Solute Distribution In Immiscible Systems

Jermane T. Flores
Department of Chemical Engineering, College of Engineering and Architecture
Cebu Institute of Technology – University
N. Bacalso Ave. Cebu City, 6000 Philippines

ABSTRACT

The experiment's purpose was to figure out how evenly a solute distributed between two
immiscible liquids. In the experiment, Nernst distribution was used to determine how much acetic
acid would dissolve in water and diethyl ether, two immiscible liquids. In order to separate
components between two immiscible liquids, liquid-liquid extraction was performed. Diethyl ether
was used to mix acetic acid at various quantities, and the acetic acid was then separated using a
separatory funnel. After reaching equilibrium, samples of each layer were taken and titrated with
sodium hydroxide using the indicator phenolphthalein. After calculating the concentration of each
layer, K was computed. Titration was performed on each upper and lower layer of 0.50N, 1.0N, and
2.0N. The distribution coefficient was then calculated, and it was found that at constant temperature,
as concentration rises, the distribution coefficient of k decreases.
 1. Introduction
This laboratory experiment was performed to measure the distribution coefficient of organic
compounds in immiscible systems using experimental data. Creating a model of the solute
distribution of organic compounds in immiscible system based on experimental data. And analyzing
the solute distribution phenomenon in immiscible system experimentally.

A dissolved substance will distribute between two immiscible solvents in contact with each
other in accordance with a specific equilibrium. The distribution coefficient K is calculated as the
ratio of the chemical A's equilibrated concentrations in the organic phase (CA, org) and aqueous
phase (CA, aq).

K = CA,organic(upper)
(1)

CA,organic(lower)

Because it includes concentrations rather than activities and might change somewhat with solute
concentration, the distribution coefficient K described by (1) is not a real equilibrium constant. If the
solute has a differing molecular weight in the two phases, the distribution coefficient's magnitude will
change quickly with concentration if it is determined by (1).

The ratio of the concentrations in the two phases does not remain constant when the
molecular weight of a solute is different in the two solvents, and vice versa, if the ratio significantly
varies with concentration, it can be assumed that the molecular weight of the solute is not the same
in the two solvents.

An,aqueous ~7 nAorganic (2)

The corresponding distribution coefficient is

(3)

In comparison to using a single portion of the same total volume of solvent, extraction
with many portions of solvent is more effective. It is feasible to create a generalized formula that
will display the quantity yet un extracted after a specified number of operations in the case of
phase distributions that meet Eq. (1). Following one extraction, the concentration in the original
solution will be x1/V and in the extracting phase (x0 - x1)/v. If V milliliters of solution initially
containing xo grams (or equivalents) of a substance are repeatedly extracted with V milliliters of
an immiscible solvent, we may calculate the number of grams xn remaining un extracted after n
extractions. Therefore, the distribution coefficient is

K= x1/V

(x0 − x1)/v (4)

After a second extraction x2 grams (or equivalents) remain in the original solvent. Thus,

(5)

The second form is obtained by substitution for x1 by use of (5). After n extractions the quantity
remaining in the original solvent is

X 2
0 = KV (6)
x0
KV + v

The technique of liquid-liquid extraction is used to purify impure substances by taking

advantage of a solubility differential of the substance in different solvents. It is different from
crystallization in that the sample can be solid or liquid. The impure sample is dissolved in solvent 1
first. Then a second solvent 2 is added in such a way that the sample migrates from the first to the
second solvent without the impurities. This, of course, requires that the two solvents 1 and 2 be
immiscible, and ideally that the sample be more soluble in solvent 2 than in solvent 1.
2. Materials and Methods

2.1 Materials and Apparatus

- Three (3) 100-mL separatory funnels

- Six (6) 100-mL Erlenmeyer flasks
- One (1) 100-mL volumetric flask
- One (1) 25-mL pipette
- Three (3) 250-mL beaker
- 0.5 M, 1 M, 2 M acetic acid
- Diethyl ether
- 0.5 M sodium hydroxide

