999 resultados para Composição físico-química


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To overcome the challenge of meeting growing energy demand in a sustainable way, biodiesel has shown very promising as alternative energy can replace fossil fuels, even partially. Industrially, the biodiesel is produced by homogeneous transesterification reaction of vegetable oils in the presence of basic species used as catalysts. However, this process is the need for purification of the esters obtained and the removal of glycerin formed after the reaction. This context, the alternative catalysts have that can improve the process of biodiesel production, aiming to reduce costs and facilitate its production. In this study, the AlSBA-15 support with Si / Al ratio = 50 was synthesized, as like as the heterogeneous catalysts of zinc oxide and magnesium supported on mesoporous AlSBA-15 silica, in the concentrations of 5, 10, 15 and 30 %, relative to the support. The textural properties and structural characterization of catalysts and supports were determined by techniques: X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) coupled to the chemical analyzer, adsorption / desorption of N2, thermal analysis (TG / DTG), absorption spectroscopy in the infrared (FTIR) and X-ray photoelectron spectroscopy (XPS). Characterization results indicated that the support AlSBA-15 retained the hexagonal ordered after the incorporation of zinc oxide and magnesium oxide in the holder. For heterogeneous catalysts, ZnO-AlSBA-15, that was observed the presence of zinc oxide nanoparticles dispersed in the surface and interior channels of the mesoporous and microporous support. The catalytic activity was evaluated by the transesterification reaction of sunflower oil via methylic route, and some reaction parameters were optimized with the most active catalyst in biodiesel production by sunflower oil. For the series of heterogeneous catalysts, the sample with 30 % ZnO supported on AlSBA-15 showed a better conversion of triglyceride to methyl esters, about 95.41 % of reaction conditions: temperature 175 °C, with molar ratio of 42:1, stirring at 200 rpm and under a pressure of 14 bar for 6 h. The catalyst MgO-AlSBA-15 showed no catalytic activity in the studied reactions

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In this study, we worked with the validation of a methodology for analysis of bioactive amines in shrimp, considering it to be one of the main products of the northriograndense trade balance, maintaining the state of Rio Grande do Norte topped the list of Brazilian exports of this product the last decade. The sector of the Brazilian shrimp works exclusively with gray shrimp Litopenaeus Vannamei since the late 1990s. This study used liquid chromatography with conductimetric detector, using as the mobile phase methylsulfonic 3 mM acid (MSA) with gradient and phase C18 column with reverse the development of methodology for the analysis of bioactive amines in shrimp. In the sample preparation was used as 5% trichloroacetic acid (TCA) extraction solution. Validation analysis of biotativas amines (putrescine - PUT, histamine - HIST, agmatine - AGM, spermidine - EPD and spermine - EPN) in shrimp, the linear working range was 0.1 to 2.0 mg L-1 to was sensitive, homoscedastic, in effect, selective, accurate and precise array. Thus, considered feasible for these determinations bioactive amines in this array. Determined the concentration of these amines in fresh shrimps (AGM = 0.61 ± 0.05 mg kg- 1 EPD = 2.57 ± 0.14 mg kg-1 and EPN = 1.79 ± 0.11 mg kg-1), and freezing weather predetermined in cooked shrimp (AGM = 6.28 ± 0.18 mg kg-1, EPD = 12.72 ± 0.02 mg kg- 1 and EPN = 22.30 ± 0.60 mg kg-1), the shrimp with twenty-four hour stay at room temperature (PUT = 879.52 ± 28.12 mg kg-1, AGM = 848.13 ± 19.40 mg kg-1, ESPD = 13.59 ± 0.97 mg kg-1 and ESPN = 18.47 + 1.57 mg kg-1). In shrimp subjected to freezing for a week, two weeks, three weeks and four weeks, the results showed that there is an increase in the content of agmatine (7.31 ± 0.21 mg kg-1) while in spermine ( 1.22 ± 0.14 mg kg-1) and spermidine (below limit of quantification) there was a decrease in the freeze time, while there is a decrease in the level of spermidine not reaching detectad. The putrescine was only found in shrimp that remained for 24 hours at room temperature and histamine was not found in any of the samples

