Maugri Grace Kristi P.

Laluma Group Number 4

November 30 and December 3, 2010 December 10, 2010

Experiment Number 2 Recrystallization and Melting Point Determination

I. Objectives 1. To clarify the meaning of purity in the chemical sense. 2. To apply the method of recrystallization in the purification of a solid sample. 3. To recognize the melting point as a physical property that can serve as an index of purity. 4. To determine the melting point of a substance using a simple apparatus. 5. To compare the melting point of a pure versus impure sample of a substance.

II. Theoretical Background

In this experiment the techniques called recrystallization will be studied and the melting point of the collected crystals will be determined to check and analyze its purity content and to check its percent recovery from the original solid organic sample. Recrystallization is a technique often use in purification of solid organic compounds to isolate the purity of the sample and extract impurities. Using this technique will enable you to achieve the highest possible state of purity of the sample. In the step-by-step process of the sample, many simple techniques of separation and solubility will be used that would in turn help in extracting the impurities in the sample.

III. Melting Point Determination TRIAL 1 Melting Point Range (Temperature 1 to Temperature 2) Change in color (if any) Shrinking of sample (if any) 118ÛC-121ÛC none Shrink and became compacted TRIAL 2 119ÛC-122ÛC It became transparent No shrinkage Recorded Measures Weight of Evaporating Dish= 58. But when it was put in an ice-water bath in the next period crystals formed cloudy-like and powdery. Crystal Form Spiky formation on top and cloudy-like formation at the bottom CCl4 No crystal formed but the solution looked immiscible having the upper layer viscose than the lower layer.9156g Weight of Crystal Formed= 0.7523g Weight of Evaporating Dish + Scraped Crystal= 58. Data and Results Characteristics of Resulting Crystals Characteristics Water Size visible Color Cloudy white SOLVENT 95% Ethanol No crystal formed but the solution looked immiscible having the upper layer viscose than the lower layer.1633g Note: This is not the total weight of the crystal since it was not measured when it crystallized in the Erlenmeyer flask. .

crystals will form when the hot solution will be allowed to cool. Its principle is behind the fact that almost all solids are more soluble in a hot than in a cold solvent. Recrystallization of solids is one of the many techniques used for purification of solid organic compounds. water should be the one to be used since in the recrystallization process there are interactions on the bonds of molecules that are polar and some are exhibiting hydrogen bonding. But then the extent of crystallization of the solid depends on the difference in its solubility with the particular chosen solvent and the solid should recover at enough temperatures or the solvent will freeze All in all for the first part of the experiment. If the solid is first dissolved in an amount of the hot solvent where it is insufficient to dissolve it when cold. It is very precise with the theoretical melting point of benzoic acid which is 121ÛC-122ÛC which means we have atleast collected back the crude sample. it may be very soluble in a cold. very polar solvent. Of course. Well in fact. the polarity of the solvent should be taken into account. the resulting crystals that formed is very visible for water but for the 95% ethanol it dissolved and in CCl4.IV. Discussions In this experiment. a solvent of intermediate polarity may be the choice for a satisfactory recrystallization. In choosing its solvent to be used among water. For the melting point determination for the collected crystal of benzoic acid and CCl4. although a highly polar compound is unlikely to be soluble in a hot. In this case. it wasn¶t sure what principle behind was to take into account so we used CCl4. Nevertheless. we have recorded it to be approximately 118ÛC-122ÛC for the two trials. Thus in choosing the good solvent. But in CCl4 when it was put in an ice-water bath in the next period it crystallized. . when we used CCl4 we had a hard time to recrystallized it but after the next period it crystallized when it was out into an ice-water bath. giving a pure solid which are the impurities. Among the three. the molecules of the other compounds dissolved in solution are excluded from the growing crystal lattice. nonpolar solvent. As the compound crystallizes from the solution. Polar compounds are normally soluble in polar solvents and insoluble in nonpolar solvents. It is a process that involves the dissolution of a solid in a chosen solvent at an elevated temperature and re-formation of crystals upon cooling. we are given benzoic acid as the crude sample. whereas nonpolar compounds are more soluble in nonpolar solvents being ³like dissolves like´. 95% ethanol and CCl4. Since the solute is insoluble at room temperature and soluble at high temperature and it is accompanied that its impurities are soluble at all temperature. water is the most polar and it was experimented that it is indeed a good solvent for benzoic acid.

giving a pure solid which are the impurities. The formed crystals should be a pure material since the impurities have dissolved in the solution and is still dissolved after it was cooled. Its structure is a unique arrangement of atoms and molecules in a crystalline liquid or solid. .V. As the compound crystallizes from the solution. And to check in the final part if the collected output is really the pure one. Also if it did not dissolve in the solution then it was removed during filtration before cooling. Recrystallization of solids is one of the many techniques used for purification of solid organic compounds. Calculations VI. Answers to Questions 1. the molecules of the other compounds dissolved in solution are excluded from the growing crystal lattice. the melting point of the solid is determined and it is compared with the original sample to check if it is really pure or not. How does recrystallization free a substance from impurities? Explain how each step in recrystallization contributes to the removal of impurities. 2. It is a process that involves the dissolution of a solid in a chosen solvent at an elevated temperature and re-formation of crystals upon cooling. What is a crystal and what is meant by recrystallization? Crystals are solids that form by a regular repeated pattern of molecules connecting together.

3. . Pure crystalline substances have a clear. (c) The boiling point of the solvent should be low enough so that it can readily be removed from the crystals. sharply defined melting point. It can be used as an index of purity since it determines if the collected output is pure by comparing the gathered melting point range with the theoretical melting point of the crude sample. What is melting point? Why can it be used as an index of purity? The melting point of a substance is the temperature at which the material changes from a solid to a liquid state. What must be considered in choosing a solvent for recrystallization? The choice of solvent is perhaps the most critical step in the process of recrystallization since the correct solvent must be selected to form a product of high purity and in good recovery or yield. (a) The desired compound should be reasonably soluble in the hot solvent and insoluble or nearly insoluble in the cold solvent. (b) Conversely. 4. (d) The boiling point of the solvent should generally be lower than the melting point of the solid being purified. the impurities should either be insoluble in the hot solvent or must remain at least moderately soluble in the cold solvent and very soluble at room temperature. It should be volatile enough for it to evaporate after it crystallized (e) The solvent should not react chemically with the substance being purified.

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