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B. OBJECTIVE OF EXPERIMENT
1. Draw the phase diagram of ternary system. Ternary system is the system that
form a pair of liquid substance that partially miscible that is chloroform,
water, and acetic acid mixture
2. Determine the location of pleit point in the phase diagram
C. LITERATURE REVIEW
Physical chemistry is a field in chemistry that studies the physical aspects
of matter and energy and their mechanisms of change. Physical chemistry is
generally divided into the fields of thermodynamics, kinetics and quantum.
Chemical thermodynamics studies matter and the energy that accompanies it,
which in essence studies the basic laws of thermodynamics, while kinetics is a
field that studies aspects of the process of changing a material in a reaction or
other interaction. In kinetics, several techniques to determine the mechanism of a
reaction are also studied (Fatimah, 2015: 2).
Phase is a homogeneous part of a system, that can separated in these
method of mechanically; homogenous in the chemical composition and also the
physical properties. So a system that contain liquid and vapor for each of them
have a part of homogeneous area. The system that area just consist of mixture in
gas form, there is only one phase of these equilibrium states because gas always
mixed homogenously. In a system that just consist of liquids at the equilibrium of
can be found one phase or more, its depend of the solution properties about the
solubility (Rohman, 2002:155).
The phase diagram of a substance is a map showing the conditions of
temperature and pressure at which its various phases are thermodynamically most
stable. For example, at point A in the illustration, the vapor phase of the
substance is thermodynamically the most stable, but at C the liquid phase is the
most stable. The boundaries between regions in a phase diagram, which are called
phase boundaries, show the values of p and T at which the two neighboring
phases are in equilibrium. For example, if the system is arranged to have a
pressure and temperature represented by point B, then the liquid and its vapor are
in equilibrium (like liquid water and water vapor at 1 atm and 100°C). If the
temperature is reduced at constant pressure, the system moves to point C, where
the liquid is stable (like water at 1 atm and at temperatures between 0°C and
100°C). If the temperature is reduced still further to D, then the solid and liquid
phases are in equilibrium (like ice and water at 1 atm and 0°C). A further
reduction in temperature to E takes the system into the region where the solid is
the stable phase (Atkins, 2011: 99-100).
A phase equilibrium involves the same chemical species present in
different phases. A reaction equilibrium involves different chemical species,
which may or may not be present in the same phase. Phase equilibrium is
considered in this section, reaction equilibrium in the next. The condition for
material equilibrium in a closed system with P - V which holds for any possible
infinitesimal change in the mole numbers. Consider a several-phase system that is
in equilibrium. For a closed system with P-V work only in thermal and
mechanical equilibrium, the phase equilibrium condition is that the chemical
potential of a given substance is the same in every phase of the
system (Levine, 2009:129).
Two phases are said to be in equilibrium if the temperature, pressure, and
chemical potential of each component involved in the two phases are equal. The
things that affect the balance system are: Pressure (P), Temperature (T), the
concentration of component A in the liquid phase (x) and the concentration of
component A in the vapor phase (y) (Nisa, 2017: 38).
Solubility is the maximum quantity of a dissolved chemical (solute) to
dissolve in a certain solvent to form a homogeneous solution. The solubility of a
basic substance is highly dependent on the physical and chemical
properties of the solute and solvent at temperature, pressure and pH of the
solution (Sari, 2016: 363).
Two-component phase diagrams can be complicated. Without the phase
rule, they would seem to have a bewildering array of unrelated behaviors. Many
two-component phase diagrams, however, can be broken down into combinations
of three simple diagrams. Two-component phase diagrams are characterized by
one more degree of freedom than pure one-component diagrams because of the
added composition variable
f=C−P+2=2−P+2=4–P
We can express composition in many ways, but the mole fraction of a two-
component system is most convenient for our purposes.
XB = nB /nA + nB
(Rogers, 2011:134).
Two component system is usually called binary have the amount of two
component (c=2), therefore the phase rule (f=c-p+2) became f=4-p. For one phase
system (p=1). The freedom degrees (f) equals to three. So, there are three
intensive variables of independent that need to state the system condition, that is
T, P, and mole fraction. Usually one from three variable are made constant. So the
other variables can be draw in a phase diagram of two dimension. The variable
that usually chose be stable are P or T (Rohman, 2002:170).
