Mixture separating mixtures

Flotation. Flotation is a gravity separation process which exploits differences in the surface properties of particles. Gas bubbles are generated in a liquid and become attached to solid particles or immiscible liquid droplets, causing the particles or droplets to rise to the surface. This is used to separate mixtures of solid-solid particles and liquid-liquid mixtures of finely divided immiscible droplets. It is an important technique in mineral processing, where it is used to separate different types of ore. 

For a heterogeneous or multiphase mixture, separation usually can be achieved by phase separation. Such phase separation should be carried out before any homogeneous separation. Phase separation tends to be easier and should be done first. 

Dibromobutane from 1 4 butanediol). In a 500 ml. threenecked flask fltted with a stirrer, reflux condenser and dropping funnel, place 154 g. (105 ml.) of 48 per cent, hydrobromic acid. Cool the flask in an ice bath. Add slowly, with stirring, 130 g. (71 ml.) of concentrated sulphuric acid. To the resulting ice-cold solution add 30 g. of redistilled 1 4-butanediol dropwise. Leave the reaction mixture to stand for 24 hours heat for 3 hours on a steam bath. The reaction mixture separates into two layers. Separate the lower layer, wash it successively with water, 10 per cent, sodium carbonate solution and water, and then dry with anhydrous magnesium sulphate. Distil and collect the 1 4-dibromo-butane at 83-84°/12 mm. The yield is 55 g. 

Di-n-amyl ether. Use 50 g. (61 5 ml.) of n-amyl alcohol (b.p. 136-137°) and 7 g. (4 ml.) of concentrated sulphuric acid. The calculated volume of water (5 ml.) is collected when the temperature inside the flask rises to 157° (after 90 minutes). Steam distil the reaction mixture, separate the upper layer of the distillate and dry it with anhydrous potassium carbonate. Distil from a 50 ml. Claisen flask and collect the fractions of boiling point (i) 145-175° (13 g.), (ii) 175-185° (8 g.) and (iii) 185-190° (largely 185-185-5°) (13 g.). Combine fractions (i) and (u), reflux for 1 hour in a small flask with 3 g. of sodium, and distil from the sodium amyloxide and excess of sodium this yields 9 5 g. of fairly pure n-amyl ether (iv). The total yield is therefore 22 - 5 g. A perfectly pure product, b.p. 184 185°, is obtained by further distillation from a Little sodium. 

Place 50 g. of anhydrous calcium chloride and 260 g. (323 ml.) of rectified spirit (95 per cent, ethyl alcohol) in a 1-litre narrow neck bottle, and cool the mixture to 8° or below by immersion in ice water. Introduce slowly 125 g. (155 ml.) of freshly distilled acetaldehyde, b.p. 20-22° (Section 111,65) down the sides of the bottle so that it forms a layer on the alcoholic solution. Close the bottle with a tightly fitting cork and shake vigorously for 3-4 minutes a considerable rise in temperature occurs so that the stopper must be held well down to prevent the volatilisation of the acetaldehyde. Allow the stoppered bottle to stand for 24-30 hours with intermittent shaking. (After 1-2 hours the mixture separates into two layers.) Separate the upper layer ca. 320 g.) and wash it three times with 80 ml. portions of water. Dry for several hours over 6 g. of anhydrous potassium carbonate and fractionate with an efficient column (compare Section 11,17). Collect the fraction, b.p. 101-104°, as pure acetal. The yield is 200 g. 

With phenylalanine and tyrosine, the sodium salt of the derivative is sparingly soluble in water and separates during the initial reaction. Acidify the suspension to Congo red the salts pass into solution and the mixture separates into two layers. The derivative is in the etheresil lay and crystallises from it within a few minutes. It is filtered off and recrystaUised. 

Indole (I) condenses with formaldehyde and dimethylamine in the presence of acetie acid (Mannich reaction see Section VI,20) largely in the 3-position to give 3 dimethylaminomethylindole or gramine (II). The latter reaets in hot aqueous ethanol with sodium cyanide to give the nitrile (III) upon boiling the reaction mixture, the nitrile undergoes hydrolysis to yield 3-indoleaeet-amide (IV), part of which is further hydrolysed to 3-indoleacetic acid (V, as sodium salt). The product is a readily separable mixture of 20 per cent, of (IV) and 80 per cent, of (V). 

