EXP262

Lizzie Clark with Andrew Lang
 * Researchers **

To recrystallize cinnamic acid using distilled water.
 * Objective **

Trans-cinnamic acid (MSDS) 125 mL erlynmeyer flask Stopper for erlynmeyer flask Weigh Paper Electronic Balance Chemical Spatula Funnel Pipette 25 mL volumetric flask 25 mL distilled water (MSDS) Hot water bath Cool water bath Thermometer Gloves Safety Goggles Lab Coat Vacuum hose Ring Stand and clamp Buchner funnel Rubber filter column Filter paper Side arm flask Plastic Spatula
 * Materials **

1. Weigh empty volumetric flask (in grams). 2. Weigh volumetric flask with 25mL of distilled water (solvent) in it. 3. Pour the 25mL of solvent into an erlynmeyer flask and place stopper on the top to prevent evaporation of solvent. 4. Calculate and measure out the amount of trans-cinnamic acid (solute) needed for the intended concentration. 5. Add measured trans-cinnamic acid to erlynmeyer flask with distilled water. 6. Place erlynmeyer flask in hot water bath and swirl periodically. 7. Gradually increase the water bath's temperature until all solute has dissolved. 8. Record temperature that the solute finally dissolves at. 9. Place flask aside to cool at room temperature. Planning Sheet for 0.25M solution Planning Sheet for 0.1M solution Planning Sheet for 0.05M solution <span style="background-color: white; font-family: Arial,sans-serif; font-size: 10pt;">Planning Sheet for 0.01M solution
 * <span style="background-color: white; font-family: Arial,sans-serif; font-size: 15.5pt;">Procedure **

We got an 80.6% return from Flask A (0.05M solution).
 * <span style="background-color: white; font-family: Arial,sans-serif; font-size: 15.5pt;">Results **


 * <span style="background-color: white; font-family: Arial,sans-serif; font-size: 15.5pt;">Log **

<span style="font-family: Arial,sans-serif;">2/21/12
<span style="font-family: Arial,sans-serif;">*Working toward a concentration of 0.25 M. <span style="font-family: Arial,sans-serif;">9:33- Empty 25mL flesk weighed 20.247g. <span style="font-family: Arial,sans-serif;">9:36- 25mL of distilled water in flask weighed to be 45.208g. <span style="font-family: Arial,sans-serif;">*Room temperature at 19.0 C. <span style="font-family: Arial,sans-serif;">9:51- Measured out experimental amount of cinnamic acid of .955g (the predicted value was 0.954g). <span style="font-family: Arial,sans-serif;">9:58- Added 25mL of distilled water to beaker and added measured cinnamic acid. Parafilmed beaker. <span style="font-family: Arial,sans-serif;">9:59- Place in hot water bath at 49.0 C and swirled. <span style="font-family: Arial,sans-serif;">10:04- Hot water bath at 53.5 C. Stopped swirling and left to sit in hot water bath while my lab partner got close to her boiling point (of around 69.0 C) because the boiling point for water is much higher. <span style="font-family: Arial,sans-serif;">* Dr. Andrew Lang later brought solution to a boiling but all the solute still did not dissolve.

