PHYSICAL CHEMISTRY LABORATORY REPORT (CHE 414L)

Department of Chemical Engineering

School of Engineering and Architecture

Saint Louis University

Group No. 6

Names of Students Signature

DIAZ, Jeany Rose

ECLAR, Jezreel Maye

FERER, Jean

FRANCISCO, Valerie Ann G.

I. Title: STEAM DISTILLATION

II. Background of the Study

When a mixture of two practically immiscible liquids are heated while being agitated

to expose the surfaces of both the liquids to the vapor phase, each constituent independently

exerts its own vapor pressure as a function of temperature as if the other constituent were not

present. Consequently, the vapor pressure of the whole system increases. Boiling begins

when the sum of the partial pressures of the two immiscible liquids just exceeds

the atmospheric pressure (approximately 101 kPa at sea level). In this way, many organic

compounds insoluble in water can be purified at a temperature well below the point at which

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decomposition occurs. The total pressure of the pot liquids can be defined by the following

equation.

(1)

Notice there are no mole fraction terms in the equation. This means that if you have lots

of water or just a little it will make the same contribution to the vapor pressure.

A helpful relationship when considering steam distillation in a theoretical sense is the

ideal gas law, PV = nRT, where P = pressure, V = volume, n = moles, R = the gas constant

and T = temperature. It is important to remember that all of these parameters refer to gaseous

molecules. Since distillation involves the expansion of a liquid into a gas in a fixed volume

(the still), the gas law can be useful in predicting the amount of water needed to complete a

steam distillation or to figure out the proportion in which the organic and aqueous layers will

co-distill. To gain a more practical expression, take the ratio of a gas law written for the

gaseous water and one written for the organic gas. If this is done, one obtains the following

expression.

(2)

Fortunately, several of the terms in the above expression cancel. The volumes cancel

because both gases occupy the same space, i.e., the still. The temperature terms cancel

because the two components are co-distilling at the same temperature. The R terms obviously

cancel.

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The equation therefore reduces to:

(3)

This simple equation sums up steam distillation because it demonstrates that the

amount of water obtained is directly proportional to the vapor pressure of water at the

distillation temperature. The same is true of the organic component . Therefore, if the organic

component has a higher boiling point than the aqueous component, it will contribute fewer

molecules to the overall push against the atmosphere. Nonetheless, the two components are

working together.

Problem. From the plots, estimate the boiling point of the mixture at the corrected barometric

pressure and then estimate the composition of the distillate, at the estimated boiling point,

expressed as grams of toluene per gram of water.

Objectives. From the densities of toluene and water from the Perry’s Chemical Engineer

Handbook 8th edition and the relative volumes of toluene and water actually obtained from

the experiment the aims of this laboratory activity is to calculate the composition of the

distillate and expressed in grams of toluene per gram of water.

Research questions (and/or hypothesis/es). Why is steam distillation useful? What Is

the Set Up For Steam Distillation?

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 Most complex organic compounds are immiscible with water, meaning they don't

dissolve in water but form a mixture instead, which separates if allowed to settle as the water

settles down and the organic compounds float on top. The steam distillation process works on

the principle that when a mixture of two or more immiscible liquids is heated while ensuring

that the surfaces of both liquids are in contact with the atmosphere, the vapor pressure

exerted by the system is increased. This is because it now becomes the sum of the vapor

pressures of all of the components of the mixture combined together. This allows for

evaporation of elements with high boiling points at much lower temperatures merely by

allowing them to form a mixture with water.

Steam distillation set up is a particular type of a separation process for temperature

sensitive materials like natural aromatic compounds. This is whereby water or steam is added

to the distillation apparatus to enhance the boiling points of compounds. After distillation the

vapors is condensed, hence yielding a two-phase system of water and the organic

compounds, that allows for decantation. The shown figure below is sample setup for steam

distillation.

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Conceptional framework. Most essential oils are obtained from the plant material by a

process known as steam distillation. Descriptions and explanations of the theory and practice

of steam distillation are given elsewhere (AMES and MATTHEWS, 1968, and DENNY,

1991).

The fundamental nature of steam distillation is that it enables a compound or mixture

of compounds to be distilled (and subsequently recovered) at a temperature substantially

below that of the boiling point(s) of the individual constituent(s). Essential oils contain

substances with boiling points up to 200C or higher, including some that are solids at normal

temperatures. In the presence of steam or boiling water, however, these substances are

volatilized at a temperature close to 100C at atmospheric pressure. The mixture of hot

vapours will, if allowed to pass through a cooling system, condense to form a liquid in which

the oil and water comprise two distinct layers. Most (but not all) essential oils are lighter than

water and form the top layer. The steam that is used for the distillation is generated either

within the steel vessel that contains the plant material (by boiling water contained at the base)

or by an external boiler.

