Isothermal nitrogen adsorption

AlTUD-1, a new mesoporous, Bronsted acidic aluminosilicate with ideal characteristics for catalyst immobilization was used for the noncovalent anchoring of hydride tungsten complex [WH2(ti -OOCCH3) (Ph2PCH2CH2PPh2)2][BPh4]. The immobilization was carried out by an adsorption process in liquid phase. The new materials were characterized by several techniques spectroscopic methods (ICP-AES, FT-IR and UVA is), X-ray techniques (XPS and XRD), isothermal nitrogen adsorption and elemental analysis. 

Fig. XVII-27. Nitrogen adsorption at 77 K for a series of M41S materials. Average pore diameters squares, 25 A triangles, 40 A circles, 45 A. Adsorption solid symbols desorption open symbols. The isotherms are normalized to the volume adsorbed at Pj = 0.9. (From Ref. 187. Reprinted with kind permission from Elsevier Science-NL, Sara Burgerhartstraat 25, 1055 KV Amsterdam, The Netherlands.)...

Fig. XVII-31. (a) Nitrogen adsorption isotherms expressed as /-plots for various samples of a-FeOOH dispersed on carbon fibers, (h) Micropore size distributions as obtained by the MP method. [Reprinted with permission from K. Kaneko, Langmuir, 3, 357 (1987) (Ref. 231.) Copyright 1987, American Chemical Society.]...

The nitrogen adsorption isotherm is determined for a finely divided, nonporous solid. It is found that at = 0.5, P/P is 0.05 at 77 K, gnd P/F is 0.2 at 90 K. Calculate the isosteric heat of adsorption, and AS and AC for adsorption at 77 K. Write the statement of the process to which your calculated quantities correspond. Explain whether the state of the adsorbed N2 appears to be more nearly gaslike or liquidlike. The normal boiling point of N2 is 77 K, and its heat of vaporization is 1.35 kcal/mol. 

Fig. 2.29 Comparison of nitrogen adsorption at 78 K on a carbon black (Sterling FT) before and after graphitization (a) The amount adsorbed on the ungraphitized sample plotted against the amount x, adsorbed on the graphitized sample, at the same pressure, b) The corresponding isotherms O, adsorption, , desorption on the ungraphitized sample (4 runs) A. adsorption A desorption, on the graphitized sample (4 runs).

When the values of the BET monolayer capacity calculated from Type III isotherms are compared with independent estimates (e.g. from nitrogen adsorption) considerable discrepancies are frequently found. A number of typical examples are collected in Table 5.1. Comparison of the value of the monolayer capacity predicted by the BET equation with the corresponding value determined independently (columns (iv) and (v)) show that occasionally, as in line 6, the two agree reasonably well, but that in the majority... 

Fig. 6. Family of adsorption isotherms for adsorption of nitrogen on 2eolite X at temperatures of -30 to 196°C (1).

Surface areas are deterrnined routinely and exactiy from measurements of the amount of physically adsorbed, physisorbed, nitrogen. Physical adsorption is a process akin to condensation the adsorbed molecules interact weakly with the surface and multilayers form. The standard interpretation of nitrogen adsorption data is based on the BET model (45), which accounts for multilayer adsorption. From a measured adsorption isotherm and the known area of an adsorbed N2 molecule, taken to be 0.162 nm, the surface area of the soHd is calculated (see Adsorption). 

Nitrogen adsorption experiments showed a typical t)q5e I isotherm for activated carbon catalysts. For iron impregnated catalysts the specific surface area decreased fix>m 1088 m /g (0.5 wt% Fe ) to 1020 m /g (5.0 wt% Fe). No agglomerization of metal tin or tin oxide was observed from the SEM image of 5Fe-0.5Sn/AC catalyst (Fig. 1). In Fig. 2 iron oxides on the catalyst surface can be seen from the X-Ray diffractions. The peaks of tin or tin oxide cannot be investigated because the quantity of loaded tin is very small and the dispersion of tin particle is high on the support surface. 

Here, N is the amount of adsorption and X is the relative pressure (P/Po). Ds can be calculated through the slope of a log-log plot of Eq. (3) by a single nitrogen adsorption isotherm data. 

The samples were characterized by chemical analysis induced coupled plasma and atomic absorption techniques apparatus), nitrogen adsorption isotherms (at 77 K), XRD patterns ( Siemens diffractometer and (3uKa radiation), SEM observations (Hitachi S800 apparatus of the University C. Bernard, Lyon I) and TGA-DTA (Setaram 92-12 apparatus). The IR spectra were recorded with a Bruker IPS 48 FTIR spectrometer. 

