Extraction alkaline

However, there are some drawbacks in alkali extraction  

Alkali solutions dissolve silica from the mineral matter and this silica contaminates the organic fractions separated from the extract. 

Alkali solutions dissolve protoplasmic and structural components from fresh organic tissues and these become mixed with the humified organic matter. 

Organic chelants acetyloacetone, cupferron, hydroxyquinoline Organic solvents Formic add (HCOOH) 

Source Data from Stevenson, F. J., Humus Chemistry Genesis, Composition, Reactions. 

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The solution will then contain the free acid and the hydrochloride of the base either of these may separate if sparingly soluble. If a sohd crystallises from the cold solution, filter, test with sodium bicarbonate solution compare Section 111,85, (i) and compare the m.p. with that of the original compound. If it is a hydrolysis product, examine it separately. Otherwise, render the filtrate alkahne with sodium hydroxide solution and extract the base with ether if the presence of the unchanged acyl canpound is suspected, extract the base with weak acid. Identify the base in the usual manner (see Section IV, 100). The acid will be present as the sodium salt in the alkaline extract and may be identified as described in Section IV,175. 

Step 1. Extraction and separation of the acidic components. Shake 5-10 g. of the sohd mixture (or of the residue R obtained after the removal of the solvent on a water bath) with 50 ml. of pure ether. If there is a residue (this probably belongs to Solubihty Group II or it may be a polysaccharide), separate it by filtration, preferably through a sintered glass funnel, and wash it with a Uttle ether. Shake the resulting ethereal solution in a smaU separatory funnel with 15 ml. portions of 5 per cent, aqueous sodium hydroxide solution until all the acidic components have been removed. Three portions of alkaU are usuaUy sufficient. Set aside the residual ethereal solution (Fj) for Step 2. Combine the sodium hydroxide extracts and wash the resulting mixture with 15-20 ml. of ether place the ether in the ETHER RESIDUES bottle. Render the alkaline extract acid to litmus with dilute sulphuric acid and then add excess of sohd sodium bicarbonate. 

Hemicellulose [9034-32-6] is the least utilized component of the biomass triad comprising cellulose (qv), lignin (qv), and hemiceUulose. The term was origiaated by Schulze (1) and is used here to distinguish the nonceUulosic polysaccharides of plant cell walls from those that are not part of the wall stmcture. Confusion arises because other hemicellulose definitions based on solvent extraction are often used in the Hterature (2—4). The term polyose is used in Europe to describe these nonceUulosic polysaccharides from wood, whereas hemicellulose is used to describe the alkaline extracts from commercial pulps (4). The quantity of hemicellulose in different sources varies considerably as shown in Table 1. 

Extra.ction St ige. The washing step after the chlorination stage removes the chlorine. In alkaline extraction, about 1.5—3.5% NaOH based on pulp is used. This typically amounts to about 55% of the CI2 demand used in the chlorination stage (% NaOH = 0.55 x % CI2 ). The target pH exiting the... 

The most widely available yeast biomass is a by-product of the brewing industry, where the multiplication of yeast during brewing results in a surplus of ceUs. Eor every barrel (117 L) of beer brewed, 0.2—0.3 kg of yeast soHds may be recovered. In the U.S., a substantial fraction is recovered and made available about 40 x 10 kg of brewers yeast aimually. The yeast is recovered from beer by centrifuging and dried on roUer dmms or spray dryers and sold as animal feed or a pet-food supplement. It can be debittered by alkaline extraction to remove the bitter hop residues, and is then sold mainly by the health-food industry. It is available as tablets, powder, or flakes and is often fortified with additional vitamins. Distillers yeast caimot be readily separated from the fermented mash and the mixture is sold as an animal feed supplement. 

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. 

Further Preparative Reactions. When pulps are to be used in the production of materials that do not retain the original fiber stmcture, such as rayon or ceUulose acetate film, the lignin, hemiceUulose, and other components must be reduced to the lowest possible concentrations. A surfactant (ionic or nonionic) is often added during a hot, weakly alkaline extraction step after chlorination. Another approach, sometimes used in addition to the surfactant step, is to treat the pulp with 6—10% NaOH after most of the oxidative bleaching is finished. This treatment removes most of the hemiceUulose. In most purification plants the final stage includes use of sulfuric acid chelators are optional. 