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The Layered Double Hydroxides has become extremely promising materials due to its range of applications, easily obtained in the laboratory and reusability after calcination, so the knowledge regarding their properties is of utmost importance. In this study were synthesized layered double hydroxides of two systems, Mg-Al and Zn-Al, and such materials were analyzed with X-ray diffraction and, from these data, we determined the volume density, planar atomic density, size crystallite, lattice parameters, interplanar spacing and interlayer space available. Such materials were also subjected to thermogravimetric analysis reasons for heating 5, 10, 20 and 25 ° C / min to determine kinetic parameters for the formation of metaphases HTD and HTB based on theoretical models Ozawa, Flynn-Wall Starink and Model Free Kinetics. In addition, the layered double hydroxides synthesized in this working ratios were calcined heating 2.5 ° C / min and 20 ° C / min, and tested for adsorption of nitrate anion in aqueous solution batch system at time intervals 5 min, 15 min, 30 min, 1h, 2h and 4h. Such calcined materials were also subjected to exposure to the atmosphere and at intervals of 1 week, 2 weeks and 1 month were analyzed by infrared spectroscopy to study the kinetics of regeneration determining structural called "memory effect"

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The present work has as main objective to contribute to the coordination chemistry of the ligand kojic acid, with the synthesis and characterization of the homoleptic compounds [Al(kj)3], [Fe(kj)3], [Fe(kj)2], [Cu(kj)2] e [Ru(kj)3], and the new heteroleptic complexes, trans- K2[Fe(kj)2(CN)2] and trans-Na2[Ru(kj)2(CN)2]. The obtained compounds were characterized by vibrational spectroscopy in the infrared region (IV) and Electronic spectroscopy in the ultraviolet and visible region (Uv-Vis). The infrared results indicated the coordination of the bidentate ligand kojic acid, due to reductions in the values of the stretching frequencies of the carbonyl and double bonds, compared to the free ligand for all complexes obtained. The presence of new vibrational modes indicated the change of symmetry of the molecules in the new compounds synthesized. Additionally, the presence of vibrational modes assigned to metal-oxygen also contributed to confirm the ligand coordinating to the metal ions. Through this technique, was also possible to perform correlations of the numbers of vibrational modes, in the region 1400-900 cm-1 and the compounds geometry. The heteroleptic compounds exhibited υC≡N in 2065 and 2053 cm-1, respectively, for the trans-K2[Fe(kj)2(CN)2] and trans-Na2[Ru(kj)2(CN)2], indicating coordination of the cyano ligand to metal ions FeII e RuII. Comparing the obtained values with literature data was possible to identify the complex isomerism as trans. In relation to the results of electronic spectroscopy, studies of pH variation of kojic acid provided information on the distribution of electron density in the molecule, showing characteristic spectral profile of kojic ion and its protonated form (Hkj, kojic acid), with two bands at 215 and 269 nm, or deprotonated (kj-), with bands at 226 and 315 nm. The electronic spectra obtained for all complexes in aqueous medium, in the ultraviolet region, exhibited variations of the energies assigned to kojic acid intraligand transitions while in the visible region, only transitions assigned to charge transfer of iron and ruthenium complex have been identified

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In this work a study was done using electrochemical cyclic voltammetry and differential pulse voltammetry for isoniazida (INH), ethambutol (EMB), rifampicina (RIF) and pyrazinamide (PZA) using the electrode boron-doped diamond (BDD) as working electrode. It also verified the applicability of the technique of differential pulse voltammetry in the quantification of the active compounds used in the treatment of tuberculosis, subsequently applying in samples of pharmaceutical formulation. Among the four active compounds studied, isoniazid showed the best results for the detection and quantification using differential pulse voltammetry. At pH 4 and pH 8, for the calibration curves to INH showed good linearity, with quantification limits of 6.15 mmol L-1 (0,844 ppm) and 4.08 mmol L-1 (0.560 ppm) for the respective pH. The proposed method can be used to determine drug isoniazid, for recovery values were obtained in approximately 100%

