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RALPH JUDE I.

JAKOSALEM Experiment 4: Distillation

CHEM 31.1 HEJ

Problem/ Questions: 1. Discuss the basic principles of the three distillation operations. Simple Distillation (for a mixture with miscible components) It is usually used only to separate liquids whose boiling points differ greatly (>70C) or to separate liquids from involatile solids or oils. In the process, all the hot vapors produced are immediately channelled into a condenser which cools and condenses the vapors. Therefore, the distillate will not be as pure. A simple distillation apparatus consists of a boiling flask (round-bottom flask) attached to an adapter holding a thermometer (to determine the boiling temperature of the liquid). The adapter connects to a condenser into which cold water is constantly passed through. The condenser leads into a collection flask for the purified liquid. Fractional Distillation (for a mixture with miscible components) It is usually employed with separation of complex mixtures at small boiling points difference (about 25C). It can separate the mixture into its component parts or fractions. It is essentially the same as simple distillation except that a fractionating column is placed between the boiling flask and the condenser. The glass beads found in the fractionating column provide "theoretical plates" on which the refluxing liquid can condense, re-evaporate, and condense again, essentially distilling the compound over and over. The more volatile liquids will tend to push towards the top of the fractionating column, while less volatile liquid will stay towards the bottom, giving a better separation between the liquids. Steam Distillation (for a mixture with immiscible components) It is the process of purifying a substance through application of steam. It deals with compounds that are heat sensitive (e.g. natural aromatic compounds). Steam distillation works on the principle that immiscible substance when mixed together can lower the boiling point of each other. Many compounds, both solids and liquids, are separated from otherwise complex mixtures by taking advantage of their volatility in steam. A compound must satisfy three conditions to be successfully separated by steam distillation. It must be stable and relatively insoluble in boiling water, and it must have a vapor pressure in boiling water that is of the order of 1 kPa (0.01 atm). But if two or more compounds satisfy these three conditions, they will generally not separate from each other but will be separated from everything else. 2. Explain the differences of the distillation curves between simple distillation and fractional distillation. The curve of fractional distillation yields a higher slope or gives a higher or sudden rise in the temperature of distillation than the curve of simple distillation. The curve of fractional distillation is more defined, while that of the simple distillation is more of a straight line characterizing almost constant temperature rise. This shows that fractional distillation yields a purer distillate than simple distillation. The sharp rise in the temperature happens when the ethanol component has almost boiled out of the mixture, thus there is an increase in the water composition of the vapors produced since water requires greater amount of heat to boil. 3. In the separation of the ethanol from water using fractional distillation, the distillate always contains about 5% water. Explain.
Not all liquids conform to Raoult's law and form ideal solutions. An example is the mixture of water and ethanol. Because of certain intermolecular interactions, a unique mixture (an azeotrope) of 95.5% ethanol and 4.5% water forms that boils below (78.1 C) the boiling point of ethanol (78.3 C). Thus, we say that ethanol/water mixtures form a low-boiling azeotrope because the boiling point of the azeotrope is lower than the boiling points of either single component. No matter how efficient is our distilling apparatus, pure 100% ethanol cannot be obtained by the distillation of a mixture of ethanol/water.

4. Illustrate the following phase diagrams: a. t vs. % concentration of ethanol-water mixture @constant pressure

b. p vs. % concentration of ethanol-water mixture @constant temperature

c. t vs. % concentration of liquid mixture, which does not form azeotrope @constant temperature

