Iodine chloride solution

Additional properties of vinyl laurate are 1.4345 and 2 0.8639. If the iodine number is determined by the Wijs method, a 200% excess of iodine chloride solution and a 1-hour reaction period should be employed in order to obtain values which are 97-99% of the theoretical value. 

Place 10 ml. of 1% starch solution (prepared as described above) in a boiling-tube, add 2 ml. of 1% sodium chloride solution and place the tube in a water-bath maintained at 38-40 . Place about 5 ml. of water in a series of test-tubes and to each add a few drops of 1% iodine solution. Now add 4 ml. of the diluted saliva solution to the starch solution, mix well and note the time. At intervals of about 30 seconds transfer 2 drops of the reacting mixture, by means of a dropping tube, to one of the test-tubes, mix and note the colour. As in the previous experiment, the colour, which is blue at first, changes to blue-violet, red-violet, red-brown, pale brown, and finally disappears at this stage the solution will reduce Fehling s solution. If the reaction proceeds too quickly for the colour changes to be observed, the saliva solution should be diluted. 

CAUTION. Ethers that have been stored for long periods, particularly in partly-filled bottles, frequently contain small quantities of highly explosive peroxides. The presence of peroxides may be detected either by the per-chromic acid test of qualitative inorganic analysis (addition of an acidified solution of potassium dichromate) or by the liberation of iodine from acidified potassium iodide solution (compare Section 11,47,7). The peroxides are nonvolatile and may accumulate in the flask during the distillation of the ether the residue is explosive and may detonate, when distilled, with sufficient violence to shatter the apparatus and cause serious personal injury. If peroxides are found, they must first be removed by treatment with acidified ferrous sulphate solution (Section 11,47,7) or with sodium sulphite solution or with stannous chloride solution (Section VI, 12). The common extraction solvents diethyl ether and di-tso-propyl ether are particularly prone to the formation of peroxides. 

Hydrochloric acid digestion takes place at elevated temperatures and produces a solution of the mixed chlorides of cesium, aluminum, and other alkah metals separated from the sUiceous residue by filtration. The impure cesium chloride can be purified as cesium chloride double salts such as cesium antimony chloride [14590-08-0] 4CsCl SbCl, cesium iodine chloride [15605 2-2], CS2CI2I, or cesium hexachlorocerate [19153 4-7] Cs2[CeClg] (26). Such salts are recrystaUized and the purified double salts decomposed to cesium chloride by hydrolysis, or precipitated with hydrogen sulfide. Alternatively, solvent extraction of cesium chloride direct from the hydrochloric acid leach Hquor can be used. 

A mixture consisting of 0.69 g (10.5 mmoles) of zinc-copper couple, 12 ml of dry ether, and a small crystal of iodine, is stirred with a magnetic stirrer and 2.34 g (0.7 ml, 8.75 mmoles) of methylene iodide is added. The mixture is warmed with an infrared lamp to initiate the reaction which is allowed to proceed for 30 min in a water bath at 35°. A solution of 0.97 g (2.5 mmoles) of cholest-4-en-3/ -ol in 7 ml of dry ether is added over a period of 20 min, and the mixture is stirred for an additional hr at 40°. The reaction mixture is cooled with an ice bath and diluted with a saturated solution of magnesium chloride. The supernatant is decanted from the precipitate, and the precipitate is washed twice with ether. The combined ether extracts are washed with saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent is removed under reduced pressure and the residue is chromatographed immediately on 50 g of alumina (activity III). Elution with benzene gives 0.62 g (62%) of crystalline 4/5,5/5-methylene-5 -cholestan-3/5-ol. Recrystallization from acetone gives material of mp 94-95° Hd -10°. 

Chlor-jod, n. iodine chloride, specif, iodine monochloride, -kali, n. chloride of potash (potassium hypochlorite) potassium chloride. -kalilOsung, /. Pharm.) solution of chlorinated potassa, Javelle water, -kalium, n. potassium chloride. 

Preparation of 4-aza-S-(N-methyl-4-piperidyll-10,11-dihydro-SH-dibenzo[a,d]cycloheptene-S-ol Add 17.4 g of N-methyl-4-chloropiperidine to a stirred mixture containing 3.2 g of magnesium, 20 ml of anhydrous tetrahydrofuran, 1 ml of ethyl bromide and a crystal of iodine. Reflux for two hours, cool to 30°-35°C and add a solution of 13 g of 4-aza-10,11 -dihydro-5H-dibenzo[a,d] cycloheptene-5-one in 25 ml of tetrahydrofuran. Stir for five hours, remove the solvent by distillation in vacuo and add 250 ml of ether. Add 100 ml of 10% ammonium chloride solution and extract the mixture with chloroform. Concentrate the chloroform solution to a residue and recrystallize from isopropyl ether obtaining 20 g of the carbinol,... 

