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NAME : FIKAFAJARIYAH ARIFIN NIM : 103194006 CLASS : INTERNATIONAL CHEMISTRY EDUCATION 2010 A. Tittle : “Two-Component Phase Equilibrium” B. Day/date of starting experiment : Friday/16 th March 2012 C. Day/date Finishing experiment : Friday/16 th March 2012 D. Objective : 1. Describe the two-component phase equilibrium in phase liquid - liquid (phenol - aquadest). 2. Determine the equivalence point on two-component phase equilibrium in phase liquid - liquid (phenol - aquadest). 3. Define phase, components, and the degrees of freedom of a two-component phase equilibrium in phase liquid - liquid (phenol – aquadest). E. Basic theory Part of something that became the center of attention and study referred to as systems. A heterogeneous system consisting of various parts of the homogeneous inter-

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NAME : FIKAFAJARIYAH ARIFIN

NIM : 103194006

CLASS : INTERNATIONAL CHEMISTRY EDUCATION 2010

A. Tittle : “Two-Component Phase

Equilibrium”

B. Day/date of starting experiment : Friday/16th March 2012

C. Day/date Finishing experiment : Friday/16th March 2012

D. Objective :

1. Describe the two-component phase equilibrium in phase liquid - liquid

(phenol - aquadest).

2. Determine the equivalence point on two-component phase equilibrium in

phase liquid - liquid (phenol - aquadest).

3. Define phase, components, and the degrees of freedom of a two-component

phase equilibrium in phase liquid - liquid (phenol – aquadest).

E. Basic theory

Part of something that became the center of attention and study referred to as

systems. A heterogeneous system consisting of various parts of the homogeneous inter-

contact with clear boundaries. Homogeneous part is called the phase can be

mechanically separated.

Pressure and temperature determine the state of a material phase equilibria of the

same material. Phase equilibria of a system must meet the requirements the following:

a. The system has more than one phase although the material is the same

b. Displacement occurs reversible chemical species from one phase to another phase

c. All parts of the system have the same pressure and temperature

Phase equilibria are grouped according to the number of constituent components

the system of one component, two component and three components of Understanding

phase behavior developed by the Gibbs phase rule.

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WHAT IS MEANT BY A ‘PHASE’ ?

A phase may be defined as : any homogeneous part of a system having all

physical and chemical properties the same throughout. A system may consist of one

phase or more than one phases.

1) A system containing only liquid water is one-phase or 1-phase system (P = 1)

2) A system containing liquid water and water vapour (a gas) is a two-phase or 2-

phase system (P = 2).

3) A system containing liquid water, water vapour and solid ice is a three-phase or

3-phase system.

A system consisting of one phase only is called a homogeneous system.

A system consisting of two or more phases is called a heterogeneous system.

WHAT IS MEANT BY ‘COMPONENTS’?

A system ‘C’ in the Phase Rule equation stands for the number of components

of a system in equilibrium. The term component may be defined as : the least number of

independent chemical constituents in terms of which the composition of every phase can

be expressed by means of a chemical equation.

Gibb’s Phase Rule is free from flaws and limitations which are a common feature

of all other generalizations of Physical Chemistry based on hypothetical assumptions as

to the nature of the constitution of matter. It may be stated mathematically as follows :

F = C – P + 2

F = degree of freedom C = components P = phase

Definition of Degree of freedom

The term Degree of Freedom represented by F in the phase Rule equation (F = C

– P + 2) is defined as follows: the least number of variable factors (concentration,

pressure and temperature) which must be specified so that the remaining variables are

fixed automatically and the system is completely defined

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Nonvariant equilibria, A system with F = 0 is known as nonvariant or having no

degree of freedom. In which neither P or T can be changed; on a phase diagram,

this is represented as a singular invariant point

Univariant equilibria, A system with F = 1 is known as univariant or having one

degree of freedom. In which either P or T can be changed independently, but to

maintain the state of the system, there must be a corresponding change in the

other variable; on a phase diagram this is referred to as a univariant curve and

Bivariant equilibria, A system with F = 2 is known as bivariant or having two

degrees of freedom. In which both P and T are free to change independently

without changing the state of the system (but bounded by the conditions defined

by the univariant equilibria).

