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Apr 3, 2024
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Chem134L 2023 Report 2 1 Report 2 Aims of the experiment and brief overview of the experimental method Aims: In experiment 3, “Volumetric Analysis,” the purpose of the experiment was to conduct volumetric analysis by titration using volumetric glassware and ideas of stoichiometry, solution concentration, and volume. This experiment aimed to investigate manufacturer claims of the amount of acetylsalicylic acid in aspirin tablets by titration against a standardized sodium hydroxide solution, resulting from a titration of an aqueous sodium hydroxide solution against a primary standard, potassium hydrogen phthalate. Sharing findings with colleagues facilitated further statistical analysis. Methods: This experiment was divided into two parts: the standardization of the sodium hydroxide titrant and the determination of the acetylsalicylic acid content of commercial aspirin tablet. In the standardization of the sodium hydroxide titrant, a measuring cylinder was used to collect 20 mL of 1.0 N NaOH stock solution and transferred to a clean 100.0 mL volumetric flask. Approximately 80 mL of deionized water was added to the volumetric flask until solution was diluted to the 100.0 mL mark. To homogenize the solution, an inversion-mixing process was carried out 10 times. To clean the buret, the buret was rinsed with deionized water three times and then with the diluted sodium hydroxide solution three times. After discarding rinsate into the waste beaker, the buret was filled with leftover sodium hydroxide solution past the 0 mL mark; excess was drained out until the meniscus was approximately at the 0 mL mark. Next, approximately 0.40-0.42 KHP was weighed in an analytical balance with a weigh boat and then transferred into a clean 250 mL Erlenmeyer flask. The weigh boat was weighed once more to use the difference to calculate the mass of the transferred KHP. Approximately 30 mL of deionized water was added into the Erlenmeyer flask along with 5-6 drops of phenolphthalein indicator solution. A magnetic bead was placed into the Erlenmeyer flask, and the flask was then placed on a magnetic stir at high speed with its opening right under the bottom of the buret. After recording initial volume on buret, the diluted sodium hydroxide solution was added dropwise into the Erlenmeyer flask while still stirring. Rinsed alongside flask with deionized water when needed. Endpoint is achieved when the solution in the flask turns pink with the addition of a single drop of titrant. End volume was recorded, and titration was repeated for a second. In the determination of the acetylsalicylic acid content of commercial aspirin tablet part, an aspirin tablet was collected, then supplier and how much aspirin was “in” the tablet was recorded. The tablet was added to a clean 250 mL Erlenmeyer flask. Approximately 20 mL of acetone was collected into a measuring cylinder and transferred into flask. The tablet was dissolved by stirring and crushing via glass rod. Approximately 20 mL of deionized water was collected in measuring cylinder and transferred into flask. 5-6 drops of phenolphthalein indicator solution was also added. Magnetic stirrer was added into flask and starting volume was recorded. Titrant was added dropwise until endpoint is reached. End volume was recorded, and experiment was repeated for a second trial.
Chem134L 2023 Report 2 2 Results and calculations Pay close attention to the precision for all the measured and calculated values throughout and be careful to include units with any values The Standardization of Sodium Hydroxide Table 1. Complete this table with the data relating to the titration of KHP by sodium hydroxide. Trial 1 Trial 2 Mass of KHP Used (g) 0.4188 0.4197 Moles of KHP used (mol) 0.002051 0.002055 V
initial
of Sodium Hydroxide (mL) 0.00 11.15 V
final
of Sodium Hydroxide (mL) 11.15 22.31 Volume of Sodium Hydroxide Solution Used (mL) 11.15 11.16 Concentration of Sodium Hydroxide Solution (
M
) 0.1839 0.1842 Sample calculations One sample calculation of each type is sufficient. Please show how you set up your calculations. Pay close attention to significant digits and always give units with values. Moles of KHP from mass of KHP: (mass KHP) (1 mol KHP/ molar mass KHP) = mol KHP Trial 1 (0.4188 g KHP) (1 mol KHP / 204.22 g KHP) = 0.002051 mol KHP Volume of sodium hydroxide solution added: [V
final
of Sodium Hydroxide (mL)] –
[V
initial
of Sodium Hydroxide (mL)] Trial 1 (11.15 mL) –
(0.00 mL) = 11.15 mL sodium hydroxide added Concentration of sodium hydroxide solution: [(mass KHP) (1 mol KHP/ molar mass KHP) (1 mol NaOH)] / Volume of NaOH (L) (0.4188 g KHP) (1 mol KHP / 204.22 g KHP) (1 mol NaOH/1 mol KHP) / [(11.15 mL)(1 L/1000mL)] = 0.1839 M
