self-reflexive manner with common pop cultural representations of gender, which becomes particularly prevalent and radically condensed in the series finale.

  5. Analysis of coals and biomass pyrolysis using the distributed activation energy model.

    Science.gov (United States)

    Li, Zhengqi; Liu, Chunlong; Chen, Zhichao; Qian, Juan; Zhao, Wei; Zhu, Qunyi

    2009-01-01

    The thermal decomposition of coals and biomass was studied using thermogravimetric analysis with the distributed activation energy model. The integral method resulted in Datong bituminous coal conversions of 3-73% at activation energies of 100-486 kJ/mol. The corresponding frequency factors were e(19.5)-e(59.0)s(-1). Jindongnan lean coal conversions were 8-52% at activation energies of 100-462 kJ/mol. Their corresponding frequency factors were e(13.0)-e(55.8)s(-1). The conversion of corn-stalk skins were 1-84% at activation energies of 62-169 kJ/mol with frequency factors of e(10.8)-e(26.5)s(-1). Datong bituminous coal, Jindongnan lean coal and corn-stalk skins had approximate Gaussian distribution functions with linear ln k(0) to E relationships.

  6. Grab That Mike: communicative issues in French Talk Show "Grab That Mike": questões comunicativas em um "Talk Show" Francês

    Directory of Open Access Journals (Sweden)

    Ludwina Van Son

    2004-12-01

    Full Text Available In this analysis we have chosen a recent French talk show to illustrate how communication is turned into some new kind of "ideology"nowadays: in other words, you have to communicate if you consider yourself a citizen of today's world. The main characteristic of issue-centered talk shows being the destabilization of the implicit rules and participation framework, we observe how the so-called democratic right to express ourselves is (misused by the talk show host to secure the dynamics of the show. In order to reveal the host's manipulations, we have examined the verbal interactions between host and guests on the following issues: topic choice, turn-taking mechanisms and identity construction of the talk show's guests. In the perspective that this kind of talk show presents itself as a public space where direct democracy can be exercised, the analysis of the discursive strategies of the talk show host reveals the impact of a mediatic participation framework.Para a presente análise escolhemos um "talk show" francês recente para ilustrar como a comunicação se transforma em um novo tipo de ideologia: em outras palavras, você deve se comunicar se você se considera um cidadão do mundo de hoje. Sendo a principal característica do talk show a desestabilização das regras implícitas e o framework de participação, observamos como o tal direito democrático de expressão é interpretado pelo apresentador para manter a dinâmica do programa. Para revelar suas manipulações, examinamos as interações verbais entre apresentador e convidados nos seguintes temas: escolha do tópico, mecanismos de tomada de turno e construção de identidade dos convidados. É nessa perspectiva que este tipo de programa se apresenta como um espaço público onde a democracia direta pode ser exercitada; a análise das estratégias discursivas do apresentador do talk show revela o impacto de um framework de participação mediada.

  7. Vibrational and thermal study of l-methionine nitrate polycrystals

    Energy Technology Data Exchange (ETDEWEB)

    Victor, F.M.S.; Ribeiro, L.H.L.; Facanha Filho, P.F.; Santos, C.A.S.; Soares, R.A.; Abreu, D.C.; Sousa, J.C.F.; Carvalho, J.O.; Santos, A.O. dos [Universidade Federal do Maranhao (UFMA), MA (Brazil)

    2016-07-01

    Full text: Intensified in studies of nonlinear optical materials has been observed over the past two decades for its wide application in telecommunications, optical modulation and optical signal processing. The goal of this work is the thermal and vibrational study of L-methionine nitrate polycrystalline. The polycrystals were obtained by the method of slow evaporation of solvent at ambient temperature of 25 ° C. The X-ray diffraction was performed to confirm the structure of the material, which has monoclinic structure (space group P21) with four molecules per unit cell structure. Refinement by Rietveld method has been optimized and good quality parameters Rwp = 7.97% , Rp = 5.74 and S = 1.92%. The thermal stability of the material was verified from Thermogravimetric analysis (TGA), Differential Thermal Analysis (DTA) and Differential Scanning Calorimetry (DSC). The measures showed a possible phase transition event at about 107°C before the melting point of the material, which took place at about 127°C. Thermogravimetric analysis showed two mass loss events of 61.5% and 30.4%. The vibrational modes of the L-methionine nitrate molecule were identified by Raman spectroscopy in the spectral range between 35cm-1 and 3500 cm-1, the scattering measurements were made from room temperature up to the melting temperature of the material (140 ° C ) in which the disappearance of bands was found in the region of normal modes at 130 ° C, thus demonstrating a irreversible structural phase transition, because the spectrum obtained after returning the sample to ambient temperature is typical of amorphous material. (author)

  8. Global morphological analysis of marine viruses shows minimal regional variation and dominance of non-tailed viruses.

    Science.gov (United States)

