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:I. Berezovska, V. Yanishpolskii, V. Tertykh, M. Burmistr, and K. Sukhyy
Effect of the presence
of I-4 Me-Ph ionene in the supramolecular template (cetyltrimethylammonium
bromide) on formation of porous structure of silicas has been studied. As-synthesized
nanocomposites were characterized by using thermal analysis. Nitrogen adsorption–desorption
measurements, X-ray diffraction and scanning electronic microscopy were applied
to determine adsorption-structural characteristics and morphology of particles
of the mesoporous templated silicas prepared in basic media.
Authors:K. Hashimoto, T. Sekine, T. Omori, and K. Yoshihara
Tris (benzoylacetonato) technetium(III) and tris (2-thenoyltrifluoroacetonato) technetium(III) were synthesized by the direct reduction of pertechnetate with dithionite in the presence of excess ligands. The geometrical isomers of the benzoylacetonate were further separated by means of a silica gel column chromatography. In the silica gel system, the adsorption distribution coefficient of the tris (-diketonato) technetium(III) decreases in the order of Tc(acac)3>fac-Tc(bzac)3>mer-Tc(bzac3)>Tc(tta)3.
Sorption of nickel, Ni2+, on SiO2 . xH2O (silica gel) has been studied as a function of time conditions: amount of silica gel: 0.10-1.00 g, nickel concentration:
5.00 . 10-5-1.20 . 10-3M, ionic strength: 0.20-1.40M NaClO4, pH 6.50 to 8.50, and temperature 273-318 K. From the kinetic data, the diffusion coefficient of Ni2+ ion was calculated to be 1.28(±0.07) . 10-11 m2 . s-1 under particle diffusion-controlled conditions. The sorption rate was determined as 3.79(±0.35) . 10-3 s-1 at 298 K, pH 8.40 in 0.20M (NaClO4). The sorption data were fitted to Freundlich, Langmuir and Dubinin-Radushkevich (D-R) isotherms. Nickel sorption on 0.20
g silica gel decreased with ionic strength from 77.70±0.70% (0.20M NaClO4) to 16.12±0.37% (1.40M NaClO4) at intial pH of 8.50±0.05. A gradual decrease in pH with increasing ionic strength suggests an ion exchange mechanism and
the sorption of Ni2+ on silica gel increasing with temperature indicates an endothermic enthalpy. The effect of different ligands such as fluoride,
carbonate, phosphate and oxalate on Ni2+ sorption on silica gel was studied.
Authors:K. Lee, Y. Yoon, S. Jeong, Y. Chae, and K. Ko
The effects of acids on the removal of impurity from 2N grade silica have been studied using five leaching acids: 0.2 M-oxalic
acid (pH 1.5 and 2.5), c-aqua regia, 2.5%—HCl/HF, and 1%—HNO3/HF. The presence of 39 impurities in the 2N grade silica and the reference material (RM, 5N grade silica) were investigated
by neutron activation analysis (NAA), X-ray fluorescence (XRF), and inductively coupled plasma mass spectrometry (ICP-MS)
methods. Major impurities of the 2N silica were Al, K, Fe, Na, Ti, Ca, Mg and P. The fractions of the eight major impurities
were 99.2% and 90.9% of total impurity in the 2N and RM silica, respectively. Among the leaching acids, almost all of the
major impurities were removed effectively by the 2.5% HCl/HF leaching acid. All the major impurities, except for phosphorous,
as well as 21 minor and trace impurities could be determined by the NAA.
Authors:Przemysław Rybiński, Grażyna Janowska, and Ludomir Ślusarski
The article presents the results of testing thermal properties and combustibility of butadieneacrylonitrile
rubber with 18% contents of bounded acrylonitrile, NBR 18. Two types of silica, Zeosil 175C and Ultrasil VN-3, with different
specific surfaces were used as filler.
Zeosil 175C and Ultrasil VN-3 were modified via cryogenic dezaggregation method. The activity of
unmodified and cryogenic modified silica toward butadiene-acrylonitrile rubber were investigated.
