Preparation and Characterization of Activated Carbon from Microwave and Conventional Heated Almond Shells Using Phosphoric Acid Activation

Activated carbon production from almond shells using phosphoric acid activation agent was achieved by applying both conventional heating and microwave heating in succession. The morphology and surface properties of activated carbon were studied using thermogravimetric and differential gravimetric analysis, Fourier-transform infrared spectroscopy, scanning electron microscopy, and Brunauer–Emmett–Teller analysis. A surface area of 1128 m²/g was achieved by optimizing the microwave power (500?W), microwave application time (15?minutes), conventional heating time (45?minutes), conventional heating temperature (500?°C), and the phosphoric acid:sample ratio (0.7:1). An adsorption capacity of methylene blue of 148?mg/g and an iodine value of 791?mg/g was obtained for the prepared activated carbon.     

Non-adiabatic thin-film (chip) nanocalorimetry

To study the kinetics of processes on a millisecond time scale a thin-film nanocalorimeter based on a commercially available microchip (thermal conductivity vacuum gauge, TCG 3880, from Xensor Integration, NL) was constructed. The gauge consists of a submicron silicon nitride membrane with a film-thermopile and a film-heater, which are located at the 100 μm × 100 μm central part of the membrane. Controlled fast cooling is possible in addition to fast heating at essentially non-adiabatic conditions. To allow fast cooling the measurements are performed in an ambient gas atmosphere. It is proved that the maximum rate of the controlled cooling can be achieved with a gas cooling agent, rather than in a system with a solid heat-sink. The advantage of the gauge TCG 3880 is that its central heated region is small enough to be considered as a point source of the heat-flow into the gas, which essentially simplifies the calorimeter calibration. The maximum cooling rate is inversely proportional to the radius of the heated region. The gauge is placed in a thermostat with controlled gas pressure and temperature to be utilized as a device for fast scanning calorimetry of sub microgram samples with sensitivity 1 nJ/K and time resolution ca. 5 ms.     

Structural changes in β-lactoglobulin by conjugation with three different kinds of carboxymethyl cyclodextrins

β-Lactoglobulin-carboxymethyl cyclodextrin (β-LG-CMCyD) conjugates were prepared by using water soluble carbodiimide. Three kinds of CMCyDs differing in molecular mass were used to investigate the effects of different CMCyD contents, net charge and hydrophobicity on the structural changes in β-lactoglobulin. The effect of CMCyDs on the structure of β-lactoglobulin was utilized to investigate the contribution of hydrophobic interactions to the stability of the protein. Spectroscopic studies suggested that the conformation around had not changed in either conjugate but the α-helix content of β-LG-CMCyD conjugates had markedly increased as compared with that of β-lactoglobulin. The differential scanning calorimetry technique confirmed that the addition of one glucose unit in β-LG-CMCyD conjugates, enthalpy change of calorimetry decreased and the denaturation temperature of each conjugate was higher than that of native β-lactoglobulin. The heat contents agreed well with the conformational transition measured by molar ellipticity at 222 nm ([θ]₂₂₂) and Stoke's radius (R_S) values. Therefore, hydrophobic forces play an important role in stabilizing and shielding of the β-LG-CMCyD conjugates.     

Details of surface features in aromatic polyamide reverse osmosis membranes characterized by scanning electron and atomic force microscopy

In the present article, some new events on the surface morphology of the aromatic polyamide thin‐film‐composite (TFC) membranes were demonstrated in conjunction with their inherent chemical nature. In addition, the detailed, quantitative understanding of the microscopic surface features was shown to be essential in controlling the water permeability and eventually developing the high performance membranes. The surface roughness and the surface area were mainly affected by the existence or nonexistence of the crosslinking and/or the free amide groups not pertinent to the formation of the hydrogen bonding, which in turn contributed to the water permeability. © 1999 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 37: 1429–1440, 1999     

Domain structure and interphase dimensions in poly(urethaneurea) elastomers using DSC and SAXS

Small‐angle X‐ray scattering (SAXS) and differential scattering calorimetry (DSC) were used to demonstrate distinct differences in domain size, phase separation, and hydrogen bonding in a series of segmented urethaneurea elastomers prepared from isocyanate‐terminated prepolymers and aromatic diamine chain extenders. Two types of prepolymers were studied. The first contained a broadly polydisperse high molecular mass oligomer with relatively high levels of free isocyanate monomer. The second type of prepolymer contained low levels of high molecular mass oligomers with mass fractions greater than 90% of the two‐to‐one adduct of toluene diisocyanate (TDI) to polytetramethylene glycol (PTMEG). The mass fraction of the residual unreacted diisocyanate was less than 0.1% in the second type. Two chain extenders, 4,4′‐methylene bis‐(2‐chloroaniline)(Mboca) and 4,4′‐methylene bis‐(3‐chloro‐2,6‐diethylaniline) (MCDEA), were used to convert the prepolymers to poly(urethaneurea) elastomers. Materials prepared from the prepolymers with low oligomer polydispersity exhibited smaller hard segment domains with more ordered morphology, greater phase separation, and more hydrogen bonding than those prepared from prepolymers with high oligomer polydispersity. These tendencies were enhanced in those elastomers prepared by chain extension with MCDEA compared to those made with Mboca. © 1999 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 37: 2586–2600, 1999     