<span style="font-family: Arial,sans-serif;">2/28/12 <span style="font-family: Arial,sans-serif;">* Restarted experiment with a new concentration of .0.1 M. This new concentration required a new value of cinnamic acid of 0.375g. <span style="font-family: Arial,sans-serif;">9:03- Funneled and pipetted 25mL of distilled water into volumetric flask. <span style="font-family: Arial,sans-serif;">9:07- Measured out 0.374g of cinnamic acid on the electric balance using weigh paper. <span style="font-family: Arial,sans-serif;">9:08- Poured the 25mL distilled water and 0.374g of cinnamic acid into a 125mL erlynmeyer flask and placed a stopper on the top. <span style="font-family: Arial,sans-serif;">9:09- Placed in 52.0 C hot water bath and swirled periodically. <span style="font-family: Arial,sans-serif;">9:11- Hot water bath temperature at 54.0 C. <span style="font-family: Arial,sans-serif;">9:32- Hot water bath temperature at 58.8 C. <span style="font-family: Arial,sans-serif;">9:37- Hot water bath temperature at 61.0 C. <span style="font-family: Arial,sans-serif;">10:00- Hot water bath temperature now at 65.0 C. <span style="font-family: Arial,sans-serif;">10:10- Hot water bath temperature now at 79.0 C. <span style="font-family: Arial,sans-serif;">10:14- Hot water bath temperature now at 82.0 C. <span style="font-family: Arial,sans-serif;">10:20- Hot water bath temperature now at 86.0 C. <span style="font-family: Arial,sans-serif;">10:29- Hot water bath temperature now at 88.0 C. <span style="font-family: Arial,sans-serif;">* No changed detected. Forced to abandon due to time constraints.

<span style="font-family: Arial,sans-serif;">3/6/12 <span style="font-family: Arial,sans-serif;">*Further altered experiment and worked with multiple flasks. Flask A represents a 0.05M solution, and Flask B represents a 0.01M solution. <span style="font-family: Arial,sans-serif;">*Room temperature at 20 C <span style="font-family: Arial,sans-serif;">Flask A: <span style="font-family: Arial,sans-serif;">8:55- Empty volumetric flask weighed 20.248g. <span style="font-family: Arial,sans-serif;">8:58- 25mL of distilled water in volumetric flask weighed 45.169g. <span style="font-family: Arial,sans-serif;">8:59- Poured 25mL of distilled water into erlynmeyer flask (Flask A) and stoppered. <span style="font-family: Arial,sans-serif;">9:06- Measured out 0.186g of cinnamic acid and placed in Flask A. <span style="font-family: Arial,sans-serif;">9:08- Placed Flask A in hot water bath at 73 C (which rose to just under 100 C throughout the course of the experiment). Swirled periodically till all solute dissolved. <span style="font-family: Arial,sans-serif;">9:19- Water bath at 80 C. <span style="font-family: Arial,sans-serif;">9:32- Temperature remained constant, so placed Flask A directly on hot plate. <span style="font-family: Arial,sans-serif;">9:34- Water in Flask A brought to nearly boiling. <span style="font-family: Arial,sans-serif;">9:35- All dissolved in Flask A. Set aside to coll at room temperature. <span style="font-family: Arial,sans-serif;">Flask B: 9:01- Empty volumetric flask weighed 20.375g. 9:02- 25mL of distilled water in volumetric flask weighed 45.189g. 9:03- Poured 25mL of distilled water in erlynmeyer flask (Flask B) and stoppered. 9:11- Measured out 0.038g of cinnamic acid and added it to Flask B. 9:13- Placed Flask B in hot water bath, now at 75 C. <span style="font-family: Arial,sans-serif;">9:19- Water bath at 80 C. <span style="font-family: Arial,sans-serif;">9:21- Flask B completed dissolved at 81 C. removed Flask B to cool at room temperature.
 * Be aware that the stopper may pop off with force during the heating process. Wear proper safety gear.**

<span style="font-family: Arial,sans-serif;">3/13/12 <span style="font-family: Arial,sans-serif;">Filtration of Flask A (0.05M solution) <span style="font-family: Arial,sans-serif;">9:40- Set up vacuum filtration system similar to what is seen here. Ran vacuum for ~30 mins. <span style="font-family: Arial,sans-serif;">10:35- Weight of the filtrate is 0.15g. <span style="font-family: Arial,sans-serif;">10:35- Filtrate placed at room temp to see if more drying is needed. <span style="font-family: Arial,sans-serif;">10:40- Weight of the filtrate remained the same, filtration is complete. <span style="font-family: Arial,sans-serif;">*Flask B will not be filtrated because we are interested in using the highest molarity possible- which was Flask A.