87.973, Ⓒ -0/1- 87.973 From the procedure 4. Add-2 g of salicylic acid and re-weigh the flask. Record the mass Mass of
Posted: Thu Jul 07, 2022 1:44 pm
From the procedure 4. Add-2 g of salicylic acid and re-weigh the flask. Record the mass Mass of Elenmeyer flask + salicylic acid (g) D 89.978
From the procedure 5. Working in a fume hood, carefully add 5 mL of acetic anhydride to the flask Volume of acetic anhydride used (mL) Graduated cylinder reading 5.1
6. Slowly add 10 drops of 85% phosphoric acid, H₂PO4 7. Stir the mixture with a stirring rod. 8. Place the flask in the boiling water bath and stir until the solid dissolves. 9. Once the solid dissolves, remove the flask from the water bath and allow it to cool to room temperature. 10. Allow the reaction mixture in the beaker to cool to room temperature. 11. While your reaction is cooling, obtain a 400 mL beaker and prepare an ice-water bath 12. Working in a fume hood, carefully add 20 drops of water to the cooled mixture. 13. Once the reaction is complete, and no further change is observed, add 50 mL of cold water. 14. Place the flask into the ice bath for about 10 minutes to cool the mixture. 15. Stir gently. Aspirin will precipitate from solution. If no crystals form, gently scratch the inside of the flask with the stirring rod. Aspirin Collection - Vacuum Filtration From the procedure 1. Obtain the necessary glassware and equipment to assemble the vacuum filtration apparatus in Figure A.3 in the lab manual. 2. Securely clamp a clean filter flask to the ring stand. The filter flask should be larger than the flask containing the solution you are about to filter. 3. Attach a piece of heavy-walled tubing onto the sidearm of the flask. Connect the tubing to the water aspirator. 4. Put a filter adapter on top of the filter flask and then place the funnel in the filter flask. Ensure that the neck of the funnel fits snugly in a rubber washer. 5. Add a piece of filter paper just large enough to cover the holes in the bottom of the funnel. Make sure the filter paper is flat and does not curl up at the sides 6. Carefully wet the filter paper using clean, ice-cold water to help the filter paper stick to the bottom of the Büchner funnel. 7. Turn on the vacuum and slowly pour the solution with the aspirin crystals onto the center of the filter paper.
my pour te UTOWOTE WENT Le 8. If any crystals remain in the flask, transfer them to the funnel using a spatula. Rinse the inside of the flask with ice-cold water and pour it onto the funnel. 9. Rinse the crystals collected with two 10 mL rinses of cold water. Spread the crystals out on the filter paper to aid in drying. 10. Once the liquid has been removed, turn off the vacuum before disconnecting the tubing. Hold the funnel in place and disconnect the hose from the water aspirator and then turn off the water. If you turn off the water before you disconnect the tubing, water will back up into your filtrate 11. Carefully remove the filter paper from the flask using a spatula and place the filter paper with the crystals on a paper towel and allow the crystals to air dry 12. Weigh a clean and dry watch glass. Record the mass Mass of empty watchglass (g) 29.869
(1pts) Mass of watchglass + dried aspirin product (0) (19pts) Calculation of Yields Mass of Erlenmeyer flask+ salicylic acid 32.249 g -0/T. 32.249 89978 0 11.
(19p Mass of Erlenmeyer flask + salicylic acid: Mass of empty Erlenmeyer flask (1pts) Mass of salicylic acid used (g) (2pts) Moles of salicylic acid (mol) Volume of acetic anhydride (2pts) Moles of acetic anhydride (mol) note: the density of acetic anhydride is 1.00 g/ml (2pts) What is the limiting reactant? 2.38 Choose.... 89.978 g 87.973 g 5.10 mL
Mass of empty watchglass (1pts) Mass of aspirin obtained (g) (2pts) Moles of aspirin obtained (mol) (3pts) Aspirin theoretical yield (g) (2pts) Product percent yield 29.869 g 11
(4pts) is your percent yield within reason of what you would expect? Explain your answer. Normal : BIU X₁ X¹ pH Test BEE (21pts) Purity of Aspirin Synthesized From the procedure 1. Obtain 4 test tubes and a test tube rack. 2. Add the following to the specified test tubes: 18 1,3 mL of 0.15% salicylic acid (reference sample) 2. A spatula tip of crushed commercial aspirin and 3 mL of water 3. A spatula tip of crushed buffered aspirin and 3 mL of water 4. A spatula tip of your aspirin product and 3 mL of water 3. Stir each solution with a stirring rod 4. Measure each solution's pH using pH paper and record. IT 90 T T
Virtual pH Paper Key 0 1 Virtual pH Tests Result 2 3 4 5 6 7 8 9 10 11 12 | 0.15% salicylic acid Commercial aspirin Buffered aspirin Using your observations about the pH paper, estimate the pH of each sample to the nearest pH unit. Aspirin product 13