The liberated iodine and the excess of iodide is determined by titration with standard potassium iodate solution the hydrochloric acid concentration must not be allowed to fall below 7JVf in order to prevent re-oxidation of the vanadium compound by iodine chloride. 

Schnepfe [83] has described yet another procedure for the determination of iodate and total iodine in seawater. To determine total iodine 1 ml of 1% aqueous sulfamic acid is added to 10 ml seawater which, if necessary, is filtered and then adjusted to a pH of less than 2.0. After 15 min, 1 ml sodium hydroxide (0.1 M) and 0.5 ml potassium permanganate (0.1M) are added and the mixture heated on a steam bath for one hour. The cooled solution is filtered and the residue washed. The filtrate and washings are diluted to 16 ml and 1ml of a phosphate solution (0.25 M) added (containing 0.3 xg iodine as iodate per ml) at 0 °C. Then 0.7 ml ferrous chloride (0.1 M) in 0.2% v/v sulfuric acid, 5 ml aqueous sulfuric acid (10%) - phosphoric acid (1 1) are added at 0 °C followed by 2 ml starch-cadmium iodide reagent. The solution is diluted to 25 ml and after 10-15 min the extinction of the starch-iodine complex is measured in a -5 cm cell. To determine iodate the same procedure is followed as is described previously except that the oxidation stage with sodium hydroxide - potassium permanganate is omitted and only 0.2 ml ferrous chloride solution is added. A potassium iodate standard was used in both methods. 

Hydrolysis An aliquot of the reaction mixture is quenched with saturated aqueous ammonium chloride solution eind extracted with ether, then injected on GC to verify that al the 4-bromobenzonifrile has been consumed, lodolysis An aliquot of the reaction mixture is added to a dry vial containing iodine after 10 min ether is added and the ethereal solution is washed with an aqueous solution of sodium thiosulfate. The organic phase is injected on... 

The halogen fluorides are usually regarded as normal covalent hquids, in spite of the fact that the iodine chlorides and iodine bromide conduct electricity both in the molten state and in solution (2). 

In the ion-exchange method, brine solution is passed through an anion-exchange resin. Iodide (and polyiodide) anions from the solution adsorb onto the resin from which they are desorbed by treatment with caustic soda solution. The resin is treated with sodium chloride solution to regenerate its activity for reuse. The iodide solution (also rich in iodate, IO3 ions) is acidified with sulfuric acid. The acid solution is oxidized to precipitate out iodine. Iodine is purified by sublimation. 

B. Norcarane. In a 500-ml. round-bottomed flask fitted with a magnetic stirrer and a reflux condenser protected by a drying tube filled with Drierite are placed 46.8 g. (0.72 g. atom) of zinc-copper couple and 250 ml. of anhydrous ether. A crystal of iodine is added, and the mixture is stirred until the brown color has disappeared (Note 4). A mixture of 53.3 g. (0.65 mole) of cydohexene and 190 g. (0.71 mole) of methylene iodide is added in one portion (Note 5). The reaction mixture is then heated under gentle reflux with stirring. After 30-45 minutes, a mildly exothermic reaction occurs which may require cessation of external heating. After the exothermic reaction has subsided (approximately 30 minutes), the mixture is stirred under reflux for 15 hours. At the end of this time, most of the gray couple has been converted to finely divided copper. The ether solution is decanted (Note 6) from the copper and unreacted couple, which are then washed with two 30-ml. portions of ether. The washes are combined with the bulk of the solution and shaken with two 100-ml. portions of saturated ammonium chloride solution (Note... 

Diiodo- -nitroaniline has.been made by the action of iodine chloride on a chloroform solution 1 and also on a glacial acetic acid solution 2 of />-nitroanilinc. 

Cyanogen, Chlorine, and Bromine.—Shake 0.5 gm. of powdered iodine with 20 cc. of water, and filter. To 10 cc. of the filtrate, add, drop by drop, decinormal sodium thiosulphate solution until decolorized, then add a granule of ferrous sulphate, 1 drop of ferric chloride solution and 2 cc. of sodium hydroxide solution. Warm to about 60° C., and add 10 cc. of hydrochloric acid. The liquid should not acquire a blue color. Filter, and to 10 cc. of the filtrate add 1 cc. of ammonia water, 5 drops of silver nitrate solution, and again filter. On adding to the filtrate 2 cc. of nitric acid no precipitate, and not more than an opalescent turbidity, should develop. ... 

Carbonates, Sulphates, and Sulphites.—To a solution of 3 gm. of sodium thiosulphate in 50 cc. of water, add deci-normal iodine solution (about 120 cc.) until the liquid has a slight yellow color on now adding barium chloride solution, no turbidity should ensue. 

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