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1.
Poly(N-vinyl-2-pyrrolidone-maleic anhydride-styrene) terpolymer was prepared using AIBN initiator with acetone as solvent. The terpolymer was grafted with anti-bacterial agents para-aminobenzoic acid and 2,4-dichlorophenol to introduce bactericidal activity to the terpolymer. The terpolymer and the grafted polymers were characterized by FTIR, 1H-NMR, and 13C-NMR spectroscopic methods. Thermal properties were determined by differential scanning calorimetric technique and thermogravimetric analysis. The glass transition temperature was found to be 111°C (terpolymer), 150°C (VMS-G-PABA) and 130°C (VMS-G-DCP). Terpolymer starts degradation at 288°C and grafted terpolymers at 104°C (VMS-G-PABA) and 129°C (VMS-G-DCP), respectively. The anti-bacterial activity of grafted terpolymers were evaluated by the shake flask method against gram positive and gram negative bacteria E. coli and S. epidermidis. The grafted terpolymers showed effective inhibition against both the bacteria, the minimum inhibition concentration was observed to be 75 µg/mL and 80 µg/mL for VMS-G-PABA and 50 µg/mL for VMS-G-DCP against E. coli and S. epidermidis, respectively. The new polymers showed 90% bacterial growth inhibition at 200 µg/mL.  相似文献   

2.
In this project, we synthesized TiO2 compounds through the molten salt method (MSM) using Ti(IV) oxysulfate, as the Ti source. Molten salts in the ratio of 0.375 M LiNO3:0.180 M NaNO3:0.445 M KNO3 were added and heated at temperatures of 145, 280, 380, and 480 °C for 2 h in air, respectively. A part of the sample prepared at 145 °C was further reheated to 850 °C for 2 h in air. X-ray diffraction studies showed that the amorphous phase was obtained when the sample was prepared at 145 °C, and polycrystalline to crystalline anatase phase was formed when heated from 280 to 850 °C, which is complementary to the results of selected area electron diffraction studies. Electrochemical properties were studied using galvanostatic cycling, cyclic voltammetry, and electrochemical impedance spectroscopy at a current density of 33 mA g?1 (0.1 C rate) and a scan rate of 0.058 mV s?1, in the voltage range 1.0–2.8 V vs. Li. Electrochemical cycling profiles for the amorphous TiO2 samples prepared at 145 °C showed single-phase reaction with a low reversible capacity of 65 mAh g?1, whereas compounds prepared at 280 °C and above showed a two-phase reaction of Li-poor and Li-rich regions with a reversible capacity of 200 mAh g?1. TiO2 produced at 280 °C showed the lowest capacity fading and the lowest impedance value among the investigated samples.  相似文献   

3.
In this study, we experimentally obtained partitioning ratios of radioiodide (125I?) in the three phases at two different temperatures, 4 and 23 °C, in order to observe the effect of biological activity for upland soil samples. Even at 4 °C, 125I emission was found; its partitioning ratio in the gas phase ranged from 0 to 27 %. As expected, the ratio at 23 °C was higher than that at 4 °C. Additionally, in comparison of the data for upland soil samples obtained in this study and our previous data for paddy soil samples, for the latter, I? was not only sorbed in the soil but also more of it was released into the air than for upland soil samples. The land-use difference for I? partitioning in soil might be attributed to the differences of exchangeable K and stable I concentrations in soil from the statistical analysis. On the other hand, there were good correlations of partitioning ratios in solid, liquid, and gas phases between the two temperatures. The results implied that the biological activity can enhance partitioning in not only the gas phase, but also the solid phase. Indeed, the soil–soil solution distribution coefficient at 23 °C was about three times as high as that at 4 °C.  相似文献   

