Extraction and Evaporation: Separating the Components of "Panacetin"

From the vial labeled “AE,” aspirin (0.533 g) was placed into a 50 mL Erlenmeyer flask with a boiling stick. Toluene (20 mL) was brought to a boil on a hot plate. The boiling toluene (10 mL) was then added to the aspirin until the solid dissolved completely. After allowing the solution to reach room temperature, the solution was placed in an ice bath for 16 minutes. After the crystals

Separation and Purification of the Components of an Analgesic Tablet. Cora Bruno, Lab Section E. Aspirin, Caffeine and Acetaminophen were separated from four analgesic tablets of Excedrin using extraction techniques. 5% wt/vol NaHCO3, 4M HCL, ethyl acetate and deionized water were used to separate the three active components. MgSO4 was used to dry each extraction. Aspirin was isolated using a hot water bath and weighed to determine the percent theoretical recovery and the actual percent recovery of aspirin. After separation, Aspirin (ASA), Caffeine (CAF), and Acetaminophen (ACE) were purified and identified using Thin Layer Chromatography (TLC). Standards and purified ASA, CAF, and ACE were spotted on the silica gel (stationary phase) of the

To begin the separation of the sucrose from the Panacetin, approximately 3 grams of Panacetin was transferred to a 125-mL Erlenmeyer flask. Added to the flask was 50 mL of dichloromethane to dissolve the Panacetin to aid in the separation. A fluted filter paper was used to filter the Panacetin and dichloromethane mixture by gravity using a glass funnel. The remaining filtrate was set aside than transferred to a separatory funnel and the substance on the filter paper was dried and weighed. The filtrate was extracted with 2 increments of 25-mL portions of aqueous 1 M sodium hydroxide. During this step the filtrate in the separatory funnel was shook and vented 3 times.

Prior to beginning the experiment, it is important to understand a few different concepts such as the distinguishing physical properties of a chemical substance and how these physical properties can be analyzed. Physical properties of a chemical substance include water solubility and melting point, both of which are used to pursue identification of the unknown component of Panacetin. Water solubility is a distinct physical feature of chemical substances that can lead to an increase or decrease in product recovered. For example, the water solubility of the two possible unknowns, acetanilide or phenacetin, are different in opposite temperature spectrums. Acetanilide’s cold water solubility is 0.54 grams/100 mL of water, whereas the substance’s boiling water solubility is 5.0 grams/100 mL of water.

Next, aspirin was extracted from the filtrate. When the filtrate was first mixed with the sodium hydroxide and inverted a couple times, an organic layer formed underneath an aqueous layer in the separatory funnel. Dichloromethane was present in the organic layer because it has a higher density than sodium hydroxide, therefore, it’s in the bottom layer. Aspirin reacts with bases like sodium hydroxide, and it forms the salt sodium acetylsalicylate. The polar salt molecules migrate from the organic layer, where they are insoluble, to the aqueous layer, where they are soluble. After the two layers were separated into two different containers, the aqueous layer, which contained sodium acetylsalicylate, was mixed with hydrochloric acid. A white, cloudy precipitate formed, which was a purer form of the salt. The HCl

Panacetin is an analgesic (pain reducing) and antipyretic (fever reducing) drug that is sold in drug stores. However, there is a suspicion that this bottle may be counterfeit, not containing the chemicals that it should. Panacetin should be made up of about 50 percent of the unknown component that we previously separated out of Panacetin for testing. We suspect that this unknown compound is either acetanilide or phenacetin, both of which can be toxic to humans. It is very important that this component is

The primary goal of this laboratory is to correctly identify an unknown substance. To achieve this task, one may use various tests that reveal both chemical and physical properties of a substance. By comparing the results of a known substance and the unknown substance, one may eliminate alternative possibilities and more accurately predict the undisclosed compound. Furthermore, by performing these tests, data can be collected and verified regarding chemical and physical properties of the unknown. Understanding the chemical properties of a known substance aids one’s understanding of the unknown based on comparative analysis of the results of the tests.