The colorant is prepared by leaching the annatto seeds with an extractant prepared from one or more approved, food-grade materials taken from a hst that includes various solvents, edible vegetable oils and fats, and alkaline aqueous and alcohoHc solutions (46,47). Depending on the use intended, the alkaline extracts are often treated with food-grade acids to precipitate the annatto pigments, which ia turn may or may not be further purified by recrystallization from an approved solvent. Annatto extract is one of the oldest known dyes, used siace antiquity for the coloring of food, textiles, and cosmetics. It has been used ia the United States and Europe for over 100 years as a color additive for butter and cheese (48—50). 

Benzene-1,2-dithiol [17534-15-5] M 142.2, m 24-25 , 27-28 , b 110-112 , pKEst(i) -6.0, p K s,(2) 9.4. Likely impurities are the oxidation products, the disulfides which could be polymeric. Dissolve in aq NaOH until the soln is alkaline. Extract with Et20 and discard the extract. Acidify with cold HCl (diluted 1 1 by vol with H2O) to Congo Red paper under N2 and extract three times with Et20. Dry the Et20 with Na2S04, filter, evaporate and distil residue under reduced press in an atmosphere of N2. The distillate solidifies on cooling. [UV J Chem Soc 3076 7 955 J Am Chem Soc 81 4939 7957 Org Synth Coll Vol V 419 1973.]... 

Aminocephalosporanic acid (5.00 g) which passed through a 100-mesh sieve was suspended in boiling ethyl acetate (200 ml), and 2-thienylacetyl chloride (Cagniant, Bull. Soc. Chim. France, 1949,847) (4.42 g, 1.5 equiv.) was added in ethyl acetate (20 ml). The mixture was boiled under reflux for 40 minutes, cooled, and filtered. Aniline (5.03 ml) was added, and after 1 hour the mixture was extracted with 3% sodium hydrogen carbonate solution (1 x 150 ml, 2 X 100 ml, 1 x 50 ml) and the alkaline extracts washed with ethyl acetate (3 x 100 ml). The aqueous solution was acidified to pH 1.2, and extracted with ethyl acetate (2 x 150 ml). The ethyl acetate extract was washed with water (4 x 40 ml), dried (MgS04), and concentrated in vacuo to low volume. The crude 7-2 -thienylacetamidocephalosporanic acid (2.5 g) which separated was collected by filtration. Evaporation of the filtrate gave a further 2.68 g (71%) of the product, which was purified by crystallization from ethyl acetate, then aqueous acetone, MP 150°Cto 157°C (decomp.). 

When addition is complete the mixture is heated under reflux during 5 hours and then the acetone is removed by distillation. The residue is dissolved in water, acidified with hydrochloric acid and the mixture extracted with chloroform. The chloroform extract is stirred with sodium hydrogen carbonate solution and the aqueous layer is separated. The alkaline extract is acidified with hydrochloric acid and filtered. The solid product is drained free from oil on a filter pump, then washed with petroleum ether (BP 40° to 60°C), and dried at 50°C. The solid residue, MP 114° to 116°C, may be crystallized from methanol (with the addition of charcoal) to give p-chlorophenoxyisobutyric acid, MP 118° to 119°C. 

A slight excess of mineral acid, such as sulfuric or hydrochloric acid is added to acidify the mixture which is then chilled and the solid which separates is filtered off. It is then treated with an aqueous solution of dilute sodium hydroxide to dissolve the hydantoin from the solid unreacted benzophenone. After filtration, the alkaline extract is then acidified to cause the separation of solid pure diphenylhydantoin which is filtered off and dried. It melts at 293° to 296°C. 

B. exo-cis-Bicyclo[3.3.0]octane-2-carboxylic acid. A mixture of 100 g. (0.440 mole) of 2-(trichloromethyl)bicyclo[3.3.0]octane and 500 ml. of 85% phosphoric acid is put into a 1-1. three-necked flask equipped with a mechanical stirrer, a reflux condenser, and a thermometer. The mixture is stirred and heated at 150° for 16 hours, during which time it evolves hydrogen chloride and darkens. The product is then allowed to cool and is poured into a separatory funnel. One liter of water is added and the resulting mixture is extracted with four 250-ml. portions of ether. The combined ether extract is then extracted with four 250-ml. portions of 2% aqueous sodium hydroxide (Note 9), and the resulting alkaline extract is washed with 100 ml. of ether to remove any neutral material (Note 10). The alkaline extract is acidified (to pH 2-3) with concentrated hydrochloric acid, and the oil which precipitates is extracted with three 250-ml. portions of ether. The resulting ether extract is dried with 15 g. of magnesium sulfate, filtered, and evaporated at 50° (30 mm.). The residue is then distilled at reduced pressure to obtain 29-32 g. 

