Separation citric acid

Citric Acid Separation. Citric acid [77-92-9] and other organic acids can be recovered from fermentation broths usiag the UOP Sorbex technology (90—92). The conventional means of recovering citric acid is by a lime and sulfuric acid process ia which the citric acid is first precipitated as a calcium salt and then reacidulated with sulfuric acid. However, this process generates significant by-products and thus can become iaefficient. 

The lanthanides form many compounds with organic ligands. Some of these compounds ate water-soluble, others oil-soluble. Water-soluble compounds have been used extensively for rare-earth separation by ion exchange (qv), for example, complexes form with citric acid, ethylenediaminetetraacetic acid (EDTA), and hydroxyethylethylenediaminetriacetic acid (HEEDTA) (see Chelating agents). The complex formation is pH-dependent. Oil-soluble compounds ate used extensively in the industrial separation of rate earths by tiquid—tiquid extraction. The preferred extractants ate catboxyhc acids, otganophosphoms acids and esters, and tetraaLkylammonium salts. 

Recovery. Citric acid fermentation broth is generally separated from the biomass using filtration or centrifugation. The citric acid is usually... 

Lime-Sulfuric. Recovery of citric acid by calcium salt precipitation is shown in Figure 3. Although the chemistry is straightforward, the engineering principles, separation techniques, and unit operations employed result in a complex commercial process. The fermentation broth, which has been separated from the insoluble biomass, is treated with a calcium hydroxide (lime) slurry to precipitate calcium citrate. After sufficient reaction time, the calcium citrate slurry is filtered and the filter cake washed free of soluble impurities. The clean calcium citrate cake is reslurried and acidified with sulfuric acid, converting the calcium citrate to soluble citric acid and insoluble calcium sulfate. Both the calcium citrate and calcium sulfate reactions are generally performed in agitated reaction vessels made of 316 stainless steel and filtered on commercially available filtration equipment. 

B. Di-tert-butyl dicarbonate. A solution of 20.0 g. (0.076 mole) of di-i-butyl tricarbonate in 75 ml. of carbon tetrachloride is placed in a 600-ml. beaker fitted with a magnetic stirrer, and 0.10 g. (0.0009 mole) of freshly sublimed l,4-diazabicyclo[2.2.2]octane (DABCO) is added (Note 9). Rapid evolution of carbon dioxide begins at once. The reaction mixture is stirred at 25° for 45 minutes to complete the loss of carbon dioxide (Note 10), and then 35 ml. of water, containing sufficient citric acid to make the aqueous layer slightly acidic, is added. The layers are separated and the organic layer is dried over anhydrous magnesium sulfate and then concentrated at 25° with a rotary evaporator. The residual liquid is distilled under reduced pressure to separate 13.3-15.1 g. (80-91%) of di-butyl dicarbonate as a colorless liquid, b.p. 55-56° (0.15 mm.) or 62-65° (0.4 mm.) n T> 1.4071-1.4072 (Note 11). 

Fig. 1 Separation of carboxylic acids (schematic representation). Citric acid (1), lactic acid (2), phthalic acid (3), sebacinic acid (4), salicylic acid (5), mixture (M).

The copper complex is very stable at neutral pH, but it fades very rapidly in the presence of hydrogen ions. Other complex formers such as tartaric acid or citric acid and thiourea interfere with the reaction and, therefore, should not be included in mobile phases used for the separation of amino acids [3]. 

To this solution there is added in about 20 minutes a solution of diethylamine in CHCI3 while the temperature is kept below 35°C. The reacting mixture is heated to boiling, water formed during the reaction being distilled off thereby. After two hours the distillate contains no more water and the reaction is finished. Water is added to dissolve diethylamine hydrochloride formed during the reaction, and the chloroform layer containing the product is separated from the aqueous layer. The product may be purified by distillation it boils at 132°C at 0.2 mm pressure. It is converted to the citrate by reaction with citric acid. 

Procedure. Dissolve 0.0393 g of pure copper(II) sulphate pentahydrate in 1 L of water in a graduated flask. Pipette 10.0 mL of this solution (containing about 100 jug Cu) into a beaker, add 5.0 mL of 25 per cent aqueous citric acid solution, render slightly alkaline with dilute ammonia solution and boil off the excess of ammonia alternatively, adjust to pH 8.5 using a pH meter. Add 15.0mL of 4 per cent EDTA solution and cool to room temperature. Transfer to a separatory funnel, add lOmL of 0.2 per cent aqueous sodium diethyldithiocarbamate solution, and shake for 45 seconds. A yellow-brown colour develops in the solution. Pipette 20 mL of butyl acetate (ethanoate) into the funnel and shake for 30 seconds. The organic layer acquires a yellow colour. Cool, shake for 15 seconds and allow the phases to separate. Remove the lower aqueous... 

