APPROVAL SHEET

The complete report of Physical Chemistry I Experiment entitled

“Determination of The Equilibrium Constant of The Triodide Ions” that
arranged by:
name : Muh. Aqrim S
ID : 1913441012
class : ICP of Chemistry Education
group : I (One)
It has been checked and corrected by assistant and assistant coordinator, so this
report was accepted.

Makassar, March 31th 2021

Assistant Coordinator Assistant,

Putri Sarimurti Yuliana

ID.1613142009 ID. 1713142006

Known by,
Responsibility lecturer

Diana Eka Pratiwi, S.Si, M.Si

ID. 19741027 00002 2 001
A. TITLE OF EXPERIMENT
Determination of The Distribution Coefficient

B. OBJECTIVE OF EXPERIMENT
Determine the Distribution Coefficient of I2 in a Water-Chloroform
System.

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).
Liquid-liquid extraction is a technique in which solution of usually
aqueous is brought into contact with a second solvent that (usually organic),
essentially immiscible with the first in order toal bring about a trans of one or
more solutes into the second solvent. The separation that can be performed are
simple, clean, rapid and convenient. In many case separation may be effected by
shaking in a separation funnel for a few minutes. The technique is equally
applicable to trace level and large amounts of material (Jeffery, 1989:161).
The term liquid–liquid partition coefficient is “not recommended” by
IUPAC in its 1993 nomenclature for liquid–liquid distribution. Since this term
was widely used, “not recommended” is read as “not forbidden” and it continues
to be preferred to the “recommended” terms that are distribution constant or
partition ratio whose symbol should be KD. To be understood by
chromatographers, the term partition coefficient will be used throughout this
article with the correct symbol, KD, but the IUPAC definitions are recalled here.
IUPAC points the common confusion made between distribution ratio and
distribution constant (Berthod, 2016: 4).
The liquid used for extracting must be immiscible with the solution to
beextract. In extracting a solution it isshaken in a separatory funnel with a liquid
in which the substanceto be extracted is readily soluble. The substances
commonlyused for this purpose are ether, chloroform, benzene, petroleumether or
ligroin, and carbon disulphide. Ether is generallyused as it is an excellent solvent
for many organic compounds,and, on account of its low boiling-point, it can be
readily removed.The disadvantages connected with the use of ether are its
greatinflammability and the fact that it is somewhat soluble in waterand dissolves
appreciable quantities of water (Norris, 1924: 21).
This observation was consistent with the limitnutrient in the regions,
which happened due to the impactof wind-induced mixing bringing nutrient-rich
and also theeffect of low SST water moving from subsurface to themixed layer
resulting in the promotion of positivedistribution of chlorophyll-a and negative
SST (Iskandar, 2017: 1550).
The process of a solute dissolved in one solvent being pulled out, or
“extracted” into a new solvent actually involves an equilibrium process. At the
time of initial contact, the solute will move from the original solvent to the
extracting solvent at a particular rate, but, after a time, it will begin tomove back
to the original solvent at a particular rate. Solvent extraction is governed by the
Nernst Distribution or Partition Law.This states that at constant temperature and
pressure, a solute, S, will always bedistributed in the same proportions between
two particular immiscible solvents.The ratio of the equilibrium concentrations
(strictly their activities inthe two phases defines a distribution or partition
coefficient, KD. Where denotes concentrations (activities) of the distributing
solute species, S,and the value of KD is independent of the total solute
concentration. In practice,the solute often exists in different chemical forms
due to dissociation (ionization),protonation, complexation or polymerization,
so a more practically usefulexpression which defines a distribution or partition
ratio (Kealey, 2002: 110)
 Thus, the amount that gets extracted depends on the relative distribution
between the two layers, which, in turn, depends on the solubilities in the two
layers. A distribution coefficient analogous to an equilibrium constant (also called
the partition coefficient) can be defined as follows:
[ A ] ext
K=
[ A ] orig
Uses of the distribution coefficient include: 1) the calculation of the amount of a
solute that is extracted in a single extraction step, 2) the determination of the
weight of the solute in the original solute (important if you are quantitating the
solute in this solvent), 3) the calculation of the optimum volumes of both the
extracting solvent and the original solution to be used, 4) the number of
extractions needed to obtain a particular quantity or concentration in the extracting
solvent, and 5) the percent extracted. The following expansion is useful for these:
Wext
Vext
K=
Worig
Vorig
in which Wext is the weight of the solute extracted into the extracting solvent,
Vext is the volume of the extracting solvent used, Worig is the weight of the