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This study investigates the chemical species produced water from the reservoir areas of oil production in the field of Monte Alegre (onshore production) with a proposal of developing a model applied to the identification of the water produced in different zones or groups of zones.Starting from the concentrations of anions and cátions from water produced as input parameters in Linear Discriminate Analysis, it was possible to estimate and compare the model predictions respecting the particularities of their methods in order to ascertain which one would be most appropriate. The methods Resubstitution, Holdout Method and Lachenbruch were used for adjustment and general evaluation of the built models. Of the estimated models for Wells producing water for a single production area, the most suitable method was the "Holdout Method and had a hit rate of 90%. Discriminant functions (CV1, CV2 and CV3) estimated in this model were used to modeling new functions for samples ofartificial mixtures of produced water (producedin our laboratory) and samples of mixtures actualproduced water (water collected inwellsproducingmore thanonezone).The experiment with these mixtures was carried out according to a schedule experimental mixtures simplex type-centroid also was simulated in which the presence of water from steam injectionin these tanks fora part of amostras. Using graphs of two and three dimensions was possible to estimate the proportion of water in the production area

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Biodiesel is a fuel made up by mono-alkyl-esters of long chain fatty acids, derived from vegetable oils or animal fat. This fuel can be used in compression ignition engines for automotive propulsion or energy generation, as a partial or total substitute of fossil diesel fuel. Biodiesel can be processed from different mechanisms. Transesterification is the most common process for obtaining biodiesel, in which an ester compound reacts with an alcohol to form a new ester and a new alcohol. These reactions are normally catalyzed by the addition of an acid or a base. Initially sunflower, castor and soybean oil physicochemical properties are determined according to standard test methods, to evaluate if they had favorable conditions for use as raw material in the transesterification reaction. Sunflower, castor and soybean biodiesel were obtained by the methylic transesterification route in the presence of KOH and presented a yield above 93% m/m. The sunflower/castor and soybean/castor blends were studied with the aim of evaluating the thermal and oxidative stability of the biofuels. The biodiesel and blends were characterized by acid value, iodine value, density, flash point, sulfur content, and content of methanol and esters by gas chromatography (GC). Also studies of thermal and oxidative stability by Thermogravimetry (TG), Differential Scanning Calorimetry High Pressure (P-DSC) and dynamic method exothermic and Rancimat were carried out. Biodiesel sunflower and soybean are presented according to the specifications established by the Resolution ANP no 7/2008. Biodiesel from castor oil, as expected, showed a high density and kinematic viscosity. For the blends studied, the concentration of castor biodiesel to increased the density, kinematic viscosity and flash point. The addition of castor biodiesel as antioxidant in sunflower and soybean biodiesels is promising, for a significant improvement in resistance to autoxidation and therefore on its oxidative stability. The blends showed that compliance with the requirements of the ANP have been included in the range of 20-40%. This form may be used as a partial substitute of fossil diesel