5. Based on the phase diagram of 4(a), what is the approximate composition of the ethanol-water mixture, which begins to distill at 80C? Approximately 92% water and 8% ethanol is present at 80C. 6. At 95C the vapor pressure of n-heptane is 684 mmHg and of n-octane is 303 mmHg. Calculate the mole ratio and weight ration of the two components in a mixture of n-heptane and n-octane, which begins to distill at 95C at 650 mmHg. P sol = 650 mmHg 684 x + 303 (1-x) = 650 684x + 303 303x = 650 x= 0.9107 1-x = 0.089 Mole ratio: 0.9107/0.089 = 10.23 (10.23 mols of n-heptane for every 1 mol of n-octane) Weight ratio: 91.25/10.17 = 8.98 (8.98 g of n-heptane for every 1 g of n-octane) 7. Explain the difference in the values of toluene/water weight ratios between the first and second fractions. The ratio of this fraction must be equal since they are extracted at the same time and behaves independently. Throughout the heating process, water and toluene molecules will escape in proportion to their respective vapor pressures at the distilling temperature. Since the water and organic components are not interacting with each other, no enrichment will occur and they will co-distill at a single temperature until all of one component is completely distilled over. Normally, steam distillations are carried out with a large excess of water. When the entire organic component has been distilled, pure water begins to distill. 8. Cite some important application of steam distillation and vacuum distillation. Steam distillation is employed in the production of essential oils like perfumes. It is also employed in the synthetic procedures of complex organic compounds. Eucalyptus oil and orange oil are obtained by this method on the industrial scale. Steam distillation is also widely used in petroleum refineries and petrochemical plants where it is commonly referred to as "steam stripping". Other industrial uses of steam distillation include the production of consumer food products such as sprayable or aerosolized condiments such as mayonnaise. Vacuum distillation is used when liquids to be distilled have high atmospheric boiling points or chemically change at temperatures near their atmospheric boiling points. Temperature sensitive materials (such as beta carotene) require vacuum distillation to remove solvents from the mixture without damaging the product.

RALPH JUDE I. JAKOSALEM EXPERIMENT 4: DISTILLATION DATA AND RESULTS Simple Distillation

CHEM 31.1 HEJ

T (C) 76 76.5 76 76 72 76 77 77.5 76.5 77 77.5 76.5 77.5 77.5 76.5 77 79 78 77 79 76.5 76 74 76.5 77

V (mL) 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1 1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.9 2 2.1 2.2 2.3 2.4 2.5

77.5 75.5 81 78 79 78 82 83 90 91.5 92 92 92 92 93 93.5 93.5 93.5 94 94 94 94 94 94 94 94 94

2.6 2.7 2.8 2.9 3 3.1 3.2 3.3 3.4 3.5 3.6 3.7 3.8 3.9 4 4.1 4.2 4.3 4.4 4.5 4.6 4.7 4.8 4.9 5 5.1 5.2
T (C) 76 90

94 94 94 94 94 94 94 94 93.5 93.5 93 93 93 93 93 93 93.5 93.5 93.5 93.5 93.5 93.5 93.5 93.5 93.5 93.5 93.5

5.3 5.4 5.5 5.6 5.7 5.8 5.9 6 6.1 6.2 6.3 6.4 6.5 6.6 6.7 6.8 6.9 7 7.1 7.2 7.3 7.4 7.5 7.6 7.7 7.8 7.9

93.5 93.5 93.5 93.5 93.5 94 94 94 94 94 94 94 94 94 94 94 94 94 94 94 94 94 94 94 94 94

8 8.1 8.2 8.3 8.4 8.5 8.6 8.7 8.8 8.9 9 9.1 9.2 9.3 9.4 9.5 9.6 9.7 9.8 9.9 10 10.1 10.2 10.3 10.4 10.5

First Distillate Second Distillate

Identity Mainly Ethanol Mainly Water

% Volume 22% 51%

Fractional Distillation

T (C) 76 76 76 76 74 66 76 76 71 77

V (mL) 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1

77 76 69 74 76 76 76 76 71 76 76.5 76

1.1 1.2 1.3 1.4 1.5 1.6 1.7 1.8 1.9 2 2.1 2.2

58 85 82 93 92 87 98 98 97 89 91 93

2.3 2.4 2.5 2.6 2.7 2.8 2.9 3 3.1 3.2 3.3 3.4

94 95 98 98 98 97 98 98 98 98 98

3.5 3.6 3.7 3.8 3.9 4 4.1 4.2 4.3 4.4 4.5

First Distillate Second Distillate

Temperature (C) 76 82

Identity Mainly Ethanol Mainly Water

% Volume 17% 15%

Steam Distillation
Volume Xylene (mL) First Fraction 0.5 Second Fraction* -no data*the experiment was unsuccessful Volume Water (mL) 1.3 -no dataWeight Ratio 0.38 : 1 -no data-