Int. J. Pharm. Sci. Rev. Res., 54(1), January - February 2019; Article No.

19, Pages: 109-112 ISSN 0976 – 044X

Research Article

Effect of the Critical Solution Temperature of a Partial Miscible Phenol-Water Solution with
Addition of Potassium Chloride
Chinmaya Keshari Sahoo*1, Hemanta Kumar Khatua2, Jimidi Bhaskar3, D. Venkata Ramana4
1
Department of Pharmaceutics, Malla Reddy College of Pharmacy (Affiliated to Osmania University), Maisammaguda, Hyderabad, Telangana-500014, India.
2
Department of Pharmaceutics, Princeton College of Pharmacy (Affiliated to JNTUH), Korremula, Hyderabad, Telangana -500088, India.
3
Department of Pharmacy, Avanthi Institute of Pharmaceutical Sciences, Gunthapally (V), Near Ramoji Film City, Hyderabad, Telangana-501505, India.
4
Department of pharmaceutical Technology, Netaji Institute of Pharmaceutical Sciences, Toopranpet, Yadadri Bhongir, Telangana -508252, India.
*Corresponding author’s E-mail: [email protected]

Received: 05-12-2018; Revised: 25-12-2018; Accepted: 08-01-2019.

ABSTRACT
Partially miscible liquids become more soluble with the increase in temperature and at a certain temperature they are completely
miscible. This temperature is known as the critical solution temperature (CST) or consolute temperature. The temperature above
the phase gets affected by the addition of impurities. To observe the miscibility temperature, the mixture was heated in a boiling
tube until the turbidity disappeared and the final temperature was noted. Then, the mixture was cooled down and the temperature
noted when the turbidity reappeared. Solutions of impurities of different concentrations were formed and their effect on the phase
was analyzed. It was found that addition of ionic compound KCl, in phenol- water system show lesser increase in CST as they
decrease the miscibility to a lesser extent.
Keywords: Critical Solution Temperature, KCl, Phenol-Water System.

INTRODUCTION To phenol–water system if impurities of ionic and

covalent substances are added, a ternary system is

A homogenous mixture of a solute and a solvent is

called as a true solution. The liquid-liquid are of
three types such as completely miscible liquid
pairs - E.g. Water-Alcohol, Water-Sulphuric acid. Partially
miscible liquid pairs - E.g. Ether-Water, Phenol-Water and
formed. For a ternary system, there are three
components co-existing in a system. The addition of a
third substance to a partially miscible system to increase
its miscibility is known as blending. This is also called as
the ‘salting-out’ in pharmaceuticals and is used to select
liquid pairs that are practically immiscible - E.g. Mercury-
the best solvent for the drugs. In this process, a salt is
Water, Nitrobenzene-water1.
added to separate the aqueous phase from the organic
When phenol and water are mixed, a certain amount of phase. If the added salt dissolves in one of the phases
the two dissolves with the other due to hydrogen bonding only, it results in an increase in the UCST, and a decrease
and two conjugate layers of liquids are obtained. The in the LCST, thus decreasing the miscibility of the system 3,
4
upper layer of this system is water dissolved in phenol . Further, if the added salt is soluble in both the phases,
and the lower layer is phenol dissolved in water. The then the UCST is lowered and the LCST is raised, thus
composition of these layers depends only on the increasing the miscibility of the system. This increase or
temperature of the system and is independent of the decrease in the CST depends on the nature and the mass
quantities of the liquids mixed. For every temperature of the added substance and the composition of the
two solubilities can be obtained, one for phenol dissolved system.
in water and the other for water dissolved in phenol.
MATERIALS AND METHODS
Generally, for partially miscible liquids solubility increases
Materials
with increasing temperature and the temperature at
2
which they are completely miscible is termed as the Potassium chloride was obtained from Qualigens Fine
critical solution temperature (CST) or consolute Chemicals, India. Phenol was purchased from standard
temperature. The temperature above which the phases of chemicals, Hyderabad, India and distilled water was
a system are completely miscible is known as the upper collected from distillation unit from college.
consolute temperature (UCT) or upper uritical solution 5
Methods
temperature (UCST). Similarly, the temperature below
which the phases of a system are completely miscible is Step I: Procedure for Calculating the CST of a Phenol-
known as the lower critical solution temperature (LCST). Water System (without added impurity)-
The phenol water system exhibits an upper critical
1. Phenol concentration scales of 8%, 15%, 40%, 55% and
solution temperature and this critical solution
80% were set in the experiment.
temperature can be used for testing the purity of the
2. Five 20 mL of the mixture of phenol and water with the
mixture.
concentration scales were prepared in the test tubes.