The systems which include mixture of ternary components: a polymer, a
solvent and a third component (such as non-solvent). This ternary system is
completely miscible over a certain composition range, but a miscibility gap has
appeared at composition over this certain composition range, as shown which
indicates an isothermal phase diagram of the ternary components. The pure
components are represented at the corners of the triangle while boundary lines
between any two corners of triangle represent mixtures of two components, and
any point inside the triangle diagram represents a mixture of all three components.
The main elements of ternary-phase diagram are: binodal and spinodal curves, a
critical point, tie lines, and a glassy region. For the studied ternary system, the
evaluation of interaction parameters for the binary mixture has allowed a
remarkably accurate prediction of the ternary phase diagram (Elgendi, 2012:62).
Suppose a small amount of a liquid B is added to a sample of another
liquid A at a temperature T′. It dissolves completely, and the binary system
remains a single phase. As more B is added, a stage comes at which no more
dissolves. The sample now consists of two phases in equilibrium with each other
(P = 2), the most abundant one consisting of A saturated with B, the minor one a
trace of B saturated with A. In the temperature–composition diagram drawn the
composition of the former is represented by the point a′ and that of the latter by
the point a″. The relative abundances of the two phases are given by the lever
rule (Atkins, 2006:185).
Type II phase diagrams describe liquid–liquid systems in which the
components are completely miscible at some temperatures but undergo phase
separation at others. Systems with a composition and temperature above the
dome-shaped coexistence curve are completely miscible. Those with a
temperature and composition below the curve split into two phases. The transition
can be brought about by cooling a miscible solution so that the temperature drops
along a vertical and enters the two phase zone or it can be brought about at
constant temperature (Rogers, 2011:136).
Any point lying on a phase boundary represents a pressure and
temperature at which there is a ‘dynamic equilibrium’ between the two adjacent
phases. A state of dynamic equilibrium is one in which a reverse process is taking
place at the same rate as the forward process. Although there may be a great deal
of activity at a molecular level, there is no net change in the bulk properties or
appearance of the sample. For example, any point on the liquid–vapor boundary
represents a state of dynamic equilibrium in which vaporization and condensation
continue at matching rates. Molecules are leaving the surface of the liquid at a
certain rate, and molecules already in the gas phase are returning to the liquid at
the same rate; as a result, there is no net change in the number of molecules in the
vapor and hence no net change in its pressure. Similarly, a point on the solid–
liquid curve represents conditions of pressure and temperature at which molecules
are ceaselessly breaking away from the surface of the solid and contributing to the
liquid. However, they are doing so at a rate that exactly matches that at which
molecules already in the liquid are settling onto the surface of the solid and
contributing to the solid phase (Atkins, 2011:100).
A three-component (or ternary) system has f = 3-p+2=5-p. For p =1, there
are 4 degrees of freedom. To make a two-dimensional plot, we must hold two
variables fixed (instead of one, as with binary systems). We shall hold both T and
P fixed. For a one-phase system, the two variables will be taken as xA and xB, the
mole fractions of components A and B. For multiphase systems, xA and xB will
be taken as the overall mole fractions of A and B in the system. Once xA and xB
are fixed, xC is fixed. We could use a rectangular plot with xA and xB as the
variables. However, Gibbs suggested the use of an equilateral-triangle plot, and
this has become standard for ternary systems (Levine, 2009: 385).
Any mixture of three components can be represented within an equilateral
triangle. All points within the triangle represent one and only one of the infinitely
many possible mixtures. Because there are now three composition variables f = C
− P + 2 = 3 − P + 2, both T and p are held constant for the three-component
triangular representation on a two-dimensional surface. If only one phase is
present, all solutions are permitted and the composition can take any point in the
triangular 2-space. When two phases are present, the composition is restricted to
the locus of points on the coexistence curve. Like the Type II phase diagram,
many three-component phase diagrams are known having a dome-shaped
coexistence curve. They are widely used for characterizing and selecting solvents
used in industrial processes. Intersections of tie lines with the coexistence curve
indicate the composition of phases in two-phase systems formed when the total
composition point is below the coexistence curve (Roger, 2011:138).
Variety of ternary mixtures of known composition within the two-phase
region were prepared and used to give different data points. After complete
separation of samples were carefully taken from each phase and analyzed to
obtain the tie lines data, volume and weight were also determined. The results
indicate that for the system, chloroform-acetic acid-water; water is a suitable
solvent for removing acetic acid from chloroform and that acetic acid solubility in
water is very large compared with its solubility in chloroform. . Correlation models
were applied to assess the reliability of the experimental tie line data of the two
ternary systems (Alamin, 2017: 29).