Phase Diagram

A phase diagram is a plot showing the conditions of pressure and temperature

under which two or more physical states can exist together in a state of dynamic

equilibrium. Fig. 19.1 is a

typical phase diagram for a

one-component system.

The diagram consists of :

(a) the Regions or Areas;

(b) the Lines or Curves;

and (c) the Triple point.

In discussing the

critical state of matter,

would more appropriately

deal with the three states of

matter simultaneously, instead of discussing two of the three substances. Phase

diagrams are a convenient way show states of matter as a function of temperature and

pressure. As a typical example, the phase diagram of water. In the phase diagram it is

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assumed that the substance is well isolated and no other substances that enter or exit the

system.

Water –phenol phase diagram

Phenol, also known as carbolic acid, hydroxybenzene and phenyl alcohol, is

produced at the rate of millions of tons per year, mostly from isopropyl benzene

("cumene"). However, phenol is poisonous. The phenol-water mixtures used in this lab

are concentrated and dangerous by contact or ingestion.

As the diagram at left indicates,

at low and high percentages of

phenol, water and phenol mix

completely, forming a single

liquid phase. However, at

intermediate compositions (and

below the critical temperature)

mixtures of phenol and water

separate into two liquid phases.

Point "h" in the figure is the

critical point. Above the critical

temperature, phenol and water

are completely miscible.

The water-phenol phase diagram contains a solid phase at high percent phenol,

near and somewhat above room temperature. The independent variable in the phase

diagram is composition.

At room temperature, a tube contains two liquid phases, one more dense than the

other. The tube is heated in a water bath until the two phases merge. The temperature at

which they merge is the "clearing temperature," also known as the "cloud" temperature,

and lies on the liquid-liquid coexistence line. By using several sample tubes, one obtains

several (% volume phenol, t) points on the coexistence line. We will fit a curve through

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those points, differentiate the curve to find its maximum, and use the maximum as the

critical temperature, tc.

System Two Component Liquid-Liquid

Two liquid miscible said most if A is soluble in a limited number, and so are the

B, soluble A in a limited number. The most common form of the TX phase diagram of

liquid-liquid at a constant pressure, usually 1 atm (shown above). The diagram above

can be obtained experimentally by adding a liquid substance into another pure liquids at

pressure with temperature variations.

Pure liquid B is gradually added little by little fluid A at fixed temperature (T1).

System starting at point C (pure substance B) and moves horizontally toward the right

in accordance with the addition of A. From point C to point D is obtained a single phase

(ie A is added late in B). At point D is obtained the maximum solubility in the liquid A

liquid B at temperature T1.

A further addition will generate two-phase system (two layers), the first layer

(L1) A saturated solution in B with the composition XA, 1 and the second layer (L2) a

saturated solution of B in A with the composition of the XA, 2. The second layer is

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called the conjugate layer (located together in the area between D and F). The overall

composition is between points D and F. At point E the overall composition is XA, 3.

The relative amounts of the two phases in equilibrium is determined by the lever rule.

At point E the first layer over much of the second layer. A further addition would

change the overall composition more to the right, while the composition of the coating

will remain XA, and XA 1, 2.

Differences caused by the addition of A is continuously located on the relative

amount of the first and second layers. Getting to the right amount will be reduced

relative to the first layer while the second layer will increase. A fluid at point F which is

added sufficient to dissolve all of B in A form a saturated solution of B in A. Thus the

system is in F into a single phase. From F to G, the addition of A is only a dilution

solution B in A. To reach the G spot in need of increasing the number of A is an infinite

number, or by doing experiments starting from pure substances A and B substances in

the added bit by bit until the reach the point F, and so on.

