1.

0 INTRODUCTION

The purity of a substance is a factor that has to be tested in order to prove that it is really pure because most of the time it can be contaminated, without even being known. There are three physical methods used for this purpose, namely melting point determination, boiling point determination and by determining the refractive index of the substance.

Pure substances have a characteristic melting point, which is expressed as the temperature range over which the solid melts to become a liquid. The transition between the solid and the liquid is extremely sharp for small samples of the substance that melting points can be measured to 0.1 C. It normally never exceeds 1 C. In the melting of crystalline solids, a sharp melting point is observed. As they melt at a very narrow range of temperatures, they are suitable to be used in determination of a substances purity. In this experiment, benzoic acid was used as the substance to be tested. Benzoic acid will be inserted into the melting point apparatus and heated. The resulting melting point is normally recorded twice, one at a higher temperature to get a stable temperature and another at a lower temperature to get an accurate temperature.

The boiling point of pure liquids is also a characteristic physical property. However, the process of determining the boiling point is considered more complex that for the melting point. It requires more material and because it is less affected by impurities, it is not a very good indication of purity. Just like the melting point the boiling point of a liquid is affected by the forces that attract one molecule to another via ionic attraction, dipole-dipole attraction, hydrogen bonding and van der Waals force. If a very clean liquid in a very clean vessel is heated,

superheating occurs and does not boil when subjected to a temperature above its boiling point. Explosions too may occur. To avoid this problem, boiling stones are a must before heating these liquids.

Lastly, refractive index is also a physical constant like the boiling point that can be used to characterize liquids. It is the ratio of the velocity of light in air to the velocity of light in liquid. The angle of refraction is a function of temperature and the wavelength of light. As the velocity of light in air is always greater that a liquid, the refractive index is always a number greater than 1, for example, hexane is n20D 1.3751. The superscript indicated the measurement was made at 20C and the subscript refers to the yellow D-line of a sodium vapour lamp, light with a wavelength of 589 nm. The measurement can be made by adding a few drops of liquid on the prism surface and adjusting the refractometer to obtain the intended readings.

The objective of the this experiment is to identify the Purity of the Organic Compounds by Identifying its Melting Point, Boiling Point and Refractive Index.

2.0 MATERIAL AND METHODOLOGY

2.1 Experimental Materials A small amount of benzoic acid, liquid ethanol and four different solutions with known composition

2.2 Experimental Apparatus Melting point apparatus, simple distillation apparatus and refractometer

2.3 Experimental Procedures Part A: Melting Point Benzoic acid solid was given to measure its melting point. i) A small amount of the sample was then put into the melting point tube and the substance was made to rest at the bottom of the melting point tube. ii) The melting point tube was then inserted into the apparatus and it was made sure that the tube went right into the end and was visible under the magnifying lens. iii) The heater of the melting point apparatus was started and left at a rate of 5 degrees per minute. iv) The substance was observed continuously as well as the temperature of the thermometer provided. The temperature at which the substance starts to melt and completely melt was noted. This was the melting range. It was visible when the solid changed to liquid. v) The experiment was repeated at a slower rate of heating to get a more accurate result.

Part B: Boiling Point i) A small amount of liquid ethanol was taken and the equipment was arranged as shown. ii) The heating was started at a rate of 5 degrees per minute until the substance started to boil. iii) The temperature at which the substance began to boil was noted. iv) The experiment was repeated at a slower heating to get a more accurate result.

Part C: Refractive Index i) The prism of the refractometer is made sure to be clean and dry. ii) 1-2 drops was placed on top of the prism and the cover was locked. iii) The temperature was noted. iv) The refractive index was read as shown. v) Four solutions with known composition and 1 unknown were provided. Their refractive index was noted and the correlation curve of refractive index against the composition of the solution mixture was plotted. The % of composition of the solution provided was read from the graph.

3.0 RESULTS AND DISCUSSION 3.1 Collection of Data Part A: Melting Point
Solid Temperature of apparatus Temperature the sample start to melt (C) Benzoic acid 5 C per minute 2 C per minute 124 124 125 125 124-125 124-125 Temperature sample completely melt (C) Melting range (C)

Part B: Boiling Point

Liquid Ethanol Temperature of apparatus 5 C per minute 2 C per minute Temperature the sample boils (C) 78 C 78C

Part C: Refractive Index

Composition % Refractive Index 1.446 1.476 1.432 1.425 1.456 20/80 40/60 50/50 60/40 Unknown

3.2 Discussion For part A, the melting point obtained for benzoic acid is within the range of 123-125 C. This means that the melting point is estimated to be at this point. The original boiling point of benzoic acid is 122.4 0C. In this experiment, the melting point seems to be slightly higher than the original melting point. This may be due to certain errors in the experiment. For part B, the boiling point obtained for ethanol is 78 C. The original boiling point of ethanol is 78.260C. Thus it can be seen that there is a very small percent of error from the original readings as the experimental readings obtained was comparably lower. Finally, for part C, the different compositions of mixtures give out different refractive indices. From the graph, it is known that the composition of the unknown solution is 26/74 %. (Refer to graph 1).

