SURFACE CHEMISTRY AND CATALYTIC PROPERTIES OF BORON PHOSPHATE: 1. SURFACE AREA AND ACIDITY

1965 ◽  
Vol 43 (6) ◽  
pp. 1680-1688 ◽  
Author(s):  
J. B. Moffat ◽  
H. L. Goltz

Surface properties of the dehydration catalyst, boron phosphate (BP), prepared by the reaction of triethyl borate and phosphoric acid, were investigated by the use of a microbalance system. During evacuation at elevated temperatures, weight changes of the BP were obtained. Nitrogen adsorption isotherms were measured after each treatment. Surface areas appear to increase, and reach a maximum in the range 200–300 °C. Weight changes are initially large but begin to level off as the temperature is increased. Ammonia isotherms were obtained at 25.00 °C on aliquots of the same BP sample after various pretreatments. Amounts of ammonia remaining adsorbed after evacuation overnight were taken as the quantity chemisorbed. An approximate value of 8.9 kcal/mole of ammonia was obtained for the heat of chemisorption of ammonia by measuring the pressure and weight change as the amount of chemisorbed ammonia is decreased on heating the BP to various temperatures in a closed system. Results are interpreted in terms of change of number of active sites with surface area and the deactivation of sites on loss of water.

1962 ◽  
Vol 40 (2) ◽  
pp. 184-188 ◽  
Author(s):  
P. L. Walker Jr. ◽  
W. V. Kotlensky

It is shown that the open pore volume within carbon blacks can be calculated from nitrogen adsorption isotherms (77°K) on the blacks. From this volume and a helium density, the apparent density of a black can be calculated. Other properties of the blacks which then can be calculated are free surface area, internal surface area, surface roughness factor, and the average pore diameter of the internal surface. These data are presented for five selected carbon blacks.


Coatings ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1115
Author(s):  
Tatiana Skripkina ◽  
Ekaterina Podgorbunskikh ◽  
Aleksey Bychkov ◽  
Oleg Lomovsky

The surface area is an important parameter in setting any biorefining technology. The aim of this study was to investigate the applicability of sorption of methylene blue to characterize the surface of the main biomass carbohydrates: α-cellulose, sigmacell cellulose, natural gum, β-glucan, and starch. The morphology of particles of the model objects was studied by scanning electron microscopy. Nitrogen adsorption isotherms demonstrate that the selected carbohydrates are macroporous adsorbents. The monolayer capacities, the energy constants of the Brunauer–Emmett–Teller (BET) equation, and specific surface areas were calculated using the BET theory, the comparative method proposed by Gregg and Sing, and the Harkins–Jura method. The method of methylene blue sorption onto biomass carbohydrates was adapted and mastered. It was demonstrated that sorption of methylene blue proceeds successfully in ethanol, thus facilitating surface characterization for carbohydrates that are either soluble in water or regain water. It was found that the methylene blue sorption values correlate with specific surface area determined by nitrogen adsorption/desorption and calculated from the granulometric data. As a result of electrostatic attraction, the presence of ion-exchanged groups on the analyte surface has a stronger effect on binding of methylene blue than the surface area does. Sorption of methylene blue can be used in addition to gas adsorption/desorption to assess the accessibility of carbohydrate surface for binding large molecules.


1996 ◽  
Vol 13 (3) ◽  
pp. 153-163 ◽  
Author(s):  
G.A. El-Shobaky ◽  
A.S. Ahmad ◽  
A.M. Ghozza ◽  
S.M. El-Khouly

Two specimens of Fe2O3/Al2O3 solids were prepared by impregnating a known mass of finely-powdered Al(OH)3 with calculated amounts of ferric nitrate solutions followed by drying at 120°C and calcination in air at 400°C for 4 h. The mixed solids thus prepared had the nominal molar compositions 0.06Fe2O3/Al2O3 and 0.125Fe2O3/Al2O3 (FeAl-I and FeAl-II). The surface and catalytic properties of various irradiated solids (15–200 Mrad) were studied using nitrogen adsorption at −196°C and catalysis of CO oxidation by O2 at 150–280°C using a static method. The results obtained revealed that γ-irradiation at doses between 15 and 80 Mrad resulted in a progressive decrease (7–22%) in the surface area of the treated solids. Treatment with doses above this limit exerted an opposite effect. γ-Irradiation also resulted in a widening of the pores of the irradiated adsorbents. The catalytic activity of the FeAl-I solid was influenced slightly by γ-rays while the FeAl-II catalyst was significantly modified by this treatment. The reaction rate constant per unit surface area of the catalytic reaction conducted at 280°C over the FeAl-II solid decreased (65%) by exposure to doses up to 120 Mrad, then increased on increasing the dose above this limit. This did not modify the mechanism of the catalytic reaction, but changed the number of catalytically-active sites taking part in chemisorption and catalysis of the CO oxidation reaction without affecting their energetic nature.