solute in the original solvent, and Vorig is the volume of the original solventused
(Kenkel, 2003: 304).
It is a well-known fact that certain substances are more soluble in some
solvents than in others. Thus iodine is very much more soluble in carbon
disulphide, chloroform, or carbon tertrachloride than it is in water. If iodine is
shaken with a mixture of carbon disulphide and water and then allowed to settle,
the iodine will be found to be distributed between the two solvents. Another
important reactant in redox titrimetry is potassium iodide, KI. KI is a reducing
agent (2I- I2 + 2e-) that is useful in analyzing for oxidizing agents. The
interesting aspect of the iodide–iodine chemistry is that it is most often used as an
indirectmethod (recall the indirect Kjeldahl titration involving boric acid
discussed previously). This means that the oxidizing agent analyte is not measured
directly by a titration with KI, but is measured indirectly by the titration of the
iodine that forms in the reaction. The KI is actually added in excess, since it need
not be measured at all. The experiment is called iodometry. This titrant is
normally sodium thiosulfate (Na2S2O3).An important application of iodometry can
be found in many wastewater treatment plant laboratories. Chlorine, Cl 2, is used in
a final treatment process prior to allowing the wastewater effluent to flow into a
nearby river. Of course, the chlorine in both the free and combined forms can be
just as harmful environmentally as many components in the raw wastewater.
Thus, an important measurement for the laboratory to make is the amount of
residual chlorine remaining unreacted in the effluent. Such chlorine, which is an
oxidizing agent, can be determined by iodometry (Kenkel, 2003: 133).
The constant Kd is known as the partition, or distribution, coefficient. The
distribution or partition law may be formulated thus: when a solute distributes
itself between two immiscible solvents there exists for each molecular species, at
a given temperature, a constant ratio of distribution between the two solvents, and
this distribution ratio is independent of any other molecular species which may be
present. The value of the ratio varies with the nature of the two solvents, the
nature of the solute, and the temperature (Svehla, 1979: 130).
No actual solutions are ideal, and many solutions deviate from ideal-dilute
behavior as soon as the concentration of solute rises above a small value. In
thermodynamics we try to preserve the form of equations developed for ideal
systems so that it becomes easy to step between the two types of system.6 This is
the thought behind the introduction of the activity, aJ, of a substance, which is a
kind of effective concentration. The activity is defined so that the expression
mo J = mJ + RT ln aJ
is true at all concentrations and for both the solvent and the solute. For ideal
solutions, aJ = xJ, and the activity of each component is equal to its, mole
fraction. For ideal-dilute solutions using the definition in eqn 3.21, aB = [B], and
the activity of the solute is equal to the numerical value of its molar concentration.
For non-ideal solutions we write
For the solvent: aA = jAxA
For the solute: aB = jB[B]
where the _ (gamma) in each case is the activity coefficient. Activity coefficients
depend on the composition of the solution (Atkins, 2006: 133).
The observed and predictedlog Kd values were compared and
the consistency between these twosets of log Kd indicated that the
adsorption models developed in this study could predict the distribution
coefficients (Tang, 2019: 1304)
It is necessary to look for the relationship between plutonium
concentrations in water and sediment in the form of distribution coefficient values
denoted by the Kd value to see the distribution and displacement of plutonium in
water bodies. The Kd value is used in calculating the retardation factor (Rf)
which is commonly used in transport models that describe the interactions
between contaminants. and geological materials such as sediment, soil
and rock (Makmur, 2016: 86).
Another example is the determination of the distribution coefficient of
rhenium and tungsten with tungsten with the extraction method using methyl ethyl
ketone as solvent. In this study it can be concluded that the research process of
Rhenium and Wolfram can be carried out using methyl ethyl ketone (MEK)
extraction. more and more. The higher the pH of the solution, the less rhenium is
removed. The KD of rhenium is greater than Wolfram. The time of shaking, the
volume of the MEK solvent and the pH setting of the solution did not affect the
tungsten extraction process (Hidayat, 2015: 105).
In both extraction and stripping, when the aqueous solution is contacted
with solvents that do not dissolve each other, the extracted components will be
found to be distributed between the two phases, namely the organic phase and the
aqueous phase. This distribution can be expressed by the distribution coefficient.
One of the important factors in the extraction-stripping separation is the
distribution coefficient, which is expressed in Eq