    Brum, Jennifer R; Schenck, Ryan O; Sullivan, Matthew B

    2013-09-01

    Viruses influence oceanic ecosystems by causing mortality of microorganisms, altering nutrient and organic matter flux via lysis and auxiliary metabolic gene expression and changing the trajectory of microbial evolution through horizontal gene transfer. Limited host range and differing genetic potential of individual virus types mean that investigations into the types of viruses that exist in the ocean and their spatial distribution throughout the world's oceans are critical to understanding the global impacts of marine viruses. Here we evaluate viral morphological characteristics (morphotype, capsid diameter and tail length) using a quantitative transmission electron microscopy (qTEM) method across six of the world's oceans and seas sampled through the Tara Oceans Expedition. Extensive experimental validation of the qTEM method shows that neither sample preservation nor preparation significantly alters natural viral morphological characteristics. The global sampling analysis demonstrated that morphological characteristics did not vary consistently with depth (surface versus deep chlorophyll maximum waters) or oceanic region. Instead, temperature, salinity and oxygen concentration, but not chlorophyll a concentration, were more explanatory in evaluating differences in viral assemblage morphological characteristics. Surprisingly, given that the majority of cultivated bacterial viruses are tailed, non-tailed viruses appear to numerically dominate the upper oceans as they comprised 51-92% of the viral particles observed. Together, these results document global marine viral morphological characteristics, show that their minimal variability is more explained by environmental conditions than geography and suggest that non-tailed viruses might represent the most ecologically important targets for future research.

  9. Study on the Properties of Microcapsulated Chlorocyclophosphazene Polypropylene Composites%三聚氯化磷腈微胶囊阻燃剂/聚丙烯复合材料的性能研究

    Institute of Scientific and Technical Information of China (English)

    刘亚青; 赵贵哲

    2007-01-01

    Microcapsulated chlorocyclophosphazenes were synthesized, and then microcapsulated chlorocyclophosphazene/polypropylene(PP) composites were prepared.The results showed that microcapsulated chlorocyclophosphazene had good high thermal stability through thermogravimetric analysis (TGA).The flammability and mechanical properties of microcapsulated chlorocyclophosphazene/polypropylene composites were investigated by limiting oxygen index experiment, UL 94V flame retardancy test, cone calorimetry, tensile experiment, and impact test, respectively.It was shown that the microcapsulated chlorocyclophosphazene/PP composites had better tensile strength, impact strength, flame retardant properties and smoke suppress properties compared with chlorocyclophosphazene/PP composites.

  10. Bulletin of Materials Science | Indian Academy of Sciences

    Indian Academy of Sciences (India)

    ... analysis and thermogravimetric/differential thermal analysis, respectively. The membrane that contains EC+ GBL exhibits maximum ionic conductivity of the order of 1.208×10-3 S cm-1 at 303 K. The temperature-dependent ionic conductivity of the polymer membranes has been estimated using AC impedance analysis.

  11. Photocatalytic properties of hierarchical ZnO flowers synthesized by a sucrose-assisted hydrothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Lv Wei [Key Laboratory of Photonic and Electric Bandgap Materials, Ministry of Education, School of Physics and Electronic Engineering, Harbin Normal University, Harbin 150025 (China); Wei Bo [Center for Condensed Matter Science and Technology, Department of Physics, Harbin Institute of Technology, Harbin 150080 (China); Xu Lingling, E-mail: xulingling_hit@163.com [Key Laboratory of Photonic and Electric Bandgap Materials, Ministry of Education, School of Physics and Electronic Engineering, Harbin Normal University, Harbin 150025 (China) and Center for Condensed Matter Science and Technology, Department of Physics, Harbin Institute of Technology, Harbin 150080 (China); Zhao Yan, E-mail: zhaoyan516@126.com [Department of Physics, Northeast Forestry University, Harbin 150040 (China); Gao Hong; Liu Jia [Key Laboratory of Photonic and Electric Bandgap Materials, Ministry of Education, School of Physics and Electronic Engineering, Harbin Normal University, Harbin 150025 (China)

    2012-10-15

    Highlights: Black-Right-Pointing-Pointer Hierarchical ZnO flowers were synthesized via a sucrose-assisted urea hydrothermal method. Black-Right-Pointing-Pointer The sucrose added ZnO flowers showed improved activity mainly due to the improved crystallinity. Black-Right-Pointing-Pointer The effect of sucrose content was studied and optimized. - Abstract: In this work, hierarchical ZnO flowers were synthesized via a sucrose-assisted urea hydrothermal method. The thermogravimetric analysis/differential thermal analysis (TGA-DTA) and Fourier transform infrared spectra (FTIR) showed that sucrose acted as a complexing agent in the synthesis process and assisted combustion during annealing. Photocatalytic activity was evaluated using the degradation of organic dye methyl orange. The sucrose added ZnO flowers showed improved activity, which was mainly attributed to the better crystallinity as confirmed by X-ray photoelectron spectroscopy (XPS) analysis. The effect of sucrose amount on photocatalytic activity was also studied.