4.
We have studied LiFePO4/C nanocomposites prepared by sol-gel method using lauric acid as a surfactant and calcined at different temperatures between 600 and 900 °C. In addition to the major LiFePO4 phase, all the samples show a varying amount of in situ Fe2P impurity phase characterized by x-ray diffraction, magnetic measurements, and Mössbauer spectroscopy. The amount of Fe2P impurity phase increases with increasing calcination temperature. Of all the samples studied, the LiFePO4/C sample calcined at 700 °C which contains ~15 wt% Fe2P shows the least charge transfer resistance and a better electrochemical performance with a discharge capacity of 136 mA h g?1 at a rate of 1 C, 121 mA h g?1 at 10 C (~70 % of the theoretical capacity of LiFePO4), and excellent cycleability. Although further increase in the amount of Fe2P reduces the overall capacity, frequency-dependent Warburg impedance analyses show that all samples calcined at temperatures ≥700 °C have an order of magnitude higher Li+ diffusion coefficient (~1.3?×?10?13 cm2 s?1) compared to the one calcined at 600 °C, as well as the values reported in literature. This work suggests that controlling the reduction environment and the temperature during the synthesis process can be used to optimize the amount of conducting Fe2P for obtaining the best capacity for the high power batteries.  相似文献   

5.
Ambazone is a pharmaceutical compound that possesses antiseptic activity and tested as well for anti-tumor properties. Metal complexes of Zn(II), Fe(III), and Cu(II) containing ambazone as ligand were synthesized using a molar ratio salt:ligand of 1:1, heating the mixture up to 50 °C for 6 h. Coordination compounds were characterized by thin-layer chromatography, FT-IR spectroscopy, elemental analysis, and thermal behavior. The non-isothermal experiments were carried out in order to investigate the thermal degradation process of these complexes and were performed in a dynamic air atmosphere at a heating rate β = 10 °C min?1 from ambient temperature, up to 500 °C. It was revealed that decomposition process is a multistadial one.  相似文献   

6.
Efficiency in HPLC can be enhanced by increasing the column length and/or decreasing the particle size. The use of high temperature in HPLC has emerged as a valuable tool to overcome the increase in column backpressure when using small packing particles, as it allows for reduction in mobile phase viscosity. In this study, high plate count was obtained by coupling sub-2 ??m columns at elevated temperature to reduce the viscosity of the mobile phase, thus reducing the column backpressure. At 80 °C, up to three columns of 15 cm × 4.6 mm I.D. packed with 1.8 ??m particles could be coupled generating ~84,000 theoretical plates for the last eluting compound. The number of theoretical plates was increased on average by a factor of ~3.6 when three columns were coupled at 80 °C compared with one column at 30 °C. The relationships between separation efficiency and column length were examined using Van Deemter plots constructed at 30 °C and 80 °C for different column lengths. The advantages of using coupled columns in combination with elevated temperature for the environmental analysis were illustrated using test mixtures comprised of eight sulfonamides separated on one column at 30 °C and three coupled columns at 80 °C by isocratic elution. Sample clean up was carried out by employing solid-phase extraction (SPE) using Oasis HLB cartridges. The method developed was validated based on parameters such as linearity, precision, accuracy, detection and quantification limits. Recoveries generally ranged from 71.7 to 99% (with the exception of sulfanilamide), with standard deviations not higher than 4.7%. The detection limits of the method ranged from 0.6?C2 ??g L?1, while limits of quantification were in the range 2?C6.7 ??g L?1 with UV detection.  相似文献   

7.
This work focuses on the thermal characterization of a calcium silicate-based material synthesized with different solid wastes (chamotte and marble) for use as thermal insulation material. Thermal and structural changes occurring during heating were accompanied by differential thermal analysis, thermogravimetric analysis, dilatometric analysis, open photoacoustic cell technique, X-ray diffraction (XRD), and scanning electron microscopy. An endothermic event at 823.2 °C was interpreted as decomposition of carbonates. An exothermic event around 900 °C is associated with the crystallization of calcium silicate phases mainly wollastonite. The themophysical properties of the calcium silicate-based material (thermal diffusivity, thermal conductivity, specific thermal capacity, and thermal effusivity) are influenced by the synthesis temperature. The thermal analysis results agree well with the XRD. The calcium silicate pieces presented low thermal conductivity values (0.227?0.376 W m?1 K?1). These results suggest that the calcium silicate-based materials produced essentially with chamotte and marble wastes has high potential to be used as thermal insulation construction material.  相似文献   