1. a) At a fast rate of heating, the melting point and boiling point of a substance is higher than the true one because, the actual melting point and boiling point would take some time to reach. This is mainly due to the fact that temperature stabilization occurs at this point. Once the temperature range is found to be stable enough, a slower heating will produce the accurate melting point and boiling point.

b) Impure substances give different readings of boiling points and melting points. Boiling happens when the vapor pressure equals to the outside pressure. The presence of impurities in solutions lowers the vapor pressure so more energy has to be added. The simple reason is this. When you add salt, for example, to water, the water molecules

interact with the salt ions. As a result, it takes energy from the surroundings to dissolve the salt. The salt-water interacted species are now more stable than just the water alone. Now when you try to turn the water into vapor, these interactions have to be broken down (the same reason water has a high boiling point than expected due to hydrogen bonding). Breaking down these interactions takes energy, so the boiling point increases because you now have to separate the water from the salt as well as vaporize it. On the other hand, the melting point may increase or decrease depending on the impurities contained in a solid. No matter what impurities they are, they are a form of matter with specific characteristics and again more energy will be needed to melt the substance which explains the difference in melting points obtained.

c) The melting point shows better indication of purity compared to boiling point. This is because the boiling point is harder to determine considering the fact that it would need more materials and it is less affected by impurities.

d) It is important to state the temperature when measuring refractive index because refractive index varies inversely with temperature. If the temperature is not stated, readings of the refractive index would be considered inaccurate.

4.0 CONCLUSION

As a conclusion, the purity of substances can be identified by determining their melting point, boiling point and refractive index with melting point determination being the most suitable method. For this experiment, the boiling point obtained for ethanol is 78 C. As its percentage of error was considerably small, the experiment was successful in determining the purity of ethanol. Similarly, the melting point of benzoic acid obtained was at a range of 124-125 C, which also proved that its purity was successfully determined. Finally, the % composition of the unknown solution was 24/76 % based on the graph.

5.0 LIMITATION OF EXPERIMENT

5.1 Limitation of technique This technique cannot bear 100 % accuracy as it is impossible to obtain absolutely pure samples to be tested on. Even though they were pure initially, while the experiment was conducted, it is absolutely possible for impurities (especially from air) to contaminate the samples.

5.2 Errors that may have occurred A few errors could have occurred during this experiment. Firstly, the starting sample may have been impure. This would explain why the melting and boiling point was slightly different than the original values. Next, the instruments may have been read inaccurately. In both cases, the occurrence of parallax error could have caused some inaccuracies in the readings obtained. On the other hand, if too much or too little sample is used, errors are bound to occur.

5.3 Improvement and Safety Precautions A few improvements can be done to reduce errors in the experiment and some safety precautions should be observed. Firstly, try to eliminate all kind of contamination while the experiments are conducted. This decreases the presence of impurities in the samples and thus increases the accuracy of the readings. Next, parallax error can be avoided if the meniscus of the thermometer is read at a position where it is parallel to the eye. Also, make sure samples are not heated too fast. Avoid heating faster than five degrees per minute as it guarantees poor results in most cases. For this experiment, it is very important to wear safety goggles as boiling substances can incur in spilling or accidents and boiling ethanol can be very harmful. Also, distillation should never be

conducted in a closed system, as the pressure of the heated gases inside the apparatus can cause ruptures. Lastly, make sure the liquid is handled with care as it is flammable and is explosive.

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REFERENCE

1. Chandy (2009), Melting Point, Boiling Point and Refractive Index, Retrieved on 8th October 2010 from http://spot.pcc.edu/~chandy/241/meltptboilptrefract.pdf

2. P. Atkins(1994), Physical Chemistry, 5th edition, Retrieved on 9th October 2010 from http://www.mynamehere.com/edu/pchem/fphased.html

3. Unknown author, (from many sources), (2010), Organic Qualitative Analysis, Retrieved on 9th October 2010 from http://faculty.swosu.edu/william.kelly/pdf/qo2.pdf

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