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 Int. J. Pharm. Sci. Rev. Res., 54(1), January - February 2019; Article No. 19, Pages: 109-112 ISSN 0976 – 044X

3. The volume of phenol and water required were the dispersion of two liquids until a clear mixture was
calculated by using the formula:- obtained.
Let X be the concentration scale of phenol: 8. The temperature at which the turbid liquid becomes
clear (T1) was observed and recorded.
Volume of phenol = 20 mL × X/100
9. The test tube was removed from the hot water and it
Volume of water = 20 mL× (100-X)/100
was cooled by applying ice bath until the liquid became
4. The measured amount of water and phenol were turbid and the temperature at this point was
transferred into a test tube. immediately recorded(T2).
5. The phenol transfer process must be done in the fume
10. Similarly15%, 40%, 55% and 80% of phenol
cupboard as the phenol is very toxic.
concentration scales in the experiment were prepared.
6. A thermometer was placed into the test tube and
sealed by using parafilm followed by aluminium foil and it 11. The average miscibility temperature for each test tube
was to make sure that the thermometer did not touch the at which two phases were no longer seen or at which two
bottom surface of the test tube. phases existed were determined.
7. During the process of heating, the test tube was shaken
gently in the water bath to increase the rate of speed of
Average miscibility of temperature of solution (T)

12. The graph of temperature against percentage of 3. Similarly 0.2 %, 0.4 %, 0.6 %, and 0.8 % w/v of KCl
phenol was plotted to produce a phase diagram and the solutions were prepared by adding 0.2, 0.4, 0.6 and 0.8
critical solution temperature was determined. grams of KCl to 100 ml of distilled water respectively in 4
different 100 ml beakers, with the help of measuring
Step II: Finding the Effect of KCl on the CST of the
cylinders.
Phenol-Water system-
4. From the prepared solution 5 ml of various w/v% KCl
Preparation of KCl solution
solutions were taken and added in the boiling tube
1. One gram of potassium chloride (KCl) salt was weighed containing different % phenol-water composition solution
by an electronic weighing machine. respectively.
2. This was dissolved in 100 ml distilled water in a beaker 5. The miscibility temperatures for the mixture prepared
to get 1% w/v KCl solution. at different concentrations of phenol were found by
repeating steps.
Calculation

Average temperature when clear (T1)

Average temperature when turbid (T2)

RESULTS AND DISCUSSION temperature decreased. Hence plotting graph

temperature vs composition of phenol nearly parabolic
From the observed tables it was found that when the
graph is obtained. The highest miscibility temperature is
concentration of phenol was increased from 8 % to 40%
known as CST. The CST obtained from pure phenol-water
the miscibility increased and consequently the miscibility
system was 67.5⁰C. All the observed values were reported
temperature increased from 51 0C to 710C.But further
in table 1 to 5.
increased concentration of phenol 55% to 80% the
miscibility decreased and consequently the miscibility
Table 1: Phenol-Water System
Temperature when Temperature when Average
Test Phenol Water 0 0 CST
clear,(T1), C turbid,(T2) C miscibility
Tube 0
% ml % ml I II Average I II Average temperature(T), C