In a 250 ml. distilling flask (1) place 122 g. (119 ml.) of p-phenylethyl alcohol and 40 g. of sodium hydroxide peUets (or 56 g. of potassium hydroxide). Heat is evolved. Warm gently until bubbles commence to form and the mixture separates into two sharply-defined layers. Distil slowly water, etc. passes over first accompamed by the gradual dis appearance of the upper phase. FinaUy the styrene passes over at 140 160° (mainly 150°) coUect this separately in a receiver containing about 0 1 g. of hydroquinone. Dry the distillate with a httle anhydrous calcium chloride or magnesium sulphate, and then distil under reduced pressure (2). C oUect the pure styrene at 42-43°/18 mm. The 3rield is 80 g. Add about 0-2 g. of hydroquinone (anti-oxidant) if it is desired to keep the phenylethylene. 

Although GGMS is the most widely used ana lytical method that combines a chromatographic sep aration with the identification power of mass spectrometry it is not the only one Chemists have coupled mass spectrometers to most of the mstru ments that are used to separate mixtures Perhaps the ultimate is mass spectrometry/mass spectrome try (MS/MS) m which one mass spectrometer gener ates and separates the molecular ions of the components of a mixture and a second mass spec trometer examines their fragmentation patterns ... 

Chromatography is a method for separating mixtures of substances into their individual components. Substances can be loosely categorized as volatile (including gaseous) and nonvolatile. The terms are... 

In addition to the Hquid—Hquid reaction processes, there are many cases in both analytical and industrial chemistry where the main objective of separation is achieved by extraction using a chemical extractant. The technique of dissociation extraction is very valuable for separating mixtures of weakly acidic or basic organic compounds such as 2,4-dichlorophenol [120-83-2] and 2,5-dichlorophenol [583-78-8] which are difficult to separate by... 

The primary disadvantage of the conjugate addition approach is the necessity of performing two chiral operations (resolution or asymmetric synthesis) ia order to obtain exclusively the stereochemicaHy desired end product. However, the advent of enzymatic resolutions and stereoselective reduciag agents has resulted ia new methods to efficiently produce chiral enones and CO-chain synthons, respectively (see Enzymes, industrial Enzymes in ORGANIC synthesis). Eor example, treatment of the racemic hydroxy enone (70) with commercially available porciae pancreatic Hpase (PPL) ia vinyl acetate gave a separable mixture of (5)-hydroxyenone (71) and (R)-acetate (72) with enantiomeric excess (ee) of 90% or better (204). 

Several N-substituted pyrroHdinones eg, ethyl, hydroxyethyl and cyclohexyl, are used primarily in specialized solvent appHcations where their particular physical properties are advantageous. For example, mixtures of l-cyclohexyl-2-pyrroHdinone and water exhibit two phases at temperatures above 50°C below that temperature they are miscible in aH proportions. This phenomenon can be used to facHitate some extractive separations. Mixtures of 1-alkyl-pyrroHdinones that are derived from coconut and taHow amines can be used at lower cost in certain appHcations where they may be used instead of the pure l-dodecyl-2-pyrroHdinone and l-octadecyl-2-pyrroHdinone. 

Many forms of chromatography have been used to separate mixtures of quinoline and isoquinoline homologues. For example, alumina saturated with cobalt chloride, reversed-phase Hquid chromatography, and capillary gas chromatography (gc) with deactivated glass columns have all been employed (38,39). 

Conversion to acetates, trifluoroacetates (178), butyl boronates (179) trimethylsilyl derivatives, or cycHc acetals offers a means both for identifying individual compounds and for separating mixtures of polyols, chiefly by gas—Hquid chromatography (glc). Thus, sorbitol in bakery products is converted to the hexaacetate, separated, and determined by glc using a flame ionisation detector (180) aqueous solutions of sorbitol and mannitol are similarly separated and determined (181). Sorbitol may be identified by formation of its monobensylidene derivative (182) and mannitol by conversion to its hexaacetate (183). 