Citric acid is also highly astringent it can be used as a skin toner. Like the related compound sodium citrate, citric acid is often an ingredient in ice creams, where it helps keep the fat globules separate. 

When the distribution coefficient for the desired solute from aqueous solutions into even the best of solvents is unfavourable it may become attractive to superimpose reaction. Consider the. separation of citric acid from aqueous solutions, for which physical extraction is unattractive. Here we can use a bulky tertiary amine, e.g. tri-2-ethylhexylamine, which has a very low solubility in water, and dissolve it in a suitable, water-insoluble solvent this will... 

Citric acid (Ruthven, 1997). In the separation of citric acid from fermentation liquors the Sorbex process can be used. In the conventional process neutralization is carried out with lime followed by acidification with sulphuric acid to produce calcium sulphate as waste. The Sorbex technology avoids lime and sulphuric acid wastage and calcium sulphate disposal. 

Extraction and Separation of Alkaloids - The air-dried ground heart-wood (2.2 kg) was extracted by percolation at room temperature with alcohol USP until a negative alkaloid test of the percolate was observed. Removal of the solvent at reduced pressure and at 40° left 71 g of residue that exhibited antimicrobial activity. A 35 g sample of the alcohol-soluble residue was partitioned between 125 ml each of ether and 2Z citric acid In water. The ether layer was extracted twice more with 125 ml of 2% citric acid, filtered to remove some lnterfaclal solids (5.8 g alkaloid negative, no antimicrobial activity), dried (sodium sulfate), and evaporated to dryness, giving 8.6 g of ether solubles that had no antimicrobial activity. 

A high performance capillary electrophoresis (HPCE) was described for the separation and simultaneous determination of OTC, TC, CTC, DC, and chloramphenicol in honey. The use of buffer pH 3.2 containing 0.02 mol/L Na2HP04 and 0.01 mol/L citric acid with addition of 4% (v/v) A-methylmorpholine and 12% (v/v) acetonitrile demonstrated a good separation of these five antibiotics within 20 min. The proposed method gave detection limit (signal to noise ratio > 5) of 20 pg/L for OTC [26],... 

Citric acid and nitriloacetic acid (NTA) lanthanide complexes were used in the earliest ion exchange separations of lanthanides from fission product mixtures (Kf = 3.2 for Ce(H3 Cit.)3 and Kf = 10.8 for CeNTA2) (Sillen and Martell, 1964). More recently such polyamino-polycarboxylic acids as ethylenediaminetetraacetic acid (EDTA), 1,2-diaminocyclohexaneacetic acid (DCTA), and diethylenetriaminepentaacetic acid (DTPA) have been prepared. Their lanthanide complexes are very stable (Table 3) and have been widely used in analysis and separation of lanthanide mixtures. They have also been used experimentally to remove internally-deposited 144Ce and other radioactive lanthanide nuclides from animals and man (Foreman and Finnegan, 1957 Catsch, 1962 Balabukha et al., 1966 Palmer et al., 1968 among others). 

Multivalent cations (antacids, iron, sucralfate, zinc, vitamins, dairy, citric acid) didanosine Decreased absorption of quinolone Separate by 2 hours... 

Chen et al. (1997a) analysed sodium saccharin in soft drinks, orange juice and lemon tea after filtration by injection into an ion-exclusion column with detection at 202 nm. Recoveries of 98-104% were obtained. They reported that common organic acids like citric and malic and other sweeteners did not interfere. Qu et al. (1999) determined aspartame in fruit juices, after degassing and dilution in water, by IC-PAD. The decomposition products of aspartame, aspartic acid and phenylanaline were separated and other sweeteners did not interfere. The recoveries of added aspartame were 77-94%. Chen et al. (1997b) separated and determined four artificial sweeteners and citric acid. 

There is increasing interest in the use of specific sensor or biosensor detection systems with the FIA technique (Galensa, 1998). Tsafack et al. (2000) described an electrochemiluminescence-based fibre optic biosensor for choline with flow-injection analysis and Su et al. (1998) reported a flow-injection determination of sulphite in wines and fruit juices using a bulk acoustic wave impedance sensor coupled to a membrane separation technique. Prodromidis et al. (1997) also coupled a biosensor with an FIA system for analysis of citric acid in juices, fruits and sports beverages and Okawa et al. (1998) reported a procedure for the simultaneous determination of ascorbic acid and glucose in soft drinks with an electrochemical filter/biosensor FIA system. 

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