Effects of cooling rate on crystallinity of i-polypropylene and polyethylene terephthalate crystallized in nonisothermal conditions

Crystallization of polyethylene terephthalate and i-polypropylene in nonisothermal conditions is studied by means of differential scanning calorimetry. Measurements, carried out at several constant cooling rates, are interpreted in terms of a new theory^1,2 that takes into account effects related to a transient, nonsteady-state course of the process as well as athermal nucleation, which may occur under such circumstances. This article gives preliminary results based on analysis of final crystallinity reached at the end of cooling. Results indicate that the classical isokinetic approach is not adequate to describe crystallization kinetics at high cooling rates. A parameter quantizing the magnitude of deviations from isokinetic law is evaluated. © 1999 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 37: 2821–2827, 1999     

Isothermal crystallization of concentrated amorphous starch systems measured by modulated differential scanning calorimetry

The slow isothermal crystallization of concentrated amorphous starch systems is measured by Modulated Differential Scanning Calorimetry (MDSC). It can be followed continuously by the evolution (stepwise decrease) of the MDSC heat capacity signal (Cp), as confirmed with data from X-ray diffractometry, Dynamic Mechanical Analysis, Raman spectroscopy, and conventional Differential Scanning Calorimetry. Isothermal MDSC measurements enable a systematic study of the slow crystallization process of a concentrated starch system, such as a pregelatinized waxy corn starch with 24 wt % water and 76 wt % starch. After isothermal crystallization, a broad melting endotherm with a bimodal distribution is observed, starting about 10°C beyond the crystallization temperature. The bulk glass transition temperature (T_g) decreases about 15°C during crystallization. The isothermal crystallization rate goes through a maximum as a function of crystallization time. The maximum rate is characterized by the time at the local extreme in the derivative of Cp (t_max), or by the time to reach half the decrease in Cp (t_1/2). Both t_max and t_1/2 show a bell-shaped curve as a function of crystallization temperature. The temperature of maximum crystallization rate, for the system studied, lies as high as 75°C. This is approximately 65°C above the initial value of T_g. Normalized Cp curves indicate the temperature dependence of the starch crystallization mechanism. © 1999 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 37: 2881–2892, 1999     

扫描隧道显微镜在有机化学中的应用

扫描隧道显微镜的最大优点是可达到原子量级的分辨率。本文综述了STM对有机分子的结构、聚集形态及其反应过程的研究。     

Voltage-Height Spectroscopy in the <Emphasis Type="Italic">Ex Situ</Emphasis> Configuration of a Scanning Tunneling Microscope

Basic regularities of electrochemical processes in the gap of an ex situ scanning tunneling microscope in conditions of condensation of air moisture at the sample surface are considered on a qualitative level. A layer of condensed moisture is viewed as an electrolyte in a two-electrode cell. The depolarizers present in this layer may experience electrochemical conversions on the tip and in an area of the sample surface near the tip. As a result, the recorded “tunneling” current includes electrochemical constituents. Depending on the electrochemical processes in the gap, various dependences of the tip-sample distance on the current and applied voltage can be expected. For preliminary diagnostics of processes in the gap it is suggested to use voltage-height spectra, whose shape and characteristic heights are sensitive to the nature and location of redox active species. Experimental data for various films on conducting supports (quasi-two-dimensional adsorbed layers of hemin and peroxidase, electrodeposited nonstoichiometric tungsten oxides, doped tin dioxide, solid electrolyte with ionic conduction) are presented as an examples.__________Translated from Elektrokhimiya, Vol. 41, No. 5, 2005, pp. 583–595.Original Russian Text Copyright © 2005 by Yusipovich, Vassiliev.     

Phase Transitions,Thermal Desorption of Gases,and Electroconduction in BaCeO<Subscript>3</Subscript>, a Base for High-Temperature Protonic Conductors

Investigations of phase transitions in barium cerate are carried out by methods of dilatometry and differential scanning calorimetry. Thermal desorption of gases and temperature dependences of electroconduction in dry and humid air are studied. Barium cerate exhibits complex polymorphism, undergoing a number of structural conversions at 300– 1300 K. The peaks in the spectra of thermal desorption of CO₂ and H₂O correlate with variations in the crystal lattice. Structural changes in BaCeO₃ affect activation energies for the carrier transport and the shares of partial conductivities.__________Translated from Elektrokhimiya, Vol. 41, No. 5, 2005, pp. 620–626.Original Russian Text Copyright © 2005 by Kuz’min, Gorelov, Vaganov, Korzun, Kazantsev, Aksenova, Khromushin.