Potassium bisulfite solutions

More definite evidence for the transient existence of the un-cyclized l-(jS-aminoethyl)-3,4-benzoquinones has been obtained recently by Kodja and Bouchilloux,77 78 who noted that a transient yellow color (Amax ca. 385 mp) was occasionally observed during the enzymic oxidations of catecholamines (particularly in unbuffered systems at low temperatures). This phenomenon was probably due to the formation of the transient o-quinones. (The absorption maximum of o-benzoquinone, the effective chromophore of the open-chain quinones, is known to occur at ca. 390 mp.79) An absorption maximum at 390 mp is characteristic of the formation of the dopa-quinone chromophore during oxidation of small C -terminal tyrosine peptides in the presence of tyrosinase.37 48 Similar spectroscopic features were observed when the oxidations were carried out with lead dioxide in sulfuric acid solutions (pH> 1). If the initial oxidation was carried out for a short period of time, it was possible to regenerate the original catecholamines by reduction (e.g. with sodium bisulfite, potassium iodide, and zinc powder) and to show that the 385 mp peak disappeared.77,78 Kodja and Bouchilloux were also able to identify 2,4-dinitrophenylhydrazones of several of the intermediate non-cyclized quinones by paper chromatography and spectroscopy (Amax n weakly acid solution ca. 350 mp with a shoulder at ca. 410 mp).77,78... 

Wear eye protection, laboratory coat, and rubber gloves. Dissolve the aniline (1 mL) in 50 mL of 3 M sulfuric acid (prepared by slowly adding 8 mL of concentrated sulfuric acid to 21 mL of water). Weigh 10 g of potassium permanganate and stir small portions of the solid into the aniline solution over a period of about 1 hour. Stir the mixture at room temperature for 48 hours, and then neutralize the solution by adding solid sodium carbonate or a 10% solution of sodium hydroxide. Add solid sodium bisulfite until solution is colorless. Decant the clear liquid into the drain and discard any brown solid with regular refuse.11,12... 

Isonaphthazarin can be synthesized by adding a solution of o-phthalaldehyde in dioxane to an aqueous solution of glyoxal bisulfite, potassium cyanide, and sodium bicarbonate and stirring the solution in the presence of air at 20°. The solution rapidly acquires an intense violet color and is acidified after 15 min. (since the product is very sensitive to alkali) to precipitate bright red isonaphthazarin. 

Ammonia Solutions. It has long been suggested that ammonia solutions age quicker than sodium or potassium solutions of sulfite. We have recorded Raman spectra of three year old 1 M ammonium bisulfite solutions in sealed ampules. These contain not only a solid elemental sulfur phase and solid ammonium sulfate phase, but the liquid phase contains also several percent of dithionate, recognizable by the vibration frequencies of 710 cm- and 1206 cm-, with an intensity ratio of l7io/ -l2Q6 = 3.2. A search for other oxyacids yielded traces of thiosulfate... 

Plating solution, chrome Potassium acid sulfate Potassum alum Potassum aluminum sulfate Potassium bicarbonate Potassium bichromate Potassium bifluoride Potassium bisulfate Potassium bisulfite Potassium bitartrate Potassium bromide Potassium carbonate Potassium chlorate Potassium chloride Potassium chromates Potassium citrate Potassium cyanate Silicone tetrachloride, dry Silicone tetrachloride, wet Silver bromide Silver chloride Silver cyanide Silver nitrate Silver sulfate Soap solutions Soda ash Sodium acetate Sodium benzoate Sodium bicarbonate Sodium bichromate Sodium bifluoride Sodium bisulfate Sodium bisulfide Sodium bisulfite Sodium borate Sodium bromate Sodium bromide Sodium carbonate... 

Analytical Methods. A classical and stiU widely employed analytical method is iodimetric titration. This is suitable for determination of sodium sulfite, for example, in boiler water. Standard potassium iodate—potassium iodide solution is commonly used as the titrant with a starch or starch-substitute indicator. Sodium bisulfite occurring as an impurity in sodium sulfite can be determined by addition of hydrogen peroxide to oxidize the bisulfite to bisulfate, followed by titration with standard sodium hydroxide (279). 

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). 

It is advisable to test the solution after the addition of the sodium bisulfite with acidified potassium iodide solution to be sure that all the hypochlorite has been destroyed. If... 