Figure 3.42. Nitrogen adsorption/desorption isotherm for a commercial y-alumina. The arrows denote the mode of changing the pressure, viz. increasing or decreasing pressure.

Catalysts Characterization Catalysts were characterized by nitrogen adsorption-desorption isotherms, XRD, XPS, TEM, and FT-IR. The concentration and the strength of the acid sites were determined using a combination of NHs-chemisorption and FTIR. Detailed procedures are given elsewhere [18, 19]. 

Nitrogen adsorption isotherms were measured with a sorbtometer Micromeretics Asap 2010 after water desorption at 130°C. The distribution of pore radius was obtained from the adsorption isotherms by the density functional theory. Electron microscopy study was carried out with a scanning electron microscope (SEM) HitachiS800, to image the texture of the fibers and with a transmission electron microscope (TEM) JEOL 2010 to detect and measure metal particle size. The distribution of particles inside the carbon fibers was determined from TEM views taken through ultramicrotome sections across the carbon fiber. 

The support and the catalysts were characterised by means of nitrogen adsorption, XPS, TPD and SEM. The nitrogen adsorption isotherms were determined at 77 K in a Coulter Omnisorp 1000 CX equipment, and were analysed by the BET equation (SBet), and by the t-plot for mesopore surface area (Smeso) and micropore and mesopore volume (Vmicr0, Vmeso), using the standard isotherm for carbon materials. The catalyst samples were previously outgassed at 120 °C. 

The analytical data of the catalysts used are given in Table II. The number of B5 sites was determined from infrared measurements and nitrogen adsorption isotherms in the way outlined by van Hardeveld and Montfoort 10). The values found are higher than those mentioned in an earlier paper 24), owing partly to an improvement of the method for determining the extinction coefficient per molecule of nitrogen adsorbed,... 

Nitrogen adsorption/desorption isotherms of all the activated carbons are of Type I, i.e. characteristic of basically microporous solids. There is a lack of adsorption/desorption hysteresis. More careful analysis permits to notice significant differences in the porous texture parameters depending on precursor origin. 

Fig. 2.28 Nitrogen adsorption (open symbol)/desorption (closed symbol) isotherms (A) as-synthesized, (B) hydrolyzed materials.

Nitrogen adsorption/desorption isotherms on Zeolite and V-Mo-zeolite are very similar and close to a type I characteristic of microporous materials, although the V-Mo-catalysts show small hysterisis loop at higher partial pressures, which reveals some intergranular mesoporosity. Table 1 shows that BET surface area, microporous and porous volumes, decrease after the introduction of Molybdenum and vanadium in zeolite indicating a textural alteration probably because of pore blocking by vanadium or molybdenum species either dispersed in the channels or deposited at the outer surface of the zeolite. The effect is far less important for the catalysts issued from ZSM-5. 

The nitrogen adsorption isotherms for the onion-like Fe-modified MLV-0.75 materials are of type IV, although their hysteresis loops are of complex types, HI, H2, and H3. The H2-type hysteresis loop indicates the presence of bottle-shaped pores. The pore sizes obtained with the BJH method can be assigned to entry windows of mesopores. For pure MLV-0.75 and Fe-modified MLV-0.75 (x = 1.25), the pore size distributions exhibit two peaks (Fig. Id). The first peak appears at 9.0 and ca. 6 nm for MLV-0.75 and Fe-MLV-0.75, respectively. The shift of the broad peak maximum of the distribution curve... 

Figure 1. Nitrogen adsorption-desorption isotherms at 77 K on (void squares) SBA-15 synthesized at 403 K, (void lozenges) SBA-15 synthesized at 343 K, (filled triangles) MCM-41.

The X-ray diffraction pattern of the spheres before the immersion in SBF shows the typical diffraction peak ascribable to the (100) reflection of the ordered mesophase with a dioo of 3.45 nm. Nitrogen adsorption-desorption isotherms are of type IV and pore size from DFT model results 2.4 nm (data not reported). 

Nitrogen adsorption-desorption isotherms of MCM-41-IBU after 2 hours of immersion in SBF show the characteristic mesopore filling at p/p° below 0.25 (type IV isotherm). 

The structure of the catalysts was characterized by X-ray diffraction, IR-spectroscopy and transmission electron microscopy, their thermal stability was followed by thermal analytical method. The specific surface area and pore size distribution of the samples were determined by nitrogen adsorption isotherms. 

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