Isolation of Ibuprofen: Fifteen 200 mg ibuprofen tablets were used, which was 3.37g (16.34 mmol, 112.3%) ibuprofen. This amount of ibuprofen was submerged in 25 mL of acetone and stirred vigorously for 5 minutes to dissolve. Red coatings of the tablet were separated and vacuum filtration was utilized to dissolve all insoluble components. The melting point range of the crude ibuprofen was 72.4-73.9°C. The major bands from the IR are, FTIR: sp3 O-H stretch, about 3200-2500 cm-1 (b, m); sp3 C-H stretch, 2991-2868 cm-1 (sh, m); sp2 =C-H stretch, 3100-3000 cm-1 (sh, w); sp2 C=O stretch, 1701 cm-1 (sh, s); and sp2-sp2, aromatic, C=C stretch (in ring), 1507 cm-1 (s, m). Formation of Diastereomeric Salts: 30 mL of 0.25 M sodium hydroxide was added to the flask that contained the crude ibuprofen. This flask was heated to 85°C with the addition of 0.9 mL of S-(-)-α-phenethylamine (d=0.94 g/mL, 6.981 mmol). The crude salt was collected via vacuum filtration for 30 minutes and the percent yield of the salt formation was 98.688 %. …show more content…
This beaker was heated in a hot water bath until the solid dissolved in the solution and was cooled in an ice water bath for 15 minutes. Crystals were gathered via vacuum filtration and the stir bar was removed. The mass of the final product was 0.52g and 57.33 % recovery, with a melting point of 166.5-170.6
To do this we created proportions. We calculated that we need to put .25 mL of salt in 50 mL of water to create .5% salinity, 1.5 mL of salt in 50 mL of water to create 3% salinity, and 2.5 mL of salt
Therefore, liquid-liquid and acid-base extraction techniques were successfully performed to separate the components of the Excedrin tablet. According to the TLC analysis results, the compounds (aspirin, acetaminophen, and caffeine) were successfully isolated from the analgesic (Excedrin tablet). In figure 1, the separation of the compound in the TLC analysis correlates with the TLC analysis in figure 2. Furthermore, Rf index calculations of the TLC analysis demonstrated that the compounds (aspirin, acetaminophen, and caffeine) were separated. The Rf calculations of aspirin in table 1 shows an Rf value of .491; however, in table 2 the Rf value of aspirin was calculated to be .784.
In order to separate KNO3 and CuSO4, which are both soluble in water, recrystallization was used. The reason the two components can be separated through recrystallization is because of the temperature dependence of solubility, KNO3 is much more soluble in hot water and insoluble in cold water while CuSO4 is only slightly more soluble in hot water. When the filtrate was heated the solution was saturated with KNO3 but when the system was cooled, the KNO3 became insoluble and pure crystals reformed while CuSO4 stayed dissolved in the
The purpose of this experiment was to understand the pharmacokinetics of the drug acetaminophen within the body, specifically focusing on its partition coefficient, drug protein interaction and its bioavailability through various form of administration. The bioavailability of the drug was determined to be 100% for IV because the drug is injected directly into the systemic circulation in its active form and this is also visible on Figure 4, where the initial concentration of drug is much higher than in PO and IP. For PO and IP administration, the bioavailability was determined to be 72.6% and 39.1%, respectively. This makes sense because both of these type of administration involve the first-pass effect where a portion of the drug is metabolized by peripheral organs, especially the liver in this case, and therefore the amount of active drug reaching the circulation is less. PO administration, however has a much higher content reaching the circulation than IP, because the IP route involves passing through the whole gastrointestinal tract before being absorbed in the liver while the IP route injects the drug into the
(1) The purpose of the separation lab procedure was to help my group members and I successfully formulate our own plan before completing the experiment, handling multiple materials and substances, etc. It acted as a step-by-step plan that guided us throughout the experiment and ensured that we were well prepared ahead of time (ie. knowing what kind of materials were necessary and gathering the correct measurements of each substance); this made the experiment day much less hectic for all of us. It made reaching our goals (achieving > 85% recovery for each substance) more realistic and convenient. (2)We predicted that we would be able to easily separate each substance from the mixture through the use of our designed procedure. By using a bar magnet, we predicted that all the iron (and only the iron) would attract and quickly maneuver its way through the beaker and into the
In this experiment, the goal was to identify the unknown monoterpene assigned by infrared spectroscopy, ultraviolet-visible spectroscopy, and 1H NMR spectroscopy. The hypothesis was that the unknown monoterpene was citronellol. The hypothesis was confirmed through the spectroscopes conducted. The ultraviolet-visible spectroscopy showed a 214nm with an absorbed energy of 1.006ε. Since it was under 220nm, it showed that there was only one double bond in the molecule.