After stirring the diazotized solution for 15 minutes, it is slowly poured through a glass-wool filter into a solution of 180 g. (3.4 moles) of potassium iodide in 600 ml. of water. After standing overnight, the heavy dark oil is separated, washed successively with 10% aqueous sodium hydroxide, water, 5% aqueous sodium bisulfite and water, and then dried over magnesium sulfate. 

A solution of 17-cyanoandrosta-5,16-dien-3jS-ol acetate (46 g) and anhydrous potassium acetate (0.46 g) in methylene dichloride (310 ml) is treated with a mixture of 40% peracetic acid (37 ml) and anhydrous potassium acetate (1.84 g) in methylene dichloride (46 ml), the temperature of the solution being maintained below 25°. The mixture is stored at room temperature for 4 hr and then washed successively with water, 5% sodium bicarbonate solution (aqueous sodium bisulfite, 10g/150g water, has been used to decompose excess reagent before workup) and water until neutral. Evaporation of the dried solution and addition of ether gives 24.1 g of 5oc,6a-epoxy-17-cyanoandrost-16-en-3 -ol acetate mp 187-190°. One recrystallization from methanol gives 20.4 g of oxirane melting at 191-194°. 

A solution of 4.36 g of sodium iodide in 100 ml of ethanol is added to a boiling mixture of 10 g of the tetrabromide in 1.5 liters of ethanol, and the mixture is refluxed for 1 hr. Water is added and the mixture is extracted with ether, the extract washed with dilute sodium bisulfite solution and water, and the ether evaporated. The residue is taken up in 1000 ml. of methanol and refluxed for 1 hr after the addition of a solution of 50 g. of potassium hydroxide in 50 ml. of water. Water is added and the mixture is extracted with ether, the extract washed with water and the ether evaporated. The alkaline layer is acidified and extracted with ether. The extracts are washed... 

Powdered potassium permanganate (94 mg) is added to an ice-cold, stirred solution of 0.1 g of the unsaturated nitrile in 3.5 ml of acetone containing 0.11 ml of piperidine. The reaction mixture is stirred at 0° for 1.5 hr, allowed to warm to room temperature (30 min) and then treated with 0.02 ml of acetic acid in 0.2 ml of acetone. After stirring at room temperature for an additional 1.5 hr the mixture is treated with chloroform, aqueous sodium bisulfite and sufficient 1 N sulfuric acid to reduce all of the manganese dioxide. 

A convenient laboratory route involves the reduction of an aqueous solution of nitrous acid or potassium nitrite with bisulfite under carefully... 

In a 25% aqueous solution of potassium bromide. The resultant solution is acidified with a 20% solution of sodium bisulfite, centrifuged, washed with water and then dried under vacuum. The product Is then recrystallized in acetic acid and 13.6 g of 2-(4 -hydroxy-3, 5 -di-bromo-benzoyl)-3-athyl coumarone obtained. MP 151°C. 

A solution of 11.2 g of potassium permanganate in 100 ml of warm water was added drop-wise to a well stirred solution of 10 g of 2-(4-chlorophenyl)-3-methyl-4-metathiazanone in 50 ml of glacial acetic acid. The temperature was kept below 30°C with external cooling. An aqueous sodium bisulfite solution was then added to remove the manganese dioxide. The thick whitish oil which separated was taken up in chloroform and the extract was washed with water. Removal of the chloroform by distillation in vacuo yielded an oily residue which solidified. The solid was recrystallized from isopropyl alcohol to give 5 g of the product, 2-(4-chlorophenyl)-3-methyl-4-metathiazanone-1,1-dioxide, MP 116.2° to 118.6°C (corr.). 

When the chlorination is complete, the reaction mixture is poured into 1,000 parts of water and treated with a dilute sodium bisulfite solution, until no more reaction may be observed with starch-potassium iodide paper. Thereby the 5,7-dichloro-8-hydroxy-quinaidine separates out in form of a weakly yellowish colored precipitate. The same is filtered off and thoroughly washed with water. 