If the experiments performed at high temperature will be obtained different

solubility limits. The higher the temperature, each solubility component increased with

each other, so that the narrowing phase. Solubility curves eventually meet at a point in a

consolute above, or also called the critical solubility temperature (Tc). Above the

mutual solubility of Tc perfect fluid in a variety of compositions

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F. Tools and Materials

Tools :

Tools size Amount

Beaker Glass 500 mL 2

Beaker Glass 250 mL 1

Test tube big 2

Thermometer 0-100°C (± 0.1°C) 1

Spatula - 1

Tripod - 1

Gauze wire 10 mL 1

Spiritus burner - 1

Graduated cylinder - 1

Pipette - 3

Materials :

Aquadest

Phenol Solution

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10 ml aquadest

Test Tube A

10 ml phenol

Test Tube B

10 ml aquadest + 2 ml phenol

10 ml phenol + 2 ml aquadest

Add 2 ml phenol Add 2 ml aquadest

aquadestNote the temperature when the solution change from turbidity become colorless (T1a)

Note the temperature when the solution change from turbidity become colorless (T1b)

Beaker glass 500 ml

Boiled aquadest

boiling

Take the test tube from beaker glass, note the temperature when the solution become turbid again

Test tube A Test Tube B

T2a T2b

G. Procedure

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10 mL aquadest

T1a

-Poured into test tube A-added 2 mL phenol-stirred and observed the change-put into the boiled aquadest in beaker glass

T2a

-take from the beaker glass-Note the temperature

H. Result of experiment

No ProcedureVolume (Ml) %

Volume

of Phenol

Temperature

(°C) Conclusion

Phenol Aquades t 1 A t 2 A

1 2

10

16.667 % 62 55 C6H5OH(l)

+H2O C6H5OH(aq)

When being heated the system made one-phase equilibrium

When being cooled down, the system made two-phase equilibrium

The more volume phenol added, the higher the solubility.

4 28.571 % 43 50

6 37.5 % 35 47

8 44.44 % 33 45

10 50 % 34 43

12 54.545 % 38 40

14 58.33 % 44 49

16 61.58 % 45 50

18 64.285 % 54 51

20 66.667 % 60 54

22 68.75 % 55 49

No Procedure Volume (Ml) % Temperature Conclusion

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10 mL aquadest

T1a

-Poured into test tube A-added 2 mL phenol-stirred and observed the change-put into the boiled aquadest in beaker glass

T2a

-take from the beaker glass-Note the temperature

Volume

of Phenol

(°C)

Phenol Aquades t 1 A t 2 A

1

10

2 83.33 % 60 46 C6H5OH(l)

+H2O C6H5OH(aq)

When being heated the system made one-phase equilibrium

When being cooled down, the system made two-phase equilibrium

The more volume phenol added, the higher the solubility.

4 71.428 % 47 33

6 62.5% 47 32

8 55.55 % 43 45

10 50 % 40 47

12 45.45 % 35 50

14 41.666 % 45 51

16 38.465 % 59 50

18 35.714 % 62 59

20 33.333 % 63 58

22 31.25 % 60 58

Grouping table

No % Volume of PhenolTemperature (°C)

t 1 A t 2 A

1 16.667 62 55

2 28.571 43 50

3 31.25 35 47

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4 33.333 33 45

5 35.714 34 43

6 37.5 38 40

7 38.3615 44 59

8 41.666 45 50

9 44.44 54 51

10 45.454 60 54

11 50 55 49

12 50 60 46

13 54.545 47 33

14 55.55 47 32

15 58.333 43 45

16 61.538 40 47

17 62.5 35 50

18 64.285 45 51

19 66.667 59 50

20 68.75 62 59

21 71.428 63 58

22 83.33 60 58

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16.66728.57131.2533.33335.71437.538.361541.66644.4445.45450 50 54.54555.5558.33361.53862.564.28566.66768.7571.42883.33

0

10

20

30

40

50

60

70

Graph Relation Between % Volume Phenol & Temperature

T1T2

I. Discussion

Test Tube A

Calculating the % volume of phenol to add phenol in 10 aquades :

% volume of phenol= volumeof phenolvolum phenol+volum aquades

×100

212

x 100% = 16.667%. In adding, 16.667% is gotten from (T1) as big as 62°C,

whereas (T2) as big as 55°C.