Chem134L 2023 Report 2 3 Determination of the Aspirin Content of Commercial Aspirin Tablets. Table 2. Complete this table with the data relating to the titration of aspirin by sodium hydroxide. Trial 1 Trial 2 Concentration of Sodium Hydroxide Solution (
M
) 0.1841 0.1841 V
initial
of Sodium Hydroxide in buret (mL) 22.31 32.28 V
final
of Sodium Hydroxide in buret (mL) 32.28 42.13 Volume of Sodium Hydroxide Solution Used (mL) 9.97 9.85 Moles of Sodium Hydroxide consumed (mol) 0.00184 0.00181 Mass of Acetylsalicylic Acid (g) 0.331 0.327 Manufacturer’s claimed content (g)
0.325 0.325 Deviation from the claimed content (%)* 1.85 0.615 *Report the sign of the deviation with the value. Sample calculations One sample calculation of each type is sufficient. Please show how you set up your calculations. Pay close attention to significant digits and always give units with values. Moles of sodium hydroxide: [Volume of Sodium Hydroxide Solution Used (mL)] x (1L / 1000mL) x [(Concentration of Sodium Hydroxide Solution (
M
)] Trial 1 (9.97 mL NaOH solution) (1L / 1000mL) (0.1841 mol/L) = 0.001835477 mol NaOH →
0.00184 mol NaOH Mass of acetylsalicylic acid from moles of sodium hydroxide: (mol NaOH) (1 mol Aspirin / 1 mol NaOH) (molar mass Aspirin / 1 mol Aspirin) Trial 1 (0.00184 mol NaOH) (1 mol Aspirin / 1 mol NaOH) (180.16g Aspirin / 1 mol Aspirin) = 0.330679 g acetylsalicylic acid →
0.331g acetylsalicylic acid Deviation from claimed acetylsalicylic acid content: [(Mass of Acetylsalicylic Acid –
Manufacturer’s claimed content
) / (Manufacturer’s claimed content)] x 100 [(0.331 g –
0.325 g)/ (0.325 g)] x 100 = 1.85%
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Chem134L 2023 Report 2 4 Statistical Analysis Table 3: Statistical analysis of class data. Quantity Value Average (mean) mass of salicylic acid (g): your two trials 0.329 Average (mean) mass of salicylic acid (g): class day trials (number of values used) 0.345 Average (mean) mass of salicylic acid (g): five values from your class day trials 0.334 Standard deviation: class day trials (g) 0.0230 Standard deviation: five values from your class day trials (g) 0.00566
Chem134L 2023 Report 2 5 Reflection Questions Be brief in your answers. If you wish, you may consult with your TF, the instructors, and your classmates when you are formulating answers to these questions but when giving your answers make sure that your answers are your own. 1.
Compare your two values for the mass of aspirin in the tablets to the class average value and to the average of five random values from the class trials. Are these values the same? Which of them do you think is closest to the true value? Explain your answer. The two values that I calculated for the mass of aspirin in the tablets were 0.331 g of aspirin and 0.327 g of aspirin. These values are less than the class average value of 0.345 g of aspirin and the average of five random values from the class trials of 0.334 g of aspirin. Both values are larger than my two values that I calculated. Since the class average included more trials (32 trials) than the five random values and my own two trials, experimental error is minimized because we can make sure the results are consistent and not altered by random events such as going far past the endpoints and/or various experimental flaws. Though my own values of the mass of aspirin were closer to what the label claimed, as the number of trials increases, the average value should theoretically get closer to the true value. Thus, I believe the class average value is the closest to the true value. 2.
How does the class average value for the mass of aspirin in the tablets compare to the manufacturer’s declared value? Suggest reasons for any difference between the found and the claimed values. Comment on any aspect of the experimental design which might contribute to any observed difference. The class average value of 0.345 g of aspirin is 0.20 g higher than what the manufacturer’s claimed to be in the tablets. The reason for this difference is because the class average comes from trials of undergraduate students compared to pharmaceutical professionals. This experiential difference could potentially be the reason that titration endpoints were overshot. Overshot titration endpoints lead to a hot pink KHP and acetate solution instead of a faint pink endpoint. This overshot volume is a probable reason the class average value of the mass of aspirin is higher than what is on the manufacturer’s label. Because of this fault,
the overshot NaOH volume would lead to an overshot value of number of moles of NaOH, which is then used to calculate and overshot mass of the aspirin in the tablet. Therefore, the class average is higher than was displayed on the manufacturer’s label. To fix this experimental flaw, a machine learning model could be used to detect the exact titration endpoint to warn the experimenter to get ready to cease drops from the buret.
Chem134L 2023 Report 2 6
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