LABORATORY REPORT : NFNF1213

Set1 Sem 1 20152016 SIFAT

FIZIKOKIMIA DADAH
Thursday, 3 December 2015

LAB 2 Phase Diagram – Mutual Solubility Curve for

Phenol and Water
TITLE 
Phase Diagram – Mutual Solubility Curve for Phenol and Water

DATE
3rd of November 2015

OBJECTIVES
i. To determine the solubility of two partially miscible liquids of phenol-water system
 ii. To construct a mutual solubility curve for phenol-water system

iii. To determine the critical solution temperature of phenol-water system

INTRODUCTION

          Miscibility is often applied to liquids and the term is meant by the extent of two
or more liquids that dissolve in each other. Miscibility can be categorized into
miscible, partially miscible and immiscible. If the liquids are said to be miscible, it
means that the liquids are completely dissolved in each other to form a
homogenous solution. For instance, water and ethanol are miscible because they
mix in all proportions. Two liquids may be partially miscible if they mix each other in
limited proportions, for example, ether-water and phenol-water. By contrast, liquids
are said to be immiscible if a significant proportion does not form a solution. Oil and
water are said to be immiscible due to the formation of two layers of liquids after
mixing.
          In general, both liquids become more soluble as the temperature increases
until a critical solution temperature is reached. Below the critical solution
temperature, the liquids will be immiscible at any temperature by forming two layers
of liquids. Above or at the critical solution temperature, miscible liquids are formed
as only one layer will be formed. Any pair of liquids are possible to form a closed
system because the existence of both upper and lower critical solution
temperatures. However, the temperatures are difficult to be determined except for
nicotine-water.
          The composition for two layers of liquids in equilibrium state is constant and
does not depend on the relative amount of these two phases at any temperature
below the critical solution temperature. Apart from temperature and pressure
factors, the presence of a third component can significantly influence the mutual
solubility of the pair of partially miscible liquids.

APPARATUS

Test Tubes

Test Tube Rack

Test Tube Holder

Measuring Cylinder
 Dropper

Water Bath

Thermometer

MATERIAL

Aluminium Foil

Distilled Water
 Ice

Parafilm

Phenol

PROCEDURE 
1.  Phenol concentration scales of 8%, 15%, 40%, 55% and 80% were set in the
experiment.
2. Five 20 mL of the mixture of phenol and water with the concentration scales were
prepared in the test tubes.   
3. The volume of phenol and water required were calculated by using the formula:-
          Let X be the concentration scale of phenol:
                                         Volume of phenol = 20mL × X/100

                                         Volume of water = 20mL× (100-X)/100

4. The volume of phenol and water in 8% of phenol mixture was calculated by using
the formula 
above and then measured by using 10mL measuring cylinder.
5. The measured amount of water and phenol were transferred into a test tube.
6. The phenol transfer process must be done in the fume cupboard as the phenol is
 very toxic.
7.  A thermometer was placed into the test tube and sealed by using parafilm
followed 
by aluminium foil and it was to make sure that the thermometer did not touch the
bottom surface of the test tube.

   
      8. The test tube was then heated in a 90 ºC water bath until it reached about 67 ºC.

  9. During the process of heating, the test tube was shaken gently in the water bath
to
  increase the rate of speed of the dispersion of two liquids until a clear mixture
  was obtained.
   
10. The temperature at which the turbid liquid becomes clear was observed and
recorded.

11. The test tube was removed from the hot water and it was cooled until the liquid 
became turbid and two layers were seen, the temperature at this point
was immediately recorded.
     12. The test tube was being cooled by applying ice to it.

13. Steps 4 until 12 were repeated with 15%, 40%, 55% and 80% of phenol
     concentration scales in the experiment.
     14. The average temperature for each test tube at which two phases were no 
     longer seen or at which two phases existed were determined.
     15. The graph of temperature against percentage of phenol was plotted to produce a
phase 
     diagram and the critical solution temperature was determined.

   

    

      RESULT

Temperature Temperature    

 Test Phenol Water when   clear, when turbid,     Average
Tube ˚C ˚C Temperature,
% ml % ml I II Average I II Average ˚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
C 40 8.0 60 12.0 74 68 71 69 61 65 68
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

CALCULATION

Average Temperature when Clear =

Temperature from set I + Temperature from set II

                                       2
Average Temperature when Turbid =

Temperature from set I + Temperature from set II

                                       2
Average Temperature =

Average temperature when clear + Average temperature when turbid

                                                      2

QUESTIONS
1. Plot the graphs of phenol composition (horizontal axis) in the different mixtures
against
    temperature at complete miscibility. Determine the critical solution temperature.
.

2. Discuss the diagrams with reference to the phase rule.

    The phase rule is expressed as below:
     F = C - P + 2          in which F = The number of degrees of freedom in the system
                                                  C = The number of components
                                                  P = The number of phases presents 
     Phenol-water system is a two phase system. The region of temperature applied
to the phenol-water system above the line graph will give out single phase system
which means the phenol is completely miscible in the water. Whereas, the region of
the temperature applied to the system will show a two phase system which forms a
two layer system as the phenol is not miscible in the water at that particular
temperature. The graph above in the results shows the graph of average
temperature at complete miscibility of solution against percentage of phenol in
water. By using the phase rule, there are 2 components in the system and the phase
presents is 1, therefore F = 2 – 1 + 2. The number of degrees of freedom in the
system, F= 3,  however, the pressure applied to the system is fixed, so the F has to
reduce to 2. It is necessary to fix both temperature and concentration to define
system. When 2 liquid phases are formed, F = 2-2+2, since is the pressure is still
fixed to the system, hence F=1. The temperature is the only factor that have to be
fixed to define the system.

