Extraction sodium acetate

Place 80 g, of hydroxylamine sulphate (or 68-5 g. of the hydrochloride), 25 g. of hydrated sodium acetate, and 100 ml. of water in a 500 ml. flask fitted with a stirrer and a reflux water-condenser, and heat the stirred solution to 55-60°. Run in 35 g (42 nil,) of -hexyl methyl ketone, and continue the heating and vigorous stirring for ij hours. (The mixture can conveniently be set aside overnight after this stage.) Extract the oily oxime from the cold mixture twice with ether. Wash the united ethereal extract once with a small quantity of water, and dry it with sodium sulphate. Then distil off the ether from the filtered extract, preferably using a distillation flask of type shown in Fig. 41 (p. 65) and of ca, 50 ml, capacity, the extract being run in as fast as the ether distils, and then fractionally distil the oxime at water-pump pressure. Collect the liquid ketoxime, b.p. 110-111713 mm. Yield, 30-32 g. 

The following are examples of the above procedure. A mixture of diethylamine and re-butyl alcohol may be separated by adding sufficient dilute sulphuric acid to neutralise the base steam distillation will remove the alcohol. The amine can be recovered by adding sodium hydroxide to the residue and repeating the distillation. A mixture of diethyl ketone and acetic acid may be treated with sufficient dilute sodium hydroxide solution to transform the acid into sodium acetate and distilling the aqueous mixture. The ketone will pass over in the steam and the non-volatile, stable salt will remain in the flask. Acidification with dilute sulphuric acid hberates acetic acid, which can be isolated by steam distillation or by extraction. 

Sodium acetate reacts with carbon dioxide in aqueous solution to produce acetic anhydride and sodium bicarbonate (49). Under suitable conditions, the sodium bicarbonate precipitates and can be removed by centrifugal separation. Presumably, the cold water solution can be extracted with an organic solvent, eg, chloroform or ethyl acetate, to furnish acetic anhydride. The half-life of aqueous acetic anhydride at 19°C is said to be no more than 1 h (2) and some other data suggests a 6 min half-life at 20°C (50). The free energy of acetic anhydride hydrolysis is given as —65.7 kJ/mol (—15.7 kcal/mol) (51) in water. In wet chloroform, an extractant for anhydride, the free energy of hydrolysis is strangely much lower, —50.0 kJ/mol (—12.0 kcal/mol) (51). Half-life of anhydride in moist chloroform maybe as much as 120 min. Ethyl acetate, chloroform, isooctane, and / -octane may have promise for extraction of acetic anhydride. Benzene extracts acetic anhydride from acetic acid—water solutions (52). 

Ash is a measure of residual sodium acetate. A simple method consists of dissolving the PVA in water, diluting to a known concentration of about 0.5 wt %, and measuring the electrical conductivity of the solution at 30°C. The amount of sodium acetate is estabUshed by comparing the result to a cahbration curve. A more lengthy method involves the extraction of the PVA with methanol using a Soxhlet extractor. The methanol is evaporated and water is added. The solution is titrated using hydrochloric acid in order to determine the amount of sodium acetate. 

Anthraquinone Blue B (Acid Blue 45, l,5-diamino-4,8-dihydroxy-9,10-anthraquinone-3,7-disulfonic acid di-Na salt) [2861-02-1] M 474.3, m >300°, Cl 63010, X.max 595nm, pKesi(1) <0, pKEst(2) 2, pKEst(3) 9. Purified by salting out three times with sodium acetate, followed by repeated extraction with EtOH [McGrew and Schneider 7 Am Chem Soc 72 2547 1950]. 

Anthraquinone Blue RXO [4403-89-8] M 445.5. Purified by salting out three times with sodium acetate, followed by repealed extraction with EtOH [McGrew and Schneider J Am Chem Soc 72 2547 1950]. 

Milling Red SWB l-[4-[4-[4-toluenesulfonyloxy]phenylazo](3,3 dimethyl-l,l -biphenyl)-4 -azo]-2-hydroxynaphthalene-6,8-disulfonic acid di-Na salt, Acid Red 114 [6459-94-5] M 830.8, m dec >250", Cl 23635, X,max 514nm. Salted out three times with sodium acetate, then repeatedly extracted with EtOH. [McGrew and Schneider J Am Chem Soc 72 2547 1950.] See Solochrome Violet R on p. 352 in Chapter 4. 

A solution of 16jS-methyl-l la,17a,21-trihydroxy-5j5-pregnane-3,20-dione 21-acetate (52), 45 g, in dioxane (297 ml) is cooled to 15° and treated over a 5 min period with a solution of bromine (34.2 g) in dioxane (594 ml) precooled to 18°. After 2 min a solution of sodium acetate (60 g) in water (600 ml) is added and the mixture poured into ice water (8 liters). The precipitate is filtered off, washed to neutrality with water, and dried to give the crude dibromide (53), 55.7 g mp 125-126° (dec.) [aJu 58°. A mixture of dibromide (53), 55.5 g, lithium bromide (27.8 g), lithium carbonate (27.8 g) and DMF (1.11 liters) is refluxed under rapid stirring for 6 hr. The mixture is concentrated under vacuum to about 250 ml, poured into ice water (8 liters) containing hydrochloric acid (250 ml), and extracted with methylene dichloride. The extracts are washed to neutrality with water and evaporated to dryness. The residue is dissolved in acetone, evaporated to dryness under reduced pressure, redissolved in acetone and crystallized by the additon of hexane. This gives the dienone (54) 24.4 g, mp 236-239°. 