8.
ZnO nanoparticles (NPs) with tunable morphologies were synthesized by a hybrid electrochemical–thermal method at different calcination temperatures without the use of any surfactant or template. The NPs were characterized by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction, dynamic light scattering, thermogravimetry–differential thermal analysis, scanning electron microscope and N2 gas adsorption–desorption studies. The FT-IR spectra of ZnO NPs showed a band at 450 cm?1, a characteristic of ZnO, which remained fairly unchanged at calcination temperatures even above 300 °C, indicating complete conversion of the precursor to ZnO. The products were thermally stable above 300 °C. The ZnO NPs were present in a hexagonal wurtzite phase and the crystallinity of ZnO increased with an increasing calcination temperature. The ZnO NPs calcined at lower temperature were mesoporous in nature. The surface areas of ZnO NPs calcined at 300 and 400 °C were 51.10 and 40.60 m2 g?1, respectively, which are significantly larger than commercial ZnO nanopowder. Surface diffusion has been found to be the key mechanism of sintering during heating from 300 to 700 °C with the activation energy of sintering as 8.33 kJ mol?1. The photocatalytic activity of ZnO NPs calcined at different temperatures evaluated by photocatalytic degradation of methylene blue under sunlight showed strong dependence on the surface area of ZnO NPs. The ZnO NPs with high surface area showed enhanced photocatalytic activity.  相似文献   

9.
Abstract

A novel hydrolysis-resistant superabsorbent composite was prepared via the solution polymerization based on acrylic acid (AA) and sodium bentonite (SBT) as monomers, tetraallylammonium bromine (TAAB) as crosslinker and ammonium persulfate (APS) as initiator. The mechanism of polymerization and the structure of the superabsorbent polymer (SAP) were studied by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (X-ray), and scanning electron microscopy (SEM). The reaction conditions such as different mass ratios of APS to AA, TAAB to AA, SBT to AA, neutralization degree of AA were optimized by orthogonal experiment, and the influence of each reaction condition on the capacity of water absorption at 150?°C was investigated via single-factor controlled experiment. The hydrolysis resistance and swelling kinetics of the SAP were studied in different solutions at 150?°C. Compared to traditional SAPs, the SAP synthesized with TAAB as crosslinker performed a more excellent hydrolysis resistance and water absorbency capacity at high temperatures. The water absorbency in distilled water or 0.1?mol L?1 NaCl solution could reach 392.6 and 145.2?g g?1at 150?°C, respectively. The SAP maintaining high swelling capacity in the pH range of 5–9 indicated its wide application values in the acidic or alkaline environment at high temperature. In addition, the SAP exhibited good reusability which could still retain about 73% of its initial water absorbency after reswelling six times at 150?°C.  相似文献   

10.
A hyaluronate lyase was obtained by cultivating Arthrobacter globiformis strain A152. The enzyme was purified to homogeneity from the supernatant by ammonium sulfate fractionation, Q Sepharose Fast Flow, and Sephadex G-100 chromatography. The purification resulted in a 32.78-fold increase in hyaluronate lyase activity with specific activity of 297.2 U/mg. The molecular weight of the enzyme determined by SDS-PAGE was approximately 73.7 kDa. Using hyaluronic acid (HA) as a substrate, the maximal reaction rate (Vmax) and the Michaelis–Menten constant (Km) of hyaluronate lyase were found to be 4.76 μmol/min/ml and 0.11 mg/ml, respectively. The optimum pH and temperature values for hyaluronate lyase activity were pH 6.0 and 42 °C, respectively. This enzyme was stable at pH 4–10, 5–7, and 5–7 at 4, 37, and 42 °C, respectively. Investigation about temperature effects on hyaluronate lyase displayed that it was stable at 30–37 °C and also showed high activity at 37 °C. The enzymatic activity was enhanced by Ca2+ and was strongly inhibited by Cu2+ and SDS. These properties suggested that the hyaluronate lyase in this study could bring promising prospects in medical and industry applications.  相似文献   