  12. Thermal, mechanical, optical and dielectric properties of piperazinium hydrogen phosphite monohydrate NLO single crystal

    Science.gov (United States)

    Rajkumar, R.; Praveen Kumar, P.

    2018-05-01

    Optical transparent crystal of piperazinium hydrogen phosphite monohydrate (PHPM) was grown by slow evaporation method. The grown crystal was characterized by single crystal X-ray diffraction analysis and the crystal belongs to monoclinic system. The functional groups present in PHPM crystal were confirmed by FTIR analysis. UV-Visible spectrum shows that the PHPM crystal is transparent in the visible region. The mechanical behavior of PHPM crystal was characterized by Vickers hardness test. Thermal stability of PHPM crystal was analyzed by thermogravimetric analysis. Dielectric studies were also carried out for the grown crystal. The third-order nonlinear parameters such as nonlinear refractive index and nonlinear absorption coefficient have been calculated using Z scan technique.

  13. Soft purification of N-doped and undoped multi-wall carbon nanotubes

    International Nuclear Information System (INIS)

    Alvizo-Paez, Edgar Rogelio; Ruiz-Garcia, Jaime; Hernandez-Lopez, Jose Luis; Romo-Herrera, Jose Manuel; Terrones, Humberto; Terrones, Mauricio

    2008-01-01

    A soft method for purifying multi-wall carbon nanotubes (N-doped and undoped) is presented. The technique includes a hydrothermal/ultrasonic treatment of the material in conjunction with other subsequent treatments, including the extraction of polyaromatic compounds, dissolution of metal particles, bundle exfoliation, and uniform dispersion. This method avoids harsh oxidation protocols that burn (via thermal treatments) or functionalize (by introducing chemical groups) the nanotubes. We show a careful analysis of each purification step and demonstrate that the technique is extremely efficient when characterizing the materials using scanning electron microscopy (SEM), energy dispersive x-ray analysis (EDAX), scanning tuneling electron microscopy (STEM), x-ray powder diffraction (XRD), diffuse reflectance Fourier transform infrared (DRFTIR) spectroscopy and thermogravimetric analysis (TGA)

  14. FLAMMABILITY OF HERBICIDE-TREATED GUAVA FOLIAGE

    Science.gov (United States)

    Guava leaves treated with herbicide were found to be less flammable than untreated green leaves or dead leaves . Differences in flammability were...determined by small-scale laboratory fires, differential thermal analysis, and thermogravimetric analysis. The herbicide-treated leaves had a higher ash

  15. Shortened carbon nanotubes and their influence on the electrical properties of polymer nanocomposites

    NARCIS (Netherlands)

    Inam, F.; Reece, M.J.; Peijs, A.A.J.M.

    2012-01-01

    Multi-wall carbon nanotubes of medium length (mCNTs) were aggressively tip-ultrasonicated to produce shortened and damaged carbon nanotubes (xCNTs). High-resolution electron microscopic analysis was performed to measure the dimensions of carbon nanotubes (CNTs). Thermo-gravimetric analysis and Raman

  16. Alkali and bleach treatment of the extracted cellulose from pineapple ...

    African Journals Online (AJOL)

    (FTIR) spectroscopy, Thermogravimetric analysis (TGA) and Differential thermal analysis (DTA). SEM micrographs revealed that alkali treatment removed the impurities in the pineapple leaf fibers and subsequent bleaching further purify the fibers leaving mostly cellulose only while hemicellulose and lignin are removed as ...

  17. Bayesian analysis of repairable systems showing a bounded failure intensity

    International Nuclear Information System (INIS)

    Guida, Maurizio; Pulcini, Gianpaolo

    2006-01-01

    The failure pattern of repairable mechanical equipment subject to deterioration phenomena sometimes shows a finite bound for the increasing failure intensity. A non-homogeneous Poisson process with bounded increasing failure intensity is then illustrated and its characteristics are discussed. A Bayesian procedure, based on prior information on model-free quantities, is developed in order to allow technical information on the failure process to be incorporated into the inferential procedure and to improve the inference accuracy. Posterior estimation of the model-free quantities and of other quantities of interest (such as the optimal replacement interval) is provided, as well as prediction on the waiting time to the next failure and on the number of failures in a future time interval is given. Finally, numerical examples are given to illustrate the proposed inferential procedure

  18. Investigation of Water Absorption and Diffusion in Microparticles Containing Xylitol to Provide a Cooling Effect by Thermal Analysis

    Science.gov (United States)

    Salaün, F.; Bedek, G.; Devaux, E.; Dupont, D.; Deranton, D.

