Experiment 3 Lab Report

ADAMSON UNIVERSITY College of Engineering Chemical Engineering Department M a n il a

Experiment no. 3

SOLUBILITY DIAGRAM OF A PARTIALLY MISCIBLE LIQUID SYSTEM

Submitted by: Lavilles, Francis Dominic Lee Gee Hyun Lojica, Kathlyn Joyce M.

Date performed: July 18, 2015 Date submitted: July 27, 2015

ABSTRACT: The purpose of this experiment is to determine the solubility diagram for a system that is made up of two partially miscible liquid components A and B which is phenol and water. This solubility diagram is an equilibrium composition of solution as a function of temperature and pressure. In the experiment, 80% phenol solution was prepared and was placed in an acid burette. Using another burette, distilled water was added to the phenol solution while stirring nonstop until a cloudy solution formed. The tube was placed in the water bath and the water in the hot bath was heated until a clear solution formed. The results showed that as the number of runs increases, the %weight of phenol also increases. The different volume ratios of mixtures prepared were subjected to constant heating and cooling in order to gather the needed temperature necessary for the construction of the solubility curve of Phenol-Water solution.

INTRODUCTION: A few liquids are miscible with each other in all proportions while others have miscibility under certain proportions only. Miscibility is to mix the liquids to form a homogeneous solution. A typical example for this is phenol and water. Under certain temperature and concentration of phenol and water, the phenol and water maybe in 1 phase condition or maybe being separated into 2 different phases. Generally, both liquids become more soluble with rising temperature until the critical solution temperature or consulate point is attained, and above that point, the liquids will turn into only 1 phase. At any temperature below the critical solution temperature, the composition for the 2 layers of liquids in equilibrium state is constant and does not depend on the relative amount of these 2 phases. The solubility for a pair of partially miscible liquids in general is extremely influenced by the presence of a third component.

REVIEW OF RELATED LITERATURE: The solubility diagram is a graph of the equilibrium composition of a mixture as function of temperature. A solubility diagram for a system made up of two partially miscible liquid components can be made. Miscible liquid mixtures are being studied in recent researches (Califano et. al., 2014). A simple phenol-water system can be examined and used in constructring a solubility diagram. The phenol-water system is the mixture used in this experiment. Other studies examine phase and solubility of other systems. For example, in a certain study the liquidliquid equibria of the water-acetic acid-butyl acetate system was investigated. (Ince, 2002). Studies are also made about the equilibria of mixtures involving water -phenol and another third component like carbon dioxide (Yoon, 2004) The study of phenol-water system has many industrial applications. It can be applied to cases that involve extraction of phenol from industrial water (Jabrou, 2012). It can also be applied to phenol removal from water in some recent study (Zhang, 2013). Another research probed the degradation of phenol in water solution by photo catalysis (Laoufi, 2008). A recent study quantified phenol in surface water by gas chromatography and mass spectroscopy (Hossain, 2009). Solubility and phase diagrams for complex mixtures of soluble and membrane proteins are being examined in recent studies (Talreja, 2010). Solubility diagrams have many applications and uses. Analysis of solubility diagrams are made on some important pharmaceutical drugs like diazepam and nitrazepam (Hadziabdic,2012). Solubility and phase diagrams for fatty acids are also being examined in some researches (Tzocheva, 2011).

METHODOLOGY: Eighty percent of phenol solution was prepared. This was done by using the graduated cylinder. About twenty ml of melted phenol was put in the graduated cylinder and distilled water was added which was equivalent to one-fourth the weight of the phenol using burette. The weight of the phenol was recorded. All the phenol solution was placed in a clean acid burette. Ten millilitre of the phenol was added in the burette and covered with a cork. A thermometer and a copper wire stirrer were fitted in the cork cover. Using another burette, distilled water was added to the phenol solution while stirring nonstop until a cloudy solution formed. The volume of phenol solution was recorded. The tube was placed in the water bath and the water in the hot bath was heated until a clear solution formed. The temperature was recorded. The tube was taken from the water bath and was stirred nonstop until a cloudy solution formed. The temperature at which the cloudy solution formed was noted. An additional 1ml of water was added from the burette and the previous step was repeated. This was done 4 times. Another ignition tube was used and 10ml of distilled water was added from a burette. Phenol solution from a burette was then added while stirring nonstop until a cloudy solution formed. Previous steps are repeated as necessary. All the data was recorded in the table. The % weight of pure phenol in all solution was computed and the density of the 80% phenol solution used is 1.05 g/mL.

RESULTS: Table 1. Water Add to Phenol Run No.

1

2

3

4

5

6

68

66

72

70

68

68

70

62

64

68

64

64

69

64

68

69

66

66

10

10

10

10

10

10

10.5

10.5

10.5

10.5

10.5

10.5

8.4

8.4

8.4

8.4

8.4

8.4

5

6

7

8

9

10

13.4

14.4

15.4

16.4

17.4

18.4

66.69

58.33

54.55

57.22

48.58

45.65

2

3

4

5

6

Clearing temperature (oC) Clouding temperature (oC) Average temperature (oC) Volume of phenol solution Weight of the phenol solution (W1) Weight of pure phenol Weight of water added to phenol (W2) Total weight of solution (WT) Weight % phenol

Table 2. Phenol Added to Water Run No.