Preparation of 5a,6a-0xido-17a-Hydroxya//opregnane-3,20-dione 3,20-Bis-(Ethy ene Ketal) A solution was prepared by heating 19.96 g (0.0477 mol) of 17a-hydroxyprogesterone 3,20-bis-(ethylene ketal) and 500 ml of benzene. After the solution was effected the flask was cooled to 5°C and a mixture of 3.68 g (0.0449 mol) of sodium acetate and 174 ml of 40% peracetic acid was added with stirring. The reaction mixture was stirred in the ice bath for 3 hours. The lower peracid layer was separated, diluted with water and extracted twice with benzene. 

The resulting mixture does not crystalize and is converted into a mixture of oximes by treatment of a solution of the mixture in 20 ml of ethanol with a solution of 1.8 g of hydroxylamine sulfate in 3 ml of water. 1.B g of sodium acetate In 5 ml of water is added, and the mixture is refluxed for 5 hours, then extracted with ethyl acetate, and the ethyl acetate solution is washed with a saturated aqueous sodium chloride solution and dried over Sodium sulfate. After evaporating the solvent, the residue is triturated with warm ether and 1.1 g of a crystalline oxime is obtained, MP 16B° to 171°C. 

The frozen shells were ground in a cold mortar with 50 mM sodium acetate buffer, pH 5.8, containing 10 mM EGTA and 0.2 M NaCl, then the mixture was centrifuged. The pellets were re-extracted with the same buffer, and centrifuged. All supernatants were combined, and the photoprotein was precipitated with ammonium sulfate. The photoprotein in the precipitate was purified by four steps of column chromatography at near 0°C. Due to the instability of the photoprotein, efforts were made to reduce the time required for purification. 

Baker et al, have obtained some kinetic data on the exchange reactions between the 1,10-phenanthroline, 2,2 -dipyridine and 2,2, 2"-tripyridine complexes of Co(III) and Co(ll) in both H2O and D2O solution. The isotopic method ( Co) and separations involving either extraction of Co(II) with organic solvents (n-hexanol-ether or saturated sodium acetate in n-hexanol) or precipitation of Co(III) as Co(phen)3(l3)3 were used. For the 1,10-phenanthroline system, a rate law... 

The CDTA- and NajCOj-soluble pectins were also used as test materials. Extracts were dialyzed against water and freeze-dried. They were then tested directly or after digestion with purified tomato PGl (treatment at 37 in sodium acetate, pH 4.5). 

Acetylcyclohexanone. Method A. Place a mixture of 24-6 g. of cyclohexanone (regenerated from the bisulphite compound) and 61 g. (47 5 ml.) of A.R. acetic anhydride in a 500 ml. three-necked flask, fitted with an efficient sealed stirrer, a gas inlet tube reaching to within 1-2 cm. of the surface of the liquid combined with a thermometer immersed in the liquid (compare Fig. II, 7, 12, 6), and (in the third neck) a gas outlet tube leading to an alkali or water trap (Fig. II, 8, 1). Immerse the flask in a bath of Dry Ice - acetone, stir the mixture vigorously and pass commercial boron trifluoride (via an empty wash bottle and then through 95 per cent, sulphuric acid) as fast as possible (10-20 minutes) until the mixture, kept at 0-10°, is saturated (copious evolution of white fumes when the outlet tube is disconnected from the trap). Replace the Dry Ice-acetone bath by an ice bath and pass the gas in at a slower rate to ensure maximum absorption. Stir for 3 6 hours whilst allowing the ice bath to attain room temperature slowly. Pour the reaction mixture into a solution of 136 g. of hydrated sodium acetate in 250 ml. of water, reflux for 60 minutes (or until the boron fluoride complexes are hydrolysed), cool in ice and extract with three 50 ml. portions of petroleum ether, b.p. 40-60° (1), wash the combined extracts free of acid with sodium bicarbonate solution, dry over anhydrous calcium sulphate, remove the solvent by... 

Soils in Uzbekistan have an average Co of 17 mg/kg. Total Cu in humic soils is in the range of 18-22 mg/kg, and total Zn is 83 mg/kg. In subdesert soils formed on loessial clayey loams and saline alkali soils, total Mo is 2.6-4.5 mg/kg, and Mo in some soils is as high as 8 mg/kg. Total Zn in subdesert soils varies from 60-112 mg/kg. Sodium acetate-extractable Zn in these subdesert soils is 2.1-3.2 mg/kg, accounting for 2.3-5.1% of total Zn. In saline alkali soils formed on loess and marine clays, total B content is 160 mg/kg. The exchangeable Mn in arid and semi-arid soils is 7-50 mg/kg, accounting for 0.7-7.8% of total Mn. Saline soils in the Ustyurt region contain 42-80 mg/kg of Pb. 

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