Bromine extraction

After the Teflon stopcock is closed, the reaction vessel is transferred to a water bath maintained at 60°. The lower end of the vessel should be immersed to within about 1 in. below the fritted-glass retainer. As refluxing of the bromine proceeds, a liquid layer should accumulate above the fritted-glass retainer. If this does not happen, some bromine should be poured through the bypass arm so that a liquid layer ca. 1 in. thick is maintained on the frit. It is essential that liquid bromine contact the tribromide in order to attain efficient conversion to tetrabromide. As the reaction proceeds, the product, dissolved in liquid bromine, extracts into the lower vessel and deposits there as fine black crystals. 

Ambient air sampling on plant property of industrial bromine extraction and bromo-organics synthesis facilities revealed the presence of tetrabromobisphenol A (N.D. —28 ng/m ), decabromobiphenyl ether (N.D. —72 ng/m3), tris(2,3-dibromopro-pyljphosphate (N.D. —60 ng/m3) and l,2-bis(tribromophenoxy)ethane (N.D. —183 ng/m3). 

Generally, as discussed previously, the mechanism involved in the cross-linking of fluoroelastomers is the removal of hydrogen fluoride to generate a cure site that then reacts with diamine [39], bisphenol [40], or organic peroxides [41] that promote a radical cure by hydrogen or bromine extraction. Preferred amines have been blocked diamines such as hexamethylene carbamate (Diak No. 1) or bis(cinnamylidene) hexamethylene diamine (Diak No. 3). Preferred phenols are hydroquinone and the bisphenols such as 4,4 -isopro-pylidene bisphenol or the corresponding hexafluoro-derivative bisphenol AF. 

Bromine extraction (Herbert Henry Dow) Dow s method for extracting bromine from brine enables bromine to be widely used in medicines and in photography. 

For chemical processes, some examples are the elimination of aromatics by sulfonation, the elimination of olefins by bromine addition on the double bond (bromine number), the elimination of conjugated diolefins as in the case of the maleic anhydride value (MAV), and the extraction of bases or acids by contact with aqueous acidic or basic solutions. 

Carbon disulphide is an excellent solvent for fats, oils, rubber, sulphur, bromine and iodine, and is used industrially as a solvent for extraction. It is also used in the production of viscose silk, when added to wood cellulose impregnated with sodium hydroxide solution, a viscous solution of cellulose xanthate is formed, and this can be extruded through a fine nozzle into acid, which decomposes the xanthate to give a glossy thread of cellulose. 

Like bromine, iodine is soluble in organic solvents, for example chloroform, which can be used to extract it from an aqueous solution. The iodine imparts a characteristic purple colour to the organic layer this is used as a test for iodine (p. 349). NB Brown solutions are formed when iodine dissolves in ether, alcohol, and acetone. In chloroform and benzene a purple solution is formed, whilst a violet solution is produced in carbon disulphide and some hydrocarbons. These colours arise due to charge transfer (p. 60) to and from the iodine and the solvent organic molecules. 

Extract the acidified solution with ether, remove the ether and identify the phenol in the usual manner (see Section IV,114).f Add a few drops of bromine water or nitric acid to the aqueous layer and test for sulphate with barium chloride solution. 

Dissolve the solid in 700 ml. of water in a 1500 ml. round-bottomed flask, and add a solution of 88 ml. of concentrated sulphuric acid in about 200 ml. of water until the liquid has a distinct odour of sulphur dioxide sufficient heat will be liberated in the neutralisation to cause the solution to boil. Immediately steam distil the liquid (Fig. II, 40, 1 it is better to use the apparatus shown in Fig. II, 41, 3) until a sample of the distillate gives only a slight precipitate with bromine water. About 700 ml. of distillate should be collected. Saturate the steam distillate with salt, extract the dl with ether, dry the extract with a little anhydrous magnesium or calcium sulphate, distil oflF the ether (compare Fig. II, 13, 4, but with a 50 ml. Claisen flask replacing the distilling flask) and distil the residue under diminished pressure. Collect the p-cresol at 95-96°/15 mm. the colourless liquid solidifies to a white crystalline solid, m.p. 31°. The yield is 24 g. 

This solution may also be employed in the test for bromine. If iodine has been found, add small amounts of sodium nitrite solution, warm shghtly and shake with fresh 1 ml. portions of carbon tetrachloride until the last extract is colourless boil the acid solution until no more nitrous fumes are evolved and cool. If iodine is absent, use 1 ml. of the fusion solution which has been strongly acidified with glacial acetic acid. Add a small amount of lead dioxide, place a strip of fluorescein paper across the mouth of the tube, and warm the solution. If bromine is present, it will colour the test paper rose-pink (eosin). 

Most of the chlorine produced is used in the manufacture of chlorinated compounds for sanitation, pulp bleaching, disinfectants, and textile processing. Further use is in the manufacture of chlorates, chloroform, carbon tetrachloride, and in the extraction of bromine. 

A member of the halogen group of elements, it is obtained from natural brines from wells in Michigan and Arkansas. Little bromine is extracted today from seawater, which contains only about 85 ppm. 

This method is by far the easiest of the two methods I descnbe, but because it uses bromine liquid as a precursor to the dibromodioxane crystals a fume cupboard (or a fucking good method of fume extraction) is absolutely essential. Surgically removing ones gonads with a blunt knife would be a much less painful way of harming yourself than messing with this stuff in the kitchen. 