The boundaries of the phase fields are in satisfactory agreement with the
experimental results. Increasing of the copper content in the alloys leads to
expansion of the homogeneity range of the phase in the ternary system. The
obtained thermodynamic model of the liquid phase was used to calculate the
cupola of stable and metastable separation of the melt. A projection of the cupola
where the solid lines correspond to the stable separation and the dashed lines
represent its metastable continuation for super cooled liquid alloys. The
magnitude of super cooling required for metastable separation of the liquid phase
can be calculated as the difference between the temperatures of equilibrium
liquidus (Dreval, 2010:135, 137).
E. WORK PROCEDURE
1. 2 pieces of burette 50 mL was prepared.
2. Every unit of burette 50 mL was filled with H2O and CH3COOH glacial.
3. 5 pieces of Erlenmeyer flask was prepared.
4. Every unit of Erlenmeyer flask was filled with CHCl 3 by 1,5ml , 2ml, 2,5
ml, 3ml and 3,5 ml. This activities was did one by one for every volume of
CHCl3.
5. 2,5 mL of H2O was inserted into Erlenmeyer flask that filled 1,5 mL of
CHCl3.
6. The mixture solution was titrated with CH3COOH glacial until formed one
phase of solution (homogeneous solution).
7. This activities was repeated for Erlenmeyer flask that filled 2 mL of CHCl3
and so on.
8. Diagram of ternary phase was maked by the calculation of P composition.
F. OBSERVATION RESULT
Mass of Mass of
Volume of
Chemicals empty Picnometer Density
Solution
Picnometer Solution
Aquadest 30. 573 gr 80. 600 gr 50 mL 1.0 gr/mL
Chloroform 30. 575 gr 104. 573 gr 50 mL 1.47 gr/mL
Acetic Acid 31. 193 gr 83. 099 gr 50 mL 1.023 gr/mL
Volume Station
Liquid Component
I II III IV V
Chloroform 1.5 mL 2 mL 2.5 mL 3 mL 3.5 mL
Aquadest 2.5 mL 2.5 mL 2.5 mL 2.5 mL 2.5 mL
Glacial Acetic Acid 3.1 mL 4.5 mL 4.9 mL 7 mL 6 mL
G. ANALYSIS DATA
1. Titration I
Known : Volume CHCl3 = 1,5 mL
Volume H2O = 2,5 mL
Volume CH3COOH = 3,1 mL
ρCHCL3 = 1,47 gr/mL
ρH2O = 1 gr/mL
ρCH3COOH = 1,05 gr/mL
Mr CHCL3 = 119,5 g/mol
Mr H2O = 18 g/mol
Mr CH3COOH = 60 g/mol
Asked : a. XCHCL3
b. X H2O
c. X CH3COOH
Solution :
a. m CHCL3 = VCHCL3× ρCHCL3
= 1,5 mL×1,47 gr /mL
= 2,20 gram
m
n CHCL3 =
Mr
2,20 gram
=
119,5 g /mol
= 0,018 mol
b. m H2O = VH2O× ρH2O
= 2,5 mL×1 gr /mL
= 2,5 gram
m
n H2O =
Mr
2,5 gram
=
18 g / mol
= 0,138 mol
c. mCH3COOH = VCH3COOH× ρCH3COOH
= 3,1 mL×1,05 gr /mL
= 3,255 gram
m
n CH3COOH =
Mr
3,255 gram
=
60 g /mol
= 0,054 mol
n total = n CHCL3 + n H2O + n CH3COOH
= 0,018 mol + 0,138 mol + 0,054 mol
= 0,21 mol
So, for the X value respectively:
n
a. XCHCL3 =
n total
0,018 mol
=
0,21 mol
= 0,085
n
b. X H2O =
n total
0,138 mol
=
0,21 mol
= 0,65
n
c. X CH3COOH =
n total
0,054 mol
=
0,21 mol
= 0,257
2. Titration II
Known : Volume CHCL3 = 2 mL
Volume H2O = 2,5 mL
Volume CH3COOH = 4,5 mL
ρCHCL3 = 1,47 gr/mL
ρH2O = 1 gr/mL
ρCH3COOH = 1,05 gr/mL