1948 ◽  
Vol 26a (2) ◽  
pp. 29-38 ◽  
Author(s):  
J. C. Arnell ◽  
G. O. Henneberry

The modified Kozeny equation has been found to be satisfactory for the measurement of the specific surfaces of carbon blacks having average particle diameters ranging from 0.01 to 0.1 μ to within ±10%. Comparative data were obtained from electron microscope counting and from low temperature nitrogen adsorption isotherms. The three methods examined gave results that were in satisfactory agreement, except when the carbon black was porous, and then the adsorption value was extremely large.


1997 ◽  
Vol 15 (6) ◽  
pp. 465-476 ◽  
Author(s):  
G.A. El-Shobaky ◽  
A.M. Ghozza ◽  
G.M. Mohamed

Two samples of Cr2O3/Al2O3 were prepared by mixing a known mass of finely powdered Al(OH)3 with a calculated amount of CrO3 solid followed by drying at 120°C and calcination at 400°C. The amounts of chromium oxide employed were 5.66 and 20 mol% Cr2O3, respectively. The calcined solid specimens were then treated with different doses of γ-rays (20–160 Mrad). The surface and catalytic properties of the different irradiated solids were investigated using nitrogen adsorption at −196°C and the catalysis of CO oxidation by O2 at 300–400°C. The results revealed that γ-rays brought about a slight decrease in the BET surface area, SBET (15%), and in the total pore volume, Vp (20%), of the adsorbent containing 5.66 mol% Cr2O3. The same treatment increased the total pore volume, Vp (36%), and the mean pore radius, r̄ (43%), of the other adsorbent sample without changing its BET surface area. The catalytic activities of both catalyst samples were found to increase as a function of dose, reaching a maximum value at 80–160 Mrad and 40 Mrad for the solids containing 5.66 and 20 mol% Cr2O3, respectively. The maximum increase in the catalytic activity measured at 300°C was 59% and 100% for the first and second catalyst samples, respectively. The induced effect of γ-irradiation on the catalytic activity was an increase in the concentration of catalytically active sites taking part in chemisorption and in the catalysis of CO oxidation by O2 without changing their energetic nature. This was achieved by a progressive removal of surface hydroxy groups during the irradiation process.


1967 ◽  
Vol 40 (5) ◽  
pp. 1305-1310 ◽  
Author(s):  
G. Kraus ◽  
K. W. Rollmann

Abstract The Harkins and Jura (HJ) absolute method of surface area determination (Harkins and Jura, J. Am. Chem. Soc. 66, 919, 1944) has been applied to a large number of carbon blacks. Surface area is calculated from the heat of immersion of the solid powder covered by a preadsorbed multilayer of the immersion liquid. For non-porous carbon blacks good agreement with nitrogen adsorption surface areas is obtained, but with porous blacks the HJ method gives smaller values since micropores are filled and bridged over by the pre-adsorbed film. Thus the HJ areas are more nearly representative of particle size and may be used to calibrate indirect methods of particle size determination. An example of this is shown using light reflectance values on dry carbon black and possible complications due to particle size distribution in the use of the reflectance test are discussed.


1964 ◽  
Vol 37 (3) ◽  
pp. 630-634 ◽  
Author(s):  
Andries Voet

Abstract Surface areas of completely nonporous carbon blacks of widely varying particle chain formation (structure) have been determined by means of the nitrogen adsorption method as well as by electron micrography. Accurately determined densities in helium were used as the basis of calculations in the latter approach. It was found that the ratio of areas measured by nitrogen adsorption to electron micrographically determined surface areas is greatly dependent upon chain formation. A higher structural build-up leads to a lower ratio, explained by the observation that fusion areas in carbon chains are necessarily, though erroneously, counted as surfaces in electron micrography. The ratio differs markedly from unity, however, in low structure blacks, where fusion areas are negligible. By accepting the area of a nitrogen molecule adsorbed in a monolayer as being equal to that in the solid state, 13.8 A2, the ratio becomes unity for nonporous low structure blacks. It appears likely, therefore, that all surface area data based on the area of a nitrogen molecule in the liquid state of 16.2 A2 are too high by about 15 per cent of presently accepted values.


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