414

x 100% = 28.571%. In adding, 28.571% is gotten from (T1) as big as 43°C,

whereas (T2) as big as 50°C.

616

x 100% = 37.5%. In adding, 37.5% is gotten from (T1) as big as 35°C,

whereas (T2) as big as 47°C.

818

x 100% = 44.4%. In adding, 44.4 is gotten from (T1) as big as 33°C, whereas

(T2) as big as 45°C.

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1020

x 100% = 50%. In adding, 50% is gotten from (T1) as big as 34°C, whereas

(T2) as big as 43°C.

1222

x 100% = 54.545%. In adding, 54.545% is gotten from (T1) as big as 38°C,

whereas (T2) as big as 40°C.

1424

x 100% = 58.333%. In adding, 58.333% is gotten from (T1) as big as 44°C,

whereas (T2) as big as 59° C.

1626

x 100% = 61.538%. In adding, 61.5%38 is gotten from (T1) as big as 45°C,

whereas (T2) as big as 50°C.

1828

x 100% = 64.285%. In adding, 64.285% is gotten from (T1) as big as 54°C,

whereas (T2) as big as 50°C.

2030

x 100% = 66.667%. In adding, 66.667% is gotten from (T1) as big as 60°C,

whereas (T2) as big as 54° C.

2232

x 100% = 68.75%. In adding, 68.75% is gotten from (T1) as big as 55°C,

whereas (T2) as big as 49°C.

Test Tube B

Calculating the % volume of phenol to add aquades in 10 phenol :

1012

x 100% = 83.333%. In adding, 83.333% is gotten from (T1) as big as 60°C,

whereas (T2) as big as 46°C.

1014

x 100% = 71.428%. In adding, 71.428% is gotten from (T1) as big as 47°C,

whereas (T2) as big as 33°C.

1016

x 100% = 62.5%. In adding, 62,5% is gotten from (T1) as big as 47°C,

whereas (T2) as big as 32°C.

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1018

x 100% = 55.5%. In adding, 55.55% is gotten from (T1) as big as 43°C,

whereas (T2) as big as 45°C.

1020

x 100% = 50%. In adding, 50% is gotten from (T1) as big as 40°C, whereas

(T2) as big as 47°C.

1022

x 100% = 45.454%. In adding, 45.454% is gotten from (T1) as big as 35°C,

whereas (T2) as big as 50°C.

1024

x 100% = 41.666%. In adding, 41.666% is gotten from (T1) as big as 45°C,

whereas (T2) as big as 51°C.

1026

x 100% = 38.461%. In adding, 38.461% is gotten from (T1) as big as 59°C,

whereas (T2) as big as 50°C.

1028

x 100% = 35.714%. In adding, 35.714% is gotten from (T1) as big as 62°C,

whereas (T2) as big as 59°C.

1030

x 100% = 33.333%. In adding, 33.333% is gotten from (T1) as big as 63°C,

whereas (T2) as big as 58° C.

1032

x 100% = 31.25%. In adding, 31.25% is gotten from (T1) as big as 60°C,

whereas (T2) as big as 58°C.

The heating of mix solution between aquades and phenol will happened one

phase equilibrium is shown with the mix solution that will become clear. But when it

cold, will happened two-phase equilibrium is shown with the color change in mix

solution.