11.
The photocatalytic conversion of CO2 and H2O to alcohols was achieved using self-organized TiO2 nanotube arrays (TNAs), which were prepared by electrochemical anodization of Ti foils in 1 M (NH4)2SO4 electrolyte containing 0.5 wt% NH4F. Experimental results revealed that the morphology and structure of self-organized TNAs could be strongly influenced by the applied voltage and anodization temperature, and the optimized TNAs were prepared by electrochemical anodization of Ti foils under optimal conditions (i.e., at 20 V for 2 h at 30 °C). The as-prepared TNAs were amorphous and could be transformed to anatase phase during the thermal treatment at 450 °C in air for 3 h. By using the annealed TNAs as a photocatalyst, the photocatalytic reduction of CO2 to alcohol, predominately methanol and ethanol, was demonstrated under Xenon lamp illumination. Based on the photocatalytic measurements, the production rates of methanol and ethanol were calculated to be ~10 and ~9 nmol cm?2 h?1, respectively. In addition, the formation mechanism of methanol and ethanol was also tentatively proposed.  相似文献   

12.
The synthesis of titanium pyrophosphate is carried out, and the material is sintered at different temperatures between 370 and 970 °C. Yttrium is added during the synthesis to act as acceptor dopant, but it is mainly present in the material in secondary phases. The conductivity is studied systematically as a function of sintering temperature, pH2O, pO2, and temperature (100–400 °C). Loss of phosphorus upon sintering above 580–600 °C is confirmed by energy dispersive spectroscopy and combined thermogravimetry and mass spectrometry. The conductivity decreases with increasing sintering temperature and decreasing phosphorus content. The highest conductivity is 5.3?×?10?4 S cm?1 at 140 °C in wet air (pH2O?=?0.22 atm) after sintering at 370 °C. The conductivity is higher in wet atmospheres than in dry atmospheres. The proton conduction mechanism is discussed, and the conductivity is attributed to an amorphous secondary phase at the grain boundaries, associated with the presence of excess phosphorus in the samples. A contribution to the conductivity by point defects in the bulk may explain the conductivity trend in dry air and the difference in conductivity between oxidizing and reducing atmospheres at 300–390 °C. Slow loss of phosphorus by evaporation over time and changes in the distribution of the amorphous phase during testing are suggested as causes of conductivity degradation above 220 °C.  相似文献   

13.
In this study, the use of the organic fraction of municipal solid waste as an abundant and low-cost raw material for producing activated carbon was investigated. For this purpose, ZnCl2 was used as a chemical activation agent and the carbonization process took place at 800 °C in N2 atmosphere. Seven sorbents were prepared by chemical activation (pyrolysis under N2 atmosphere at temperature of 800 °C after impregnation with ZnCl2) with different ratios of ZnCl2. The optimum ratio of organic fraction of municipal solid waste to ZnCl2 was inspected via methylene blue number and iodine number (ASTM Designation: D4607–94). The results showed that the adsorbent with 60 % ZnCl2/raw material was the most appropriate one with a satisfactory adsorption capacity, 112.4 mg g?1 for methylene blue and 134.0 mg g?1 for iodine. In addition, the structural analysis of this sorbent was performed using FT-IR, BET surface area, SEM–EDX and thermal analysis. Application of this sorbent to remove Cr(VI) from wastewater was studied to find an adsorption capacity of 66.7 mg g?1. The experimental adsorption equilibrium data were fitted to Langmuir adsorption model with an acceptable adsorption capacity of 66.7 mg g?1.  相似文献   

14.
In this work, the influence of the mineral composition of the synthesized calcium silicate hydrates on their hydraulic activity after thermal treatment was determined. Primary mixture, consisting of quartz sand and burnt limestone (CaO/SiO2 = 2), was treated hydrothermally with NaOH additive at 200 °C. It was determined that α-C2SH prevailed in the product after 4 h of the synthesis. The results of DSC and XRD analysis revealed that α-C2SH was partially decomposed after 12 h of the synthesis and newly formed compounds were identified—killalaite, portlandite and C–S–H. The products of 4 and 12 h synthesis were treated thermally at temperatures between 450 and 1000 °C. It was determined that dellaite and x-C2S formed already at 450 °C, β-C2S at 600 °C and α′L-C2S at 800 °C when the 4 h synthesis product, in which α-C2SH prevailed, was treated thermally. On the other hand, killalaite remained stable up to 600 °C, and the temperature values, at which mentioned calcium silicates formed, increased in case of a 12 h synthesis product. Heat flow values of the main hydration reaction and total heat release exceeded 3.1 mW g?1 and 140 J g?1 accordingly in case of the samples in which α-C2SH prevailed. However, increase in the thermal treatment temperature resulted in a decrease in the mixtures hydraulic activity. It was proved that killalaite formation in the product of the 12 h hydrothermal synthesis vividly decreases its hydraulic activity after the thermal treatment in the temperature range of 450–1000 °C. No increment in the heat flow values that could be attributed to the main hydration reaction (acceleration period) was witnessed in all the curves of the heat flow analysis in this case.  相似文献   

