Seperating and Extracting the Components of panacetin Aim: To measure, analyze, through extraction and seperation of the components of chemical, Panacetin, which will conclude whether the label attached measures adequate amounts and contains US grade safe contents to which the drug, Panacetin, is originally produced by. Extraction of the chemicals Sucrose, Aspirin, and an Unknown substance is tested to determine the legitimacy of the label and drug. Theory: The percent composition is calculated for accuracy and to conclude the “label is accurate”.
The formula for the percent composition is adding the sums of all the extracts, then dividing the total sum by each of the three (3) individual extract; Sucrose, Aspirin, Unknown. By separating and extracting the three (3) substances from the original drug, Panacetin, analysis can conclude whether it has been smuggled from overseas, which contains toxins, or has been made inside the US, with USP orders and specifications. Materials: The materials used for this experiment are a 15 mL centrifugation tube and cap to add 0. 40 g of the drug, Panacetin, and a graduated cylinder to measure 8. 0 mL of dichloromethane, and filter paper.
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A digital scale, a centrifuge, two (2) test tubes, 4. 0 mL of 5. 0% NaHCO3, micropipette (glass with rubber suction top), a stirring rod, and a vial. A 50 mL beaker, 2 x 1. 0 mL of 6. 0 M HCl, pH paper, a vacuum chamber, a test tube rack, scooper, ice bath, hot water bath, hot plate, Hirsche funnel, and a rubber tube are all necessary to perform the experiment. Method: Weigh and add 0. 40 g of Panacretin to a 15. 0 mL centrifuge tube with a rubber stopper. Add 8. 0 mL of dichloromethane to the 0. 40 g of Panacretin and shake thoroughly, then place in a centrifuge, at three (3) speed for three (3) minutes.
Extract the Sucrose and weigh using a digital scale (must be tared for accuracy). Separate the 8. 0 mL of DCM to two (2) test tubes, each containing 4. 0 mL of DCM. Add 4. 0 mL of NaHCO3 (Sodium bicarbonate) to each of the two (2) test tubes and stir using a stirring rod until two (2) layers are visible, a thin top layer and thick-filmy bottom layer. Extract the bottom layers from the two (2) test tubes to a vial using a glass micropipette and a rubber suction cap/top and seal immediately. Conjoin the two (2) top layers to a 50 mL flask and add 1. 0 mL of 6. M HCl to the beaker containing the solution and stir until the fizzing subsides. Test the pH of the solution with 6. 0 M HCl added using pH paper, which has a color chart to analyze the results. Continue to add 1. 0 mL of 6. 0 M HCl until the pH of the solution is two (2) or less. Place the solution with the pH of 2 or less into an ice bath/cold water bath to form crystallization of aspirin for approximately five (5) minutes. After the five (5) minutes, establish a funnel system using a Hirsche Funnel attached to a vacuum filtration system located on/in the hood, to extract the Aspirin crystals formed from the ice bath/cold water bath.
Weigh the crystals of aspirin using a digital scale (tared) and filter paper. This aspirin may be confiscated to the Professor, discarded, or saved for future work. Uncap the vial, which contains the thick-filmy bottom layer extracted and place in a hot bath, located under the hood, until all of the liquid has dissolved and only a solid unknown precipitate remains. Vacuum-dry the unknown solid precipitate and vial to further ensure a decreased marginal error for weight. Extract the unknown solid precipitate and weigh using a digital scale and filter paper, and place the unknown precipitate back in the vial and seal.
Calculate the percent composition of each extracted and separated substance y finding the sum of the three (3) masses and dividing the sum by each individual extract mass. Results: Mass of each individual extract separated: a. Sucrose: 0. 135 g b. Aspirin: 0. 301 g c. Unknown: 0. 416 g Total mass: 0. 851 g Calculation of percent composition: a. Sucrose: 0. 851 g / 0. 135 g = 16% b. Asprin: 0. 851 g / 0. 301 g = 35% c. Unknown: 0. 851 g / 0. 416 g = 49% Conclusion: Experiment the drug, Panacetin, separate and extract three (3) substances to analyze and conclude whether they are counterfeit or not, or if the drug is illegitimate or not.
After experimenting and analyzing the chemicals, the drug is not counterfeit and made of proper chemicals to satisfy US-grade safety. Each chemical is available in the Panacetin in sufficient amounts based on the mass and percent composition, which concludes this drug is not made overseas using toxins and incorrect amounts of substances. Problems: 2a. After adding DCM to Panacetin, if it were not shaken or stirred (or centrifuged) properly, the sucrose would not be separated completely and would not suffice the weight and percent composition needed to conclude this drug is not a counterfeit. b.
Failure to mix the aq and organic layers thoroughly after adding 5% NaHCO3 will result in incomplete separation of the unknown substance from the aspirin containing aqueous solution. This will cause a discrepancy in the masses of each extracted and separated substance and will misconceive the conclusion that this drug is not a counterfeit drug. c. Extracting DCM with 5% HCl rather than 5% NaHCO3 will cause the aspirin contained in the solution to dissipate due to the acidity of the 6. 0 M HCl solution. It will cause excessive fizzing and bubbling and destroy all or most of the aspirin which will conclude the legitimacy of the label and drug.