The extraction procedure was undertaken in order to separate the acid, base and neutral components of the solution into separate phases. This procedure was executed using different solvents with different polarities in order to extract the different solutes. The recrystallization procedure was undertaken in order to purify the solutes further by removing any contaminants. This was done by using hot solvent and then allowing it to cool, which causes the compound to precipitate out. This creates purified crystals that have less other associated compounds.
Data and Results The initial mass of the acid was 0.33 grams. The pure mass that was measured after recrystallization was 0.127 grams, which gives a recovery percentage of 38.5%. The melting point of the purified crystals was found to be between 157C and 160C. As the melting point of salicylic acid is between 158C and 160C, it is likely that the acid is salicylic acid. The initial mass of the base was 0.33 grams. The pure mass that was measured after recrystallization was 0.125 grams, which gives a recovery percentage of 37.9%. The melting point of the purified crystals was found to be between 142C and 145C.
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The three solutes, the acid, base and neutral, were able to be extracted using different solvents and were then able to be further purified using the recrystallization technique. They were not extracted fully, however, because the percent yields were only 38.5%, 37.9%, and 40.0% for the acid, base and neutral solutes respectively. Since only approximately 40% of each solute was extracted, that means the rest was left in the other phases of the extraction or were not crystallized out of solution during the recrystallization. This could have been due to incomplete extraction of the extraction solutions during the extraction procedure or from incomplete cooling in the recrystallization. However, overall, the expected principles were
In the first section, the Synthesis of Aspirin, salicylic acid was weight to be 3.029 grams using mass by difference since it was weighed on a 150 milliliter beaker. 9.23 milliliters of the acetic anhydride and 14 drops of 85 percent phosphoric acid were added to this beaker. A Bunsen burner provided by the laboratory was then used to boil the just mixed combination by producing a flame underneath the positioned beaker on top, and then allowed to cool for several minutes after the Bunsen burner flame was terminated. Two quantities of distilled water were then added to this mixture to make it cool even further, which were 41 drops and 30 milliliters. After cooling for some time, this beaker was placed into an ice bath in order to start the crystallization process. A glass rod was used to scratch around the bottom and the sides to catch all of the crystallized Aspirin that was being formed during this whole process. Then, by using a Buchner funnel and filter paper, which was placed on top of the flask connected to a water aspirator with rubber tubing, the excess liquid was removed from the just scraped Aspirin crystals when the Aspirin was placed on the filter paper. Using a medicine dropper, the Aspirin crystals on the filter paper were washed with distilled water just so that any non-pure substances were removed from the crude product. When these crystals were then ultimately dry, they were placed on a watch glass and put into an oven for 30 minutes. Then they were weighed by mass by difference to yield 2.4667 grams of crude s...
Based on our observations during the separation techniques and some speculation, we were able to identify eight components of our mixture: graphite from the filtration residue, Epsom salt from crystallization, water and acetic acid through distillation, red and orange dye, iron metal, marble chips, and sand.
Firstly, an amount of 40.90 g of NaCl was weighed using electronic balance (Adventurer™, Ohaus) and later was placed in a 500 ml beaker. Then, 6.05 g of Tris base, followed by 10.00 g of CTAB and 3.70 g of EDTA were added into the beaker. After that, 400 ml of sterilized distilled water, sdH2O was poured into the beaker to dissolve the substances. Then, the solution was stirred using the magnetic stirrer until the solution become crystal clear for about 3 hours on a hotplate stirrer (Lab Tech® LMS-1003). After the solution become clear, it was cool down to room temperature. Later, the solution was poured into 500 ml sterilized bottle. The bottle then was fully wrapped with aluminium foil to avoid from light. Next, 1 mL of 2-mercaptoethanol-β-mercapto was added into fully covered bottle. Lastly, the volume of the solution in the bottle was added with sdH2O until it reaches 500 ml. The bottle was labelled accordingly and was stored on chemical working bench.
When making an organic compound, it is important to separate the compound from other compounds to make it as pure as possible, this is called crystallization.
Salicylic Acid(SA) was measured was by measuring 0.5g of plant tissue. The tissue was ground to a fine powder with liquid nitrogen. The acid was then extracted twice with Methan...
The actual amount of crude product was determined to be 3.11 grams. The percent yield of the crude product was determined to be 67.75 %. The actual amount of pure product formed was found to be 4.38 grams. The percent yield of the pure product was determined to be 95.42%. Regarding the thin layer chromatography, the line from the solvent front is 8 centimeters.