A 8 1.6 92 18.4 54 50 52 49 47 48 50
B 15 3.0 85 17.0 56 54 55 55 51 53 54
67.5
C 40 8.0 60 12.0 73 67 70 68 62 65 67.5
D 55 11.0 45 9.0 70 66 68 62 58 60 64
E 80 16.0 20 4.0 58 54 56 50 46 48 52

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Int. J. Pharm. Sci. Rev. Res., 54(1), January - February 2019; Article No. 19, Pages: 109-112 ISSN 0976 – 044X

Table 2: Effect of 0.2% KCl on the miscibility of Phenol-Water System

Temperature when Temperature when Average

Test Phenol Water CST
clear,(T1), 0C turbid,(T2) 0C miscibility
Tube temperature, C
0
% ml % ml I II Average I II Average

A 8 1.6 92 18.4 54 52 53 51 47 49 51
B 15 3.0 85 17.0 58 54 56 54 50 52 54
68
C 40 8.0 60 12.0 75 67 71 68 62 65 68
D 55 11.0 45 9.0 69 63 66 64 56 60 63
E 80 16.0 20 4.0 59 54 56 52 48 50 53

Table 3: Effect of 0.4 % KCl on the miscibility of Phenol-Water System

Temperature when Temperature when Average

Test Phenol Water 0 0 CST
clear,(T1), C turbid,(T2) C miscibility
Tube temperature, C
0
% ml % ml I II Average I II Average
A 8 1.6 92 18.4 57 53 55 51 47 49 52
B 15 3.0 85 17.0 61 55 58 56 52 54 56
69
C 40 8.0 60 12.0 76 66 71 72 62 67 69
D 55 11.0 45 9.0 71 65 68 67 57 62 65
E 80 16.0 20 4.0 60 52 56 54 50 52 54

Table 4: Effect of 0.6% KCl on the miscibility of Phenol-Water System

Temperature when Temperature when Average

Test Phenol Water CST
clear,(T1) 0C turbid,(T2), 0C miscibility
Tube temperature, C
0
% ml % ml I II Average I II Average

A 8 1.6 92 18.4 57 51 54 52 48 50 52
B 15 3.0 85 17.0 60 54 57 55 51 53 55
70
C 40 8.0 60 12.0 77 69 73 73 61 67 70
D 55 11.0 45 9.0 70 64 67 65 57 61 64
E 80 16.0 20 4.0 62 52 57 55 51 53 55

Table 5: Effect of 0.8 % KCl on the miscibility of Phenol-Water System

Temperature when Temperature when

Test Phenol Water 0 0
Average miscibility CST
clear,(T1), C turbid,(T2), C
Tube temperature 0C
% ml % ml I II Average I II Average

A 8 1.6 92 18.4 58 54 56 54 50 52 54
B 15 3.0 85 17.0 62 56 59 58 52 55 57
71
C 40 8.0 60 12.0 76 70 73 72 66 69 71
D 55 11.0 45 9.0 73 63 68 65 57 62 65
E 80 16.0 20 4.0 61 51 56 57 51 54 55

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Int. J. Pharm. Sci. Rev. Res., 54(1), January - February 2019; Article No. 19, Pages: 109-112 ISSN 0976 – 044X

Comparison quantities of the liquids mixed. Due to addition of

potassium chloride there was increase in the critical
From the data comparison it was found that CST was
solution temperature. It was observed that the UCST of
affected by the concentration of potassium chloride. All
phenol-water system increases with increase in
the observed values were depicted in table 6.
concentrations of impurities irrespective of their nature.
Table 6: Comparison of CST with different concentration
Acknowledgements: Authors wish to thanks their
of KCl addition
respective authorities of Institutions for providing
Concentration of KCl added laboratory facilities to complete this research article.
Sl. No. CST, 0C
(% w/v)
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Source of Support: Nil, Conflict of Interest: None.

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