Ever wonder about the chemical makeup of tablets that people take for pain relief? Before a tablet can be successfully made, the limiting and excess reactants must be considered. The limiting reactant will affect the amount of the product that can be made. Another reason why the starting reactants must be determined carefully is to make reduce the amount of the reactant in excess so that reactants are not wasted. This experiment uses an Alka-Seltzer tablet. Alka-Seltzer dissolves in water and is an antacid and a pain reliever1. The Alka-Seltzer tablet has many uses such as relief of headaches, ingestion, heart burns, or even upset stomachs2. The active ingredients in an Alka-Seltzer tablet is aspirin, also known as acetyl-salicylic acid (C8H12O4), citric acid (C6H8O7), and sodium bicarbonate (NaHCO3)2. The aspirin in the Alka-Seltzer tablet helps with pain relief. Because of the acid-base chemistry (Brønsted-Lowry), citric acid and sodium bicarbonate produce O2, which makes the tablet fizz when it is dropped in liquid. The Brønsted-Lowry theory shows how the Brønsted-Lowry acid donates a hydrogen ion while the Brønsted-Lowry base accepts the hydrogen ions3. The remaining NaHCO3 that is in excess post reaction with the citric acid is what is used to neutralize stomach acid which helps relief heart burn2. The problem in

Sucrose has a molar mass of 342.3 g/mol. It has a melting point range of 185-187°C and can be an irritant.

We made sure the solution is strongly acidic by testing it with litmus paper getting a pH of 2. We then cooled the mixture to room temperature swirling the flask occasionally in an ice bath. We collected the aspirin by vacuum filtration and washed the aspirin on the filter with cold distilled water. We let it air dry for 30-35 minutes and then weighed the aspirin. It weighed out at 0.513g. The unknown component was calculated and weighed at 0.738g.

HCl will not react with aspirin to form a water soluble salt, so the aspirin will stay in the organic layer and will not be obtained. So that leaves the reported weight of the unknown to be too high.

Thus, leaving us with a layer of aspirin and another layer of CH2Cl2. During the unknown separation, the aspirator evaporated the the solvent. But by cooling the substance we were able to recover the dichlormethane and then re evaporate until I only saw the solid substance remain. Although we succeeded with losing barely any substance, as I will prove later in the calculations section.

This report presents the synthesis of Aspirin (acetylsalicylic acid), as the product of the reaction of salicylic acid with ethanoic anhydride under acidic conditions. Aspirin was purified through recrystallisation by vacuum filtration, followed by desiccation of the Aspirin crystal over silica gel. The percentage yield was calculated as 44.89% and a sample of Aspirin was analysed using infra-red spectroscopy and compared to the spectrum of pure Aspirin, this served as an introduction to the identification of functional groups in organic compounds. The melting point was calculated using an IA9000M apparatus and recorded to be 35.2°C, which was slightly below the melting point of pure Aspirin; known to be between 138-140°C. Both IR spectroscopy and melting point measurement were used verify the purity of synthetic Aspirin made, which proved to be fairly pure under these laboratory conditions.

N-(4-Ethoxyphenyl)acetamide, otherwise known as Phenacetin, is considered to be an analgesic. Since Phenacetin is an analgesic, it means that the purpose of the drug is to relieve pain and reduce fever symptoms, such as an increases body temperature. The drug has an approximate molar mass of 179.22 daltons and has a molecular formula of C10H13NO2. After calculating the molecule’s degrees of unsaturation, one can tell that there are 5 degrees of unsaturation, meaning that the molecule contains five rings, five double bonds, or any combination of the two possibilities which come to equal five. In this instance, the combination is one ring and four double bonds,

Spray dried powder samples (5 mg) were weighed accurately and dissolved using a mixture of water/ methanol (80:20% v/v) in a 100 mL volumetric flask. The flasks were shaken at room temperature for 60 min on an orbital mixer incubator (Ratek Instruments Pty. Ltd., Victoria, Australia) at a speed of 200 rpm followed by bath sonication using an ultrasonic cleaner (Misonix Inc., NY, USA) for 15 min. The solutions were filtered, and the drug content of filtrates was quantified by HPLC analysis.