Calcium chloride purification

Purification of the Methylamine HCI is in order now, so transfer all of the crude product to a 500mL flask and add either 250mL of absolute Ethanol (see end of FAQ for preparing this) or, ideally, n-Butyl Alcohol (see Footnote 4). Heat at reflux with a Calcium Chloride guard tube for 30 minutes. Allow the undissolved solids to settle (Ammonium Chloride) then decant the clear solution and cool quickly to precipitate out Methylamine HCI. Filter rapidly on the vacuum Buchner funnel and transfer crystals to a dessicator (see Footnote 3). Repeat the reflux-settle-cool-filter process four... 

Salt that is substantially free of sulfate and other impurities is the cell feed. This grade may be purchased from commercial salt suppHers or made on site by purification of cmde sea or rock salt. Dried calcium chloride or cell bath from dismanded cells is added to the bath periodically as needed to replenish calcium coproduced with the sodium. The heat required to maintain the bath ia the molten condition is suppHed by the electrolysis current. Other electrolyte compositions have been proposed ia which part or all of the calcium chloride is replaced by other salts (61—64). Such baths offer improved current efficiencies and production of cmde sodium containing relatively Htde calcium. 

The purification of diethyl ether (see Chapter 4) is typical of liquid ethers. The most common contaminants are the alcohols or hydroxy compounds from which the ethers are prepared, their oxidation products (e.g. aldehydes), peroxides and water. Peroxides, aldehydes and alcohols can be removed by shaking with alkaline potassium permanganate solution for several hours, followed by washing with water, concentrated sulfuric acid [CARE], then water. After drying with calcium chloride, the ether is distilled. It is then dried with sodium or with lithium aluminium hydride, redistilled and given a final fractional distillation. The drying process should be repeated if necessary. 

B. (l-Azido-3,3-dimethoxy-l-propenyl)benzene. In a 2-1., one-necked, round-bottomed flask equipped with a magnetic stirrer and powder funnel are placed 156 g. (0.45 mole) of the iodoazide from Part A and 1500 ml. of anhydrous ether. The solution is stirred and cooled in an ice-salt bath (— 5° to 0°), and 62 g. (0.55 mole) of potassium <-butoxide (Note 6) is added. The powder funnel is then replaced by a calcium chloride drying tube and the mixture is stirred for 4 5 hours at 0°. At the end of this time 350 ml. of water is added while the mixture is still cold. The ethereal layer is then separated and washed with three 350-ml. portions of water and dried over magnesium sulfate. The solvent is removed with a rotary evaporator without heating, leaving 67-75 g. (68-76%) of (l-azido-3,3-dimethoxy-l-propenyl)-benzene as a dark oily liquid (Note 7). This material can be used without further purification for Part C (Note 8). 

Pure Commercial Benzene, obtained from coal-tai naphtha, should distil w lthin one degiee (80—Si ), and solidify completely when cooled to 0°. Other tests are as follow s shaken with concentrated sulphuric acid for a few minutes, the acid should not darken, and a drop of bromine water should not be immediately decolourised. A single distillation over a few small pieces of sodium, which absorb any traces of water, is usually a sufficient purification. If the benzene impart a brown or black colour to the sulphuric acid, it must be repeatedly shaken with about 20 per cent, of the acid until the lattev becomes only slightly yellow on standing. This is done in a stoppered separating funnel, and after shaking fora few minutes the mixture is allow ed to settle, and the low er layer of acid diawn off. The benzene is then shaken tw o 01 three times with water to free it from acid, carefully separated from the aqueous layer, and left in contact with fused calcium chloride until the liquid becomes clear. It is then decanted, frozen in ice, and any liquid (carbon bisulphide, paraffins) carefully drained off, and die benzene finally distilled over sodium. 

A mixture of 125 g of o-(pethyl chlorocarbonate in 150 ml of ether. The mixture is kept at room temperature for 3 days, diluted with about 500 ml of water and extracted with 300 ml of ether. The ethereal extract Is washed with 300 ml of water, dried over calcium chloride, filtered and concentrated. The resulting ethyl o-(pnext step without further purification. 

Through the separatory funnel are introduced 1600 cc. of water, 500 cc. of c. p. acetone, and 372 cc. of glacial acetic acid. The stirrer is started and the temperature of the water bath is raised to 70-80°, so that the mixture in (he flask is at about 65° (Note 2). Then 354 cc. (7.3 moles) of bromine is carefully added through the separatory funnel. The addition is so regulated as to prevent the accumulation of unreacted bromine (Note 3). The addition requires one to t wo hours. As a rule the solution is decolorized in about twenty minutes after the bromine has been added. When the solution is decolorized, it is diluted with 800 cc. of cold water, cooled to io°, made neutral to Congo Red with about 1000 g. of solid anhydrous sodium carbonate, and the oil which separates is collected in a separatory funnel and dried with 80 g. of anhydrous calcium chloride. After drying, the oil is fractionated and the fraction boiling at 38 48°/13 mm. is collected. The yield is 470 480 g. (47—48 per cent of the theoretical amount). It may be used without further purification for the preparation of acetol (p. 1), but if a purer product is desired, the above product is refractionated... 