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Topics of research related to energy and environment have significantly grown in recent years, with the need of its own energy as hydrogen. More particularly, numerous researches have been focused on hydrogen as energy vector. The main portion of hydrogen is presently obtained by reforming of methane or light hydrocarbons (steam, oxy, dry or auto reforming). During the methane steam reforming process the formation of CO2 undesirable (the main contributor to the greenhouse effect) is observed. Thus, an oxide material (sorbent) can be used to capture the CO2 generated during the process and simultaneously shifting the equilibrium of water gas shift towards thermodynamically more favorable production of pure hydrogen. The aim of this study is to develop a material with dual function (catalyst/sorbent) in the reaction of steam reforming of methane. CaO is well known as CO2 sorbent due to its high efficiency in reactions of carbonation and easy regeneration through calcination. However the kinetic of carbonation decreases quickly with time and carbonation/calcination cycles. A calcium aluminate (Ca12Al14O33) should be used to avoid sintering and increase the stability of CaO sorbents for several cycles. Nickel, the industrial catalyst choice for steam reforming has been added to the support from different manners. These bi-functional materials (sorbent/catalyst) in different molar ratios CaO.Ca12Al14O33 (48:52, 65:35, 75:25, 90:10) were prepared by different synthesis methodologies, among them, especially the method of microwave assisted self-combustion. Synthesis, structure and catalytic performances of Ni- CaO.Ca12Al14O33 synthesized by the novel method (microwave assisted selfcombustion) proposed in this work has not being reported yet in literature. The results indicate that CO2 capture time depends both on the CaO excess and on operating conditions (eg., temperature and H2O/CH4 ratio). To be efficient for CO2 sorption, temperature of steam reforming needs to be lower than 700 °C. An optimized percentage corresponding to 75% of CaO and a ratio H2O/CH4 = 1 provides the most promising results since a smaller amount of water avoids competition between water and CO2 to form carbonate and hydroxide. If this competition is most effective (H2O/CH4 = 3) and would have a smaller amount of CaO available for absorption possibly due to the formation of Ca(OH)2. Therefore, the capture time was higher (16h) for the ratio H2O/CH4 = 1 than H2O/CH4 = 3 (7h) using as catalyst one prepared by impregnating the support obtained by microwave assisted self-combustion. Therefore, it was demonstrated that, with these catalysts, the CO2 sorption on CaO modifies the balance of the water gas-shift reaction. Consequently, steam reforming of CH4 is optimized, producing pure H2, complete conversion of methane and negligible concentration of CO2 and CO during the time of capture even at low temperature (650 °C). This validates the concept of the sorption of CO2 together with methane steam reforming

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This work is directed to the treatment of organic compounds present in produced water from oil using electrochemical technology. The water produced is a residue of the petroleum industry are difficult to treat , since this corresponds to 98 % effluent from the effluent generated in the exploration of oil and contains various compounds such as volatile hydrocarbons (benzene, toluene, ethylbenzene and xylene), polycyclic aromatic hydrocarbons (PAHs), phenols, carboxylic acids and inorganic compounds. There are several types of treatment methodologies that residue being studied, among which are the biological processes, advanced oxidation processes (AOPs), such as electrochemical treatments electrooxidation, electrocoagulation, electrocoagulation and eletroredution. The electrochemical method is a method of little environmental impact because instead of chemical reagents uses electron through reactions of oxide-reducing transforms toxic substances into substances with less environmental impact. Thus, this paper aims to study the electrochemical behavior and elimination of the BTX (benzene, toluene and xylene) using electrode of Ti/Pt. For the experiment an electrochemical batch system consists of a continuous source, anode Ti/Pt was used, applying three densities of current (1 mA/cm2, 2,5 mA/cm2 and 5 mA/cm2). The synthetic wastewater was prepared by a solution of benzene, toluene and xylene with a concentration of 5 ppm, to evaluate the electrochemical behavior by cyclic voltammetry and polarization curves, even before assessing the removal of these compounds in solution by electrochemical oxidation. The behavior of each of the compounds was evaluated by the use of electrochemical techniques indicate that each of the compounds when evaluated by cyclic voltammetry showed partial oxidation behavior via adsorption to the surface of the Ti/Pt electrode. The adsorption of each of the present compounds depends on the solution concentration but there is the strong adsorption of xylene. However, the removal was confirmed by UV-Vis, and analysis of total organic carbon (TOC), which showed a percentage of partial oxidation (19,8 % - 99,1 % TOC removed), confirming the electrochemical behavior already observed in voltammetry and cyclic polarization curves