The sulphur and peroxide vulcanizates contained 20, 30, 40, and 50 phr. of the filler were studied.
The article discusses also the test results of thermal stability and flammability of NBR 18 containing
silica prepared "in situ" from alkoxysilane precursor.
The test results were obtained with the use of derivatograph, measurements of flammability by the
method of oxygen index, and in air.
The effect of the silica modification on the SEM and AFM was also examined.
The method of cryogenic modification enables to achieve increase of mineral fillers activity towards
elastomer and reduction in the flammability of NBR 18 vulcanizates.
It has been found that the modification of the vulcanizates of NBR 18 with tetraethoxysilane that
makes it possible to form silica "in situ" reduces the flammability of cross-linked rubbers.
Authors:Helena Majstorović, Danijela Ratkov-Žebeljan, Živoslav Tešić, and Dušanka Milojković-Opsenica
The chromatographic behavior of some phenolic compounds has been studied with the objective of understanding the role of cyano groups in the processes of chromatographic separation on thin layers of CN-silica gel. For this purpose separations were performed on thin layers of CN-silica gel, unmodified silica gel, and polyacrylonitrile adsorbent (PANS) using fourteen mobile phases, nine of which resulted in normal-phase systems. On the basis of the results obtained the effect of compound structure (i.e. properties of
substituents of the compounds separated) on their retention is discussed. The dependence of the order of retention of the phenols on the properties of the adsorbent was also considered. Plots of retention data (
) determined by use of different chromatographic systems were used to characterize the systems used. The results enabled hypotheses to be formulated about possible mechanisms involved in the separations of the phenols on these adsorbents.
Authors:T. C. K. Yang, W. H. Chang, and D. S. Viswanath
Thermal degradation of poly(vinyl butyral) (PVB) and its mixtures with alumina, mullite and silica was investigated by non-isothermal thermogravimetry in the temperature range of 323 to 1273 K. The analysis of the data was carried out using a three-dimensional diffusion model. Results showed that the kinetic parameters (activation energy and pre-exponential factor) of the PVB degradation are different for polymer alone, and ceramic/polymer composites. The overall weighted mean apparent activation energy showed an increasing reactivity in the order of PVB<alumina+PVB<mullite+PVB<silica+PVB. This shows that the acidic and basic surface characteristics of the ceramics promote the thermal degradation of PVB and, the more acidic silica affects the degradation more than mullite and alumina. The effect of pellet compression pressure in the range of 4000 to 8000 psig is also investigated.
Authors:C. L. Beaudry, L. C. Klein, and R. A. McCauley
Thermogravimetric analyses of sol-gel derived silica and silica-poly(vinyl acetate) (PVAc) materials show that the loss in weight between 35 and 900°C can be attributed to three distinct reactions. Samples were prepared by dissolving the reactants tetraethyl orthosilicate (TEOS), poly(vinyl acetate) (PVAc), and water in mixtures of ethanol and formamide. The lowest temperature weight loss is due to the decomposition/removal of the solvents, while the intermediate weight loss corresponds to decomposition of the PVAc. The highest temperature weight loss is related to the dehydroxylation of the silica surface. The relative amounts of ethanol and formamide have a considerable effect on processing time, drying behavior, and the resulting thermal behavior of the gels.
Authors:Masanobu Nogami, Yuichi Sugiyama, and Yasuhisa Ikeda
As a part of the development of resins with selectivity to U(VI) in HNO3 media, adsorptivities of U(IV) onto some silica-supported monoamide resins in HNO3 solutions have been examined. It was found that resins consisting of N,N-dimethylacrylamide (Silica-DMAA resins) showed higher selectivity to U(VI) than U(IV) in the concentration range of HNO3 up to 9 mol/dm3. On the other hand, a resin consisting of N-methyl-N-vinylbenzylacetamide (Silica-MVBAA) was found to show a higher selectivity to U(IV) under the same concentration range of
HNO3. Differences in the selectivity among the resins were explained by the difference in the conformation between the functional
carbonyl groups of the monoamide resins and U species.