The use of steam generated within the vessel requires that the leaf be supported above

some boiling water by a grid. The water is heated either directly using a fire or by heat

exchanger coils. The simplicity of the method makes it suitable for small-scale distillation of

essential oils.

If steam is generated, instead, by an external boiler it is introduced into the base of the

vessel via an open coil, jets or similar device(s). The advantages of this type of distillation

are that it is relatively rapid and capable of greater control by the operator. The vessel can be

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emptied and recharged quickly and with the immediate reintroduction of steam there is no

unnecessary delay in the commencement of the distillation process. Oils produced by this

means are more likely to be of acceptable quality than those produced using the more direct

method.

Significance. Steam distillation is employed in the manufacture of essential oils, for instance,

perfumes. In this method, steam is passed through the plant material containing the desired

oils. Eucalyptus oil and orange oil are obtained by this method on the industrial scale. Steam

distillation is also sometimes used to separate intermediate or final products during the

synthesis of complex organic compounds.

Steam distillation is also widely used in petroleum refineries and petrochemical plants

where it is commonly referred to as "steam stripping" .

Steam distillation is also used in a wide variety of applications in commercial food

preparation. As with essential oil steam distillation, flavors and aromas can be heightened or

intensified by steam distillation. Alcoholic beverages are often subjected to steam distillation

as a method of manipulating chemical ratios and modifying flavors. Foods with high fat or

oil concentrations are also steam distilled to deodorize the fat and oil to make packaged foods

more palatable to the end consumer. The chemicals that lead to disagreeable aromas and

flavors are carefully targeted and either reduced or removed using precise steam temperatures

and sophisticated distillation equipment.

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Apparutus:

 500 mL round bottom flask  Long glass tubing

 500 mL didtilling flask  2 clamps

 condenser  2 bunsen burner

 adapter  2 rubber tubings

 2-holed corks  Water bath

 100 mL graduated cylinder  2 wire gauze

 150 ˚C thermometer  Boiling chips

 Bent glass tubings

 Iron stands

Reagents:

 Toluene

 Distilled water

 Distilled water (for rinsing

 Hydrochloric acid ( for cleansing)

Method/Procedure

The bent glass tubing serves as a steam delivery tube,with one end starting from just

under the cork of the round bottom flask, and the other going to the bottom of the distilling

flask. Insert a three feet length of glass tubing in the round bottom flask cork as a safety tube;

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this should run to the bottom of the round bottom flask. Insert a thermometer into the

distilling flask cork, setting the bulb just opposite the exit tube of the flask.

Place 300 mL of toluene in the distilling flask and connect it to the water condenser.

Partly immerse the flask in a water bath heated to about 80˚C. Add distilled water to the

steam generator (round bottom flask). Regulate the rate of boiling so that about two drops of

distillate per second fall into a 100mL graduated cylinder. Under this condition, the

thermometer should record a temperature which remains constant within about 0.2 ˚C. Reject

the first 10-20 mL of distillate, pouring it into a residue bottle.

When distillation is proceeding under equilibrium conditions, start collecting the

distillate until 10 mL obtained. Also record the barometric pressure. When the layers in the

distillate have separated completely, record the temperature and the respective volumes and

pour the mixtures into the residues bottle. Also pour the mixture remaining in the distilling

flask into the residues bottle.

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IV. Conclusion and Recommendation

Based on findings of this experiment that we have performed and data’s that we have

presented, we therefore conclude that the process of steam distillation works because when

two immiscible liquids are distilled, the boiling point of the mixture is below the boiling

point of the both pure compounds. Since water has a significantly lower boiling point than

toluene, a much greater proportion of water molecules were vaporizing at any time during the

distillation. Even though the components of toluene have low vapor pressure, they are

volatile enough to vaporize to some extent and a small amount will lifted off with the water

molecules. This boiling will occur when the independent internal vapor pressures are equal to

760 torr, which is the external vapor pressure. It is noted that steam distillation, unlike

regular distillation, it does not follow Raoult’s Law.

We also recommend that to be able to have definite results we must read and follow the

instructions carefully in preparing and performing the experiment, measure accurately the

solutions that are needed in the experiment, refrain from being careless in using the

apparatus, in weighing the pycnometer be efficient in reading the values and most

importantly to achieve common goal have a teamwork!

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V. References

AMES, G.R. and MATTHEWS, W.S.A. (1968) The distillation of essential oils. Tropical
Science, 10, 136-148.

DENNY, E.F.K. (1991) Field Distillation for Herbaceous Oils. Lilydale, Tasmania:
Published by the author (PO Box 42).

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SET UP.