Extraction with Water

1 This extraction is meant for the determination of chloride (Cl), nitrite-nitrogen (NOj), nitrate-nitrogen (NO3) and sulphate-sulphur (SO/). 

1 The anions that are free in the plant material are extracted as such by water. 

Dried plant material may easily stick to glass when the relative humidity of the air is low. These 

1 Weigh, to the nearest 0.001 g, approximately 0.5 g of the dried plant material sample in a metal weighing funnel and transfer the sample to a 50-mL erlenmeyer flask. Add 25 ml water and shake for 30 min at room temperature. Filter over fine paper (4.1). 

Collect the filtrate and filter this very portion of filtrate again over the same piece of paper. Use the last filtrate for analysis. 

Glycosides may also be extracted with water. The extract is carefully concentrated to a syrupy consistency and then taken up in alcohol. The precipitate formed can often be discarded. 

Other suitable concentration procedures are liquid/liquid partition of the extracts, e. g., between water and ether or benzene and formamide. Precipitation with lead and, recently with success, column chromatography on polyamide [60, 171] can be used for purification. 

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Tin(IV) oxide is insoluble in water, but if fused with sodium hydroxide and the mass extracted with water, sodium hexahydroxo-stannate(IV) is formed in solution ... 

This reaction is also used on a large scale, to obtain iodine from seaweed. The ash from burnt seaweed ( kelp ) is extracted with water, concentrated, and the salts other than iodides (sulphates and chlorides) crystallise out. The more soluble iodides remain and the liquor is mixed with sulphuric acid and manganese dioxide added the evolved iodine distils off and is condensed. 

The green manganate(VI) is extracted with water, then oxidised to manganatefVII). This is usually carried out electrolytically. at an anode, but in the laboratory chlorine may be used ... 

When an organic compound is heated with a mixture of zinc powder and sodium carbonate, the nitrogen and halogens are converted into sodium cyanide and sodium hahdes respectively, and the sulphur into zinc sulphide (insoluble in water). The sodium cyanide and sodium hahdes are extracted with water and detected as in Lassaigne s method, whilst the zinc sulphide in the residue is decomposed with dilute acid and the hydrogen sulphide is identified with sodium plumbite or lead acetate paper. The test for nitrogen is thus not affected by the presence of sulphur this constitutes an advantage of the method. 

Sodium bismuthate (oxidation of manganese) heat 20 parts of NaOH nearly to redness in an iron or nickel crucible, and add slowly 10 parts of basic bismuth nitrate which has been previously dried. Add 2 parts of sodium peroxide, and pour the brownish-yellow fused mass on an iron plate to cool. When cold break up in a mortar, extract with water, and collect on an asbestos filter. 

When PET is extracted with water no detectable quantities of ethylene glycol or terephthaUc acid can be found, even at elevated extraction temperatures (110). Extractable materials are generally short-chained polyesters and aldehydes (110). Aldehydes occur naturally iu foods such as fmits and are produced metabohcaHy iu the body. Animal feeding studies with extractable materials show no adverse health effects. 

The methyl a-hydroxyisobutyrate produced is dehydrated to MMA and water in two stages. First, the methyl a-hydroxyisobutyrate is vaporized and passed over a modified zeoHte catalyst at ca 240°C. A second reactor containing phosphoric acid is operated at ca 150°C to promote esterification of any methacrylic acid (MAA) formed in the first reactor (74,75). Methanol is co-fed to improve selectivity in each stage. Conversions of methyl a-hydroxyisobutyrate are greater than 99%, with selectivities to MMA near 96%. The reactor effluent is extracted with water to remove methanol and yield cmde MMA. This process has not yet been used on a commercial scale. 

Use of excess sodium drives the reaction, usually done under an argon or helium blanket, to completion. After cooling, the excess sodium is leached with alcohol and the sodium and potassium fluorides are extracted with water, leaving a mass of metal powder. The metal powder is leached with hydrochloric acid to remove iron contamination from the cmcible. 

After epoxidation a distillation is performed to remove the propylene, propylene oxide, and a portion of the TBHP and TBA overhead. The bottoms of the distillation contains TBA, TBHP, some impurities such as formic and acetic acid, and the catalyst residue. Concentration of this catalyst residue for recycle or disposal is accompHshed by evaporation of the majority of the TBA and other organics (141,143,144), addition of various compounds to yield a metal precipitate that is filtered from the organics (145—148), or Hquid extraction with water (149). Low (<500 ppm) levels of soluble catalyst can be removed by adsorption on soHd magnesium siUcate (150). The recovered catalyst can be treated for recycle to the epoxidation reaction (151). 