[ Unsur ] organik
Kd=
[ Unsur ]aqueous
The distribution coefficient value for extraction is expected to be high,
while the distribution coefficient value for stripping is expected to be
low (Ferliana, 2016: 28).
If into a two-phase liquid system that cannot mix with each other, a third
substance that can dissolve in both of them is added, the third substance will be
distributed between the two phases in a certain amount. When the saturated
solution of I2 in CHCl3 is shaken with water that is not soluble in CHCl3,
then I2 will be divided into water and in CHCl3 at a constant temperature.
This situation is a direct result of the law of thermodynamics in
equilibrium (Tim Penyusun, 2021: 11).

D. APPARATUS AND CHEMICALS

1. Apparatus
a. Beaker 200 mL (1 piece)
b. Beaker 250 mL (1 piece)
c. Graduted cylinder 50 mL (2 pieces)
d. Graduted cylinder 10 mL (2 pieces)
e. Erlenmeyer flask 250 mL (4 pieces)
f. Burette 50 mL (2 pieces)
g. Separation funnel (1 piece)
h. Stative and Clamp (2 pieces)
i. Drop pipette (2 pieces)
j. Funnel (1 piece)
k. Stirrer (1 piece)
l. Spray bottle (1 piece)
2. Chemicals
a. Saturated Solution of I2 in CHCl3 (I2 In CHCl3)
b. Sodium Thiosulphate Solution 0,02 M (Na2S2O3)
c. Aquadest (H2O)
d. Tissue
E. WORK PROCEDURES
1. 135 mL of I2 in CHCl3 was filled in Erlenmeyer 250 mL.
2. 100 mL of H2O was filled in Erlenmeyer 250 mL.
3. Erlenmeyer was filled in Separating funnel 250 mL.
4. Separating funnel was shaked until 15 minutes.
5. Separating funnel was leaved until form 2 layer.
6. 4 pieces of Erlenmeyer 250 mL was prepared
7. Bottom layer and top layer was taken into Erlenmeyer different.
8. 2 pieces of burette 50 mL was prepared.
9. Bottom layer of solution was titrated with Na 2S2O3 0,02 M until colorless
of solution.
10. Top layer of solution was titrated with Na2S2O3 0,02 M until colorless of
solution.
11. This activities was repeated for next Erlenmeyer flask.
12. Volume of Na2S2O3 0,02 M was recorded by use the titrated.

F. OBSERVATION RESULT
No Activity Result
1. 135 ml of I2 in CHCl3 Purple Soltion

2. 100 ml of H2O Colorless Solution

2 layer solution
3. Shake until 15 minutes Water (Top) is Colorless
Chloroform (Down) is dark purple
Titration 1: 6,1 ml (colorless)
Bottom layer was titrated
4. Titration 2: 5,5 ml (colorless)
with Na2S2O3
Titration 3 : 5,2 mL (colorless)
Titration 1: 1,2 ml (colorless)
Top layer was titrated with
5. Titration 2: 1,2 ml (colorless
Na2S2O3
Titration 3: 1,2 ml (colorless)

G. ANALYSIS DATA
Known:
M [Na2S2O3] = 0,02 M
V I2 in CHCl3 solution = 2,5 mL
V I2 in H2O solution = 2,5 mL
Volume Na2S2O3 of titration I2 in CHCl3
Titration I = 6,1 mL
Titration II = 5,5 mL
Titration III = 5,2 mL
Volume Na2S2O3 of titration I2 in H2O
Titration I = 1,2 mL
Titration II = 1,2 mL
Titration III = 1,2 mL
Asked: (Kd) = ...?
Answer :
The reaction :
Na2S2O3 2Na++ S2O32-
Reduction = I2 + 2e- 2I
Oxidation = 2SO2O3 S4O62- + 2e-
I2 + 2S2O3 2I- + S4O52-
The complex reaction:
2Na2S2O3(aq) + I2(aq) 2 NaI(aq) + Na2S4O6(aq)
(sodium thiosulfate) (iod) (sodium iodide) (sodium tetrationate)
From the reaction : 2 mmol Na2S2O3 : 1 mmol I2
1 mmol Na2S2O3 : ½ mmol I2

