Precipitation and Concentration

Thou must take notice, brother Sancho, that this adventure and those like it are not adventures of islands, but of cross-roads, in which nothing is got except a broken head or an ear the less. 

Protein is precipitated to get rid of ions or agents that interfere with the protein determination or gel electrophoresis, and/or to concentrate the protein. The method of choice for samples less than 500 J,1 is the chloroform/methanol precipitation. However, the native conformation of the proteins gets lost. 

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Factors that affect the growth of protein crystals also affect the growth of protein-DNA cocrystals. These factors include the nature of the buffering system, pH, ionic strength, temperature, concentration and nature of precipitant, and concentration of the complex (McPherson, 1990). Examples of crystallization... 

Toxins and a large group of compounds (e.g. quaternary ammonium bases and dioxins) that require special isolation techniques, using ion pairs or ion exchange resins, formation of derivatives, continuous extraction, precipitation and concentration... 

As the L/S ratio remains high, a concentration stage must be kept in the purification process. Evaporation is an expensive step that may be replaced by membrane filtration. Ultrafiltration was therefore investigated for its capability to achieve purification (in the same way as the alcohol precipitation) and concentration at the same time. Ultrafiltration was tested using differents membranes with an MWCO ranging from 1 to 50 kDa in order to obtain a minimum concentration ratio (CR) of 2 with a minimal organic matter loss. 

Precipitate and concentrate PCR products as follows (a number of kits are available for purifying PCR products in 96-well format however, we have exclusively used isopropanol precipitation) ... 

Catalyst 1 Kneading and evaporation Catalyst 2 Precipitation and concentration Catalyst 3 Coprecipitation and filtration Commercial ... 

In all the above methods, the sulphur dioxide obtained is impure. Dust is removed by first allowing the gases to expand, when some dust settles, then by passage through electrostatic precipitators and finally by washing with water. Water is removed by concentrated sulphuric acid which is kept in use until its concentration falls to 94%. 

Anhydrous cupric sulphate is white but forms a blue hydrate and a blue aqueous solution. The solution turns yellow when treated with concentrated hydrochloric acid, dark blue with ammonia, and gives a white precipitate and brown solution when treated with potassium iodide. A yellow-brown aqueous solution of ferric chloride becomes paler on acidification with sulphuric or nitric... 

Hydrolyse the 5 g. of 3-indoleacetamide by heating it under reflux for 4 hours with a solution of 6 g. of sodium hydroxide in 40 ml. of water. Cool to 5°, treat with decolourising carbon (if necessary), filter, render strongly acid with concentrated hydrochloric acid (pH about 1 5). Collect the acid which precipitates and dry it at 70° the crude acid weighs 4 5 g. Purify as above. 

Place 2 ml. of the periodic acid reagent in a small test tube, add one drop (no more—otherwise the silver iodate, if formed, will fail to precipitate) of concentrated nitric acid, and shake well. Add one drop or a small crystal of the compound to be tested, shake the mixture for 15-20 seconds, and then add 1-2 drops of 3 per cent, silver nitrate solution. The instantaneous formation of a white precipitate of silver iodate is a positive test. Failure to form a precipitate, or the appearance of a brown precipitate which redissolves on shaking, constitutes a negative test. 

A mixture of 0.10 mol of the acetylenic alcohol, 0.12 mol of triethylamine and 200 ml of dichloromethane (note 1) was cooled to -50°C. Methanesulfinyl chloride (0.12 mol) (for its preparation from CH3SSCH3, (08300)30 and chlorine, see Ref. 73) was added in 10 min at -40 to -50°0. A white precipitate was formed immediately. After the addition the cooling bath was removed and the temperature was allowed to rise to -20°0, then the mixture was vigorously shaken or stirred with 100 ml of water. The lower layer was separated off and the aqueous layer was extracted twice with 10-ml portions of CH2CI2. The combined solutions were dried over magnesium sulfate and concentrated in a water-pump vacuum (note 2). The yields of the products, which are pure enough (usually 96%) for further conversions, are normally almost quantitative. 

Diethyl oxalate (29.2 g, 0.20mol) and 4-bromo-2-nitrotoluene (21.6 g, O.lOmol) were added to a cooled solution of sodium cthoxide prepared from sodium (4.6 g, 0.20 mol) and ethanol (90 ml). The mixture was stirred overnight and then refluxed for 10 min. Water (30 ml) was added and the solution refluxed for 2h to effect hydrolysis of the pyruvate ester. The solution was cooled and concentrated in vacuo. The precipitate was washed with ether and dried. The salt was dissolved in water (300 ml) and acidified with cone. HCl. The precipitate was collected, washed with water, dried and recrystallizcd from hexane-EtOAc to give 15.2 g of product. 