Stannous Sulfate. Stannous sulfate (tin(Il) sulfate), mol wt 214.75, SnSO, is a white crystalline powder which decomposes above 360°C. Because of internal redox reactions and a residue of acid moisture, the commercial product tends to discolor and degrade at ca 60°C. It is soluble in concentrated sulfuric acid and in water (330 g/L at 25°C). The solubihty in sulfuric acid solutions decreases as the concentration of free sulfuric acid increases. Stannous sulfate can be prepared from the reaction of excess sulfuric acid (specific gravity 1.53) and granulated tin for several days at 100°C until the reaction has ceased. Stannous sulfate is extracted with water and the aqueous solution evaporates in vacuo. Methanol is used to remove excess acid. It is also prepared by reaction of stannous oxide and sulfuric acid and by the direct electrolysis of high grade tin metal in sulfuric acid solutions of moderate strength in cells with anion-exchange membranes (36). 

Some hemicelluloses are partiaUy extractable with water, but they are usuaUy extracted with alkaline solutions foUowing removal of Upids and lignin. DeUgnifted plant material is termed, holoceUulose. Neutralization of the alkaline extract effects precipitation of the more linear and less acidic hemicelluloses, termed the hemiceUulose A [63100-39-0] fraction. The more acidic and more branched material, termed hemiceUulose B [63100-40-3], is precipitated with ethanol (70%). HemiceUulose B types type are usuaUy water-soluble after extraction. 

N-(4 Methoxyphenyl)-N-benzoyl-3-chloro-3-chloroantranlllc acid (4) 2 To ice cooled NaoEt (Irom 0 11 g Na and 10 mL ElOH) was added in rapid succession meltiyl 2 chloro 6 hydroxybenzoate 2 (0 86 g 4 7 mmol) and N (4 methoxyphenyl)benzimidyl chloride 1 (t 14 g 4 7 mmol) in EI2O (30 mL) The mixture was stirred vigorously and allowed to stand at rt tor 48 h The oily solid obtained alter evaporation was heated to 210 215°C lor 70 min under N2 The product was diluted with water (5 4 mL) ElOH (10 8 mL) and treated with 1 M NaOEt (5 4 mL) The mixture was relluxed lor 90 mm the solvent evaporated and the aqueous solution acldilied The dark oil was heated with NaOH (7 5 g) m EtOH (22 mL) Alter removal ol benzoic acid by exhaustive extraction with water the product was recrystallized Irom EtOH to give 0 36 g ol 4 (27 7%), mp 139 5 140 5°C... 

Sodium anthraquinone-l,5-disulfonate (HjO) [853-35-0] M 412.3. Separated from insoluble impurities by continuous extraction with water. Crystd twice from hot water and dried under vacuum. 

The identification of camphene is best carried out by its conversion into isobomeol under the influence of acetic acid in the presence of sulphuric acid. In order to effect this conversion, 100 grams of the fraction containing the terpene in substantial quantity are mixed with 250 grains of glacial acetic acid and 10 grams of 50 per cent, sulphuric acid. Tne mixture is heated for two to three hours on a water-bath to a temperature of 50° to 60°. At first the liquid separates into two layers, bat soon becomes homogeneous and takes on a pale red colour. Excess of water is added, and the oil which is precipitated, and which contains the isobomeol in the form of its acetate, is well washed with water repeatedly. It is then saponified by heating with alcoholic potash solution on a water-bath. The liquid is then evaporated and extracted with water, and the residue recrystallised from petroleum ether. 

It was dissolved in ethyl acetate (700 ml) and hydrogenated at ambient conditions over a palladium (5%) on carbon catalyst (18 g). The catalyst was removed by filtration and washed with ethyl acetate. The combined filtrates were extracted with water at pH 2.5 by addition of dilute hydrochloric acid. Lyophilization of the aqueous phase gave the hydrochloride of r-ethoxycarbonyloxyethyl 6-(D-a-aminophenylacetamido)penioillinate (94 g), MP... 