Iron(III) Chloride Test From the procedure 5. To each test tube from the pH Test, add 5 drops of 1% FeCl3, Free salicylic acid reacts with the FeCl3 to produce a purple color. The higher the amount of salicylic acid, the deeper the purple color. 6. Record the colors of each aspirin product. 7. Compare the purity of each aspirin product to the reference sample and record. Inspect the following images, making observations about the presence of salicylic acid in each sample. Virtual FeCl3 Tests: Result 0.15% Salicylic acid Commercial Aspirin Buffered Aspirin Aspirin Product
Use the observations you have made to complete the following table. Recall that free salicylic acid reacts with the FeCl, to produce a purple color, Select the option from the "Observation Report Table A.1: pH and Iron(III) Chloride Tests pH and Iron(II) chloride test results Salicylic acid Commercial aspirin Buffered aspirin Aspirin product column that best matches your observation. PH FeCl₂ Test Observations Choose Choose... Choose Choose Choose... Choose Choose... Table view List view Is Salicyclic acid present? Choose Choose... - Choose Choose... - Choose Choose - Choose
(2pts) What does FeCl3 react with to produce a positive result? What information does the iron(III) chloride test provide? BIU BET&Fil Normal : (3pts) What do the results of these tests tell you about the purity of Normal : XIX² BIU ELELE Commercial asperin Buffered aspirin Your synthesized asperin BIBE EIT EI (20pts) Analysis of Analgesics by Thin Layer Chromatography From the procedure 1. Obtain a 400-ml beaker to use as the developing chamber, enough plastic wrap to cover the mouth of the beaker, and a rubber band 2. Pour a small amount of solvent into the chamber so it is -0.55 cm deep. The solvent should be below the spots on the plate. 3 Cover the heaker with the plastic wran securing it with a rubber band T T. Ⓒ
5. Mark the origin, as shown in Figure A.5, by drawing a line in pencil -1 cm from the bottom of the plate. 6. On the origin, mark 6 equally spaced dots and number them 1 through 6. 1. Aspirin 2. Ibuprofen 3. Acetominophen 4. Naproxen 5. Caffeine 6. Unknown over the counter medication 7. Using a separate and clean capillary pipette for each solution, spot a very small amount of each solution onto the dots on the TLC plate. 8. Remove the plastic wrap from the chamber and carefully place the TLC plate into the developing chamber ensuring that it enters the solvent evenly and that the solvent is below the origin. 9. Cover the chamber with the plastic wrap and secure it with the rubber band. 10. Allow the solvent to travel up the plate undisturbed. 11. Once the solvent is 1 cm from the top of the plate, remove the plastic wrap and remove the plate. 12. Mark the solvent front on the plate with a pencil and allow the plate to dry in the hood. 13. Dispose of materials as instructed by your TA or lab instructor. Virtual TLC Analysis The image shown below represents a TLC was prepared according to the procedure above. The lanes on the TLC are labelled as follows 1. Aspirin 2. Ibuprofen 3. Acetominophen 4. Naproxen
5. Caffeine 6. Unknown over the counter medication After developing the TLC plate, the solvent front was marked with a pencil and it was placed under a UV light. The background of the plate fluoresces green with compounds that absorb UV-light appearing as darker spots. The spots are circled with a pencil. Use the following image to "measure" the distance traveled by the solvent and by each of the spots Virtual TLC 2 3 4 5 6 -5
Complete the following table with your measurements and calculate the R, of each spot. Report distances to at least the nearest 0.1 cm. Note: Your unknown sample may contain one, two, or three analgesics . If your sample only has one spot, enter it in the row for the lower or only spot." If your sample has two or more spots, the lower spot (that did not travel as far) is listed first and the upper spot (which traveled the furthest) is listed fast • If a there are more entries than needed for your unknown sample, enter zero for the excess distance traveled and R, entries. Do NOT leave them blank. (1pts) Enter the distance the solvent travelled (cm) TLC Analysis TLC Analysis Lane #1: Aspirin Distance spot traveled (cm) Table view List view R
Lane #2: Ibuprofen Lane #3: Acetaminophen Lane #4: Naproxen Lane #5: Caffeine Lane #6: Unknown 4 Lower or only spot smallest distance traveled if multiple Middle spot (enter zero if none present) Upper spot (enter zero if none present) largest distance traveled if multiple Based upon the TLC analysis, what is the likely most identity of each spot in Unknown 4?
Based upon the TLC analysis, what is the likely most identity of each spot in Unknown 4? (2pts) Lower or only spot (smallest distance traveled if multiple) (2pts) Middle spot (2pts) Upper spot (largest distance traveled if multiple) i (1pts) Which brand of OTC pain reliever best matches the composition of unknown 47 Choose Choose Choose Choose...