BET-surface area

ASAP2010M [Micromeritics, USA] is used—a fully automatic computer controlled setup for physical adsorption of gases [nitrogen, argon, carbon dioxide, etc] for pressures down to 1 mPa. The measurement is based on the adsorption and desorption of an inert gas on the whole surface of the sample at the same temperature. The adsorption and desorption isotherms are usually measured in the range of p/Po 0.001 to 0.999 in liquid nitrogen. The surface area 

Samples were measured by Krypton. Table 5.3 shows the results which is evident that the addition of even 0.5 g of PEDOT-PSS causes an increment of the surface area. However, no significant change was observed in the surface area with increasing content of PEDOT-PSS. 

---

Flere is the volume of gas required to saturate the monolayer, V the total volume of gas adsorbed, P the sample pressure, P the saturation vapour pressure and C a constant related to the enthalpy of adsorption. The resulting shape of the isothemi is shown plotted in figure Bl.26.6 for C = 500. A plot of P/V(P - Pq) against P/Pq should give a straight line having a slope (C - )/y C and an intercept The BET surface area is... 

Molecular area, a ,(Ar), of argon at 77 K on nonporous oxides (Argon BET plots constructed withp (liquid) BET surface areas calculated from nitrogen isotherms, with a (Na) = 16-2 A )... 

It would be difficult to over-estimate the extent to which the BET method has contributed to the development of those branches of physical chemistry such as heterogeneous catalysis, adsorption or particle size estimation, which involve finely divided or porous solids in all of these fields the BET surface area is a household phrase. But it is perhaps the very breadth of its scope which has led to a somewhat uncritical application of the method as a kind of infallible yardstick, and to a lack of appreciation of the nature of its basic assumptions or of the circumstances under which it may, or may not, be expected to yield a reliable result. This is particularly true of those solids which contain very fine pores and give rise to Langmuir-type isotherms, for the BET procedure may then give quite erroneous values for the surface area. If the pores are rather larger—tens to hundreds of Angstroms in width—the pore size distribution may be calculated from the adsorption isotherm of a vapour with the aid of the Kelvin equation, and within recent years a number of detailed procedures for carrying out the calculation have been put forward but all too often the limitations on the validity of the results, and the difficulty of interpretation in terms of the actual solid, tend to be insufficiently stressed or even entirely overlooked. And in the time-honoured method for the estimation of surface area from measurements of adsorption from solution, the complications introduced by... 

The small (10 -lm) coating particles are typically aluminum oxide [1344-28-1/, Al O. These particles can have BET surface areas of 100 to 300 m /g. The thermal and physical properties of alumina crystalline phases vary according to the starting phase (aluminum hydroxide or hydrate) and thermal treatment (see ALUMINUM COMPOUNDS, ALUMINUM OXIDE). 

The development of microporosity during steam activation was examined by Burchell et al [23] in their studies of CFCMS monoliths. A series of CFCMS cylinders, 2.5 cm in diameter and 7.5 cm in length, were machined from a 5- cm thick plate of CFCMS manufactured from P200 fibers. The axis of the cylinders was machined perpendicular to the molding direction ( to the fibers). The cylinders were activated to bum-offs ranging from 9 to 36 % and the BET surface area and micropore size and volume determined from the Nj adsorption isotherms measured at 77 K. Samples were taken from the top and bottom of each cylinder for pore sfructure characterization. 

The micropore volume varied from -0.15 to -0.35 cmVg. No clear trend was observed with respect to the spatial variation. Data for the BET surface area are shown in Fig. 14. The surface area varied from -300 to -900 mVg, again with no clear dependence upon spatial location withm the monolith. The surface area and pore volume varied by a factor -3 withm the monolith, which had a volume of -1900 cm. In contrast, the steam activated monolith exhibited similar imcropore structure variability, but in a sample with less than one fiftieth of the volume. Pore size, pore volume and surface area data are given in Table 2 for four large monoliths activated via Oj chemisorption. The data in Table 2 are mean values from samples cored from each end of the monolith. A comparison of the data m Table 1 and 2 indicates that at bum-offs -10% comparable pore volumes and surface areas are developed for both steam activation and Oj chemisorption activation, although the process time is substantially longer in the latter case. 

Monolith ID Bum-off %) BET surface area (mVg) DR micropore volume (cm /g) DA microporc diameter (nm)... 

Fig. 14. BET surface area as a function of position in a large CFCMS monolith with 10.4 4% bum-off [27].

Specimen No Burn-off (%) BET Surface Area (mVg) CO2 Capacity (Liters) ... 