    2009-08-01

    Polyurethane microparticles containing xylitol as a sweat sensor system were prepared by interfacial polymerization. The structural and thermal properties of the resultant microparticles were studied. The surface morphology and chemical structure of microparticles were investigated using an optical microscope (OM) and a Fourier-transform infrared spectroscope (FTIR), respectively. The thermal properties of samples were investigated by thermogravimetric analysis (TGA) and by differential scanning calorimetry (DSC). Thus, two types of microparticles were synthesized by varying the percentage of monomers introduced. The obtained morphology is directly related to the synthesis conditions. DSC analysis indicated that the mass content of crystalline xylitol was up to 63.8 %, which resulted in a high enthalpy of dilution of 127.7 J · g-1. Furthermore, the water release rate monitored by TGA analysis was found to be faster from the microparticles than from raw xylitol. Thus, the microparticles could be applied for thermal energy storage and moisture sensor enhancement.

  19. Modifications of Atlantic salmon by-product oil for obtaining different ω-3 polyunsaturated fatty acids concentrates: An approach to comparative analysis

    Directory of Open Access Journals (Sweden)

    Monjurul Haq

    2018-04-01

    Full Text Available Omega-3 polyunsaturated fatty acids (ω-3 PUFAs rich 2-monoacylglycerols (2-MAG, omega-3 polyunsaturated free fatty acids (ω-3 PUFFAs concentrate, and PUFA enriched acylglycerols were prepared from salmon frame bone oil (SFBO by enzymatic alcoholysis, urea complexation, and enzymatic esterification, respectively. The yields of 2-MAG, ω-3 PUFFAs concentrate, and PUFA enriched acylglycerols were 40.25, 16.52, and 15.65%, respectively. ω-3 PUFFAs concentrate and PUFA enriched acylglycerols showed darker red color than SFBO and 2-MAG due to aggregation of astaxanthin pigment in ω-3 PUFFAs concentrate during urea complexation. The viscosity and specific gravity of SFBO and PUFA enriched acylglycerols showed similar values whereas 2-MAG and ω-3 PUFFAs showed significantly (p < 0.05 lower values. Stability parameters like acid value, peroxide value, free fatty acid value, and p-anisidine value of SFBO and ω-3 PUFAs concentrates were within acceptable limits except extreme high acid value and free fatty acid value of ω-3 PUFFAs concentrate. Thermogravimetric analysis showed similar and higher thermal stability of SFBO and PUFA enriched acylglycerols than 2-MAG and ω-3 PUFFAs concentrate. The ω-3 PUFAs content in 2-MAG, ω-3 PUFFAs concentrate, and PUFA enriched acylglycerols was increased to 20.81, 52.96, and 51.74% respectively from 13.54% in SFBO. ω-3 PUFFAs concentrate and PUFA enriched acylglycerols showed higher DPPH and ABTS radical scavenging activity than SFBO and 2-MAG. The results obtained from this study suggest the production of PUFA enriched acylglycerols rich in ω-3 PUFAs supplements from fish oil for human and pet animals. Keywords: Comparative analysis, ω-3 PUFFAs concentrate, Salmon frame bone oil, PUFA enriched acylglycerols, 2-MAG

  20. Structural and optical properties of electrodeposited molybdenum oxide thin films

    International Nuclear Information System (INIS)

    Patil, R.S.; Uplane, M.D.; Patil, P.S.

    2006-01-01

    Electrosynthesis of Mo(IV) oxide thin films on F-doped SnO 2 conducting glass (10-20/Ω/□) substrates were carried from aqueous alkaline solution of ammonium molybdate at room temperature. The physical characterization of as-deposited films carried by thermogravimetric/differential thermogravimetric analysis (TGA/DTA), infrared spectroscopy and X-ray diffraction (XRD) showed the formation of hydrous and amorphous MoO 2 . Scanning electron microscopy (SEM) revealed a smooth but cracked surface with multi-layered growth. Annealing of these films in dry argon at 450 deg. C for 1 h resulted into polycrystalline MoO 2 with crystallites aligned perpendicular to the substrate. Optical absorption study indicated a direct band gap of 2.83 eV. The band gap variation consistent with Moss rule and band gap narrowing upon crystallization was observed. Structure tailoring of as-deposited thin films by thermal oxidation in ambient air to obtain electrochromic Mo(VI) oxide thin films was exploited for the first time by this novel route. The results of this study will be reported elsewhere

  1. Synthesis and Thermal and Photo Behaviors of New Polyamide/Organocaly Nanocomposites Containing Para Phenylenediacrylic Moiety

    Science.gov (United States)

    Faghihi, Khalil; Soleimani, Masoumeh; Shabanian, Meisam; Abootalebi, Ashraf Sadat

