Extraction Post Lab (2)
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Post Lab Report for the Extraction of Sucrose, Acetylsalicylic Acid, and Acetanilide
Suzanne Varughese, L16
Objective The experimental goal was to complete an acid-base extraction of sucrose, acetylsalicylic acid, and acetanilide.
Materials and Methods
First, 1.7 g of phensuprin was measured out and added to a 125 mL Erlenmeyer flask.
Then, 40 mL of ethyl acetate was added, and the solution was stirred until no more solid
appeared. The clumps were broken up, and differences in solid structure seen was with
sucrose. The size of the clumps was small and white colored. A dry piece of fluted filter weighed
1.425g. Then the leftover solid was collected using that same flute paper through gravity
filtration. The gravity filtration was done by placing fluted filter paper in a beaker, and then the
mixture was added to the fluted filter paper. The sucrose was collected by the paper, and the
remaining mixture was filtered into the beaker. The amount of sucrose collected was 1.17 g.
The leftover acetylsalicylic acid was washed with 5 mL of ethyl acetate and saved in the flute
filter paper until the next lab period. Then the ethyl acetate solution was extracted with 20 mL of 5% sodium bicarbonate solution. Using the separatory funnel, the aqueous layers were combined in the same beaker. First, the aqueous layer of sodium bicarbonate was collected in a beaker. The ethyl acetate solution was extracted a second time with another 20 mL of sodium bicarbonate. The sodium bicarbonate solution was acidified to a pH of 2 using 11 M HCl, cooled on an ice bath, and allowed crystals to form. The pH was tested using a pH test strip. After cooling on an ice bath, the solution was placed onto strip and showed a pH of 2. Then, this acetyl salicylic acid was collected by vacuum filtration and washed with water. In the Erlenmeyer flask, the acetyl salicylic acid was saved until the next lab period. The weight of the acetyl salicylic acid was 0.649 g. Once, the organic layer was dried over anhydrous sodium sulfate it was transferred to a 250
mL round-bottom flask using a pipet or gravity filtration. The following lab period the solvent was
evaporated using a rotary evaporator. The 250 mL round-bottom flask weighed 116.173 g without the substance and 117.173 with the substance. The acetanilide solid weighed 1.00 g. The results of this experiment were that the sucrose product weighed 1.17 g, the acetyl salicylic acid product weighed 0.649 g and the acetanilide product weight 1.00g.
Results
First, the calculations of the mass of each component assuming a 100% recovery: (The mixture was a 1:2:1 mix of sucrose/acetylsalicylic acid/acetanilide.)
Sucrose: (1.623/4) = 0.40575 g
Acetylsalicylic Acid: (1.623/2) = 0.8115 g
Acetanilide: (1.623/4) = 0.40575 g
The calculations of percent recovery of each component:
Actual mass / expected mass * 100 = percent recovery for that component.
Sucrose: (1.17 g/0.40575 g) 100 = 288%
Acetylsalicylic acid: (0.649 g /0.8115 g) 100 = 80.0%
Acetanilide: (1.00 g / 0.40575 g) 100 = 246%
Melting Point and Purity The sucrose melting point was 181 – 186 C. This suggests that our sample has some impurities, due to the range being greater than 2 C. Now the acetyl salicylic acid melting point was 130 – 133 C. This suggests that our sample has a little bit of impurity, not a large amount due to the close range of the melting point. However, the range is greater than 2 C, this suggests there may be a small amount of impurity. The acetanilide melting point was 104 – 109 C. This suggests that our sample has some impurities, due to the range being greater than 2 C.
Percent recovery A reason our percent recovery of sucrose was extremely high may be the acetyl salicylic
acid and acetanilide in phensuprin may not have dissolved completely in the ethyl acetate. Acetanilide is high due to the 11mL of HCl, producing a greater amount of solid. Another reason
could have been due to excess mass due to impurities within the glassware which could increase the product amount
. Discussion A similar study called, “Double Acid-Base Extraction of Silicic Acid from Quartz Sand,” focuses
on the extraction of ortho-silicic acid from Bangka-Belitung quartz sand. The experiment was
done with an acid-base extraction method that was used to extract OSA from 325-mesh size
quartz sand (Santi et al., 2017). Then, the sand was boiled in HCl solution at different
concentrations, and the optimal concentration was determined (Santi et al., 2017). Then using
x-ray diffraction and electron microscopy they found that the acid-base extraction method
hindered the quartz mineral structure, thus releasing ortho-silicic acid. The relationship between
both experiments is that we also used HCl solution as a dissolving reagent with NaHCO
3
.
Additionally, they used the acid-base extraction method to extract ortho-silicic acid solids, just
as we did to extract acetanilide.
References Santi, Laksmita Prima; Mulyanto, D.; Goenadi, Didiek Hadjar. Double Acid-Base Extraction of Silicic Acid from Quartz Sand - Eprints UPN “Veteran” Yogyakarta.
Upnyk.ac.id
2017
. http://eprints.upnyk.ac.id/18203/1/Double%20acid-djoko%20m..pdf
.
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