System ethanol-ethyl acetate

Sketch the distillation line map (residue curve map) for the system ethanol-ethyl acetate-methanol at 1 atm and 5 atm from the data in Table 12.1. Does the system have a distillation boundary Is the position of the boundary sensitive to pressure ... 

Concentration Units. Predictions of distribution thus far described are based on mole fraction concentration units. It should be noted that distribution coefficients in terms of weight fractions are different from those in terms of mole fractions, although ordinarily the direction of distribution is the same for both unit systems. In a few cases, where there is an unusual combination of molecular weights, this will not be the case. For example, in the system ethanol-ethyl acetate-water, higher concentrations of ethanol are in the water-rich layer on a weight basis but in the ester layer on a mole basis. Where the ternary-solubility curve is available, corrections from one system to another can easily be made. If the distribution is estimated from data on the binaries alone, then at zero concentration of C,... 

Griswold, Chu, and Winsauer [Ind, Eng, Chem, 41, 2352 (1949)] provide very complete data on the liquid-liquid and vapor-liquid equilibria in the system ethanol-ethyl acetate-water. Design a plant and solvent-recovery system for the recovery of 99.8% ethanol from 50,000 gal./day of a 5% solution in water, using ethyl acetate as extracting solvent. Solvent concentration in the raffinate phase is to be no greater than 0.001%. 

The crude product (48.4 grams, 80.9% yield) was recrystallized from an absolute ethanol-ethyl acetate solvent system by suspending the salt in boiling anhydrous ethyl acetate and just enough absolute ethanol was gradually added to effect solution after which the solu-... 

Figure 2. Thin-layer radiochromatogram of urine (100 il) from rats injected with labeled PbTx-3. TLC plates were developed in two sequential solvent systems chloroform ethyl acetate ethanol (50 25 25 80 10 10). Radioactive zones were scraped and counted in a liquid scintillation counter. Native PbTx-3 runs at 13 cm.

Table 12.1 Data for the ethanol-ethyl acetate-methanol system.

In Eq. (88), dn0/dl expresses how the refractive index % of the binary solvent alone varies with its composition expressed as volume fraction 4>y of liquid-1. Clearly, if liquids 1 and 3 are iso-refractive or nearly so, then M = M2, that is, a LS experiment will yield the true molecular weight irrespective of the composition of the mixed solvent. This situation is exemplified133) by the system polystyrene -ethyl-acetate (l)-ethanol (3) for which the molecular weight in mixed solvents of different 0i is the same as that obtained in pure ethylacetate (Fig. 40). The values of dn /d0j for the mixed solvents are only of the very small order of ca. 0.01, whilst the values of dn/dc for the polymer solutions are large (ca. 0.22 ml/g). 

A suggested procedure would be equal volumes of the sample and a 4% (by volume) benzene in pure ethanol. This is easily set up using a G.C.-Computer system Note Ethyl Acetate can also be detd by Standard Method ASTM Designation DI617—69, described here under Ethyl Acetate 4.3.10 Methyl-isobutyl-kefone (MIBK). The rest is iisted but not described in MIL-E-463B, but it seems that the Test 4.6.1.8 for determination of Acetone and other ketones, described... 

Separation of a number of keto acid hydrazones may be accomplished as their free hydrazones [37], as sodium salts [38] or as ammonium salts [39]. For TLC separation of the sodium salts a plate (20 X 20 cm) is coated with a 0.25-mm layer of a mixture of silica gel and 0.1 N sodium bicarbonate (1 2 w/v). The plate is activated by heating at 110 °C for 40 min and is then cooled and kept in a desiccator until required. The solvent systems are ethyl acetate (saturated with 0.1 N sodium bicarbonate)-methanol (5 1) and butanol-ethanol-0.1 N sodium bicarbonate (10 3 10) (upper layer). The plates are developed for 2.5 h at room temperature. For quantitation, the spots may be removed from the plate and dissolved in 2.07V sodium hydroxide for color development and determination in solution. Treatment of the plate directly with base (as a spray) should also be possible for quantitation in situ. The wavelengths of the absorption maxima of a number of DNPH-keto acids in aqueous base are listed in Table 4.6... 