To a solution of 6.36 parts of 17(3-hydroxy-17a-methyl-5o -androst-Ten-3-one in 95 parts of acetic acid and 12 parts of water is added 40 parts of lead tetracetate and 0.6 part of osmium tetroxide. This mixture is stored at room temperature for about 24 hours, then is treated with 2 parts of lead tetracetate. Evaporation to dryness at reduced pressure affords a residue, which is extracted with benzene. The benzene extract is washed with water, and extracted with aqueous potassium bicarbonate. The aqueous extract is washed with ether, acidified with dilute sulfuric acid, then extracted with ethyl acetate-benzene. This organic extract is washed with water, dried over anhydrous sodium sulfate, and concentrated to dryness in vacuo. To a solution of the residual crude product in 20 parts of pyridine is added 10 parts of 20% aqueous sodium bisulfite and the mixture is stirred for about 20 minutes at room temperature. 

The crude ester is cooled, an equal volume of benzene is added, then the free acid is neutralized by shaking with about 250 cc. of a 10 per cent solution of sodium carbonate (Note 4). The benzene solution is poured into 1300 cc. of a saturated solution of sodium bisulfite (about 60 g. of technical sodium bisulfite per 100 cc.), contained in a wide-neck bottle equipped with an efficient stirrer, and the mixture stirred for two and a half hours. The mixture soon warms up a little and becomes semi-solid. It is filtered through a 20-cm. Buchner funnel and carefully washed, first with 200 cc. of a saturated solution of sodium bisulfite, finally with two 150-cc. portions of benzene (Notes 5 and 6). The white pearly flakes of the sodium bisulfite addition product are transferred to a 3-I. round-bottom wide-neck flask equipped with a mechanical stirrer and containing 700 cc. of water, 175 cc. of concentrated sulfuric acid, and 500 cc. of benzene. The flask is heated on a steam bath under a hood, the temperature being kept at 55°, and the mixture is stirred for thirty minutes (Note 7). The solution is then poured into a separatory funnel, the benzene separated and the water layer extracted with a 200-cc. portion of benzene. The combined benzene solution is shaken with excess of 10 per cent sodium carbonate solution to remove free acid and sulfur dioxide (Note 8). The benzene is washed with a little water and then dried over anhydrous potassium carbonate (Note 9). The benzene is distilled at ordinary pressure over a free flame from a 500-cc. Claisen flask, the solution being added from a separatory funnel as fast as the benzene distils. It is advisable to distil the ester under reduced pressure although it can be done under ordinary pressure. The fraction distilling around n8°/5mm., 130710 mm., 138715 mm., 148725 mm., 155735 mm., or... 

When a few cubic centimeters of the solution no longer liberate iodine from a slightly acid potassium iodide solution, enough sodium bisulfite has been added. 

In the flask are placed 200 cc. of dioxane, 100 g. (1.02 moles) of mesityl oxide, and a solution of 4.6 moles of potassium hypochlorite in 3 1. of water (Note 1), and the stirrer is started. The mixture becomes warm immediately, and within five minutes chloroform begins to reflux. When the reaction becomes very vigorous the stirrer is stopped and the flask is cooled with running water (Note 2). The stirring is resumed as soon as feasible and is continued for three or four hours, when the temperature of the mixture will have dropped to that of the room. Sodium bisulfite (about 5 g.) is then added to react with the excess hypochlorite (Note 3). 

CONOSOX A complex flue-gas desulfurization process using potassium carbonate solution as the wet scrubbing medium. The product potassium bisulfite is converted to potassium thiosulfate and then reduced with carbon monoxide to potassium carbonate for re-use. The sulfur is recovered as hydrogen sulfide, which is converted to elemental sulfur by the Claus process. Developed by the Conoco Coal Development Company and piloted in 1986. 

The kinetics and mechanism of the ketone-bisulfite addition were studied by the use of the polarographic technique (Rao Salunke, Reaction Kinetics and Catalysis Letters 26 273, 1984).The specific rate was found to depend on pH. For an equimolar solution of bisulfite and acetone in a deaerated solution of potassium hydrogen phthalate buffer containing potassium iodide as the... 

The following alternative procedure may be used to prepare a solution of disodium hydroxylaminedisulfonate. Sodium nitrite (15 g., 0.217 mole) and 41.6 g. (0.40 mole) of sodium bisulfite are added to 250 g. of ice. With stirring, 22.5 ml. (0.40 mole) of acetic acid is added all at once and the mixture is stirred for 90 minutes in an ice hath. At the end of the stirring period the reaction solution is pH 5 and a potassium iodide-starch test is negative. A solution of 50 g. (0.47 mole) of sodium carbonate in water (total volume 250 ml.) is added. This buffered solution of disodium hydroxylaminedisulfonate may be used for electrolytic oxidation. 

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