A.

THE TITLE OF EXPERIMEN

Constant Distributi onof Iod in The Water Chloroform System.
B. OBJECTIVE OF EXPERIMENT
Determine the ion distribution constant in a water-chloroform solvent by Batch
extraction.
C. LITERATURE RIVIEW
The extent to which solutes, both inorganic and organic, distribute themselves
between two immiscible liquids differs enormously, and these differences have been used for
decades to separate chemical species. This section considers applications of the distribution
phenomenon to analytical separations. The partition of a solute between two immiscible
phases is an equilibrium process that is governed by the distribution law. Distribution
constants are useful because they permit us to calculate the concentration of an analyte
remaining in a solution after a certain number of extractions. They also provide guidance as
to the most efficient way to perform an extractive separation
[ A ]i=¿
(Skoog, 2014: 852-853).
Solvent extraction has one of its most important applications in the separation of
metal cations. In this technique, the metal ion, through appropriate chemistry, distributes
from an aqueous phase into a water-immiscible organic phase. Solvent extraction of metal
ions is useful for removing them from an interfering matrix, or for selectively (with the right
chemistry) separating one or a group of metals from others. The technique is widely used for
the spectrophotometric determination of metal ions since the reagents used to accomplish the
extraction often form colored complexes with the metal ion. It is also used in flame atomic
absorption spectrophotometry for introducing the sample in a nonaqueous solvent into the
flame for enhanced sensitivity, and removal of matrix effects. The separation can be
accomplished in several ways. You have noted above that the uncharged organic molecules
tend to dissolve in the organic layer while the charged anion from the ionized molecules
remains in the polar aqueous layer. This is an example of “like dissolves like (Christian,
2014: 583).
From experience with many determinations, we find that the distribution of replicate
data from most quantitative analytical experiments approaches that of the Gaussian curve.
Ten milliliters of water were transferred to the flask with the pipet, and the flask was
stoppered. The flask, the stopper, and the water were then weighed again. The temperature of
the water was also measured to determine its density. The mass of the water was then
calculated by taking the difference between the two masses. The mass of water divided by its
density is the volume delivered by the pipet. The experiment was repeated 50 times (Skoog,
2014: 92).
A solute S will distribute itself between two phases (after shaking and allowing the
phases to separate) and, within limits, the ratio of the concentrations of the solute in the two
phases will be a constant:
[S]1
K D=
[S]2
where KD is the distribution coefficient and the subscripts represent solvent 1 (e.g.,an organic
solvent) and solvent 2 (e.g., water). If the distribution coefficient is large, the solute will tend
to be quantitatively partitioned in solvent 1. Many substances are partially ionized in the
aqueous layer as weak acids. The extraction now becomes dependent on the pH
of the solution. Consider, for example, the extraction of benzoic acid from an aqueous
solution into either (Christian, 2014: 579-580).
A liquid–liquid extraction is one of the most important separation techniques used in
environmental, clinical, and industrial laboratories. Two examples from environmental
analysis serve to illustrate its importance. Before their analysis by gas chromatography,
trihalomethanes are separated from their aqueous matrix by a liquid–liquid extraction using
pentane. A liquid–liquid extraction is also used in screening orange juice for the presence of
organophosphorous pesticides. A sample of orange juice is mixed with acetonitrite and
filtered. Any organophosphorous pesticides that might be present in the filtrate are extracted
with petroleum ether before a gas chromatographic analysis. In a simple liquid–liquid