The aqueous alkaline extract is heated to ioo° to remove ether and volatile impurities. The solution is then cooled with ice and acidified with 25 per cent sulfuric acid, and the organic acid separated. The water layer is distilled from a 2-1. flask until no more oily solution comes over, The distillate is saturated with salt and the acid layer is separated. This water layer together with the low boiling fraction from distillation of the crude trimethylacetic acid is distilled and the distillate salted out as before. 

Tribromophenol may be recovered by acidification of the aqueous alkaline extracts and can be reapplied in the preparation of the tetrabromo-compound after crystallization from petroleum ether (b.p. 80-100°). 

Thermoplastic xylan derivatives have been prepared by in-hne modification with propylene oxide of the xylan present in the alkaline extract of barley husks [424,425]. Following peracetylation of the hydroxypropylated xylan in formamide solution yielded the water-insoluble acetoxypropyl xylan. The thermal properties of the derivative quahfy this material as a potential biodegradable and thermoplastic additive to melt-processed plastics. Xylan from oat spelts was oxidized to 2,3-dicarboxyhc derivatives in a two-step procedure using HI04/NaC102 as oxidants [426]. 

The most common method to extract xylan is the alkaline extraction. Several pretreatment methods can be used in association in order to break the covalent bonds that exist between xylan and other carbohydrates during the extraction (Wang Zhang, 2006). A number of articles studied the use of ultrasound on the xylan extraction. Hromadkova and coworkers reported that 36.1% of xylan was extracted from corn cobs with 5% NaOH solution at 60°C for 10 min of ultrasonication in comparison with 31.5% of xylan in the classical extraction. Both extractive methods yielded xylan with immunogenic properties (Hromadkova et al., 1999). 

The efficiency of extraction was observed to be inversely proportional to the corn cob particle size. This was expected because the size reduction corresponds to an increase in total particle surface area. An increase in the time of the alkaline extraction and in the NaOH concentration also improves the efficiency of xylan extraction. This happened because when the NaOH concentration was lower, the xylan present in corn cobs could not be fully dissolved in the solution. Thus, it resulted in lower efficiency of xylan extraction. However, when the NaOH concentration was higher than 2 M, the yields decreased with continuously increasing of the NaOH concentration. This is probably due to the alkaline degradation of xylan chains, proceeding at the higher NaOH concentration, which indicated that the ideal NaOH concentration in the extraction was between 1.5 and 1.8 M (Unpublished data). 

Similarly, after a longer time of incubation, no significant changes in the cell proliferation rate was detected, as can be seen in the data for 72 h (Figure 13). In fact, this was expected due to the biocompatible nature of xylan. As a natural polyssacharide, this type of biomaterial is considered to be highly stable, non-toxic and hydrophilic (Liu et al., 2008). Accordingly, the alkaline extraction of xylan from corn has proved to be a safe approach for obtaining the polymer with no relevant toxicity (Unpublished data). 

NaOH in ihe presence of NaBH4 for 6 h at room temperature. The alkaline extraction was repeated twice and the supernatant combined the NaOH extract acidified to pH 5 with 50 % acetic acid, exhaustively dialyzed, polysaccharide precipitated with EtOH (2 vol.) and washed with EtOH and Me2CO. 

Table IV. Yield and monosacharide composition of Fractions obtained by aqueous and alkaline extractions.

Experiments examined a chlorocatechol-contaminated sediment, and interstitial water prepared from it. These showed that the concentrations of total 3,4,5-tri- and tetrachloro-catechols (i.e., including the fraction that is released only after alkaline extraction) were apparently unaltered during prolonged incubation even after addition of cnltnres with established dechlorinating capability for the soluble chlorocatechols (Allard et al. 1994). 

The recovery is low on extracting n from soil by refluxing with water containing methanol. Metabolite n in soil can be extracted by sonication with alkaline methanol. Using this alkaline extraction procedure, another metabolite, 2-chlorobenzylsulfonic acid, is also extracted simultaneously. ... 

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