Ice Bath Observations

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Observations In step one an ice bath was prepared. Then in step two, a pipette was used to measure 1 mL of concentrated nitric acid into a 10 mL graduated cylinder. The concentrated nitric acid was placed into a reaction tube and clamped in the water bath. In step four, 1 mL of concentrated sulfuric acid was added slowly to the traction tube with nitric acid. Then the mixture was left to sit in the ice water bath for at least five minutes. A small plastic bag was filled with ice and a towel was wrapped around the bag. A towel was used to wrap the bag to insure that the bag was properly insulated. Then in step nine, using a 1 mL syringe, one portion of 0.250 mL of unknown 8B was added to the reaction tube. Immediately after the unknown was …show more content…
It was observed that it took about ten minutes for the bag to become opaque and thick. It was also observed that once the reaction tube became thick the mixture turned a yellow and orange color. Once the mixture thickened, in step twelve a 30 mL beaker was filled with ice chips to the 5 mL line. The mixture was immediately pouted over the ice and stirred with a glass rod. The mixture was stirred in the beaker until all the ice had melted. Then in step fifteen, vacuum filtration was used to separate the solid from the ice-col mother liquor. The solution was stirred to suspend the solid and the crystals were poured onto the Hirsch funnel. The reaction tube was washed with a small amount of ice water to wash any impurities off the surface of the crystals. In step twenty-one, the solid was transferred to a reaction tube and the solid was recrystallized with a small amount of 95% ethanol. It was observed that it took four increments of 0.5 mL of ethanol to become clear. During this step, it was observed that to much of ethanol was added, therefore the mixture had to be distilled for about 25 minutes. The solution was removed and allowed to cool in a nest of glass wool in a 100 mL beaker. Once the beaker cooled down, the redaction tube was placed in a beaker …show more content…
Nitration occurs when benzene is treated with a mixture of nitric acid and sulfuric acid. The reaction proceeds from an electrophilic aromatic substitution, where a nitronium ion acts as then electrophile. Nitration of aromatics is one of the oldest and industrially most important reactions. A reaction between an organic compound and a nitrating agent leads to the introduction of a nitro group onto a carbon, nitrogen or oxygen atom of that organic compound. Examples of nitration used in numerous applications such as in the production of explosives and pharmaceutical compounds. Also nitration is an irreversible reactionThe unknown assigned was 8B. After recrystallizing, the crystals had a melting point of 68 degrees Celsius and identified as 1-(2-bromoethyl)-4-nitrobenzene because 1-(2-bromoethyl)-4-nitrobenzene has a melting point between 67-69 degrees Celsius. Because nitration is taking place unknown 8B identified as unknown (2-bromoethyl)-benzene. In this experiment 0.250 ml of unknown was used, 1 mL of concentrated nitric acid, and 1 mL of concentrated sulfuric acid was used. This experiment resulted in a low percent yield of 12.86%. There could be many explanations to account for the low percent yield. One could be that not all crystals were collected and that some could still be located in the funnel. Another

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