15.
To investigate the pharmacokinetics of ZS-1 following intravenous injection in rats, ZS-1 was administered at doses of 20, 30 and 45 mg kg?1, respectively. Blood samples were collected at 0.5, 3, 8, 12, 15, 20, 30, 40 and 45 min. ZS-1 in rat plasma was measured by LC. The limit of detection (LOD) was 0.02 μg mL?1. The relative standard deviation (RSD) of intra- and inter-day precisions were <10%, and the accuracy of intra- and inter-day were >94%. The mean extraction recovery of ZS-1 was 86.1%. After intravenous injection at doses of 20, 30 and 45 mg kg?1, the concentration–time curves of ZS-1 fitted well to one compartment model. Area under the concentration–time curves (AUC) increased with dose. Clearance rates (CL) and elimination half-lives (T 1/2) had no significant difference between different dose groups (P > 0.05). ZS-1 was stable in plasma after at 25 °C for 2, 4, 6 h, after three freeze–thaw cycles, after ?20 °C for a month, and after ?80 °C for 3 months. The accuracy of ZS-1 was between 96.8 and 106.9%. The results indicated there was no significant degradation. These data indicated that the method for analysis of ZS-1 was reliable and the pharmacokinetic data could guide dosing regimens to be tested in future clinical pharmacokinetic study.  相似文献   

16.
《Analytical letters》2012,45(11):1519-1525
The thermal decomposition behavior and kinetics of pyridoxine in nitrogen-only and air atmospheres were studied using thermogravimetry analysis (TGA). Kinetic interpretation of thermal analysis data for pyridoxine decomposition was carried out using Ozawa and ASTM E698 isoconversional methods. The activation energy of the decomposition process varied with the degree of decomposition and was different in the nitrogen and air atmospheres. At a 5% decomposition level, the activation energy and the pre-exponential factor were found to be 28.3 kcal mol?1 and 1.2 × 1014 min?1, respectively, in the nitrogen-only atmosphere. Thermal stability was determined by calculating the time for 5% of the pyridoxine vitamer to decompose at 25°C. The calculated shelf life for the pyridoxine vitamer obtained via TGA was surprisingly smaller in nitrogen (0.9 years) than in air (1.5 years). This is speculated to be the result of a more complex decomposition mechanism in air, involving thermo-oxidative decomposition in the presence of oxygen.  相似文献   

17.
The research shows theoretical calculations on the thermodynamics of digestion/gasification processes where glucose is used as a surrogate for biomass. The change in Enthalpy (?H) and Gibbs Free Energy (?G) is used to obtain the Attainable Region (AR) that shows the overall thermodynamic limits for digestion/gasification from 1 mol of glucose. Gibbs Free Energy and Enthalpy (GH) plots were calculated for the temperature range 25–1500 °C. The results show the effect of temperature on the AR for the processes when water is in both liquid and gas states using 25 °C, 1 bar as the reference state. The AR results show that the production of CO, H2, CH4 and CO2 are feasible at all temperatures studied. The minimum Gibbs Free Energy becomes more negative from ?418.68 kJ mol?1 at 25 °C to ?3024.34 kJ mol?1 at 1500 °C while the process shifts from exothermic (?141.90 kJ mol?1) to endothermic (1161.80 kJ mol?1) for the respective temperatures. Methane and carbon dioxide are favoured products (minimum Gibbs Free Energy) for temperatures up to about 600 °C, and this therefore includes Anaerobic Digestion. The process is exothermic below 500 °C, and thus Anaerobic Digestion requires heat removal. As the temperature continues to increase, hydrogen production becomes more favourable than methane production. The production of gas is endothermic above 500 °C, and it needs a supply of heat that could be done, either by combustion or by electricity (plasma gasification). The calculations show that glucose conversion at temperatures around 700 °C favours the production of carbon dioxide and hydrogen at minimum G. Generally, the results show that the gas from high-temperature gasification (>~800 °C) typically carries the energy mainly in syngas components CO and H2, whereas at low-temperature gasification (<500 °C) the energy is carried in CH4. The overall analysis for the temperature range (25–1500 °C) also suggests a close relationship between biogas production/digestion and gasification as biogas production can be referred to as a form of low-temperature gasification.  相似文献   