extraction the solute is partitioned between two immiscible phases. In most cases one of the
phases is aqueous, and the other phase is an organic solvent such as diethyl ether or
chloroform (Harvey, 2000: 215).
In analytical measurements, the data collected are an estimate of the true value (ì)
that is usually represented by the arithmetic mean X of the data. This is due to only a small
set of values being collected that is known as a “sample” of the population while an infinite
set of data values would in fact represent the population itself as ì. Let us look at what is
known as the normal distribution curve (also referred to as the probability curve or error
curve) when an infinite number of data points are obtained and only random errors are
present. The curve a bell or Gaussian symmetrical shape, where the y-axis represents the
probability of the occurrence of a measurement, and the x-axis represents the distribution of
the data centered around the population mean μ (Ham, 2016: 94).
Earlier we learned that the partitioning of a solute between two phases is described
by a partition coefficient. If the solute is initially in an aqueous phase and is extracted into an
organic phase
Saq ↔ S org
the partition coefficient is
[S ¿¿ org]
K D= ¿
[S¿¿ aq ]¿
A large value for KD indicates that the extraction of the solute into the organic phase is
favorable. In evaluating the efficiency of an extraction, however, we must consider the
solute’s total concentration in each phase (Harvey, 2000: 216).
The distribution ratio D is a constant independent of the volume ratio. However, the
fraction of the solute extracted will depend on the volume ratio of the two solvents. If a larger
volume of organic solvent is used, more solute must dissolve in this layer to keep the
concentration ratio constant and to satisfy the distribution ratio. The fraction of solute
extracted is equal to the millimoles of solute in the organic layer divided by the total number
of millimoles of solute. The millimoles are given by the molarity times the milliliters. Thus,
the percent extracted it given by
[ S]0 V 0
%E= × 100 %
[S ]0 V 0 +[ S ]a V a
(Christian, 2014: 581).
This distinction between KD and D is important. The partition coefficient is an
equilibrium constant and has a fixed value for the solute’s partitioning between the two
phases. The value of the distribution ratio, however, changes with solution conditions if the
relative amounts of forms A and B change. If we know the equilibrium reactions taking place
within each phase and between the phases, we can derive an algebraic relationship between
KD and D (Harvey, 2000: 216).
Iodometric titration used Na2SO3 0.01 N as a previously standardized titrant with potassium
dichromate to determine the actual normality of Na 2S2O3 used. The volume of thiosulfate
used during titration explains that the volume of thiosulfate will continue to increase as time
increases in heating. Kinetics and stoichiometry of S-oxidation reaction of sodium Azl by
means of potassium hydrogen perox omono sulfate in aqueous solutions at pH 2–4 using
iodometric titration method were studied. The new procedure was developed and ability of
quantitative determination of penicillin in pharmaceutical preparation Securopen by
iodometric method (Karpova at.al, 2018: 510-511).
In a system of two intermittent liquid phases a third substance is added which can dissolve in
both so that all three will be distributed between the two phases in a certain amount. To
determine the optimum conditions for back extraction of Hg (II) from the organic phase
loaded into the fresh phase, the shaking of the organic phase loaded was carried out with
different molar concentrations (0.01 mol dm - 3 to 1.0 mol dm - 3) of sodium thiosulfate,
ammonium chloride, hydrochloric acid and distilled water. At this concentration of Na 2S2O3,
S2O3-2 ion replaces extraction reagents to form metal complexes extracted in the organic
phase which are insoluble in the organic phase and stripped into aqueous media (Abbasi
at.all, 2019: 7).