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This study used the Thermogravimetry (TG) and molecular absorption spectroscopy in UV-visible region to determine the iron content in herbal medicinal ferrous sulfate used in the treatment of iron deficiency anemia. The samples were characterized by IR, UV, TG / DTG, DTA, DSC and XRD. The thermoanalytical techniques evaluated the thermal stability and physicochemical events and showed that the excipients interfere in the decomposition of the active ingredients. The results of thermogravimetry showed that the decomposition temperature of the active principle Fe2(SO4)3 (T = 602 °C) is higher as compared to samples of tablets (566 586 °C). In the DTA and DSC curves were observed exothermic and endo events for samples of medicines and active analysis. The infrared spectra identified key functional groups exist in all samples of active ingredients, excipients and compressed studied, such as symmetric and asymmetric stretching of OH, CH, S=O. The analysis by X-ray diffraction showed that all samples had crystallinity and the final residue showed peaks indicating the presence of silicon dioxide, titanium dioxide and talc that are excipients contained in pharmaceutical formulations in addition to iron oxide. The results obtained by TG to determine the iron content of the studied drugs showed a variance when compared with those obtained by theoretical and UV-visible, probably due to formation of a mixture of Fe2O3 and Fe2(SO4)3. In one tablet was obtained FE content of 15.7 % and 20.6 % for TG by UV-visible, the sample EF 2 was obtained as a percentage of 15.4 % and 21.0 % for TG by UV-visible . In the third SF samples were obtained a content of 16.1 % and 25.5 % in TG by UV-visible, and SF 4 in the percentage of TG was 16.7 % and 14.3 % UV-visible

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The aromaticity index is an important tool for the investigation of aromatic molecules. This work consists on new applications of the aromaticity index developed by teacher Caio Lima Firme, so-called D3BIA (density, delocalization, degeneracy-based index of aromaticity). It was investigated its correlation with other well-known aromaticity indexes, such as HOMA (harmonic oscillator model of aromaticity), NICS (nucleus independent chemical shielding), PDI (para-delocalization index), magnetic susceptibility (), and energetic factor in the study of aromaticity of acenes and homoaromatic species based on bisnoradamantanyl cage. The density functional theory (DFT) was used for optimization calculations and for obtaining energetic factors associated with aromaticity and indexes HOMA and NICS. From quantum theory of atoms in molecules (QTAIM) it was obtained the indexes D3BIA, PDI and . For acenes, when the over-mentioned indexes were applied it was observed no correlation except for D3BIA and HOMA (R2=0.752). For bisnoradamantenyl dication and its derivatives, it was obtained a good correlation between D3BIA and NICS. Moreover, it was evaluated solely one of the factors used on D3BIA calculation, the delocalization index uniformity (DIU), so as to investigate its possible influence on stability of chemical species. Then, the DIU was compared with the formation Gibbs free energy of some pairs of carbocations, isomers or not, which each pair had small difference in point group symmetry and no difference among other well-known stability factors. The obtained results indicate that DIU is a new stability factor related to carbocations, that is, the more uniform the electron density delocalization, the more stable the is carbocation. The results of this work validate D3BIA and show its importance on the concept of aromaticity, indicating that it can be understood from degeneracy of atoms belonging the aromatic site, the electronic density in the aromatic site and the degree of uniformity of electron delocalization

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In this work were synthesized the materials called vanadyl phosphate, hydrogen vanadyl phosphate and vanadyl phosphate doped by transition metals with the aim in adsorption the following compounds: ammonia, hydrogen sulfide and nitrogen oxide. To characterize the starting compounds was used DRX, FTIR, FRX and TG analysis. After the characterization of substrates, proceeded de adsorption of NH3 and H2S gases in reactor, passing the gases with continuous flow for 30 min and room temperature. Gravimetric data indicate that the matrices of higher performance in adsorption of ammonia was those doped by aluminum and manganese, obtaining results of 216,77 mgNH3/g and 200,40 mgNH3/g of matrix, respectively. The matrice of higher performance in adsorption of hydrogen sulfide was that doped by manganese, obtaining results of 86,94 mgH2S/g of matrix. The synthesis of substrates VOPO4.2H2O and MnVOPO4.2H2O with nitrogen oxide was made in solution, aiming the final products VOPO4.G.nH2O and MnVOPO4.G.nH2O (G = NO and n = number of water molecules). The thermo analytical behavior and the infrared spectroscopy are indicative of formation of VOPO4.2,5NO.3H2O compound. Results of scanning electron microscopy (SEM) and Energy dispersive spectroscopy (EDS) of materials vanadyl phosphate and vanadyl phosphate modified after reaction in solid state or in solution with the gases show morphology changes in substrates, beyond the formation of orthorhombic sulfur crystals over their respective hosts when these adsorb hydrogen sulfide