    2011-06-01

    New type of aromatic polyamide/montmorillonite nanocomposites were produced using solution process in N-methyl-2-pyrolidone. Amide chains were synthesized from 4,4'-diaminodiphenyl sulfone and p-phenylenediacrylic acid in N-methyl-2-pyrolidone. The resulting nanocomposite films containing 5-15 mass % of organoclay were characterized for FT-IR, scanning electronmicroscopy (SEM), X-ray diffraction (XRD), thermogravimetric analysis (TGA), optical transparency and water absorption measurements. The distribution of organoclay and nanostructure of the composites were investigated by (XRD) and SEM analyses. Thermogravimetric analysis indicated an increase in thermal stability of nanocomposites as compared to pristine polyamide. The percentage optical transparency and water absorption of these hybrids was found to be much reduced upon the addition of modified layered silicate indicating decreased permeability.

  2. Oxidation behavior of U-Si compounds in air from 25 to 1000 C

    Science.gov (United States)

    Sooby Wood, E.; White, J. T.; Nelson, A. T.

    2017-02-01

    The air oxidation behavior of U3Si2, USi, and U3Si5 is studied from room temperature to 1000 C. The onsets of breakaway oxidation for each compound are identified during synthetic air ramps to 1000 C using thermogravimetric analysis. Isothermal air oxidation tests are performed below and above the breakaway oxidation onset to discern the oxidation kinetic behavior of these candidate accident tolerant fuel forms. Uranium metal is tested in the same manner to provide a reference for the oxidation behavior. Thermogravimetric, x-ray diffraction, and scanning electron microscopy analysis are presented here along with a discussion of the oxidation behavior of these materials and the impact of the lack of oxidation resistance to their deployment as accident tolerant nuclear fuels.

  3. Synthesis, crystal structures, molecular docking and urease inhibition studies of Ni(II) and Cu(II) Schiff base complexes

    Science.gov (United States)

    Sangeeta, S.; Ahmad, K.; Noorussabah, N.; Bharti, S.; Mishra, M. K.; Sharma, S. R.; Choudhary, M.

    2018-03-01

    [Ni(L)2] 1 and [Cu(L)2] 2 [HL = 2-((E)-(2-methoxyphenylimino)methyl)-4,6-dichlorophenol] Schiff base complexes have been successfully synthesized and were characterized by FT-IR, UV-Vis, fluorescence spectroscopy and thermogravimetric analysis. The crystal structures of the two complexes were determined through X-ray crystallography. Its inhibitory activity against Helicobacter pylori urease was evaluated in vitro and showed strong inhibitory activity against H. pylori urease compared with acetohydroxamic acid (IC50 = 42.12 μmolL-1), which is a positive reference. A docking analysis using the AutoDock 4.0 program could explain the inhibitory activity of the complex against urease.

  4. Chemical and Pyrolytic Thermogravimetric Characterization of Nigerian Bituminous Coals

    Directory of Open Access Journals (Sweden)

    Nyakuma Bemgba Bevan

    2016-12-01

    Full Text Available The discovery of new coal deposits in Nigeria presents solutions for nation’s energy crises and prospects for socioeconomic growth and sustainable development. Furthermore, the quest for sustainable energy to limit global warming, climate change, and environmental degradation has necessitated the exploration of alternatives using cleaner technologies such as coal pyrolysis. However, a lack of comprehensive data on physico-chemical and thermal properties of Nigerian coals has greatly limited their utilization. Therefore, the physico-chemical properties, rank (classification, and thermal decomposition profiles of two Nigerian bituminous coals – Afuze (AFZ and Shankodi-Jangwa (SKJ – were examined in this study. The results indicate that the coals contain high proportions of C, H, N, S, O and a sufficiently high heating value (HHV for energy conversion. The coal classification revealed that the Afuze (AFZ coal possesses a higher rank, maturity, and coal properties compared to the Shankodi-Jangwa (SKJ coal. A thermal analysis demonstrated that coal pyrolysis in both cases occurred in three stages; drying (30-200 °C, devolatilization (200-600 °C, and char decomposition (600-1000 °C. The results also indicated that pyrolysis at 1000 °C is not sufficient for complete pyrolysis. In general, the thermochemical and pyrolytic fuel properties indicate that the coal from both places can potentially be utilized for future clean energy applications.