Although a correlation between BET surface areas from 77 K nitrogen isotherms and methane uptake at 298 K and 3.5 MPa has been shown for many carbon adsorbents, [11, 20], deviations from this relationship have been observed [20]. However, as a primary screening process for possible carbonaceous adsorbents for natural gas, this remains a useful relationship. It should be noted that this correlation only seems to be applicable for active carbons. 

The single-point BET surface area measurement was used to check for open pores. The results for some soft and hard carbon samples heated at 700°C and 1000°C are presented in Table 2 for comparison. The hard carbon samples studied here have about ten times more open porosity than the soft carbons. 

The presence of closed pores was demonstrated by Kozawa [22] by measuring the BET surface area of EMD samples of various particle sizes. Kozawa s new method for the determination of the closed pore is based on the relationship of the BET surface area and the particle size, by extrapolating the surface area value to zero particle size (Fig. 17). Table 8 shows the percentage of closed pores of various EMD samples. 

Figure 17. Example of BET surface area vs average particle size (APS).

Abbreviations APS, average particle size of the original sample at 50wt.% S, BET surface area of original sample S(T), total BET surface area obtained by extrapolation. 

The physicochemical properties of carbon are highly dependent on its surface structure and chemical composition [66—68], The type and content of surface species, particle shape and size, pore-size distribution, BET surface area and pore-opening are of critical importance in the use of carbons as anode material. These properties have a major influence on (9IR, reversible capacity <2R, and the rate capability and safety of the battery. The surface chemical composition depends on the raw materials (carbon precursors), the production process, and the history of the carbon. Surface groups containing H, O, S, N, P, halogens, and other elements have been identified on carbon blacks [66, 67]. There is also ash on the surface of carbon and this typically contains Ca, Si, Fe, Al, and V. Ash and acidic oxides enhance the adsorption of the more polar compounds and electrolytes [66]. 

A platinum on silica gel catalyst was prepared by impregnation of silica gel (BDH, for chromatographic adsorption) by a solution containing 0.5% (wt.) of sodium hydroxide and 0.5% (wt.) of chloroplatinic acid (both of analytical grade). The dried catalyst contained 1% (wt.) of platinum and a corresponding amount of the alkaline component. The BET surface area of the catalyst was 40 m2/g, the mean pore radius 150 A. The catalyst was always reduced directly in the reactor in a stream of hydrogen at 200°C for 2 hr. 

Thorium oxide on activated carbon was prepared by absorption of thorium nitrate from its solution in anhydrous acetone on the activated carbon Supersorbon. The excess solution was decanted, the catalyst was dried at 80 °C, and the adsorbed thorium oxide was decomposed by excess 5% ammonium hydroxide solution. After repeated washing and decanta-nation with distilled water and acetone, the catalyst was dried at 180°C. It was then stabilized by heating to 360°C for 5 hr in a stream of nitrogen. The content of thorium oxide was 2.9% (wt.). The BET surface area was 870 m2/g. Prior to kinetic measurements, the catalyst was modified by passing over acetic acid vapors (100 g acid/1 g catalyst). 

A sulfonated ion exchanger catalyst (Research Institute of Synthetic Resins and Varnishes, Pardubice, Czechoslovakia) was a macroreticular styrene-divinylbenzene copolymer containing 25% divinylbenzene and 2.4 meq/g of —SO3H groups. It was dried prior to using at 90°C/14 Torr. The BET surface area, determined in a dry state, was 49 m2/g, and the mean pore size was around 100 A. 

Table 17.2 presents results of physical-chemical testing of the silica powders. The A1 sample has the lowest Cetultrimethyammonium bromid (CTAB) and Brunaues, Emmett, and Teller (BET) surface area, higher structure (DBF) and more silanol (-OH) groups on surface per unit area. 

The responses chosen all relate to important foam properties. We believed that yi, the emulsion droplet size, determines y2, the cell size in the resultant foam, and we wished to determine whether this is true over this range of formulations. The foam pore size ys should determine the wetting rate y7, so these responses could be correlated, and yg, the BET surface area, should be related to these as well. The density y and density uniformity ys are critical to target performance as described above, and ys, the compressive modulus, is an important measure of the mechanical properties of the foam. 

Catalysts were characterized using SEM (Hitachi S-4800, operated at 15 keV for secondary electron imaging and energy dispersive spectroscopy (EDS)), XRD (Bruker D4 Endeavor with Cu K radiation operated at 40 kV and 40 mA), TEM (Tecnai S-20, operated at 200 keV) and temperature-programmed reduction (TPR). Table 1 lists BET surface area for the selected catalysts. 

---