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Since many new substances of interest are very poorly soluble in water, the assessment of the pKa in aqueous solution can be dif cult and problematic Potentiometry can be a quick technique for such assessment, provided the solubility of the substance is at least 100 mM (Solutions as dilute as 10 mM can still be analyzed, but special attention must be given to electrode calibration, and ambient carbon dioxide must be excluded) If the substance is soluble to only 1 10 mM and possesses a pH-sensitive UV chromophore, then spectrophotometry can be applied CE methods may also be useful since very small sample quantities are required, and detection methods are generally quite sensitive If the compound is virtually insoluble (<1 mM), then a pH-metric mixed-solvent approach can be tried [112] For example, the pKa of the antiarrhythmic amiodarone, 906 014, was estimated from water methanol mixtures, though the intrinsic solubility of the molecule is $0008 mM (6 ng/mL) [pION] The most frequently explored solvent systems are based on water alcohol mixtures [119,164,166,181 210] DMSO water [211 215], dioxane water [216 220], and other systems [221,222] have been explored Where possible, methanol is the solvent of choice, because its general effect on pKa values has been studied so extensively It is thought to be the least error-prone of the common solvents Mixed-solvent solutions of various cosolvent water proportions are titrated and psKa (the apparent pKa ) is measured in each mixture The aqueous pKa is deduced by extrapolation of the psKa values to zero cosolvent This technique was rst used by Mizutani in 1925 [181 183] Many examples may be cited of pKa estimated by extrapolation in mixtures of methanol [119,161,162,191,192,196,200], ethanol [184,188 190,193], propanol [209], DMSO [212,215], dimethylformamide [222], acetone [221], and dioxane [216] Plots of psKa versus weight percent organic solvent, Rw 0 60 wt%, at times show either a hockey-stick or a bow shape [119] For Rw > 60 wt%, S-shaped curves are sometimes observed (Generally, psKa values from titrations with Rw > 60 wt% are not suitable for extrapolation to zero cosolvent because KCl and other ion pairing interferes signi cantly in the reduced dielectric medium [223]) For values of Rw < 60 wt%, the nonlinearity in psKa plots can be ascribed partly to electrostatic long-range ion ion interactions Extensions of the Born electrostatic model, drawing on Bjerrum s theory of ion association [223], were introduced by Yasuda [194] and Shedlovsky [201] It was recognized that equilibrium quotients in mixed solvents of varying proportions ought explicitly to incorporate the concentration of water, since constancy in water activity cannot be expected in cosolvent mixtures It was thus proposed that the plot of psKa log [H2O] versus 1/E should produce a straight line for solutions with dielectric constant E, > 50, which for methanol at 25 C means Rw < 60 wt% The slope in such a plot is expected to be inversely proportional to the average ionic diameter of the solvated molecule [201] The Yasuda Shedlovsky procedure is now widely used to assess pKa values of very sparingly soluble pharmaceutical compounds [119,150,166,172, 224,225]. barcode font excel 2013 free [SOLVED] Generate barcode in excel free - Spiceworks Community
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