  5. Thermal stability and degradation kinetics of polyphenols and polyphenylenediamines enzymatically synthesized by horseradish peroxidase

    Energy Technology Data Exchange (ETDEWEB)

    Park, Hansol; Ryu, Keungarp [University of Ulsan, Ulsan (Korea, Republic of); Kwon, Oyul [Seoul National University of Science and Technology, Seoul (Korea, Republic of)

    2015-09-15

    Various substituted phenols and phenylenediamines were enzymatically polymerized by horseradish peroxidase in 80% (v/v) organic solvents-aqueous buffer (100 mM sodium acetate, pH 5) mixtures with H{sub 2}O{sub 2} as the oxidant. The thermal stability of the polymers was investigated by thermogravimetric analysis (TGA) and represented by the char yield (wt% of the initial polymer mass) after being heated at 800 .deg. C. Poly(p-phenylphenol) had the highest thermal stability among the synthesized polymers with a char yield of 47 wt%. The polymers containing amino groups such as poly(p-aminophenol) and polyphenylenediamines were also shown to possess high thermal stabilities. The activation energies for the thermal degradation of the polymers determined by derivative thermogravimetric analysis (DTG) using Horowitz-Metzger's pseudo-first-order kinetics were in the range between 23-65 kJ/mol and comparable to those of the chemically synthesized polymers. Dynamic structural changes of the enzymatically synthesized polymers upon heating were studied by differential scanning calorimetry (DSC). The DSC curves of poly(p-phenylphenol) showed a broad exothermic peaks between 150-250 .deg. C, indicating that the polymer undergoes complex structural transitions in the temperature range. On the other hand, the DSC curves of the poly(p-aminophenol) and the poly(p-phenylenediamine) which contain amino groups showed strong sharp endothermic peaks near 150 .deg. C, implying that these polymers possess homogeneous oriented structures which undergo a concerted structural disintegration upon heating.

  6. Thermal stability and degradation kinetics of polyphenols and polyphenylenediamines enzymatically synthesized by horseradish peroxidase

    International Nuclear Information System (INIS)

    Park, Hansol; Ryu, Keungarp; Kwon, Oyul

    2015-01-01

    Various substituted phenols and phenylenediamines were enzymatically polymerized by horseradish peroxidase in 80% (v/v) organic solvents-aqueous buffer (100 mM sodium acetate, pH 5) mixtures with H 2 O 2 as the oxidant. The thermal stability of the polymers was investigated by thermogravimetric analysis (TGA) and represented by the char yield (wt% of the initial polymer mass) after being heated at 800 .deg. C. Poly(p-phenylphenol) had the highest thermal stability among the synthesized polymers with a char yield of 47 wt%. The polymers containing amino groups such as poly(p-aminophenol) and polyphenylenediamines were also shown to possess high thermal stabilities. The activation energies for the thermal degradation of the polymers determined by derivative thermogravimetric analysis (DTG) using Horowitz-Metzger's pseudo-first-order kinetics were in the range between 23-65 kJ/mol and comparable to those of the chemically synthesized polymers. Dynamic structural changes of the enzymatically synthesized polymers upon heating were studied by differential scanning calorimetry (DSC). The DSC curves of poly(p-phenylphenol) showed a broad exothermic peaks between 150-250 .deg. C, indicating that the polymer undergoes complex structural transitions in the temperature range. On the other hand, the DSC curves of the poly(p-aminophenol) and the poly(p-phenylenediamine) which contain amino groups showed strong sharp endothermic peaks near 150 .deg. C, implying that these polymers possess homogeneous oriented structures which undergo a concerted structural disintegration upon heating.

  7. DIRECT GROWTH OF VERTICALLY ALIGNED CARBON ...

    African Journals Online (AJOL)

    diffraction, thermogravimetric analysis, and Raman spectroscopy. Scanning electron ... be a good precursor of iron nanoparticles suitable to catalyze CNT growth [16-17]. .... chitosan-CdS and its biosensoring for glucose. Electrochem.

  8. Effect of acid treated carbon nanotubes on mechanical, rheological and thermal properties of polystyrene nanocomposites

    KAUST Repository

    Amr, Issam Thaher; Al-Amer, Adnan M J; Selvin, Thomas P.; Al-Harthi, Mamdouh Ahmed; Girei, Salihu Adamu; Sougrat, Rachid; Atieh, Muataz Ali

    2011-01-01

    In this work, multiwall carbon nanotubes (CNT) were functionalized by acid treatment and characterized using Fourier Transform Infrared Spectroscopy (FTIR) and thermogravimetric analysis (TGA). Polystyrene/CNT composites of both the untreated

  9. Synthesis, characterization and ion exchange properties of ...

    Indian Academy of Sciences (India)

    sodium tungstate, potassium iodate and 1 mol L–1 orthophosphoric acid to aqueous ... titration, Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis. ..... moderate concentration whereas it is less stable in bases.