As an alternative purification procedure, the checkers have esterified the crude acid by refluxing it for 2 hours with three times its weight of methanol and 2 ml. of 98% sulfuric acid. The solution is poured into 10 volumes of water and extracted with the minimum amount of chloroform required to give a clean separation of layers. The chloroform solution is washed with water, dried over calcium chloride, and distilled from a Claisen flask with an indented neck. Methyl 1-adamantanecarboxylate is collected at 77-79° (1 mm.) m.p. 38-39°. Hydrolysis of the ester with the calculated amount of 1A potassium hydroxide followed by acidification yields 1-adamantanecarboxylic acid m.p. 175-176.5° 90% overall recovery. 

The nitrosophenol is precipitated from the cooled aqueous solution by acidification with dilute sulphuric acid and is extracted with ether in a separating funnel. After brief drying over calcium chloride the brownish-green solution is concentrated on the water bath. The sparingly soluble compound crystallises from the ether on cooling. Melting point 120°-130° (decomp.). Complete purification of nitrosophenol is difficult. 

Purification entails use of an immunoaffinity column containing immobilized murine antifactor VII antibody. It is initially produced as an unactivated, single chain 406 amino acid polypeptide, which is subsequently proteolytically converted into the two-chain active factor Vila complex. After sterilization by filtration, the final product is aseptically filled into its final product containers and freeze-dried. The excipients present in the product include sodium chloride, calcium chloride, polysorbate 80, mannitol and glycylglycine. When freeze-dried in the presence of these stabilizing substances and stored under refrigerated conditions, the product displays a shelf-life of at least 2 years. It has proved effective in the treatment of serious bleeding events in patients displaying anti-factor VIII or IX antibodies. 

The moist crude bromohexadiene is quaternized in water without further purification. The submitters report that, if desired, the crude mixture may be dried over anhydrous calcium chloride and fractionally distilled through a 10-in. stainless-steel-packed column at reduced pressure. Crude bromohexadiene (220-230 g.) from 147 g. (1.50 moles) of l,5-hexadiene-3-ol was found to give the fractions listed in Table I. The yield of the... 

Materials. Imidazole, benzimidazole, and glucosamine hydrochloride were obtained from the Eastman Kodak Co., and used without further purification, after drying for several days over anhydrous calcium chloride. Stock solutions of nickel nitrate and nickel chloride were analyzed by precipitation with dimethyl-glyoxime. Stock solutions of cadmium nitrate were analyzed gravimetrically by conversion to cadmium sulfate. 

B. Bis(2,4,6-trimethylpyridine)iodine(l) hexafluorophosphate. A 1-L, threenecked, round-bottomed flask equipped with a mechanical stirrer, condenser topped with a drying tube containing calcium chloride, and a stopper is charged with 500 mL of dry methylene chloride (Note 6), 82.5 g of bis(trimethylpyridine)silver(l) hexafluorophosphate (0.166 mol), and 41.9 g of iodine (0.165 mol). The mixture is stirred until all the iodine is consumed (1 hr - 2 hr) (Note 7). The resulting yellow solid (silver iodide) is suction filtered, and washed with 100 mL of dry methylene chloride. The filtrate is concentrated on a rotary evaporator at a maximum bath temperature of 30°C to give 68-76 g (80-88%) of yellowish solid bis(2,4,6-trimethylpyridine)iodine(l) hexafluorophosphate (mp 132-133°C) (Notes 8, 9, and 10). This product is suitable for reactions without further purification. 

The checkers used anhydrous sulfur dioxide supplied in cylinders by the Matheson Co., Inc., East Rutherford, New Jersey, without further purification. Traces of moisture will not interfere with the reaction, and it is sufficient if the liquid sulfur dioxide is clear and colorless. If necessary, however, the gaseous sulfur dioxide may be dried with anhydrous calcium chloride before condensing it. 

Liquid membranes of the water-in-oil emulsion type have been extensively investigated for their applications in separation and purification procedures [6.38]. They could also allow extraction of toxic species from biological fluids and regeneration of dialysates or ultrafiltrates, as required for artificial kidneys. The substrates would diffuse through the liquid membrane and be trapped in the dispersed aqueous phase of the emulsion. Thus, the selective elimination of phosphate ions in the presence of chloride was achieved using a bis-quaternary ammonium carrier dissolved in the membrane phase of an emulsion whose internal aqueous phase contained calcium chloride leading to phosphate-chloride exchange and internal precipitation of calcium phosphate [6.1]. 

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