Calorimetry Lab Report

Reaction 2 - 1.Used a Beral- type pipet, added about 2mL (40 Drops) of 1M hydrochloric acid solution to a small test tube.

The aqueous extracts were combined in an Erlenmeyer flask and cooled down in an ice bath to 10C.

1.5ml of nitric acid was added to .30g of benzoin in a conical vial with a stir vane. The mixture was then heated in a 70 degree Celsius water bath, while stirred, for one hour. The mixture in the conical vial was then cooled to room temperature and, using a pipette, the solution was transferred to a beaker containing 4ml of ice water. The mixture slowly crystallized in the beaker and the crystallized product was filtered on a hirsch funnel with vacuum. 5 ml of cold water was used to wash the product and then the product was allowed to dry.

Cool solution in the ice bath before adding 2 mL of methylene chloride. Mix the two phases by drawing and squirting methylene chloride into aqueous layer.

Discard the solution in the appropriate container as directed to you by your lab instructor.

1.8 ml is saved to freeze for restriction digests. Then add 200 μl of resuspension solution inacti-

Fill granulated cylinder with water by submerging and make sure no bubbles at the top.

Boil up the mixture on medium warmth until the water is decreased by a third and after that let it cool for some time.

This was done for 15 minutes until there were no visible vapors coming from the reaction mixture. The reaction mixture was then poured into a 50-mL beaker containing 5g of ice. The reaction flask was rinsed three times with 2 mL of dichloromethane. The rinsing was also added to the ice mixture.

Apply heat to a hot water vapor, 5-7 minutes, constantly messing, until the mixture is homogenous.

As moisture starts to condense in the upper part of the test tube, carefully heat the entire length of the tube. Continue doing this for 2-3 minutes until all of the moisture is driven from the tube. Repeat steps 3 and 4 for the other two tubes.

Use either bowl, sink or tub with warm to hot water. Adjust the temperature to your preference, but it needs to be warm for this process.

Reflux the mixture for 30 minutes, adjusting the flame to ensure smooth boiling. Ensuring that the mixture is refluxed for 30 minutes guarantees the reaction completes so that the vapours continuously condense for re boiling. 6. Put 20cm3 of distilled water into a separating funnel. Pour the cooled mixture into the separating funnel.

Test Tube C- The test tube settled and came to room temperature. We added a crystal of sodium thiosulphate pentahydrate and it dissolved slightly. The test tube became slightly colder.

Place the sealed end of the two tubes into the melting point apparatus as follows: your product on the left and pure acetylsalicylic acid on the right. You may need to share a melting point apparatus with another two lab partners. In this case, since there are only three sample slots in the apparatus, put the pure acetylsalicylic acid in the middle and