  10. Non-Parametric Kinetic (NPK Analysis of Thermal Oxidation of Carbon Aerogels

    Directory of Open Access Journals (Sweden)

    Azadeh Seifi

    2017-05-01

    Full Text Available In recent years, much attention has been paid to aerogel materials (especially carbon aerogels due to their potential uses in energy-related applications, such as thermal energy storage and thermal protection systems. These open cell carbon-based porous materials (carbon aerogels can strongly react with oxygen at relatively low temperatures (~ 400°C. Therefore, it is necessary to evaluate the thermal performance of carbon aerogels in view of their energy-related applications at high temperatures and under thermal oxidation conditions. The objective of this paper is to study theoretically and experimentally the oxidation reaction kinetics of carbon aerogel using the non-parametric kinetic (NPK as a powerful method. For this purpose, a non-isothermal thermogravimetric analysis, at three different heating rates, was performed on three samples each with its specific pore structure, density and specific surface area. The most significant feature of this method, in comparison with the model-free isoconversional methods, is its ability to separate the functionality of the reaction rate with the degree of conversion and temperature by the direct use of thermogravimetric data. Using this method, it was observed that the Nomen-Sempere model could provide the best fit to the data, while the temperature dependence of the rate constant was best explained by a Vogel-Fulcher relationship, where the reference temperature was the onset temperature of oxidation. Moreover, it was found from the results of this work that the assumption of the Arrhenius relation for the temperature dependence of the rate constant led to over-estimation of the apparent activation energy (up to 160 kJ/mol that was considerably different from the values (up to 3.5 kJ/mol predicted by the Vogel-Fulcher relationship in isoconversional methods

  11. Synthesis and Characterization of Lanthanum Complexes with Amino Acid Schiff Base

    Institute of Scientific and Technical Information of China (English)

    张秀英; 张有娟; 杨林

    2001-01-01

    Six new complexes of lanthanum with amino acid Schiff base ligands, A-F, were prepared in methanol-aqueous solution. The composition and properties of the title complexes were characterized by elemental analysis, molar conductance, infrared, electronic spectra, 1H NMR, thermogravimetric and differential thermal analysis.

  12. Physicochemical properties of nanoparticles titania from alcohol ...

    African Journals Online (AJOL)

    The synthesized TiO2 were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), thermal analysis (thermogravimetric analysis, TGA, and differential scanning calorimetry, DSC), and surface area Brunauer–Emmett–Teller (BET) method. The photocatalytic activity of TiO2 nanoparticles was ...

  13. Marmosets, Raree shows and Pulcinelle: an Analysis and Edition of a Hitherto-Unpublished Carnival Play by Antonio de Zamora

    Directory of Open Access Journals (Sweden)

    Fernando Plata

    2013-05-01

    Full Text Available This paper is an analyisis, annotation and edition of the Mojiganga del mundinovo (‘The raree show, a carnival play’ by Antonio de Zamora. The play was performed in 1698 Madrid by the troupe of Carlos Vallejo, along with the sacramental one-act play El templo vivo de Dios (‘The living temple of God’. The hitherto unpublished text is based on the only two extant manuscripts, located in archives in Madrid. Despite the play’s title, my analysis argues that the novelty in this play is not so much the raree show, a contraption popularized four decades earlier in Golden Age theater, as the marmosets. The death of two marmosets and the ensuing desolation of their owner, Ms. Estupenda, both trigger the play and provide it with a plot. The marmosets, too, point to a changing mentality in late 17th-century society, regarding the possession among ladies of marmosets and other monkeys as pets.

  14. Meta-analysis of diffusion tensor imaging studies shows altered fractional anisotropy occurring in distinct brain areas in association with depression.

    LENUS (Irish Health Repository)

    Murphy, Melissa L

    2011-09-01

    Fractional anisotropy anomalies occurring in the white matter tracts in the brains of depressed patients may reflect microstructural changes underlying the pathophysiology of this disorder. We conducted a meta-analysis of fractional anisotropy abnormalities occurring in major depressive disorder using voxel-based diffusion tensor imaging studies. Using the Embase, PubMed and Google Scholar databases, 89 relevant data sets were identified, of which 7 (including 188 patients with major depressive disorder and 221 healthy controls) met our inclusion criteria. Authors were contacted to retrieve any additional data required. Coordinates were extracted from clusters of significant white matter fractional anisotropy differences between patients and controls. Relevant demographic, clinical and methodological variables were extracted from each study or obtained directly from authors. The meta-analysis was carried out using Signed Differential Mapping. Patients with depression showed decreased white matter fractional anisotropy values in the superior longitudinal fasciculus and increased fractional anisotropy values in the fronto-occipital fasciculus compared to controls. Using quartile and jackknife sensitivity analysis, we found that reduced fractional anisotropy in the left superior longitudinal fasciculus was very stable, with increases in the right fronto-occipital fasciculus driven by just one study. In conclusion, our meta-analysis revealed a significant reduction in fractional anisotropy values in the left superior longitudinal fasciculus, which may ultimately play an important role in the pathology of depression.

  15. Effect of high-temperature heat treatment duration on the purity and ...

    Indian Academy of Sciences (India)

    Thermogravimetric analysis (TGA), X-ray diffraction, Raman spectroscopy, transmission electron microscopy ..... atoms break away from the ordered structure, the metal cat- alyst forms ... treatment of MWCNTs, even after all metal impurities are.