Magnesium sulfate heptahydrate may be prepared by neutralization of sulfuric acid with magnesium carbonate or oxide, or it can be obtained directly from natural sources. It occurs abundantly as a double salt and can also be obtained from the magnesium salts that occur in brines used for the extraction of bromine (qv). The brine is treated with calcium hydroxide to precipitate magnesium hydroxide. Sulfur dioxide and air are passed through the suspension to yield magnesium sulfate (see Chemicals frombrine). Magnesium sulfate is a saline cathartic. 

Oil Fields. Oil field waters in the United States containing lithium have been identified in 10 states. The greatest concentrations are in waters from the Smackover formation of southern Arkansas and eastern Texas. Concentrations from this formation have been measured from 300—600 ppm in waters originating at a 2500—3300 m depth. Recovery of lithium from this resource would only be commercially feasible if a selective extraction technique could be developed. Lithium as a by-product of the recovery of petroleum (qv), bromine (qv), or other chemicals remains to be exploited (12). 

Dissolved Minerals. The most significant source of minerals for sustainable recovery may be ocean waters which contain nearly all the known elements in some degree of solution. Production of dissolved minerals from seawater is limited to fresh water, magnesium, magnesium compounds (qv), salt, bromine, and heavy water, ie, deuterium oxide. Considerable development of techniques for recovery of copper, gold, and uranium by solution or bacterial methods has been carried out in several countries for appHcation onshore. These methods are expected to be fully transferable to the marine environment (5). The potential for extraction of dissolved materials from naturally enriched sources, such as hydrothermal vents, may be high. 

Quantitatively, sulfur in a free or combined state is generally determined by oxidizing it to a soluble sulfate, by fusion with an alkaH carbonate if necessary, and precipitating it as insoluble barium sulfate. Oxidation can be effected with such agents as concentrated or fuming nitric acid, bromine, sodium peroxide, potassium nitrate, or potassium chlorate. Free sulfur is normally determined by solution in carbon disulfide, the latter being distilled from the extract. This method is not useful if the sample contains polymeric sulfur. 

Later, recovery of bromine from brine wells in Midland County, Michigan was developed. Brines in Michigan, Ohio, and West Virginia suppHed the principal portion of production in the United States until 1935. Michigan brines are stiU a source of bromine today. A significant source of bromine in 1991 came from wells in southwest Arkansas. Bromine is found in Seades Lake brine and was produced there at one time, but commercial extraction has been discontinued. 

Another ancient dye is the deep blue indigo [482-89-3], the presence of two bromine atoms at positions gives the dye Tyrian purple [19201 -53-7] once laboriously extracted from certain sea shells and worn by Roman emperors. 

Hydroxyquinoline forms the complex with Cu(II) in ratio 1 1 at pH 5-7. The composition of the complex is changed on 1 2 at pH>7. 8-Hydroxy-quinoline accepts bromine therefore its excess has been removed with NaOH solution. The complex was extracted with chloroform. It was shown that double extraction was enough to extract the complex. The detection limit is 5x10 M during 10c and at current generation IxlO A. 

In a 5-1, 3-necked flask fitted with a mechanical stirrer (Note 1), a dropping funnel, and a thermometer for reading low temperatures is placed 790 ml. (7 moles) of 48% h drobromic acid. The fl.ask and contents are cooled to 10-20 in an ice-salt bath, and 150 g, (1.59 moles) of 2-aminopyridine (Note 2) is added over a period of about 10 minutes. While the temperature is kept at 0° or lower, 240 ml. (4.7 moles) of bromine is added dropwise (Note 3). A solution of 275 g. (4 moles) of sodium nitrite in 400 ml. of water is added dropwise over a period of 2 hours, the temperature being carefully maintained at 0° or lower (Note 4). After an additional 30 minutes of stirring, a solution of 600 g. (15 moles) of sodium hydroxide in 600 ml. of water is added at such a rate that the temperature does not rise above 20-25° (Note 5). The nearly colorless reaction mixture is extracted with... 

To the acid chloride, mechanically stirred and heated on the steam bath, is added 2.5 kg. (805 ml. 15.6 moles) of dry bromine as rapidly as it will react (Note 5). The addition requires about 12 hours. The contents of the flask are stirred and heated an additional 2 hours, transferred to a dropping funnel (Note 6), and added in a thin stream to 5 1. of absolute ethyl alcohol, which has previously been placed in a 12-1. flask provided with a stopper carrying an effleient reflux condenser, a separatory funnel, and a mechanical stirrer. The resulting vigorous reaction is controlled by external cooling. After the dibromoacid chloride has been added, the reaction mixture is allowed to stand at room temperature overnight and is then poured into 5 1. of cold water. The top alcoholic aqueous layer is decanted and extracted once with 8 1. of ether. The oily bottom layer is dissolved in the ether extract, washed first with 1 1. of a 2% sodium bisulfite solution, then with two 1-1. portions of 3% sodium carbonate solution, and finally with several portions of water. The ether solution is dried over 175 g. of potassium carbonate the solvent is distilled on the steam bath. The yield of residual ester (Note 7) amounts to 2260-2400 g. (91-97% of the theoretical amount). 

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