2.2 Methods

100 milliliters of approximately 0.5 N, 1 N, and 2 N solution acetic acid were

prepared. This was done by diluting the original 29.7% acetic acid with water using the
data from pre-lab calculations. After they were prepared, 25 milliliters of each solution
were pipette into different closed 100-mL separatory funnels. The solvent, diethyl ether,
was added into the separatory funnels next. The separatory funnels filled with the
immiscible mixture were placed in a water bath to lower its temperature to 20 degrees
Celsius. A close rubber tubing was placed over the outlets to keep the water away from
the water bath. After the solutions have come to equilibrium, the separatory funnels were
removed from the water bath. The lower layer was collected into a breaker while
carefully not allowing the upper layer to pass through the opening valve. 10 milliliters of
each lower layer sample were poured to an Erlenmeyer flask to be used for titration with
sodium hydroxide, using phenolphthalein as an indicator. The procedure was repeated
for the lower layer as well. It was then titrated with the 0.5 M sodium hydroxide. Data
was collected and the distribution coefficient was computed.
3. Results

3.1 Different concentrations of acetic acid solution

0.5 N acetic acid solution

1N acetic acid solution

 2N acetic acid solution

3.2 Laboratory Set-up

4. Discussions
This experiment aims to determine the distribution coefficient of organic compounds in an
immiscible system, develop a model of the solute distribution of organic compounds, and
investigate the solution phenomena. The results demonstrate the varying distribution
coefficients, K, of the several acetic acid solutions (0.5N, 1N, and 2N).

Diethyl ether, water, and 0.5 N acetic acid constitute the initial solution. The second combination
consists of diethyl ether, water, and acetic acid at a concentration of 1.0 N. In addition, the third
solution is a combination of diethyl ether, water, and 2.0N acetic acid. The solution was
separated into two layers. Diethyl ether forms the organic layer in the solution's uppermost
layer, while water and acetic acid form the aqueous layer at the solution's base. There is a
specific ratio of solute distribution in immiscible liquids, resulting in a liquid volume below the
saturation point. The ratio is represented by the distribution coefficient K, a constant. The
findings demonstrate that the molarity and volume of NaOH utilized in the titration increase as
the acetic acid concentration rises.

Additionally, it is noted that more NaOH is consumed in the aqueous layer than in the organic
layer, resulting in a decrease in K as the solute concentration rises. K denotes the ratio of the
concentration of the upper layer to the concentration of the lower layer. As the concentration of
acetic acid rises, K's distribution coefficient falls. The concentration of the bottom layer exceeds
that of the higher layer. It indicates that there are more moles of acetic acid in the aqueous
phase than in the organic phase.

5. Conclusion
The experiment was performed under the pretense of separating immiscible solvents by
a layer of a dissolved substance which distributes itself accordingly to a definite equilibrium. To
observe how the reaction would took place, two immiscible solvents are used, water, and diethyl
ether. Three controlled set-ups are to be used, by diluting different concentrations of acetic acid,
while using phenolphthalein as an indicator. The experiment was performed using liquid-liquid
extraction, as the catalyst in the experiment used were both immiscible liquids. When the
solvents were titrated in to the different test tubes, a layer of solution formed in the middle of the
test tube, which was concluded to be the equilibrium solution that is the ratio of both organic and
aqueous phases. After performing the experiment, the researchers have found out that the pink
endpoint for the solution has not been reached, due to a miscalculation in the preliminary
computation of data. The researchers have reviewed the experimental data and found out that
there is a significant difference between the required amount of acetic acid to be used in the
experiment and the amount actually used. The results for the different variables were found out
to be dependent on the amount of the concentration of the acetic acid used in the initial
aqueous solution. Increasing the concentration of acetic acid in water might further improve the
accuracy in the results.
6. References

[1] Libretexts. (2020, August 14). 14.8: Distribution of a single species between immiscible
phases - extraction and separation. Chemistry LibreTexts. Retrieved September 22, 2022,
from https://chem.libretexts.org/Bookshelves/General_Chemistry/Map
%3A_Principles_of_Modern_Chemistry_(Oxtoby_et_al.)/
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14.8%3A_Distribution_of_a_Single_Species_between_Immiscible_Phases_-
_Extraction_and_Separation

[2] Russell, P. M. (2019, September 23). Distribution of iodine between two immiscible solvents.
YouTube. Retrieved September 22, 2022, from https://www.youtube.com/watch?
v=u4yQe_pFzNI

[3] Wilson, J. (1968). Experiments in physical chemistry. Elsevier. https://doi.org/10.1016/c2013-

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