1. Bottom Layer (I2in CHCl3)

The average volume of Na2S2O3in titration I2 in CHCl3
( 6,1+5,5+5,2 ) mL
=
3
= 5,6 mL
nNa2S2O3 = [Na2S2O3] x V Na2S2O3
= 0,02 mol/mL x 5,6 mL
 = 0,112 mol
1
n I2in CHCl3 = x mmol Na2S2O3
2
1
= x 0,112 mmol
2
= 0,056 mmol
So, consentration I2 in CHCl3
mol I 2 in CHCl 3
[I2] CHCl3 =
v I2 in CHCl3
0,056 mmol
=
2,5 mL
= 0,0224 M
2. Top Layer (I2in H2O)
The average volume ofNa2S2O3in titration I2in CHCl3
(1,2+1,2+1,2 ) mL
¿
3
= 1,2 mL
nNa2S2O3 = [Na2S2O3] x V Na2S2O3
= 0,02 mol/L x 1,2 mL
= 0,024 mmol
1
n I2 dalam H2O = x mmol Na2S2O3
2
1
= x 0,024 mmol
2
= 0,012 mmol
So Concentration I2 in H2O :
mol I 2 in H 2O
[I2] H2O =
v I2 in H2 O
0,012 mmol
=
2,5 mL
= 0,0048 M

So, distribution coefficient

 [I 2 ] CHCl3
Distribution Coefficient (Kd) =
[I 2] H2 O
0,0224 M
=
0, 0048 mL
= 4,67 M

H. DISCUSSION
Menurut hukum distribusi Nernst, bila kedalam dua pelarut yang tidak
saling bercampur dimasukkan solute yang dapat larut dalam kedua pelarut
tersebut maka akan terjadi pembagian kelarutan. Kedua pelarutr tersebut umunya
pelarut organik dan air.Pada perbandingan konsentrasi solut di dalam kedua
pelarut tetap dan merupakan suatu tetapan pada suhu tetap. Tetapan tersebut
tetapan distribusi atau koefisien distribusi dengan simbol Kd. Tujuandari
percobaan ini yaitu menentukan koefisien distribusi I2 dalam sistem air kloroform.
Nilai KD dalam percobaan ini perlu ditentukan untuk mengetahui banyaknya I 2
yang terdistribusi kedalam pelarut organik (kloroform) dan air.
Prinsip dasar percobaan ini yaitu distribusi zat terlarut I2 kedalam dua
pelarut yang tidak saling bercampur yaitu air dan kloroform.Adapun prinsip kerja
yakni, pengukuran, pencampuran, pengocokan, pemisahan dan penitrasian.Titrasi
yang digunakan yaitu titrasi iodimetri yakni metode analisis yang melibatkan
reaksi redoks secara langsung, dimana tidak memerlukan reaksi antara untuk
menghasilkan I2.Sedangkan pada titrasi iodometrri adalah jenis titrasi tidak
langsung yang memerlukan reaksi antara untuk menghasilkan I2 yaitu
mereaksikan sampel dengan iodium, maka pada proses iodometri sampel yang
bersifat oksidator direduksi dengan KI berlebih dan akan menghasilkan I 2 yang
selanjutnya dititrasi dengan larutan baku natrium tiosulfat
(Na2S2O3).
Dalam percobaan ini larutan jenuh I2 dalam CHCl3 sebanyak 135 mL
dicampurkan dengan air 100 ml dalam corong pisah. Tujuan dari perlakuan ini
untuk mempercepat proses distribusi I2 dalam kloroform dan air. Selain itu,
perlakuan merupakan proses sederhana yang merupakan suatu teknik dalam suatu
larutan (berupa air) dibuat bersentuhan dengan suatu pelarut kedua (berupa pelarut
organik) yang pada dasarnya tidak saling bercampur dan menimbulkan
perpindahan satu atau lebih zat terlarut (solut) kedalam kedua pelarut ini.

