Solvent selection procedure

Vandenburg et al. [37,489] have described the use of Hildebrand solubility parameters in a simple and fast solvent selection procedure for PFE of a variety of polymers. Hildebrand parameters for several common solvents and polymers are presented in Tables 3.2 and 3.34, respectively. When the proper solvent mixture for the polymer was determined, PFE resulted in essentially the same recoveries as the traditional extraction methods, but used much less time and solvent. PFE can be used to give very fast extractions and appears to offer the greatest flexibility of solvents and solvent mixtures. The method is ideal for a laboratory which analyses a large number of different polymers. 

Recommended Solvent Selection Procedure. Resin contaminants have been identified only recently. Until 1977, only the following resin contaminants were identified naphthalene, ethylbenzene, and benzoic acid (36). The resin cleaning procedure of Junk et al. (5), which uses a series of three solvents of decreasing polarity, removes the widest possible variety of organic contaminants from the resins. This method is necessary when many compounds must be removed. 

You can identify the solubility characteristics of your compound using the solvent selection procedure shown in Box 13.1 and modifications for mixed solvent selection are given in Box 13.2. 

Clearly, this solvent selection procedure will not always result in optimal preparative chromatographic conditions, but it offers a method that can be applied immediately. 

The author thanks Wesley French in developing the solvent selection procedure described above. Thanks are also due to PPG Industries, Inc. for permission to publish this work. 

Hansen (86) has modified the method of Nelson, et al. by incorporating solubility parameters for the three component forces in the solubility parameter, viz, dispersion, polar, and hydrogen bonding forces. The solvent selection procedure was designed for use by plant laboratories on a time sharing terminal. The enlistment of the computer in the selection of solvent blends has been a boon to the formulator, but the use of older methods is still very useful. 

Salcomine is a useful catalyst for the selective oxygenation of 2,6-disubstituted phenols to the corresponding p-benzoquinones when dimethylformamide is used as the solvent laborious procedures are avoided and high yields of pure p-benzoquinones are obtained. Following the procedure described above, the authors have prepared 2,6-diphenyl-p-benzoquinone (m.p. 134—135°, yield 86%) and 2,6-dimethoxy-p-benzoquinone (m.p. 252°, yield 91%) from the appropriate phenols. 

Cobalt, sepn. of from nickel, (cm) 532 Codeine and morphine, D. of 740 Coefficient of variation 135 Colloidal state 418 See also Lyophilic, Lyophobic Colorimeters light filters for, 661 photoelectric, 645, 666 Colorimetric analysis 645 criteria for, 672 general remarks on, 645, 672 procedure, 675 solvent selection, 674 titration, 652... 

While most polymer/additive analysis procedures are based on solvent or heat extraction, dissolution/precipita-tion, digestions or nondestructive techniques generally suitable for various additive classes and polymer matrices, a few class-selective procedures have been described which are based on specific chemical reactions. These wet chemical techniques are to be considered as isolated cases with great specificity. 

Extrinsic wastes are more functional in nature and are not necessarily inherent to a specific process configuration. These may occur as a result of unit upsets, selection of auxiliary equipment, fugitive leaks, process shutdown, sample collection and handling, solvent selection, or waste handling practices. Extrinsic wastes can be, and often are, reduced readily through administrative controls, additional maintenance or improved maintenance procedures, simple recycling, minor... 

Significant improvements in yields or reaction conditions can be achieved, together with considerable simplification of operating procedures. The powerful synergistic combination of PTC and microwave techniques has certainly enabled an ever increasing number of reactions to be conducted under clean and mild conditions. The inherent simplicity of the method can, furthermore, be allied with all the advantages of solvent-free procedures in terms of reactivity, selectivity, economy, safety, and ease in manipulation. 