In this lab, three unknown compounds were separated from a mixture and identified by melting point. Unknown mixture #124 has components of acid, base and neutral compound. The compounds were identified by melting point and matched up with the known melting points from a given list. In order to identify the compound it was important to separate by dissolving the mixture in an organic solvent which was not soluble in water, and then extracting the solution first with HCl, and then dilute sodium hydroxide solution. From the separation mixture, the aqueous layer were obtained and labeled as TT-1 (base), TT-2(acid) and TT-3 (neutral) in three different test tubes for later recovery.
Pages 96-98 in Chemistry 110 Lab Manual. Wilfrid Laurier University, ON, Canada. Abstract: The purpose of this experiment was to determine the level of purity by using the values for melting point and absorbance and chemically synthesizing aspirin by using phosphoric acid as a catalyst.
In this lab, we tested 8 known ingredients to find what ingredients was in our unknown A and unknown B medications. We first tested the water solubility of our knowns and unknowns. We found that of the knowns, cornstarch and acetaminophen were the only ones not water soluble. The unknowns were also not water soluble. Th next test was the pH test.
Intro: Separation and purification of an unknown/complex compound can be done by using techniques such as liquid-liquid extraction, solid-liquid extraction, recrystallization, melting point, and thin layer chromatography. In this experiment, these techniques were used to separate excedrin’s components containing caffeine, excedrin, and acetaminophen, Each component has its own chemical properties and characteristics such as polarity, reactivity, and solubility. Knowing how to separate and purify compounds from each other is an important skill within in a lab setting. A few techniques for first initially separating compounds apart are liquid-liquid extraction and solid liquid extraction. Liquid-Liquid extraction involves using a seperatory funnel and release on varying solubities and different solids in immiscible solvents.
The mixture was then distilled. When the temperature was reached to about 59℃, half vial of distillate (1V) and 1 mL of the liquid residue (1L) were collected. For 61.0℃, the distillation was then continued. Samples (2V, 2L) were taken at about 61.0℃.
The results were an indicative for expected IR spectrum of pure phenacetin. The IR spectrum showed peaks at (3281.67 cm-1) which indicate the presence of the N=H stretch, (3131.40 cm-1 and 3073.97 cm-1) representing the Sp2 C-H stretches, (2982.26 cm-1, 2927.60 cm-1 and 2885.53 cm-1) expressing the Sp3 C-H stretches, also (1656.82 cm-1) indicating the C =O amide stretch, and finally a wavelength at (1603.51 cm-1) representing the aromatic C =C stretch of the phenacetin molecule, respectively. Such IR spectrum results from phenacetin in comparison with an acetaminophen IR spectrum clearly showed the elimination of the hydroxide (OH) bond present at the acetaminophen molecular structure, which resulted in the IR spectrum not indicating the presence of a strong and broad (alcohol-phenol) band at about 3500 cm-1
Purpose/Introduction The process of recrystallization is an important method of purifying a solid organic substance using a hot solution as a solvent. This method will allow the separation of impurities. We will analyze Benzoic Acid as it is dissolved and recrystallized in water and in a solvent of Methanol and water. Reaction/Summary
Introduction: In this lab, of water in a hydrate, or a substance whose crystalline structure is bound to water molecules by weak bonds, is determined by heating up a small sample of it. By heating, the water of hydration, or bound water, is removed, leaving only what is called an anhydrous compound. Based on the percent water in the hydrate, it can be classified as one of three types: BaCl2O ⋅ 2H20, with a percent water of about 14.57%, CuSO4
The hydrolysis formed salicylic concentration which was mixed with iron(III) solution to form a purple complex. This was then use to study under the UV/Visible absorption spectroscopy which gave absorbance values recorded at 525nm to determine the concentration of salicylic acid using the Beer Lambert’s Law and later corrected to find the actual concentrations. The concentrations of aspirin at various intervals was found from salicylic concentrations. Upon plotting a graph of ln(aspirin) vs time, it produced a linear equation from which the gradient gave the rate constant of 0.0083min-1 and the overall shape of the graph concluding this reaction to be pseudo first order with respect to the concentration of aspirin with the deviations and improvements as