Lab 1 - Crystallization

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Northeastern University *

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2322

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Chemistry

Date

Feb 20, 2024

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pdf

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4

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Experiment 1 Crystallization Marina Gobbi Lab Partner Tochi Chukwuemeka Teaching Assistant Arezou Dilmaghanimarand Date Performed January 30, February 7, 2024 Date Due February 8, 2024
Gobbi 2 Experimental Objective This week, the melting point of an unknown compound was determined through crystallization. We dissolved an impure compound, filtered it, and crystallized the pure substance to find its melting point, and determine what compound it is. Theoretical Yield As per the student data sheet and procedure, weights and amounts of substances were not considered, meaning theoretical yield is not being calculated for this week’s lab. Procedure Given an unknown packet with carbon and an unknown compound, we had been set to isolate the unknown and find its melting point. This allowed us to determine the unknown compound's melting point, and therefore, its identity. Roughly 20 mL of water was boiled in a 50 mL Erlenmeyer flask, where we submerged, and dissolved, a test tube with 0.250 grams of the unknown sample (packet #342). A glass funnel covered with an 11 cm filter paper was then used to filter the charcoal from the hot solution into a 20 mL beaker. It was made sure that all the unknown sample was filtered by pouring more hot water into the test tube and around the glass funnel. After cooling the solution on the benchtop for 2 minutes, the same beaker was then submerged in an ice bath and stirred for approximately 10 minutes. Crystals were formed by this point, which were aspirated using a clamped filter flask. After suction, the crystals left outside the flask were placed on a piece of filter paper which were then left to dry for a week. After the week, the dried crystals were placed in a capillary tube, and then a melting-point apparatus to determine the melting point of the unknown substance alone. Observations
Gobbi 3 The procedure was followed for the lab. Some purification was noticed during the first (gravity) filtering process, but full purification and isolation from the carbon was not. In a perfect experiment, crystals were to be a cloudy white color, but it was found to be grey-ish during this experiment. After melting, the same grey crystals were turned into a liquid of the same grey color. Characterization When in the melting-point apparatus, the crystals melted between the temperatures of 150.4°C and 156.3°C. With a range of 5.9°C, our crystals were found to be impure. Conclusion As mentioned above, our crystals had a melting point range of 150.4°C-156.3°C, leading us to identify the unknown compound as adipic acid, as it has a similar melting point of 151°C to 153°C. It is noteworthy, however, to mention that with a melting point range of 5.9°C, our crystals were found to be impure (anything above a range of 2°C is impure (p. 73)). During the first filtering process, the filter paper burst, meaning some of the impurities (carbon) were allowed into the beaker that were going to form the crystals. Because of this, we cannot exactly determine our unknown, but instead have a relative guess. Question on Data Sheet Group 1 had the better data, since their melting point range was less than 2°C. This meant their unknown was pure, and the group was better suited to determine what their compound was. Group 2 could improve their results by double checking if any filters burst while using any funnels. The gravity and suction isolations are both examples of when a filter is used and can fail separating the crystals from liquid or impurities. Additionally, the group should double check that the unknown was fully dissolved during the first step of the procedure. References
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Gobbi 4 Zubrick, James W. The Organic Chem Lab Survival Manual: A Student’s Guide to Techniques . 11th ed., Hoboken, NJ, Wiley, 2020, pp. 73 74.