A stirred mixture of 11 g of 6-chloro-a-methylcarbazole-2-acetic acid ethyl ester, 100 ml ethanol and 100 ml of 3N sodium hydroxide was heated (N2 atmosphere). After 2 hours at reflux, the reaction mixture was concentrated to dryness under reduced pressure. Water (300 ml) and ice (200 g) were added to the residue and concentrated hydrochloric acid was added until the mixture was strongly acid. The acidic mixture was extracted with ether (3 X 200 ml). The ether extracts were combined, washed by extraction with water (3 x 100 ml) and dried over anhydrous magnesium sulfate. Following filtration of the desiccant and evaporation of the solvent, a yield of 9.8 g (98.2%) was obtained. Crystallization from CHCI3 yielded 6.2 g (62.0%) of 6-chloro-0 -methylcarbazole-2-acetic acid, MP 197°-198°C. A second crop of 1.6g,MP 195°-199°C was obtained from the mother liquors. 

Prepares solution of sodium methylate by dissolving 3.9 g of sodium metal in 500 ml of methanol. Add 39.0 g of 7-chloro-1,3-dihydro-5-phenyl-2H-1,4-benzodiazeplne-2-one. Evaporate the reaction mixture to a residue and dissolve the residue in 170 ml of dimethylformamide. Add 30 g of 2,2,2-trifluoroethyl Iodide and stir at room temperature for Vi hour, then heat to 60°C to 70°C for an additional 7 hours. Add 19 g of 2,2,2-trifluoroethyl iodide and resume the heating and stirring at 60°C to 70°C for an additional 16 hours. Filter off the solids and evaporate the filtrate to a residue in vacuo. Triturate the residue with water and extract with ethyl ether. Wash the ethereal extract with water, dry over anhydrous sodium sulfate and evaporate the solvent to a residue. 

The mixture is then slowly heated to the boiling point of toluene and kept boiling for one hour under reflux. After the mixture has been allowed to cool the sodium chloride which precipitates is separated by extraction with water. The solution of toluene is then extracted with dilute hydrochloric acid. From the hydrochloric acid extract the basic substance is separated in the form of an oil by means of caustic soda solution and is introduced into ether. The ethereal solution Is dried with the aid of potassium carbonate and then distilled. 

Sodium (9.6 parts) was dissolved in butanol (192 parts) and di-n-butyl ethyl 1 -methyl-n-butylmalonate (62,B parts) and urea (14.4 parts) were added to the warm solution with agitation. The mixture was then heated to reflux temperature in three quarters of an hour and maintained for 2 hours. The reaction mass was kept, water (150 parts) added, the aqueous portion separated, and the butanol layer extracted with water (3 x 50 parts). The combined aqueous extracts were then given 3 small extractions with benzene, the aqueous liquors separated, charcoaled,filtered and precipitated with concentrated hydrochloric acid (acid to congo-paper). The solid was collected, washed with water, dissolved in N-sodium hydroxide and reprecipitated with carbon dioxide. On recrystallization, from aqueous alcohol, the pentobarbitone was obtained. 

The dried dimethyleminoethyl chloride solution is poured into the toluene solution of the sodium salt of o-benzylphenol, heated to reflux, end refluxed 16 hours. After refluxing, enough water is added to the mixture to dissolve the precipitated solid. The layers ere separated, end the toluene layer is further washed with water until the water extract is just slightly elkeline. The toluene solution is then mede acid with 6N hydrochloric acid end extracted with water until no cloudiness is produced when the extract is mede elkeline. The acidic aqueous extract is washed with ether, then mede elkeline with 20% sodium hydroxide solution, end extracted into ether. The ether solution is washed several times with water, then with saturated salt solution, end is dried over anhydrous potassium carbonate. The dried solution Is filtered end distilled. The product distills at 143.5°C/1 mm 69.7 g of pale yellow oil ere recovered. 

Bj Pivaloyloxymethyl D(—)-Ot-aminobenzylpenicillinate. hydrochloride To a solution of pivaloyloxymethyl D(—)-a-azidobenzylpenicillinate (prepared as described above) in ethyl acetate (75 ml) a 0.2 M phosphate buffer (pH 2.2) (75 ml) and 10% palladium on carbon catalyst (4 g) were added, and the mixture was shaken in a hydrogen atmosphere for 2 hours at room temperature. The catalyst was filtered off, washed with ethyl acetate (25 ml) and phosphate buffer (25 ml), and the phases of the filtrate were separated. The aqueous phase was washed with ether, neutralized (pH 6.5 to 7.0) with aqueoussodium bicarbonate, and extracted with ethyl acetate (2 X 75 ml). To the combined extracts, water (75 ml) was added, and the pH adjusted to 25 with 1 N hydrochloric acid. The aqueous layer was separated, the organic phase extracted with water (25 ml), and the combined extracts were washed with ether, and freeze-dried. The desired compound was obtained as a colorless, amorphous powder. 

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