Gambar 1: I2 dalam CHCl3 + H2O

Pemisahan ini dapat dilakukan dengan mengocok larutan dalam corong

pisah selama bebrapa menit. Fungsi pengocokan yaiotu agar I 2 terdistribusi
sempurna kedalam kedua pelarut yaitu air dengan kloroform.Selain itu, untuk
mempercepat terjadinya distribusi yang disebabkan karena tumbukan tumbukan
antara partikel campuran tersebut. Adapun reaksi yang terjadi:
[I2]H2O [I2]CHCl3

Gambar 2 : Corong pisah dikocok

Setelah pengocokan campuran didiamkan agar campuran dapat terpisah

sempurna dan diperoleh dua lapisan.Lapisan atas merupakan I 2 dalam H2O dan
lapisan bawah merupakan I2 dalam CHCl3. Hal ini dikarenakan H2O bersifat polar
dan CHCl3 mempunyai sifat nonpolar. Adapun air berada pada lapisan atas dan
kloroform pada bagian bawah karena perbedaan massa jenis yakni massa jenis
CHCl3 lebih besar dibandingkan massa jenis air. Adapun massa jenis air 1 g/cm 3
sedangkan massa jenis kloroform 1,485 g/cm3

Gambar 3: larutan didiamkan dan terbentuk 2 lapisan

Setiap lapisan baik I2 dalam CHCl3 (berwarna ungu) dan I2 dalam H2O
(berwarna coklat muda) dititrasi dengan larutan standar Na2S2O3 0,02 M. Titrasi
dilakukan sebanyak tiga kali untuk diperoleh hasil yang lebih akurat. Titrasi
dilakukan hingga larutan menjadi bening. Pada titrasi terjadi reaksi redoks dimana
ion tertationat yang tidak berwarna sehingga menghasilkan larutan yang tidak
berwarna.

Gambar 4: Titrasi I2 dalam Gambar 5: Titrasi I2 dalam

CHCl3 dengan Na2S2O3 H2O dengan Na2S2O3.
Adapun reaksinya:
Na2S2O3 2 NaI + S2O32-
Reduksi = I2 + 2e- 2I
Oksidasi =2SO2O3 S4O62- + 2e-
I2 + 2S2O3 2I- + S4O52-
reaksi lengkap:
2Na2S2O3(aq) + I2(aq) 2 NaI(aq) + Na2S4O6(aq)
(natrium tiosulfat) (iod) (natrium iodida) (natrium tetrationat)
Berdasarkan hasil percobaan volume titran yang diperoleh pada lapisan (I 2
dalam kloroform) yaitu volume titran I, II, dan III secara berurutan 6,1 mL, 5,5
mL, dan 5,2 mL. Sedangkan pada lapisan atas (I2 dalam air) yaitu volume titran I,
II dan III secara berurutan 1,2 mL, 1,2 mL, dan 1,2 mL. Dari data volume titran
dapat diketahui bahwa volume titran yang digunakan pada lapisan bawah lebih
banyak dibandingkan lapisan atas yang berarti iod lebih banyak terdistribusi
kedalam kloroform dibandingkan ke dalam air. hal ini disebabkan oleh sifat
kloroform yang hampir sama dengan I2 dibandingkan dengan air. I2 yang bersifat
semi polar, kloroform bersifat nonpolar sedangkan air bersifat polar.

Gambar 6 : Hasil Titrasi

Koefisien distribusi (KD) dapat diperoleh dari perbandingan konsentrasi

iod yang terdistribusi ke fasa organik dengan konsentrasi iod yang terdistribusi ke
fasa air. berdasarkan hasil analisis data KD yang diperoleh pada percobaan ini
yaitu 4,67 dengan konsentrasi I2(CHCl3) = 0,0224 M dan I2(H2O) = 0,0048 M.
hasil yang diperoleh telah sesuai dengan teori yang mengatakan bahwa jika harga
KD besar, solut secara kualitatif akan cenderung terdistribusi lebih besar/banyak
ke dalam pelarut organik begitupula dengan sebaliknya
I. CONCLUSSION
The KD obtained in this experiment is 4,67 with a concentration of
I2 (CHCl3) = 0.0224 M and I2 (H2O) = 0.0048 M. which means I2 is more
distributed in CHCl3 (organic solvent) compared to water solvent. because the
value of KD> 1.

J. SUGGESTION
It is hoped that the next practitioner will be more careful in the titration
and shaking process which is carried out constantly so that the results obtained
can be in accordance with the theory.