3. Explain the effect of adding foreign substances and show the importance of this
effect in
    pharmacy.
    The addition of foreign substances will alter the critical solution temperature to a
marked extent. When the addition of the third substance dissolves in only one of the
two liquids, then the mutual solubility of the latter will diminish. The temperature
which the system becomes homogeneous is raised in case the system having an
upper critical solution temperature and lowered in case the system having a lower
critical solution temperature. In case of water-phenol system, the critical consolute
temperature is raised by the addition of potassium chloride to the mixture of critical
composition. The increase in temperature is due to the salting out of water. When
the added substances dissolve in both liquids, the critical solution temperature is
lowered due to negative salting out effect. The increase in mutual solubility of two
partially miscible liquid is known as blending. The importance of this effect in
pharmacy is that it can help in selecting the suitable solvent of a drug. Besides, it
can also overcome problems arising during preparation of pharmaceutical solution.

DISCUSSION      

                          
          Phenol and water system is an example of two-component systems
containing liquid phases. Phenol and water is a system that exhibit partial miscibility
(or immiscibility) so they will produce a two-phase diagram. In this experiment,
N-shaped curve is obtained after plotting average temperature versus composition
of phenol. The N-shaped curve shows the limits of temperature and concentration
within which two liquid phases, phenol and water exist in equilibrium. The region
outside the curve represents the two-component system having one phase which
means that both the phenol and water are completely miscible.
          Starting from 100% of water at 50 °C, the addition of known increments of
phenol to a fixed weight of water, the whole being maintained at 50 °C, will result in
the formation of a single liquid phase. From the graph plotted, it can be observed
that at 52 °C, a minute amount of a second phase occurs. The concentration of
phenol and water at which this occurs is 11% by weight of phenol in water. As we
prepared mixtures containing increasing quantities of phenol, which is as we
proceed from the 8% to 80% of phenol in water, the amount of phenol-rich phase
continually increase. At the same time, the amount of the water-rich phase
decreases.
          A system that prepared on a tie line which is from point A- B will always
parallel to the base line in two-component systems. The phenol-water system that
prepared on the tie line at equilibrium will separate into phrases of constant
composition. These phases are termed conjugate phases. For example in test tube
2 containing 15% by weight of phenol and 85% by weight of water at equilibrium will
have two liquid phases present in the tube. Phenol will lie below the water since the
density of phenol is much higher than water.  
           In this experiment, phase rule is used to calculate the degree of freedom in
practice to formulate systems containing more than components which may be
advantageous to achieve a single liquid-phase product. The phase rule is dependent
on the condition of the different phases present. When phenol is completely
miscible with water, the system has one phase so the degree of freedom, F = 2-1+2 =
3. Since the pressure is fixed so F = 2 and it is necessary to fix both temperature and
concentration to define the system. When phenol is immiscible with water (two
phases present), the degree of freedom, F = 2-2+2 = 2 since pressure is fixed so only
temperature that need to be defined in order to completely defined the system.
          From the plotted graph, the critical temperature or upper consolute
temperature is 68.4°C. In the case of phenol and water, the mutual solubility
increases with an increase in temperature. At this temperature, all the combination
of phenol and water are completely miscible and yield one-phrase liquid systems.
The critical solution temperature obtained was slightly different from the theoretical
value of 66.8°C. This could possibly due to several errors that occurred during the
experiment which include the tubes are not tightly sealed and heat will lose to the
surrounding which will in turn affect the temperature measured. As we known that
phenol is a volatile component so it will easily evaporates into the surrounding and
this will in turn reduce the concentration of the phenol. Besides, parallax error might
occur while we are taking the reading of the thermometer or measuring the volume
of relative phenol and water. Other than that, we must be aware and alert when
taking the temperature of the solution become clear and cloudiness. This is because
the changes in temperature might be too fast and we might fail to obtain accurate
results.
           Thus, there are some precautions that need to be taken such as sealed the
tube tightly using aluminum foil and foil to prevent the evaporation of phenol.
Parallax error should be avoided as we must place our eyes perpendicularly to the
lower meniscus of the liquid. The reading of the thermometer when the solution
turns cloudy and clear should be taken immediately to increase the accuracy of the
results.    

CONCLUSION

          The critical solution temperature of the phenol-water system is 68.4 °C. The
solubility of two partially miscible liquids of phenol-water system is depends on two
factors which are the temperature and the concentration of phenol in the water by
volume.

REFERENCE

1. Retrieved from: https://jeplerts.wordpress.com/2008/12/21/partially-miscible-

liquids determination-of-mutual-  solubility-of-phenol-water/

2. Retrieved from :Patrick J. Sinko, Lippincott Williams and Wilkins. Martin’s

Physical Pharmacy and Pharmaceutical Sciences, 5th Edition
Bryan Ong at 21:56

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1 comment:

Jade Graham 13 August 2016 at 05:17

One of the precaution should be taken is to adhere the film on top of the boiling
tube by placing the thermometer in the middle of mouth of boiling tube after
addition of phenol. Live Public Auctions of Former Test & Measurement
Reply

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