Mr CHCL3 = 119,5 g/mol
Mr H2O = 18 g/mol
Mr CH3COOH= 60 g/mol
Asked : a. X CHCL3
b. X H2O
c. X CH3COOH
Solution :
a. m CHCL3 = V CHCL3 × ρCHCL3
= 2 mL ×1,47 gr /mL
= 2,94 gram
m
n CHCL3 =
Mr
2,94 gram
=
119,5 g /mol
= 0,024mol
b. m H2O = V H2O× ρH2O
= 2,5 mL×1 gr /mL
= 2,5 gram
m
n H2O =
Mr
2,5 gram
=
18 g / mol
= 0,138 mol
c. m CH3COOH = V CH3COOH× ρCH3COOH
= 4,5 mL× 1,05 gr /mL
= 4,725 gram
m
n CH3COOH =
Mr
4 ,725 gram
=
60 g /mol
= 0,078 mol
n total = n CHCL3 + n H2O + n CH3COOH
= 0,024 mol + 0,138 mol + 0,078 mol
= 0,24 mol
So, for the X value respectively:
n
a. X CHCL3 =
n total
0,024 mol
=
0,24 mol
= 0,1
n
b. X H2O =
n total
0,138 mol
=
0,24 mol
= 0,57
n
c. X CH3COOH =
n total
0,078 mol
=
0,24 mol
= 0,325
3. Titration III
Known : Volume CHCL3 = 2,5 mL
Volume H2O = 2,5 mL
Volume CH3COOH = 4,9 mL
ρCHCL3 = 1,47 gr/mL
ρH2O = 1 gr/mL
ρCH3COOH = 1,05 gr/mL
Mr CHCL3 = 119,5 g/mol
Mr H2O = 18 g/mol
Mr CH3COOH= 60 g/mol
Asked : a. X CHCL3
b. X H2O
c. X CH3COOH
Solution :
a. m CHCL3 = V CHCL3 × ρCHCL3
= 2,5 mL×1,47 gr /mL
= 3,675 gram
m
n CHCL3 =
Mr
3,675 gram
=
119,5 g /mol
= 0,030 mol
b. m H2O = V H2O× ρH2O
= 2,5 mL×1 gr /mL
= 2,5 gram
m
n H2O =
Mr
2,5 gram
=
18 g / mol
= 0,138 mol
c. m CH3COOH = V CH3COOH× ρCH3COOH
= 4,9 mL× 1,05 gr /mL
= 5,145 gram
m
n CH3COOH =
Mr
5,145 gram
=
60 g /mol
= 0,085 mol
n total = n CHCL3 + n H2O + n CH3COOH
= 0,030 mol + 0,138 mol + 0, 085 mol
= 0,253 mol
So,for the X value respectively:
n
a. X CHCL3 =
n total
0,030 mol
=
0,253 mol
= 0,118
n
b. X H2O =
n total
0 ,138 mol
=
0,253 mol
= 0,545
n
c. X CH3COOH =
n total
0,085 mol
=
0,253 mol
= 0,336
4. Titration IV
Known : Volume CHCL3 = 3 mL
Volume H2O = 2,5 mL
Volume CH3COOH = 7 mL
ρCHCL3 = 1,47 gr/mL
ρH2O = 1 gr/mL
ρCH3COOH = 1,05 gr/mL
Mr CHCL3 = 119,5 g/mol
Mr H2O = 18 g/mol
Mr CH3COOH= 60 g/mol
Asked : a. X CHCL3
b. X H2O
c. X CH3COOH
Solution :
a. m CHCL3 = V CHCL3 × ρCHCL3
= 3 mL ×1,47 gr /mL
= 4,41 gram
m
n CHCL3 =
Mr
4,41 gram
=
119,5 g /mol
= 0,036 mol
b. m H2O = V H2O× ρH2O
= 2,5 mL×1 gr /mL
= 2,5 gram
m
n H2O =
Mr
2,5 gram
=
18 g / mol
= 0,138 mol
c. m CH3COOH = V CH3COOH× ρCH3COOH
= 7 mL × 1,05 gr /mL
= 7,35 gram
m
n CH3COOH =
Mr
7,35 gram
=
60 g /mol
= 0,1225 mol
n total = n CHCL3 + n H2O + n CH3COOH
= 0,036 mol + 0,138 mol + 0,1225 mol
= 0,2965 mol
So,for the X value respectively:
n
a. X CHCL3 =
n total
0,036 mol
=
0,2965 mol
= 0,1214
n
b. X H2O =
n total
0 , 138 mol
=
0,2965 mol
= 0,465
n
c. X CH3COOH =
n total
0,1225 mol
=
0,2965 mol
= 0,413
5. Titration V
Known : Volume CHCL3 = 3,5 mL
Volume H2O = 2,5 mL
Volume CH3COOH = 6 mL
ρCHCL3 = 1,47 gr/mL
ρH2O = 1 gr/mL
ρCH3COOH = 1,05 gr/mL
Mr CHCL3 = 119,5 g/mol
Mr H2O = 18 g/mol
Mr CH3COOH= 60 g/mol
Asked : a. X CHCL3
b. X H2O
c. X CH3COOH
Solution :
a. m CHCL3 = V CHCL3 × ρCHCL3
= 3,5 mL×1,47 gr/ mL
= 5,145 gram
m
n CHCL3 =
Mr
5,145 gram
=
119,5 g /mol
= 0,043 mol
b. m H2O = V H2O× ρH2O
= 2,5 mL×1 gr /mL
