Salts solution separation

Afonso, M.D., Hagmeyer, G., and Gimbel, R., Streaming potential measurements to assess the variation of nanofiltration membrane surface charge with the concentration of salt solutions, Separ. Purl Tech., 22, 529, 2001. 

Fig. 4 Plot of permeation rates Pr of NaCl and MgClj versus the concentration c of the aqueous salt solution. Separating membrane 60 layer pairs of PVA/PVS adsorbed from NaCl-containing polyelectrolyte solutions.

Copper salt, (a) Add aqueous copper acetate solution to an aqueous solution of glycine. Note the formation of a blue colour which is considerably deeper than the colour of the original copper acetate solution. On heating the solution, blue needles of the copper salt usually separate. 

Benzylthiouronium salts. Add 0 5 g. of sulphanilic acid to 10 ml. of water and 5 ml. of 10% NaOH solution, zndgently warm the shaken mixture until a clear solution is obtained. Cool, add 1 drop of phenol-phthalein solution, and then add dilute HCl dropwise with shaking until the pink colour is just discharged. Now add very dilute NaOH solution until the pink colour yt/rZ returns. Cool and add with shaking a solution of 0-5 g. of benzylthiouronium chloride in 5 ml. of water. The thiouronium salt rapidly separates filter at the pump, wash with water, drain and recrystallise from ethanol. Colourless crystals, m.p. 185°. (M.ps., p. 548.)... 

In a 1500 ml. round-bottomed flask, carrying a reflux condenser, place 100 g. of pure cydohexanol, 250 ml. of concentrated hydrochloric acid and 80 g. of anhydrous calcium chloride heat the mixture on a boiling water bath for 10 hours with occasional shaking (1). Some hydrogen chloride is evolved, consequently the preparation should be conducted in the fume cupboard. Separate the upper layer from the cold reaction product, wash it successively with saturated salt solution, saturated sodium bicarbonate solution, saturated salt solution, and dry the crude cycZohexyl chloride with excess of anhydrous calcium chloride for at least 24 hours. Distil from a 150 ml. Claisen flask with fractionating side arm, and collect the pure product at 141-5-142-5°. The yield is 90 g. 

Ethyl S-n-butyl xanthate. Use 32 g. of potassium ethyl xanthate, 37 g. (23 ml.) of n-butyl iodide (Section 111,40) and 50 ml. of absolute ethyl alcohol. Reflux on a water bath for 3 hours. Pour into 150 ml. of water, saturate with salt (in order to facilitate the separation of the upper layer), remove the upper xanthate layer, wash it once with 25 ml. of saturated salt solution, and dry with anhydrous calcium chloride or anhydrous calcium sulphate. Distil from a 50 ml. Claisen flask under reduced pressure. Collect the pale yellow ethyl S-n-butyl xanthate at 90-91°/4 mm. The yield is 34 g. 

Biopolymer Extraction. Research interests involving new techniques for separation of biochemicals from fermentation broth and cell culture media have increased as biotechnology has grown. Most separation methods are limited to small-scale appHcations but recendy solvent extraction has been studied as a potential technique for continuous and large-scale production and the use of two-phase aqueous systems has received increasing attention (259). A range of enzymes have favorable partition properties in a system based on a PGE—dextran—salt solution (97) ... 

This shift in emphasis by the mining iadustry has led to the development and use of a variety of improved techniques, in particular the commercial avadabihty of several metal specific extractants. These techniques are particularly useful in the separations and recycling of metals from metal sludges and metal salt solutions. 

An important publication by Kost et al. (63JGU525) on thin-layer chromatography (TLC) of pyrazoles contains a large collection of Rf values for 1 1 mixtures of petroleum ether-chloroform or benzene-chloroform as eluents and alumina as stationary phase. 1,3- and 1,5-disubstituted pyrazoles can be separated and identified by TLC (Rf l,3>i y 1,5). For another publication by the same authors on the chromatographic separation of the aminopyrazoles, see (63JGU2519). A-Unsubstituted pyrazoles move with difficulty and it is necessary to add acetone or methanol to the eluent mixture. Other convenient conditions for AH pyrazoles utilize silica gel and ethyl acetate saturated with water (a pentacyanoamine ferroate ammonium disodium salt solution can be used to visualize the pyrazoles). 

According to the literature, the product obtained in this manner may contain ethyl adipate. To remove this, the product is cooled to 0° and run slowly into 600 cc. of 10 per cent potassium hydroxide solution maintained at 0° with ice-salt. Water is added until the salt which separates has dissolved, and the cold alkaline solution is extracted twice with 200-cc. portions of ether. The alkaline solution, kept at 0°, is run slowly into 900 cc. of 10 per cent acetic acid solution with stirring, the temperature remaining below 1° (ice-salt). The oil which separates is taken up in 400 cc. of ether, and the aqueous solution is extracted with four 250-cc. portions of ether. The ether extract is washed twice with cold 7 per cent sodium carbonate solution and dried over sodium sulfate. After removal of the ether the residue is distilled, b.p. 7g-8i°/3 mm. The recovery is only 80-85 per cent, and in a well-conducted preparation the ethyl adipate eliminated amounts to less than one per cent of the total product. Unless the preparation has proceeded poorly the tedious purification ordinarily is best omitted. 

After an additional 10 min, a 1 % solution of hydrochloric acid (100 ml) is slowly added to the stirred reaction mixture and the resultant mixture is transferred to a separatory funnel. The ether layer is separated and washed sequentially with water, 5 % sodium bicarbonate solution, water and saturated salt solution. The washed ether solution is dried over anhydrous sodium sulfate, filtered, and evaporated to give an oily residue (0.45 g). Chromatography of the crude product on silica gel (50 g) followed by crystallization of the solid thus obtained (0.18 g) from ethanol gives 3 -hydroxy-B-homo-cholest-5-en-7a-one acetate (67 0.14 g) mp 90-91° [a]o 99° (CHCI3). 

With dinitriles a slightly different procedure is necessary due to their water solubility. After the reaction has cooled, 150 ml of chloroform is added to the flask, and this mixture is then poured into saturated salt solution. Enough water is added to dissolve precipitated salt and the chloroform layer is separated. The aqueous layer is extracted once with chloroform. The combined extracts are then washed twice with salt solution, dried, and distilled. 

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