1

Clearing temperature (oC)

65

70

72

70

65

61

72

63

64

68

66

66

68.5

66.5

65

69

65.5

63.5

10

11

12

13

14

15

10.5

11.55

12.6

13.65

14.70

16.75

8.4

9.24

10.08

10.92

11.76

12.6

10

10

10

10

10

10

18.4

19.24

20.08

20.92

21.76

22.6

45.65

48.02

50.20

51.20

52.45

55.25

Clouding temperature (oC) Average temperature (oC) Volume of phenol solution Weight of the phenol solution (W1) Weight of pure phenol Weight of water added to phenol (W2) Total weight of solution (WT) Weight % phenol

DISCUSSION: In most cases, partially miscible liquids become more soluble in each other with increasing temperature until the critical solution temperature is reached, above which there is complete miscibility. In this experiment mixtures of known composition are heated until they dissolve completely. This is easily recognized by the disappearance of cloudiness due to two phases.

From the table A, on the water added to phenol, the results showed that as the number of runs increases, the weight% of the phenol decreases. From the table B, on the phenol added to water, the results showed that as the number of runs increases, the weight % of phenol also increases. If a small amount of liquid phenol is added to a large quantity of water, it gives a single phase system, which means the solution of phenol in water. If a small amount of water is added to a large quantity of liquid phenol, it gives a single phase system, which means the solution of water in phenol. When water and liquid phenol are mixed in ‘comparable’ proportion, a two phase system results in one phase. The solubility of partially miscible liquids rises with temperature. In this case, the solubility curve exhibits a maximum at the “critical solution temperature” above which the two liquids become completely miscible at all proportions. The possible sources of error are personal errors. Personal errors may emerge from the fault of the researcher in determining the correct temperature reading, or failing to give an accurate volume reading.

CONCLUSION AND RECOMMENDATION: From the water added to phenol, as the volume of phenol solution increases, the weight percent of phenol decreases. From the phenol added to water, as the volume of phenol solution increases, the weight percent of phenol also increases. Partially miscible liquids become more soluble in each other with increasing temperature until the critical solution temperature is reached, above which there is complete miscibility.

The researchers recommend avoiding any solution of phenol. Also avoid spilling and clean up immediately with large amounts of water, and to never pipette by mouth.

APPENDIX: Sample computations: Ave .temperature=

clouding temperature+clearing temperature 2

Ave .temperature=

68+70 =69℃ 2

density of phenol solution=

mass of phenol solution volume of phenol solution

mass of phenol solution=1.05

g ∗10 ml=10.5 g ml

total weight of solution=mass of pure phenol+ mass of water total weight of solution=8.4 g+10 g=18.4 g

weight of phenol=

mass of phenol x 100 mass of solution

weight of phenol solution=

8.4 x 100 =45.65 18.4

REFERENCES: 1. Yoon J.H., Lee H., 2004. Clathrate phase equilibria for the water–phenol–carbon dioxide system. AIChE Journal. Vol. 43, Issue 7, pp 1884–1893

2. Talreja S., Perry S.L., Guha S., Bhamidi V., Zukoski C.F., Kenis P.J.A., 2010. Determination of the Phase Diagram for Soluble and Membrane Proteins. Journal of Physical Chemistry B, 2010, 114 (13), pp 4432–4441 3. Hadziabdic J., Elezovic A., Rahic O., 2012. Indira MujezinEffect of Cyclodextrin Complexation on the Aqueous Solubility of Diazepam and Nitrazepam: Phase-Solubility Analysis, Thermodynamic Properties. American Journal of Analytical Chemistry. 2012, Vol 3, pp 811-819 4. Tsocheva S.S., Kralchevsky P.A. , Danov K., Georgieva G.S., Post A.J., Ananthapadmanabhan K.P., 2011. Solubility limits and phase diagrams for fatty acids in anionic (SLES) and zwitterion (CAPB) micellar surfactant solutions. Journal of Colloid and Interface Science, 2011, Vol. 369, pp 274-286 5. Wang L., Cheng Y., Xiao X., and Xi Li X., 2007. Liquid−Liquid Equilibria for the Ternary Systems Acetic Acid + Water + Butyl Acetate and Acetic Acid + Water + 2Methyl Propyl Acetate at 304.15 K, 332.15 K, and 366.15 K. American Chemical Society, 2007. 52 (4), pp 1255–1257 6. Jabrou S.N., 2012. Extraction of Phenol from Industrial Water Using Different Solvents .Research Journal of Chemical Sciences, 2012. Vol. 2(4), pp 1-12. 7. Zhang J., 2013. Phenol Removal from Water with Potassium Permanganate Modified Granular Activated Carbon. Journal of Environmental Protection, 2013, Vol. 4, pp 411417 8. Laoufi N.A., Tassalit D., Bentahar F., 2008. The Degradation of Phenol in Water Solution by TiO2 photocatalysis in a Helical Reactor. Global Nest Journal, 2008, Vol. 10 No. 3, pp 404-418 9. Hossain M.A., Salehuddin S.M., 2009. Quantification of phenol in surface water by gas chromatography and mass spectroscopy. Asian Journal on Energy and Environment, 2009, Vol 10, pp 91-98

10. Califano F., Nozadze G., Manh A.L.V, Farhat A., 2014. Study of miscibility of liquid mixtures with a critical point: A new experiment for a physical chemistry course. International Journal of Physical Sciences. 2014, Vol. 9(16) pp 350-359