Sewage sludge-derived materials were used as adsorbents of hydrogen sulfide from moist air. The adsorbent obtained by carbonization at 950 degrees C has a capacity twice of that of coconut-shell-based activated carbon. The capacity of the sludge-derived materials increases with increasing carbonization temperature. It is likelythatduring carbonization at 950 degrees C a mineral-like phase is formed that consists of such catalytically active metals as iron, zinc, and copper. The results obtained demonstrate that the presence of iron oxide significantly increases the capacity of commercial carbon and activated alumina. The sludge-derived adsorbents are efficient for hydrogen sulfide removal until the pore entrances are blocked with sulfur as the product of oxidation reaction. For materials in which the catalytic effect is predominant, hydrogen sulfide is adsorbed until all pores are filled with sulfur. There is also indication that chemisorption plays a significant role in the removal of hydrogen sulfide from moist air.
Sewage sludge-derived materials carbonized at temperatures between 400 and 950 degrees C were used for adsorption of sulfur dioxide from dry and moist air. The materials were characterized using sorption of nitrogen and thermal analysis. The sulfur dioxide capacity was measured according to a laboratory-developed breakthrough test. It was found that the capacity of the adsorbents increases with increasing temperature of carbonization. It is likely that during carbonization at high temperatures such catalytic metals as calcium become active. They play a significant role in the SO2 removal process by neutralization of sulfuric acid formed as a result of oxidation of sulfur dioxide in wet conditions. Besides sulfuric acid, various sulfur-containing salts are formed. It was shown that, after their removal using waterwashing,the SO2 capacitysignificantly decreased.
The dependence of the several sources of solute retention in chromatography-bulk liquid partition, liquid interfacial adsorption, and solid support adsorption-on solvent volume and on surface areas is considered for a variety of practical situations. The relative magnitudes of the individual contributions may then be qualitatively predicted over a wide range of stationary phase loadings, for the situations of (a) constant sample size and (b) constant concentration of solute in the mobile phase. The individual contributions are finally summed to show qualitatively the various forms of variation of the net retention volume with liquid loading which may be met with in practice. The results are presented in graphical form. Certain features are found in these curves which are useful for diagnosis of interfacial adsorption effects in chromatography. The predicted curves are in formal agreement with published experimental plots, Means for the recognition of and correction for interfacial adsorption effects in experimental data are suggested, For chromatographic systems in which all three mechanisms occur, only bulk liquid partition coefficients can be determined unequivocally by chromatography alone.The range of application of chromatography to the measurement of physicochemical data is considerably broadened by these conclusions.
Sewage-sludge-derived fertilizer, Terrene, was used as a precursor of adsorbents tested for removal of hydrogen sulfide from moist air. The adsorbents were obtained by pyrolysis of zinc chloride-impregnated granular fertilizer at 400, 600, 800, and 950°C in a nitrogen atmosphere. Subsamples of the materials obtained were washed with hydrochloric acid to remove the excess zinc chloride and other soluble chlorides. This treatment results in a significant increase in the sample porosity. The highest H 2 S removal capacity was obtained for the sample carbonized at 600°C. This results from release of zinc chloride vapor during heat treatment, which acts to form micropores in the carbonaceous deposit. When inorganic oxides and salts are present in sufficient quantities, hydrogen sulfide undergoes surface reactions and is left on the surface in the form of nonvolatile sulfides and sulfates. The pores are gradually filled as the surface reaction proceeds. If catalytic metal oxides are removed, hydrogen sulfide is oxidized predominantly to sulfuric acid through the catalytic effect of the adsorption sites in the small micropores of the carbonaceous deposit. The removal of H 2 S occurs until all pore entrances are blocked with the oxidation product.
Baseline separation of 15 taxanes including paclitaxel (Taxol) was achieved on pentafluorophenyl (PFP) HPLC columns. Methods using aqueous acetonitrile gradients on each of two commercial PFP columns were developed that are suitable for the determination of potency, content uniformity, and degradation profile of the paclitaxel bulk drug and injectable dosage form. The elution order is apparently related to molecular size, the number of acetylated hydroxyl groups, and the substitution of a xylosyl group at the 7-position. The resolution of several of the taxanes is a sensitive function of the starting eluent composition and the programming rate, which requires optimization of the methods on both columns. Retention of 10 of the taxanes was studied over the temperature range from 30 to 70 degrees C, and enthalpies of transfer, delta H degree, were determined. Conversion of a hydroxy group to an acetyl group, which can interact more strongly with the fluorines on the PFP, has a large effect on the delta H degree, as does the addition of a xylosyl derivative to the 7-hydroxy. The methods developed for the injectable drug form allow good resolution of the taxanes from the excipient Cremophor EL, a polyethoxylated castor oil used with ethanol to solubilize the paclitaxel. The methods for the bulk drug were fully validated in terms of accuracy, precision, specificity including forced degradation, limits of detection and quantitation, and linearity and range.
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