= 2,5gram
m
n H2O =
Mr
2, 5 gram
=
18 g/mol
= 0,138 mol
c. m CH3COOH = V CH3COOH× ρCH3COOH
= 6 mL × 1,05 gr /mL
= 6,3 gram
m
n CH3COOH =
Mr
6,3 gram
=
60 g /mol
= 0,105 mol
n total = n CHCL3 + n H2O + n CH3COOH
= 0,043 mol + 0,138 mol + 0, 105mol
= 0,286 mol
So,for the X value respectively:
n
a. X CHCL3 =
n total
0,043 mol
=
0,286 mol
= 0,150
n
b. X H2O =
n total
0 ,138 mol
=
0,286 mol
= 0,482
n
c. X CH3COOH =
n total
0,105 mol
=
0,286 mol
= 0,367
Mole reaction table :
Titration XCHCl3 XH O
2 XCH COOH
3
0.9 0.1
0.8 0.2
0.7 0.3
0.6 0.4
0.5 0.5
0.4 0.6
0.3 0.7
0.2 0.8
0.1 0.9
0 1
XCHCl3 1 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0 XH2O
H. DISCUSSION
Diagram terner merupakan diagram yang menggambarkan komposisi tida
campuran yang tidak saling bercampur. Sistem tiga komponen membentuk
sepasang zat cair yang saling bercamour sebagian yang artinya antara larutan satu
dengan larutan lain membentuk dua fasa tetapi ketika ditambahkan larutan tiga,
maka larutan tiga tersebut akan memperbesar atau memperkecil daya saling larut
A dan B. Adapun tujuan dalam percobaan ini adalah menggambarkan diagram
fase sistem terner dan memperhatikan atau menentukan letak “pleit point” atau
titik jalin pada diagram fasenya. Sistem terner yang dimaksud yaitu sistem yang
membentuk sepasang zat cair yang bercampur sebagian yaitu campuran
kloroform-air dan asam asetat.
1. Penentuan massa jenis
Percobaan ini dilakukan untuk menentukan massa jenis larutan yakni
kloroform, air dan asam asetat glasial. Penentuan massa jenis perlu dilakukan
untuk mempermudah dalam perhitungan fraksi mol setiap larutan. penentuan
massa jenis larutan dapat dilakukan dengan menggunakan piknometer. Prinsip
piknometer didasarkan atas penentuan massa cairan dan penentuan ruang yang
ditempati larutan tersebut. Langkah awal yang dilakukan yaitu, piknometer dicuci
terlebih dahulu dengan air. Hal ini bertujuan untuk membersihkan piknometer
dari zat pengotor. Selanjutnya dikeringkan untuk menghilangkan sisa-sisa air yang
dapat mempengaruhi berat piknometer.
Piknometer kosong kemudian ditimbang dan diisi dengan larutan
CH3COOH, CHCl3 dan H2O lalu ditimbang kembali. Dari penimbangan tersebut
dapat diperoleh massa yang digunakan dalam penentuan massa jenis.
Berdasarkan hasil analisis data diperoleh massa jenis tiap-tiap larutan yaitu,
kloroform sebesar 1,47 g/mL, air sebesar 1,0 g/mL, dan asam asetat glasial
sebesar 1,023 g/mL.
Kemudian sediakan 5 erlenmeyer yang akan diisi larutan kloform dengan volume
1,5 mL, 2 mL, 2,5 mL, 3 mL, 3,5 mL.
Setelah erlenmeyer diisi oleh kloform kemudian diisi dengan aquadest sebanyak 2
mL kemudian kocok hingga terbentuk dua fase.
Gambar 2.4 : Kloroform + 2 mL Aquadest
J. SUGGESTION
It is expected that when weighing, the pycnometer must be in a dry state
and be more careful when performing titrations so that the results obtained can be
in accordance with the theory.