The paper presents evaluation of energy distribution of n-octane and pore-size distribution functions on the alumina oxide surface (e.g. total heterogeneity) of on the basis one experimental
run. the Q-TG mass loss and derivative Q-DTG mass loss curves of n-octane thermodesorption from the alumina oxide sample were made using a hungarian derivatograph with an analyser equipped
with an automatic ultraslow procedure and a special crucible of maintaining the quasi-isothermal heating procedure to increase
the resolution of thermal analysis. a new theoretical and experimental procedure was developed for evaluation of distribution
functions of liquid preadsorbed on the mesoporous surface from special thermogravimetry. An example of the approach to quantitative
description of the energetic and structural heterogeneities of alumina oxide surface is given.
Energetic heterogeneity of adsorbents is conditioned by the differences in topology of adsorption centres, dispersion of pore sizes and other factors. This paper describes theoretical and experimental studies that demonstrate a method for estimation of the energetic heterogeneity of adsorbents by making use of the results from single thermogravimetry Q-TG and Q-DTG curves, recorded under quasi-equilibrium conditions, for preadsorbed liquid on a porous solid surface.
Authors:M. Błachnio, P. Staszczuk, and G. Grodzicka
Modified carbon multiwall nanotubes were prepared via the oxidation process by means of 65% nitric acid or ferric nitrate
dissolved with 65% nitric acid. Using special thermogravimetry and sorptometry methods physicochemical properties of pure
and modified nanotube surfaces were investigated. A numerical and analytical procedure for the evaluation of total heterogeneous
properties on the basis of liquid thermodesorption from the sample surfaces under the quasi-equilibrium conditions are presented.
The calculations of the fractal dimensions of carbon nanotubes using the sorptometry and thermogravimetry data is presented.
Authors:G. Chądzyński, V. Kutarov, and P. Staszczuk
In this paper the theoretical approach and applications of Cahn ultramicrobalance to kinetic study on the thermal decomposition
of the high-temperature Y1Ba2Cu3O7-x superconductor are presented. Thermogravimetric in situ measurements of oxygen loss from Y1Ba2Cu3O6 samples heated isothermally in a relatively high dynamic vacuum were performed with a Cahn RG electrobalance. Single-phase
orthorhombic samples of composition Y1Ba2Cu3O7-x (highest oxygen content) were synthesized from stoichiometric (1:2:3) mixtures of high-purity Y2O3, BaCO3 and CuO. The original 1:2:3 mixture was prepared by the two-stage procedure described earlier. The crystal structure of the
sample in the original orthorhombic phase was controlled by the X-ray powder method (CuKα radiation) using a Stadi P Stoe diffractometer with a position-sensitive detector. Activation energy is estimated from appropriate
The gravimetric measurement of the moisture content of solids is discussed in comparison to other usual methods. Results of
measurements of silica gel are reported. Furthermore, we inform on standardisation work.
Authors:P. Staszczuk, D. Sternik, and G. Chądzyński
Using thermo-analytical and sorptometric methods physicochemical properties and especially surface heterogeneity of HgBa2Ca2Cu3O8+, (Hg-1223) was investigated. The desorption energy distribution was derived from mass loss Q-TG and differential mass loss Q-DTG curves of thermodesorption in quasi-isothermal conditions of pre-adsorbed n-octane and water vapour. It is shown that the superconducting Hg-1223 phase is highly sensitive to water vapours. The mechanism of water adsorption depends largely on the activation time. By water vapour saturation in a period of 90 min, physisorption takes place. Prolonged periods result in a chemical decomposition. From nitrogen ad- and desorption isotherms the fractal dimension of superconductors were calculated. A new approach is proposed to calculate fractal dimension from Q-TG curves.
The Q-TG mass loss and first derivative Q-DTG mass loss accompanying benzene thermodesorption from silica gel samples under
quasi-isothermal conditions were studied with a Derivatograph Q-1500 D (MOM, Hungary). The isotherms of adsorption-desorption
of benzene vapour on different porous silica gels were measured gravimetrically by using a McBain balance. The benzene mass
loss in the adsorption region, obtained from the Q-TG curves, and the adsorption capacity, established gravimetrically, exhibited
a satisfactory correlation.
Authors:G. W. Chądzyński, P. Staszczuk, D. Sternik, and M. Błachnio
The porous structure of MgB2 has been investigated using atomic force microscopy (AFM) and sorption techniques. The fractal dimension and surface roughness parameters were evaluated from (AFM) and nitrogen adsorption–desorption isotherms measured at −196 °C for MgB2 sample. Adsorption capacity, specific surface area, and fractal dimensions were determined from adsorption–desorption isotherms. The sorption isotherms of MgB2 samples were S-shaped and belong to type II according to the IUPAC classification. The results of fractal dimensions of MgB2 surface determined on the basis sorptometry and AFM data are compared.
Authors:P. Staszczuk, M. Płanda-Czyż, M. Błachnio, and V. Kutarov
The new method of diffusion coefficient calculations
from thermogravimetry Q-TG data has been presented. Programmed thermodesorption
of polar and apolar liquids from aluminium oxide and montmorillonite-Na and
-La samples in quasi-isothermal conditions has been made. The result from
above method was compared with literature data and good correlation were obtained.
Authors:P. Staszczuk, M. Majdan, S. Pikus, D. Sternik, and M. Błachnio
Complex studies of physicochemical properties of pure and modified of aluminia oxides samples are presented. The presence
of Mn2+ and Ni2+ modifiers on the aluminium oxide surface causes increase in water adsorption capacity and decrease in benzene and n-octane adsorption. This is due to decrease of specific surface area, volume and radius of pores as a result of surface impregnation
and microcrystal formation during modification with manganese and nickel chlorides. Microcrystal formation on the surface
and porosity decrease as confirmed by AFM, EDX and powder diffraction studies using automated diffractometer by step scanning.
From the Q-TG and Q-DTG data, the energies of liquid desorption from the surface of the samples and the functions of desorption,
energy distribution were calculated. High degree of nonlinearity of the functions resulting from great heterogeneity of the
studied surface was found. Adsorption of cations creates more homogeneous surface in aluminium oxide, and it is responsible
for the change in adsorbate molecule interaction energy and changes mechanism of adsorption and desorption as well as thickness
and structure of the adsorbed film. From the experimental data some parameters characterizing adsorption properties and porosity
of the studied samples were determined using the complex measuring methods (thermal analysis, sorptometry, porosimetry, AFM