Since each student prepared their own thiosulfate solution, the students. Precision of
[S2O32-] was analyzed, but their accuracy was not considered. Students precision was
compared using COVPPT based on ≥ 3 replicate titrations. As part of a multi-week lab project
in our quantitative analysis course, second and third year undergraduate chemistry and
biochemistry students determined the mass percent of Co (%Co) in a coordination
compound of unknown (to the student) stoichiometry by performing an iodometric redox
titration using thiosulfate that they standardized. The procedure to determine %Co was
independent of the oxidant used to standardize thiosulfate, but the value of %Co
depended on the accuracy of students (S2O32–) (Randall, 2014: 1332-1333).

Discussion

In this experiment iodine distribution constants have been carried out in the water
chloroform system, where the determination of the distribution coefficient is done through
iodine solutes in chloroform and water solvents. Certain substances are more soluble in
certain solvents compared to other solvents. So iod is far more soluble in carbon disulfide,
chloroform or carbontetrachloride than in water (Svehla, 1990: 139). The basic principle of
this experiment is batch extraction or solvent extraction, this extraction is useful in the
separation of a substance that uses other intermixed solvents (Analytical Chemistry Lecturer
Team, 2017: 5). While the principle of work in this experiment is pengcokan, separation and
titration.

1. Standardize Iodine solution.

In this experiment, the iodine solution was titrated with 0.1 N sodium thiosulfate
standard solution, where the sodium thiosulfate solution as the primary standard solution
whose concentration was known and the concentration remained in storage. The iodine
solution needs to be standardized so that the concentration can be known as a comparison
with the concentration in water or chloroform.

Titration is done until the color changes from brown (iod color) to clear. Titration is
carried out 3 times in order to obtain more accurate data. At three times the titration, the
volume of sodium thiosulfate solution used was 5.5 mL, 5.2 mL, and 5.3 mL with an average
volume of 5.33 mL. From these results iodine concentrations of 0.106 N. were obtained. The
reaction:

2Na2S2O3 + I2 2NaI + Na2S4O6

2. Iodine concentration in each solvent.

In this experiment, iodine solution was put into three separating funnels after which
chloroform was added and shaken, while the shaking function was to get iod perfectly
distributed into two solvents namely chloroform and water and accelerate the distribution of
iodine caused by collisions between mixed particles is also fast, more lam and powerful way,
shakes iod that is distributed many more. Furthermore the mixture is allowed to stand until
the solution is completely separated into two layers where the lower layer is purple
chloroform while the top layer of water is brown, the formation of these two layers due to
differences in density of water and chloroform where water has a density of 1 gr / ml and
chloroform of 1.48 gr / ml. The two layers are then separated and housed in a sharpened
Erlenmeyer.

The two layers are then titrated using 0.1 N Na2S2O3 standard solution. The
chloroform layer is titrated until the color changes from purple to clear, in the chloroform
penetration process it does not use starch because in chloroform there is an iod where iod is
an autoindicator (can be an indicator for himself). Na2S2O3 0.1 N volume used in
erlenmeyer 1 was 18.5 mL, Erlenmeyer 2 was 18.3 mL, and Erlenmeyer 3 was 18.5 mL so
that iodine concentrations in chloroform were obtained respectively 0.0,074 N, 0.0, 0732 N,
and 0.074 N.

The water layer is then titrated with 0.1 N Na2S2O3 standard solution until the color
changes from brown to clear. In this titration the starch indicator is used to determine whether
all iodine has reacted or not. Na2S2O3 volume of 0.1 N used in erlenmeyer 1 was 6.8 mL,
Erlenmeyer 2 was 8.5 mL, and Erlenmeyer 3 was 8.2 mL to obtain iodine concentration in
water respectively 0.0272 N, 0.034 N, and 0.0328 N.
 3. Determination of the Iod Distribution Setting (KD)

From the concentrations obtained in both the aqueous and chloroform layers, the iod
distribution constant (KD) can be obtained by the formula

C 1 [I ¿¿ 2]kloroform
K D= = ¿
C2 [ I 2 ] air
Where KD is the ratio between the concentration of solutes in the organic phase with
the concentration of solutes in the aqueous phase. So from the formula above, KD is obtained
on Erlenmeyer 1 as much as 1.0277 on Erlenmeyer 2 is 2.1470 on Erlenmeyer 3 is 2.3125.
These results indicate that KD> 1 which means iod is more distributed into the chloroform
layer than the water layer. Based on the results of experiments already in accordance with the
theory which states that if the value of KD> 1 then the solute will tend to be distributed into
organic solvents compared to water solvents (Seobagio, 2000).

The reactions that occur, namely:

−¿¿
reduction : I 2+ 2e ↔2 I
2−¿+ 2e ¿

Oxidation : 2 S 2 O32−¿↔ S O
4 6 ¿

2−¿¿
−¿+ S 4 O6 ¿

I 2+ 2 S2 O 32−¿ ↔2 I ¿

Complete reaction :
2Na2S2O3 + I2 2NaI + Na2S4O6
 BIBLIOGRAPHY

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Brooks/Cole Cengage Learning