18.
LiFePO4/carbon complexes were prepared by electrospinning to improve rate performance at high C-rate and their electrochemical properties were investigated to be used as a cathode active material for lithium ion battery. The LiFePO4/carbon complexes were prepared by the electrospinning method. The prepared samples were characterized by SEM, EDS, XRD, TGA, electrometer, and electrochemical analysis. The LiFePO4/carbon complexes prepared have a continuous structure with carbon-coated LiFePO4 and the LiFePO4 in LiFePO4/carbon complex has improved thermal stability from carbon coating. The conductivity of LiFePO4/carbon complex heat-treated at 800 °C is measured as 2.23 × 10?2 S cm?1, which is about 106–107 times more than that of raw LiFePO4. The capacity ratio of coin cell manufactured from raw LiFePO4 is 40%, whereas the capacity ratio of coin cell manufactured from LiFePO4/carbon complex heat-treated at 800 °C is 61% (10 C/0.1 C). The improved rate performance of LiFePO4/carbon complex heat-treated at 800 °C is due to the carbon coating and good electrical connection.  相似文献   

19.
Four nanoporous carbons obtained from different polymers: polypyrrole, polyvinylidene fluoride, sulfonated styrene–divinylbenzene resin, and phenol–formaldehyde resin, were investigated as potential adsorbents for carbon dioxide. CO2 adsorption isotherms measured at eight temperatures between 0 and 60 °C were used to study adsorption properties of these polymer-derived carbons, especially CO2 uptakes at ambient pressure and different temperatures, working capacity, and isosteric heat of adsorption. The specific surface areas and the volumes of micropores and ultramicropores estimated for these materials by using the density functional theory-based software for pore size analysis ranged from 840 to 1990 m2 g?1, from 0.22 to 1.47 cm3 g?1, and from 0.18 to 0.64 cm3 g?1, respectively. The observed differences in the nanoporosity of these carbons had a pronounced effect on the CO2 adsorption properties. The highest CO2 uptakes, 6.92 mmol g?1 (0 °C, 1 atm) and 1.89 mmol g?1 (60 °C, 1 atm), were obtained for the polypyrrole-derived activated carbon prepared through a single carbonization-KOH activation step. The working capacity for this adsorbent was estimated to be 3.70 mmol g?1. Depending on the adsorbent, the CO2 isosteric heats of adsorption varied from 32.9 to 16.3 kJ mol?1 in 0–2.5 mmol g?1 range. Overall, the carbons studied showed well-developed microporosity and exceptional CO2 adsorption, which make them viable candidates for CO2 capture, and for other adsorption and environmental-related applications.  相似文献   

20.
Hydrogen is a green energy carrier. Chemical looping reforming of biomass and its derivatives is a promising way for hydrogen production. However, the removal of carbon dioxide is costly and inefficient with the traditional chemical absorption methods. The objective of this article is to find a new material with low energy consumption and high capacity for carbon dioxide storage. A metal organic framework (MOF) material (e.g., CuBTC) was prepared using the hydrothermal synthesis method. The synthesized material was characterized by X-ray diffraction, ?196 °C N2 adsorption/desorption isotherms, and thermogravimetry analysis to obtain its physical properties. Then BET, t-plot, and density functional theory (DFT) methods were used to acquire its specific surface area and pore textural properties. Its carbon dioxide adsorption capacity was evaluated using a micromeritics ASAP 2000 instrument. The results show that the decomposition temperature of the synthesized CuBTC material is 300 °C. Besides, high CO2 adsorption capacity (4 mmol g?1) and low N2 adsorption capacity were obtained at 0 °C and atmospheric pressure. These results indicate that the synthesized MOF material has a high efficiency for CO2 separation. From this study, it is expected that this MOF material could be used in adsorption and separation of carbon dioxide in chemical looping reforming process for hydrogen production in the near future.  相似文献   

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