The equation reaction is : C6H5OH(l) + H2O C6H5OH(aq)

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The temperature that we got from the adding of every 2 mL phenol and adding

of every 2 mL aquades are variation. Sometimes the temperature that we got increase

and sometimes decrease. But average from this experiment, we got the temperature is

far from the theory. Theoretically, every add 2 mL of phenol will affect in decreasing

temperature. The greater volume of phenol was added the solution of the more easily

soluble. Because the boiling point of phenol solution is lower than aquades. The higher

the temperature the solubility of each component increases.

When we added 10 mL of aquadest and 2 mL of phenol in the first test tube (A).

Phenol solution is under of aquadest, it happened because the density of phenol is

greater than aquadest.

Theoretically, As the diagram at water-phenol diagram is shown indicates, at

low and high percentages of phenol, water and phenol mix completely, forming a single

liquid phase. If we saw in water-phenol phase graph we will see that %volume of

phenol is about >50%, whereas our experiment is >50%, so it indicate that our

experiment is should pass through. If our experiment pass through, the phase when heat

is should be in one phase.

As the diagram at water-phenol diagram is shown indicates , at intermediate

compositions (and below the critical temperature) mixtures of phenol and water separate

into two liquid phases. Point "h" in the figure is the critical point. Above the critical

temperature, phenol and water are completely miscible. so it in indicates that our

experiment should pass through the critical point, and when cold is should be in two

phase. But, Our experiment is shown the changing in phase when it was added 11 times

phenol and 11 times water. It happened because, we got trouble in determining the

accuracy between when of one-phase and when two-phase occur.

Theoretically, Tc of the two-component, between phenol-water is 66.8°C,

whereas the temperature of experiment between phenol-water is less than 66.8°C, it is

happened because some error, the scale in temperature was still moving up and down,

so it is affected in our experiment results. The second error in our experiment because

the heat that produced in spirtus is not in constant condition, so it is affected in our

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results. The third error is because, we don’t know the pressure in the laboratorium that

affected in our experiment.

J. Conclusion

After we did the experiment, we can conclude that :

1. the graph of two-component phase equilibrium in phase liquid – liquid ,is

getting from combining data of %volume phenol and temperature in test tube

A and B.

2. Equivalence point in our experimental results is different so far from the

theoretical equivalence point on the phase equilibrium of two component

phenol – water, we got 45°C , but the theoretical equivalence point is 66.8 oC

3. At low and high percentages of phenol, water and phenol mix completely, forming a single liquid phase, but at intermediate compositions (and below the critical temperature) mixtures of phenol and water separate into two liquid phases. The phenol-water equilibrium system is made up of : Phasa = 1 (liquid) Component = 2 (phenol and water) Degree o freedom = c-p+2

= 2-1+2= 3

K. Question answer

1. Draw a two-component phase equilibrium in phase liquid - liquid

(phenol - water) from the data already obtained !

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16.66728.57131.2533.33335.71437.538.361541.66644.4445.45450 50 54.54555.5558.33361.53862.564.28566.66768.7571.42883.33

0

10

20

30

40

50

60

70

Graph Relation Between % Volume Phenol & Temperature

T1T2

2. From the graph above, we get the equivalence of phenol and water is

45˚C when the phenol is 58.333 % .

References

Tim Kimia Fisika II. 2011. Buku Petunjuk Praktikum Kimia Fisika II. Surabaya: Unesa

Press.

Rohman, Ijang, Sri Mulyani. 2004. Kimia Fisika I. Jica. Indonesia.

Bahl, Arun, B.S. Bahl, G.D. Tuli. 2002. Essential Of Physical Chemistry. New Delhi: S.

Chand & Company LTD.

Kartohadiprojo, Irma I. 1999. Kimia Fisika (Jilid 1, Edisi keempat). Jakarta:Erlangga

Atkins, P.W. 1999. Kimia Fisika Jilid I Edisi  keempat. Jakarta: Erlangga

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ATTACHMENTS

No. Picture Information

1.

Test tube B and test tube A

2.

One phase

3.

Two phase