  16. Thermo-mechanical characterization of a monochlorophenyl, hepta isobutyl polyhedral oligomeric silsesquioxane/polystyrene composite

    International Nuclear Information System (INIS)

    Blanco, Ignazio; Bottino, Francesco A.; Cicala, Gianluca; Cozzo, Giulia; Latteri, Alberta; Recca, Antonino

    2014-01-01

    The thermal and mechanical properties of a monochlorophenyl, hepta isobutyl Polyhedral Oligomeric Silsesquioxane/Polystyrene (ph,hib-POSS/PS) composite were studied and compared with those of pristine polymer. ph,hib-POSS/PS system was prepared by solubilization and precipitation of Polystyrene (PS) in the presence of POSS. Scanning Electron Microscopy (SEM) was performed to check the distribution of the filler in the polymer matrix. Dynamic Mechanical Analysis (DMA) was carried out to measure viscoelastic properties of solid samples. Degradations were carried out into a thermobalance and the obtained thermogravimetric (TG) and differential thermogravimetric (DTG) curves were discussed and interpreted

  17. Biorelevant characterisation of amorphous furosemide salt exhibits conversion to a furosemide hydrate during dissolution

    DEFF Research Database (Denmark)

    Nielsen, Line Hagner; Gordon, Sarah; Pajander, Jari Pekka

    2013-01-01

    , as well as of crystalline furosemide salt and acid showed a higher rate of dissolution of the salt forms in comparison with the two acid forms. The measured dissolution rates of the four furosemide forms from the UV imaging system and from eluted effluent samples were consistent with dissolution rates...... obtained from micro dissolution experiments. Partial least squares-discriminant analysis of Raman spectra of the amorphous acid form during flow through dissolution showed that the amorphous acid exhibited a fast conversion to the crystalline acid. Flow through dissolution coupled with Raman spectroscopy...... showed a conversion of the amorphous furosemide salt to a more stable polymorph. It was found by thermogravimetric analysis and hot stage microscopy that the salt forms of furosemide converted to a trihydrate during dissolution. It can be concluded that during biorelevant dissolution, the amorphous...

  18. Synthesis and characterisation of star polymer/silicon carbide nanocomposites

    International Nuclear Information System (INIS)

    Majewski, Peter; Choudhury, Namita Roy; Spori, Doris; Wohlfahrt, Ellen; Wohlschloegel, Markus

    2006-01-01

    A new type of composite material's preparation and property are reported in this paper. The composite was formed by solution blending a styrene ethylene butylenes (SEBS) star polymer with silicon carbide at various compositions. The composites were characterised using spectroscopic, microscopic and thermal techniques. Photo-acoustic Fourier transform infrared spectroscopy (PA-FT-IR) and transmission electron microscopy (TEM) results show that the SiC resides uniformly in the organic network. Thermogravimetric analysis (TGA) of the hybrid shows that the thermal stability of the composite is higher than that of the star polymer. The maximum decomposition temperature increases by 73 deg. C. Dynamic mechanical analysis (DMA) of the hybrid shows that the storage modulus of the star polymer increases after the composite formation, indicating the existence of thermodynamically stable SiC nanoparticles mostly in the micro-phase separated multiarm structure of the polymer

  19. Effect of doping of multi-walled carbon nanotubes on phenolic based carbon fiber reinforced nanocomposites

    International Nuclear Information System (INIS)

    Saeed, Sadaf; Hakeem, Saira; Faheem, Muhammad; Alvi, Rashid Ahmed; Farooq, Khawar; Hussain, Syed Tajammul; Ahmad, Shahid Nisar

    2013-01-01

    We report on the effect of multi-walled carbon nanotubes (MWCNTs) on different properties of phenolic resin. A low content of MWCNTs (∼ 0.05 wt%) was mixed in phenolic resin and a stable dispersion was achieved by ultrasonication, followed by melt mixing. After curing the characterization of these composites was done by using scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and Fourier transform infra-red spectroscopy (FTIR). The thermal and ablative properties of carbon fiber reinforced MWCNTs-phenolic nanocomposites were also studied. The addition of MWCNTs showed improvement in thermal stability and ablation properties.

  20. Research of the chemical activity of microgrinding coals of various metamorphism degree

    Science.gov (United States)

    Burdukov, A. P.; Butakov, E. B.; Kuznetsov, A. V.

    2017-09-01

    In this paper, we investigate the effect of mechanically activating grinding of coals of various degrees of metamorphism by two different methods - determination of the flash time in a vertical tubular furnace and thermogravimetric analysis. In the experiments, the coals that had been processed on a vibrating centrifugal mill and a disintegrator, aged for some time, were compared. The experiments showed a decrease in the ignition temperature of mechanically activated coals - deactivation of fuel, as well as the effect of mechanical activation on the further process of thermal-oxidative degradation.