NAME NIM CLASS A.

Tittle

: FIKAFAJARIYAH ARIFIN : 103194006 : INTERNATIONAL CHEMISTRY EDUCATION 2010 : Two-Component Phase Equilibrium : Friday/16th March 2012 : Friday/16th March 2012
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B. C. D.

Day/date of starting experiment Day/date Finishing experiment 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 intercontact 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.

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 2phase 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.

Gibbs 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=CP+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

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

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

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

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

F.

Tools and Materials Tools : Tools Beaker Glass Beaker Glass Test tube Thermometer Spatula Tripod Gauze wire Spiritus burner Graduated cylinder Pipette Materials : Aquadest Phenol Solution size 500 mL 250 mL big 0-100C ( 0.1C) 10 mL Amount 2 1 2 1 1 1 1 1 1 3

G.

Procedure

Test Tube A 10 ml aquadest Add 2 ml phenol 10 ml aquadest + 2 ml phenol Beaker glass 500 ml Note the temperature when the solution change from turbidity become colorless (T1a) aquadest boiling Boiled aquadest

Test Tube B 10 ml phenol Add 2 ml aquadest 10 ml phenol + 2 ml aquadest Note the temperature when the solution change from turbidity become colorless (T1b)

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

Test tube A

Test Tube B

T2a

T2b

H.

Result of experiment Temperature (C) Conclusion

Volume (Ml) No Procedure Phenol 1

10 mL aquadest -Poured into test tube A -added 2 mL phenol -stirred and observed the change -put into the boiled aquadest in beaker glass -take from the beaker glass -Note the temperature T2a

% Volume

Aquades

of Phenol 16.667 % 28.571 % 37.5 % 44.44 % 50 % 62 43 35 33 34 38 44 45 54 60 55 55 50 47 45 43 40 49 50 51 54 49 The more volume phenol added, the higher the solubility. When being cooled down, the system made twophase equilibrium C6H5OH(l) +H2O C6H5OH(aq) When being heated the system made one-phase equilibrium

2 4 6 8 10 12 14 16 18 20 22 10

54.545 % 58.33 % 61.58 % 64.285 % 66.667 % 68.75 %

T1a

Volume (Ml) No Procedure Phenol 1

10 mL aquadest -Poured into test tube A -added 2 mL phenol -stirred and observed the change -put into the boiled aquadest in beaker glass -take from the beaker glass -Note the temperature T2a

% Volume

Temperature (C) Conclusion

Aquades 2 4 6 8 10 12

of Phenol 83.33 % 71.428 % 62.5% 55.55 % 50 % 45.45 % 41.666 % 38.465 % 35.714 % 33.333 % 60 47 47 43 40 35 45 59 62 63 46 33 32 45 47 50 51 50 59 58 The more volume phenol added, the higher the solubility. C6H5OH(l) +H2O C6H5OH(aq) When being heated the system made onephase equilibrium When being cooled down, the system made twophase equilibrium

10 14 16 18 20

T1a

22

31.25 %

60

58

Grouping table Temperature ( C) No % Volume of Phenol

16.667

62

55

2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21

28.571 31.25 33.333 35.714 37.5 38.3615 41.666 44.44 45.454 50 50 54.545 55.55 58.333 61.538 62.5 64.285 66.667 68.75 71.428

43 35 33 34 38 44 45 54 60 55 60 47 47 43 40 35 45 59 62 63

50 47 45 43 40 59 50 51 54 49 46 33 32 45 47 50 51 50 59 58

22

83.33

60

58

Graph Relation Between % Volume Phenol & Temperature

70 60 50 40 30 20 10 0 83.33 71.428 68.75 66.667 64.285 62.5 61.538 58.333 55.55 54.545 50 50 45.454 44.44 41.666 38.3615 37.5 35.714 33.333 31.25 28.571 16.667 T1 T2

I.

Discussion Test Tube A Calculating the % volume of phenol to add phenol in 10 aquades :

x 100% = 16.667%. In adding, 16.667% is gotten from (T1) as big as 62C, whereas (T2) as big as 55C. x 100% = 28.571%. In adding, 28.571% is gotten from (T1) as big as 43C, whereas (T2) as big as 50C. x 100% = 37.5%. In adding, 37.5% is gotten from (T1) as big as 35C, whereas (T2) as big as 47C. x 100% = 44.4%. In adding, 44.4 is gotten from (T1) as big as 33C, whereas (T2) as big as 45C.

x 100% = 50%. In adding, 50% is gotten from (T1) as big as 34C, whereas (T2) as big as 43C. x 100% = 54.545%. In adding, 54.545% is gotten from (T1) as big as 38C, whereas (T2) as big as 40C.

x 100% = 58.333%. In adding, 58.333% is gotten from (T1) as big as 44C, whereas (T2) as big as 59 C. x 100% = 61.538%. In adding, 61.5%38 is gotten from (T1) as big as 45C, whereas (T2) as big as 50C. x 100% = 64.285%. In adding, 64.285% is gotten from (T1) as big as 54C, whereas (T2) as big as 50C. x 100% = 66.667%. In adding, 66.667% is gotten from (T1) as big as 60C, whereas (T2) as big as 54 C. x 100% = 68.75%. In adding, 68.75% is gotten from (T1) as big as 55C, whereas (T2) as big as 49C.

Test Tube B Calculating the % volume of phenol to add aquades in 10 phenol : x 100% = 83.333%. In adding, 83.333% is gotten from (T1) as big as 60C, whereas (T2) as big as 46C. x 100% = 71.428%. In adding, 71.428% is gotten from (T1) as big as 47C, whereas (T2) as big as 33C. x 100% = 62.5%. In adding, 62,5% is gotten from (T1) as big as 47C, whereas (T2) as big as 32C. x 100% = 55.5%. In adding, 55.55% is gotten from (T1) as big as 43C, whereas (T2) as big as 45C.

x 100% = 50%. In adding, 50% is gotten from (T1) as big as 40C, whereas (T2) as big as 47C. x 100% = 45.454%. In adding, 45.454% is gotten from (T1) as big as 35C, whereas (T2) as big as 50C.

x 100% = 41.666%. In adding, 41.666% is gotten from (T1) as big as 45C, whereas (T2) as big as 51C. x 100% = 38.461%. In adding, 38.461% is gotten from (T1) as big as 59C, whereas (T2) as big as 50C. x 100% = 35.714%. In adding, 35.714% is gotten from (T1) as big as 62C, whereas (T2) as big as 59C. x 100% = 33.333%. In adding, 33.333% is gotten from (T1) as big as 63C, whereas (T2) as big as 58 C. x 100% = 31.25%. In adding, 31.25% is gotten from (T1) as big as 60C, whereas (T2) as big as 58C.

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)

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 66.8C, whereas the temperature of experiment between phenol-water is less than 66.8C, 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 results. The third error is because, we dont 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 45C , 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 Question answer 1. Draw a two-component phase equilibrium in phase liquid - liquid

K.

(phenol - water) from the data already obtained !

Graph Relation Between % Volume Phenol & Temperature

70 60 50 40 30 20 10 0 83.33 71.428 68.75 66.667 64.285 62.5 61.538 58.333 55.55 54.545 50 50 45.454 44.44 41.666 38.3615 37.5 35.714 33.333 31.25 28.571 16.667 T1 T2

2.

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

45C 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

ATTACHMENTS
No. 1. Picture Information Test tube B and test tube A

2.

One phase

3.

Two phase