The crude product (48.4 grams, 80.9% yield) was recrystallized from an absolute ethanol-ethyl acetate solvent system by suspending the salt in boiling anhydrous ethyl acetate and just enough absolute ethanol was gradually added to effect solution after which the solution was concentrated to about two-thirds of the original volume on the steam bath, charcoal treated, and suction-filtered through Celite filter aid. The white crystals of 2-dimethylaminoethanol p-acetylaminobenzoate obtained, dried at room temperature at a pressure of 0.08 mm Hg for 15 hours, melted at 159.0°-161.5°C. 

The phase regions for micellar solutions and lyotropic liquid crystals form a complicated pattern in water/amphlphile/hydrocarbon systems. The present treatment emphasizes the fact that they may be considered as parts of a continuous solubility region similar to the one for water/short chain amphiphilic systems such as water/ethanol/ethyl acetate. 

For the UNIQUAC equation, there are two adjustable equation parameters for each binary. For the binary that is partially miscible, the best way to determine the two binary parameters is to fit the mutual solubility data. For the completely miscible binaries, useful interaction parameters can be obtained from vie data. However, fitting vie data to within experimental accuracy does not uniquely determine the binary parameters. The choice of a particular set of parameters can have a significant effect on the representation of the ternary lie. For the ternary system of chloroform, water, and acetone at 333°K, for example, the two binary parameters are first determined from mutual solubility data for chloroform and water and then the other binary parameters for the two miscible binaries. Somewhat improved predictions occur by fitting binary parameters to the miscible binaries. Similar predictions have also been found for ternary systems of ethyl acetate, ethanol, and water. 

In approximate distillation column calculations, the relative volatility is sometimes assumed to be a constant (independent of composition, temperature, and pressure). Test this assumption for the ethanol-ethyl acetate system using the following data ... 

A thin layer chromatographic method for the separation of trimethobenzamide hydrochloride from its possible metabolites has been developed. The adsorbent was silica gel G and the solvent system was ethyl acetate ethanol NH OH (90 10 5). The solvent front is allowed to ascend for 15 cm. The plate is then air dried and sprayed with potassium iodoplatlnate detecting reagent (16). The approximate Rj values are given in Table V below. 

The solvent system is ethyl acetate ethanol water=3 l 3, with heavy phase as the stationary phase, the light phase as mobile phase the solute acetyl acetone (AR) acetyl acetone solution 5 mg/ml as the feed liquid automatic fraction collector spiral countercurrent extraction device ... 

FIG. 13-10 Vap or-liqiiid equilibriums for the ethyl acetate-ethanol and chloroform-acetone systems at 101.3 kPa (1 atm). 

Ethyl acetate-ethanol Minimum-hoiling azeotrope Higher esters or alcohols, aromatics Process similar for other alcohol-ester systems... 

C) Preparation of Doxapram Hydrochloride [3,3-Diphenyl-1-Ethyl-4-(2-Morpholino-Ethylj-2-Pyrrolidinone Hydrochloride Monohydrate] A solution of 25 grams (0.076 mol) of 4-(2-chloroethyl)-3,3-diphenyl-1-ethyl-2-pyrrolidinone and 13.3 grams (0.153 mol) of morpholine in 500 ml of absolute ethanol was heated at 95°-120°C for 21 hours in a closed system and concentrated in vacuo. The residue was dissolved in 3(X) ml of two normal hydrochloric acid and extracted with 150 ml of ethyl acetate. A solid crystallized (13 g) during the extraction and was removed by filtration. MP 217°-219°C. The acid extracts were made basic with sodium hydroxide and extracted with ether, and the ether solution was concentrated in vacuo and the residue was suspended in six normal hydrochloric acid. Additional crystalline product formed and was recrystallized from two normal hydrochloric acid. Yield, 10 grams MP 217°-219°C. Total yield, 23 grams (70%). 

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