A mixture of l-(r-Boc)indol-2-yl-tri- -butylstannanc (1.2 mmol) and 4-bromo-benzonitrile (1.0 mmol) and Pd(PPh3)2C , (0.02 mmol) in dry dioxane (5 ml) was heated at I00°C overnight under nitrogen. The reaction mixture was cooled, diluted with EtOAc and stirred for 15 min with 15% aq. KF. The precipitate was removed by filtration and washed with EtOAc. The EtOAc layer was separated, washed with brine, dried (Na2S04) and concentrated. The residue was purified by chromatography on silica. The yield was 66%. 

Most metals will precipitate as the hydroxide in the presence of concentrated NaOH. Metals forming amphoteric hydroxides, however, remain soluble in concentrated NaOH due to the formation of higher-order hydroxo-complexes. For example, Zn and AP will not precipitate in concentrated NaOH due to the formation of Zn(OH)3 and Al(OH)4. The solubility of AP in concentrated NaOH is used to isolate aluminum from impure bauxite, an ore of AI2O3. The ore is powdered and placed in a solution of concentrated NaOH where the AI2O3 dissolves to form A1(0H)4T Other oxides that may be present in the ore, such as Fe203 and Si02, remain insoluble. After filtering, the filtrate is acidified to recover the aluminum as a precipitate of Al(OH)3. 

Besides pH, other preparative variables that can affect the microstructure of a gel, and consequendy, the properties of the dried and heat-treated product iaclude water content, solvent, precursor type and concentration, and temperature (9). Of these, water content has been studied most extensively because of its large effect on gelation and its relative ease of use as a preparative variable. In general, too Httie water (less than one mole per mole of metal alkoxide) prevents gelation and too much (more than the stoichiometric amount) leads to precipitation (3,9). Other than the amount of water used, the rate at which it is added offers another level of control over gel characteristics. 

Catalyst recovery is a major operational problem because rhodium is a cosdy noble metal and every trace must be recovered for an economic process. Several methods have been patented (44—46). The catalyst is often reactivated by heating in the presence of an alcohol. In another technique, water is added to the homogeneous catalyst solution so that the rhodium compounds precipitate. Another way to separate rhodium involves a two-phase Hquid such as the immiscible mixture of octane or cyclohexane and aliphatic alcohols having 4—8 carbon atoms. In a typical instance, the carbonylation reactor is operated so the desired products and other low boiling materials are flash-distilled. The reacting mixture itself may be boiled, or a sidestream can be distilled, returning the heavy ends to the reactor. In either case, the heavier materials tend to accumulate. A part of these materials is separated, then concentrated to leave only the heaviest residues, and treated with the immiscible Hquid pair. The rhodium precipitates and is taken up in anhydride for recycling. 

Lime Soda. Process. Lime (CaO) reacts with a dilute (10—14%), hot (100°C) soda ash solution in a series of agitated tanks producing caustic and calcium carbonate. Although dilute alkaH solutions increase the conversion, the reaction does not go to completion and, in practice, only about 90% of the stoichiometric amount of lime is added. In this manner the lime is all converted to calcium carbonate and about 10% of the feed alkaH remains. The resulting slurry is sent to a clarifier where the calcium carbonate is removed, then washed to recover the residual alkaH. The clean calcium carbonate is then calcined to lime and recycled while the dilute caustic—soda ash solution is sent to evaporators and concentrated. The concentration process forces precipitation of the residual sodium carbonate from the caustic solution the ash is then removed by centrifugation and recycled. Caustic soda made by this process is comparable to the current electrolytic diaphragm ceU product. 

Aluminum hydroxide gel may be prepared by a number of methods. The products vary widely in viscosity, particle size, and rate of solution. Such factors as degree of supersaturation, pH during precipitation, temperature, and nature and concentration of by-products present affect the physical properties of the gel. 

Industrial Wastewater Treatment. Industrial wastewaters require different treatments depending on their sources. Plating waste contains toxic metals that are precipitated and insolubiHzed with lime (see Electroplating). Iron and other heavy metals are also precipitated from waste-pidde Hquor, which requires acid neutralization. Akin to pickle Hquor is the concentrated sulfuric acid waste, high in iron, that accumulates in smokeless powder ordinance and chemical plants. Lime is also useful in clarifying wastes from textile dyeworks and paper pulp mills and a wide variety of other wastes. Effluents from active and abandoned coal mines also have a high sulfuric acid and iron oxide content because of the presence of pyrite in coal. 

Other recovery methods have been used (10). These include leaching ores and concentrates using sodium sulfide [1313-82-2] and sodium hydroxide [1310-73-2] and subsequentiy precipitating with aluminum [7429-90-3], or by electrolysis (11). In another process, the mercury in the ore is dissolved by a sodium hypochlorite [7681-52-9] solution, the mercury-laden solution is then passed through activated carbon [7440-44-0] to absorb the mercury, and the activated carbon heated to produce mercury metal. Mercury can be extracted from cinnabar by electrooxidation (12,13). 

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