A facile method for the oxidation of alcohols to carbonyl compounds has been reported by Varma et al. using montmorillonite K 10 clay-supported iron(III) nitrate (clayfen) under solvent-free conditions [100], This MW-expedited reaction presumably proceeds via the intermediacy of nitrosonium ions. Interestingly, no carboxylic acids are formed in the oxidation of primary alcohols. The simple solvent-free experimental procedure involves mixing of neat substrates with clayfen and a brief exposure of the reaction mixture to irradiation in a MW oven for 15-60 s. This rapid, ma-nipulatively simple, inexpensive and selective procedure avoids the use of excess solvents and toxic oxidants (Scheme 6.30) [100]. Solid state use of clayfen has afforded higher yields and the amounts used are half of that used by Laszlo et al. [17,19]. 

Lipids can be extracted from biological samples using a variety of organic solvents. A chloroform-methanol solvent is suitable for all lipids but it is possible to extract different classes of lipid selectively on the basis of their solubility in different organic solvents. This may be achieved by the addition of a solvent that will effect either the precipitation or the extraction of the lipids of interest. An example of the former is the precipitation of high concentrations of phospholipids with cold, dry acetone, and of the latter, the extraction of fatty acids into ether or heptane at an acid pH. However, like all solvent extraction procedures these are not entirely specific. 

As can be seen from the list, there are many competing procedures for leaching, selective separation of the metals, and generation of products. Thus, the detailed design of a specific recovery process often involves a number of selected procedures, combined in unique ways. This chapter discusses processes containing a solvent extraction separation procedure. 

The use of Zn-Cr(III) alloy plating has almost replaced the use of Cr(VI) in the electroplating industry due to its excellent corrosion resistance and its lower toxicity. Recently, a solvent extraction procedure for separating and selectively recovering the two metals, zinc and chromium, from electroplating wastewaters has been demonstrated [10]. 

Both round 0 data (before affinity selection) and round 3 data (after three rounds of affinity selection) are shown, where round 0 represents a sampling prior to any ultrafiltration. Round 0 and round 3 samples undergo identical denaturation/solvent extraction procedures. Data were generated... 

Solvents used here for a general liquid-liquid extraction method were selected from Snyders solvent selectivity triangle. As extraction liquids have to be composed of mixtures of three solvents which may enter into maximum interaction with the analyte, three solvents had to be selected that represent a wide variety of selective interactions. In addition, the solvents should be sufficiently polar to ensure quantitative extraction. Besides selectivity and polarity requirements, the solvents should also meet a few other criteria, mainly for practical reasons they should not be miscible with water, have low boiling points (for relatively fast evaporation procedures) and have densities sufficiently different from the density of water, for pure solvents as well as for selected binary or ternary mixtures of solvents. 

Mention must be made of the use of an internal standard to monitor a reaction by g.l.c. analysis, and also to calculate the g.l.c. yield. Here, a known weight of the standard, inert to the reaction conditions and conforming to the other criteria of selection noted above, is added initially to the reaction mixture. In the case where samples of the mixture can be removed and loaded directly on to the column, the subsequent analysis presents no problem and may be deduced from the discussion above. In the case of samples which require evaporation of solvent prior to chromatographic examination, it is only necessary to ensure that the standard, and indeed the components to be analysed, do not volatilise under the conditions of concentration. If the samples require more involved solvent extraction procedures, then further experimentation is required to establish that... 

The technique used to develop the four-solvent systems was based on procedures elucidated by Lehrer (6), Rohrschneider (7), and Glajch (8). After trials with individual solvents chosen from the comers of the Snyder solvent-selectivity triangle—a system of classification of solvents by the degree to which they function as proton donors, proton acceptors, or dipole interactors—an ideal solvent system was calculated. Ethanol, acetonitrile, and tetrahydrofuran were the reverse-phase solvents used, and water was the carrier solvent. Once the ideal solvent strength of one solvent-water combination was empirically determined, that of the other combinations could be estimated by use of the following equation (9) ... 

The present model predicts how solvent selectivity will vary with mobile-phase composition, and this allows the selection of extreme solvents for maximum differences in selectivity. This information plus the ability to calculate solvent strength versus composition of the mobile phase then allows development of a general strategy for optimizing retention of any sample, so as to maximize resolution. This four-solvent approach can be further refined by use of computer-assisted procedures, such as the overlapping-resolution-mapping technique. 

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