The crude extract obtained by solvent extraction was subjected to various qualitative tests to detect the presence of common chemical constituents as:
Extraction is a separation method that is often used in the laboratory to separate one or more components from a mixture. Sucrose was separated at the beginning because it is the most immiscible and it’s strongly insoluble. Next Acetylsalicylic Acid was separated which left Acetanilide alone. Variety steps could have led to errors occurring. For example the step of separation, when dichloromethane layer was supposed to be drained out, it could be possible some aqueous layer was drained with it. Which could make the end result not as accurate. Also errors could have occurred if possibly some dichloromethane was not drained out. Both way could interfere with end result of figuring the amount of each component in the mixture. The solids percentage were 22.1% more than the original. That suggests that solids weren’t separated completely which clarifies the reason the melting points that were recorded were a slightly lower than the actual component’s melting point. The melting point for Acetylsalicylic Acid is 136 C but that range that was recorded during the experiment was around 105 C to 118 C. The melting points were slightly lower than the literature value. Sucrose was the purest among all component due to its higher melting point which follows the chemical rule that the higher the melting point the more pure the component
Aspirin (acetylsalicylic acid) is a type of acid categorized as a salicylate, this acid works as a pain reliever in the body because once digested it lowers the amount of substances already in the body that cause pains, fevers and flare ups. Also, this chemical is administered to people for prevention of heart attacks, strokes, and angina which is also known as severe chest pains. Aspirin is created by chemically synthesizing salicylic acid through the acetylation with acetic anhydride, synthesizing aspirin comprises of three steps, synthesis of it, isolation and purification of it, and testing the purity of the aspirin made. Synthesizing aspirin is done by reacting salicylic acid and acetic anhydride with a catalyst, in which phosphoric acid (H3PO4) is used. After the aspirin has been prepared (synthesized), it must be isolated and purified. Aspirin is insoluble in cold water, therefore it can be isolated by filtering the cold solution product of the reaction. In order to remove the unreacted salicylic acid, acetic anhydride, acetic acid product and phosphoric acid the solution must be purified, the acetic anhydride is decomposed simply through the use of adding water after the reaction has finished (C4H602 + H20 2C2H402). Acetic acid and phosphoric acid can be removed from the solution by soaking the aspirin in cold water since they are soluble in water. The final ending step of purifying the aspirin is through a process referred to as recrystallization. This is when the aspirin is placed in warm ethanol, the solution is cooled, and the aspirin crystallizes leaving the salicylic acid and other impurities inside the solution. Lastly testing the purity of the finished product is achieved mainly from a melting point test a common...
Saturated sodium chloride solution, also known as brine solution, is used to wash the distillate mixture. The distillate mixture is the phosphoric acid the co-distilled with the product. The brine solution also removes most of the water from the 4-methylcyclohexane layer. When six drops of 4-methylcyclohexene were added with two
It could have been lower than 100% because some product was lost during the recrystallization process, or due to an incorrect separation of the impurities when cooling the mixtures. The melting point data confirmed that the synthesized crystals were likely identical to the methoxybenzyl phenol ether because the mixed melting point was the same as the purified crystals. If the products were different or the synthesized product had to many impurities in it then the mixed melting point would have been lower than that of just the crystals, by themselves. The TLC made sense, after looking at the TLC plates under UV light and the calculation of the Rf values, it was confirmed that the 4- Methoxy-phenol was present in the unknown.
The solvents used in this experiment were sodium hydroxide as the aqueous layer and the ethyl acetate and unknown benzocaine as the organic phase. These phases are separated with an emulsion line which is a distinct line that shows where the aqueous and organic layers meet but do not mix. This method of separation relies on portioning the preferential dissolution of a compound into one solvent over another (2).
Starting this experiment, we knew that the extraction was going to form varies layers due to the density differences. When placing three different substances, we saw that two layers formed because the Clove Oil is soluble in MTBE, but not in water. In order, to get the organic layer we used separatory funnel to take out the excess substances and leave the oil layer. Then we transferred to a beaker and dried with Magnesium Sulfate. Lastly, we filtered the liquid using funnel; we placed the liquid to boil, let it cool to room temperature. The purpose of drying and evaporation is to help us with the Gas Chromatography analysis of the product.
After the some time, we filter it through a Büchner funnel before it is recrystallized and filtered again. The mass was recorded as it was dry. By adding sodium carbonate, we will now test whether what obtained is benzoic acid or not, because one can observe bobbles if it is an acid. After that we burn it to test if it is aromatic.
3.0g of salicylic acid was weighed (salicylic acid was formed from Step 1) into a 100mL beaker. In a 10mL graduated cylinder, 5.0mL of acetic anhydride was measured and was transferred into the 100mL beaker. 5 drops of concentrated sulphuric acid was also added into the beaker.