Rx mixture separates, H2O often added to facihtate color bodies partially removed into separated spent H2SO4... 

Chromatography is a technique for separating and quantifying the constituents of a mixture. Separation techniques are essential for the characterization of the mixtures that result from most chemical processes. Chromatographic analysis is used in many areas of science and engineering in environmental studies, in the analysis of art objects, in industrial quahty control (qv), in analysis of biological materials, and in forensics (see Biopolymers, analytical TECHNIQUES FiNE ART EXAMINATION AND CONSERVATION FoRENSic CHEMISTRY). Most chemical laboratories employ one or more chromatographs for routine analysis (1). 

Traditionally, sodium dichromate dihydrate is mixed with 66° Bh (specific gravity = 1.84) sulfuric acid in a heavy-walled cast-iron or steel reactor. The mixture is heated externally, and the reactor is provided with a sweep agitator. Water is driven off and the hydrous bisulfate melts at about 160°C. As the temperature is slowly increased, the molten bisulfate provides an excellent heat-transfer medium for melting the chromic acid at 197°C without appreciable decomposition. As soon as the chromic acid melts, the agitator is stopped and the mixture separates into a heavy layer of molten chromic acid and a light layer of molten bisulfate. The chromic acid is tapped and flaked on water cooled roUs to produce the customary commercial form. The bisulfate contains dissolved CrO and soluble and insoluble chromic sulfates. Environmental considerations dictate purification and return of the bisulfate to the treating operation. 

Even though the simple distillation process has no practical use as a method for separating mixtures, simple distillation residue curve maps have extremely usehil appHcations. These maps can be used to test the consistency of experimental azeotropic data (16,17,19) to predict the order and content of the cuts in batch distillation (20—22) and, in continuous distillation, to determine whether a given mixture is separable by distillation, identify feasible entrainers/solvents, predict the attainable product compositions, quaHtatively predict the composition profile shape, and synthesize the corresponding distillation sequences (16,23—30). By identifying the limited separations achievable by distillation, residue curve maps are also usehil in synthesizing separation sequences combining distillation with other methods. 

There are three distinct modes of electrophoresis zone electrophoresis, isoelectric focusing, and isotachophoresis. These three methods may be used alone or in combination to separate molecules on both an analytical (p.L of a mixture separated) and preparative (mL of a mixture separated) scale. Separations in these three modes are based on different physical properties of the molecules in the mixture, making at least three different analyses possible on the same mixture. 

It is generally preferable to meter each of the individual components of a two-phase mixture separately prior to mixing, since it is difficult to meter such mixtures accurately. Problems arise because of fluctuations in composition with time and variations in composition over the cross section of the channel. Information on metering of such mixtures can be obtained from the following sources. 

When multicomponent mixtures are to be separated into three or more products, sequences of simple distillation columns of the type shown in Fig. 13-1 are commonly used. For example, if aternaiy mixture is to be separated into three relatively pure products, either of the two sequences in Fig. 13-4 can be used. In the direct sequence, shown in Fig. 13-4, all products but the heaviest are removed one by one as distillates. The reverse is true for the indirect sequence, shown in Fig. 13-4 7. The number of possible sequences of simple distillation columns increases rapidly with the number of products. Thus, although only the 2 sequences shown in Fig. 13-4 are possible for a mixture separated into 3 products, 14 different sequences, one of which is shown in Fig. 13-5, can be synthesized when 5 products are to be obtained. 

Equations (14-168) and (14-170) have been developed for binaiw mixture separations and hold for cases where the operating hne and equilibrium line are straight. Thus, when there is curvature, the equations should be used for sections of the column where hnearity can be assumed. When the eqiiihbriiim line and operating line have the same slope, HETP = Hog and Nog = (theoretical stages). 

Modes of Operation There is a close analogy between sedimentation of particles or macromolecules in a gravitational field and their elec trophoretic movement in an electric field. Both types of separation have proved valuable not only for analysis of colloids but also for preparative work, at least in the laboratoiy. Electrophoresis is applicable also for separating mixtures of simple cations or anions in certain cases in which other separating methods are ineffectual. 

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