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Metal Organic Frameworks (MOFs) are supramolecular structures consisted of ions or metal clusters coordinated to organic ligands which are repeated in two or three dimensions. These structures have atracted much attention due to their properties such as low density, high specific surface area and large volume of pores. In this work, MOFs consisted of zinc clusters connected by ditopic ligands, terephthalic acid (1,4- H2BDC) or isophthalic acid (1,3-H2BDC) were synthesized. To obtain the proposed materials, different routes and synthetic parameters were tested, such as the molar ratio of the precursors, the addition of template molecules, the type of solvente, the addition of organic base or the type of a counter-ion of Zn salt. It was found that the variation of these parameters led to the formation of different metalorganic structures. The solids obtained were characterized by XRD, SEM and IR. For the samples identified as MOF- 5, it was verified that the structure was composed of both interpenetrated and non interpenetrated structures. These samples showed a low stability, becoming totally transformed into another structure within less than 72 hours. The addition of the nickel and/or cobalt was found to be a promissing method for increasing the stability of MOF- 5, which in this case, still remained unconverted to another structure even after 15 days of exposure to air. The samples prepared from 1,3-H2BDC were probably new, still unknown Metal Organic Frameworks

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The construction of wells is one of the most important activities of the oil industry. The drilling process is the set of activities and operations to design, program and perform the opening thereof. During this process, the cuttings are removed by the drilling fluid, or mud, and carted to the surface. This fluid is injected into the drill string and returns to the surface through the annular space between the well walls and the drill string. After the descent of the column casing, the annular space between the casing string and the walls of the borehole is filled with cement so as to secure the spine and prevent any migration of fluids between the various permeable zones traversed by the well behind of the coating. To ensure the good quality of the cementation scrubbers are used mattresses which are pumped ahead of the cement slurry so as to avoid contamination of the drilling fluid paste, or vice versa, and assist in the removal of plaster, formed by drilling fluid of the borehole walls, thus enabling a better cement bond to the well. Within this context, this work aims to evaluate the efficiency of mattresses scrubbers, the basis of ionic and nonionic surfactants, on the removal of nonaqueous drilling fluid, based on n-paraffin in oil wells, and the compatibility between the Mattress relations washer / drilling fluid bed scrubber / cement paste mattress washer / cement slurry / drilling fluid and the drilling fluid / cement slurry using laboratory tests rheology, thickening time and compressive strength. Also technique was performed X-ray diffraction (XRD) for a more detailed analysis of these mixtures with hydrated cement paste. In compatibility tests the conditions of temperature and pressure used in the same laboratory procedure simulating the conditions of oil wells, the well is considered the depth of 800 m. The results showed that the compositions of the mattress washer nonionic, KMS obtained a 100% efficient in removing the non-aqueous drilling fluid, and the best formulation showed good results with respect to compliance testing

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Textile activity results in effluents with a variety of dyes. Among the several processes for dye-uptaking from these wastewaters, sorption is one of the most effective methods, chitosan being a very promising alternative for this end. The sorption of Methyl Orange by chitosan crosslinked particles was approached using equilibrium and kinetic analyses at different pH s. Besides the standard pseudo-order analysis normally effectuated (i.e. pseudo-first-order and pseudo-second-order), a novel approach involving a pseudo-nth-order kinetics was used, nbeing determined via non-linear regression, using the Levenberg-Marquardt method. Zeta potential measurements indicated that electrostatic interactions were important for the sorption process. Regarding equilibrium experiments, data were well fitted to a hybrid Langmuir-Freundlich isotherm, and estimated Gibbs free energy of adsorption as a function of mass of dye per area of chitosan showed that the process of adsorption becomes more homogeneous as the pH of the continuous phase decreased. Considering the kinetics of sorption, although a pseudo-nth-order description yielded good fits, a kinetic equation involving diffusion adsorption phenomena was found to be more consistent in terms of a physicochemical description of the sorption process