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Experiment 6 Determination of Acetylsalicylic Acid in Aspirin Group 5 BS Biology 2A
Experiment 6 Determination of Acetylsalicylic Acid in Aspirin Group 5 BS Biology 2A
Experiment 6 Determination of Acetylsalicylic Acid in Aspirin Group 5 BS Biology 2A
6
Determination of Acetylsalicylic Acid in an Aspirin Tablet Sample
The ultimate objective in this activity is to properly perform a back-titration to evaluate the purity
of an aspirin tablet by finding out the actual percent content by mass of acetylsalicylic acid
(C9H8O4) (% ASA) in a readily available aspirin tablet. Finding out the actual % ASA in an aspirin
tablet is significant because it indicates a specific aspirin tablet’s potency and efficiency as a drug,
by comparing it to the expected % ASA of 70% ASA for effective aspirin tablets. However, the
calculated % ASA was only 21.29%, which was significantly lower than the expected value. It can
be attributed to the difference in the expected molar concentration of the standardized 0.1 M NaOH
and HCl solutions, to the actual molarity values of 0.086 M NaOH and 0.126 M HCl solutions
used in this experiment. Having calculated only 21.29% ASA, the group believes that the results
are erroneous. Hence, having such results leads the group to conclude this experiment as a failure
and must be repeated with lesser or no errors at all to determine the actual percent content of
acetylsalicylic acid (% ASA) in an aspirin tablet, which must be closely accurate to the expected
% ASA.
Chapter I
Introduction
Aspirin, also known as Acetylsalicylic Acid (ASA), is the product of reaction of Acetic
Acid (CH3COOH) and Salicylic Acid (HOC6H4COOH). Aspirin tablet, however, is an analgesic,
antipyretic drug that is not purely composed of only Acetylsalicylic Acid. ASA is its active
ingredient but certain inactive ingredients or fillers are added for it to be commercially accepted
and consumed based on certain drug standards.
Alkaline hydrolysis of the sample by Sodium Hydroxide (NaOH), into neutrality is first
required. The aspirin solution is reacted with a measured amount of NaOH solution, which will
exceed the amount of aspirin present. The reaction is represented as:
Then, the excess NaOH from the alkaline hydrolysis will be reacted with HCl in a process
called as back-titration, wherein the amount of hydrochloric acid needed to neutralize the
unreacted sodium hydroxide in the solution will be determined using a phenolphthalein indicator
that will turn the pink solution into colorless upon reaching the equivalence point (“Back
Titration,” n.d.). Knowing these values will then determine the amount of acetylsalicylic acid
present in an aspirin tablet. The reaction is shown as:
NaOH + HCl → NaCl + H2O
Sodium Hydrochloric Sodium Water
hydroxide acid chloride
In this experiment, the students are expected to be able to develop the proper techniques
for the proper dilution of a solution to a definite volume, know how to properly use a transfer
pipette, and ultimately, conduct a back-titration to evaluate the purity of an aspirin tablet by finding
out the actual percent content by mass of acetylsalicylic acid (C9H8O4) in a readily available aspirin
tablet.
Chapter II
Methodology
A. Standardization of 0.10 M NaOH solution against Potassium Acid Phthalate (KHP) using
Direct Titration
Trials 1 2 3
Weight of KHP (g) 0.5740 g
Volume of 0.1 M prepared NaOH
34.0 mL 32.0 mL 32.0 mL
solution (mL)
Average Volume of 0.1 M prepared
32.7 mL
NaOH solution (mL)
Average Molarity of standardized 0.1 M
0.086 M
prepared NaOH solution (M)
Table 1 shows the compiled data values that were obtained and calculated based from
the results after conducting the standardization of 0.10 M NaOH solution against 0.5740 grams
(g) of Potassium Acid Phthalate (KPH) using direct titration conducted during the previous
activity, since the remaining 0.1 M standardized NaOH solution from the past activity was
used in this experiment.
Based from the average final volume reading of the unreacted NaOH solution in the
three direct titration trials, which was 32.7 milliliters (mL), it was calculated that the actual
molarity of the NaOH solution required to react with 0.5740 g KHP in order to achieve the
titration’s equivalence point was not 0.10 M NaOH, but instead was 0.086 M NaOH, which
was more diluted and had lower concentration than expected. Hence, the standardized molarity
of the NaOH solution used was 0.086 M NaOH.
Trials 1 2 3
Volume of HCl (mL) 25.0 mL
Volume of NaOH used (mL) 30.9 mL 31.5 mL 32.2 mL
Average Volume of NaOH used (mL) 31.5 mL
Average Molarity of standardized 0.1000
0.126 M
M prepared HCl solution (M)
Table 2 shows the obtained and calculated data values from performing the
standardization of 0.1000 M HCl solution against the standardized 0.086 M NaOH solution
using direct titration. The three titration trials yielded an average final volume reading of 31.5
mL NaOH solution that did not react with the 25.0 mL HCl solution to achieve the titration’s
equivalence point, and from this, the average molarity of the 0.1000 M prepared HCl solution
was calculated to be actually 0.126 M, which means that the HCl solution had a higher
molarity, meaning that it was more concentrated than expected. The standardized HCl solution
for this experiment was 0.126 M HCl.
Table 3 summarizes the data values obtained from performing the back-titration of the
50.0 mL aliquot of diluted solution containing 0.3000 grams aspirin and 10.00 mL of
standardized 0.086 M NaOH solution with 25.0 mL of standardized 0.126 M HCl solution.
28.5 mL was the average final volume reading of 0.126 M standard HCl solution (0.1 M HCl
solution) upon reaching the titration’s endpoint. Using these values, the moles of
acetylsalicylic acid present in 0.3000 g previously ground aspirin within the 50.0 mL aliquot
was calculated to be 0.0003545 mol C9H8O4, thus having a mass of 0.0638663655 g C9H8O4.
With this, the calculated average percent by mass of C9H8O4 present in 0.3000 grams of aspirin
tablet was 21.29% C9H8O4, which was lower than the expected percent content of an effective
and potent aspirin tablet that has 70% acetylsalicylic acid (ASA) (Medrano, Pasco, Lubrin, &
Manrique, 2014).
There are many possible sources of error in the experiment that led to having a low
calculated ASA content in the aspirin tablet with only 21.29% C9H8O4. It includes the faulty
titration and standardization of solutions, since the 0.1 M NaOH and 0.1 M HCl solutions were
found out to be actually 0.086 M NaOH and 0.126 M HCl solutions upon standardization.
Other errors could have been the faulty weighing and measuring of samples, and incomplete
hydrolysis of the solutions that could have led to over titration and wrong calculation results
(Austria, 2013).
Chapter IV
Summary and Conclusion
The supposedly 0.1 M NaOH and 0.1 M HCl solutions used in this experiment were
standardized, wherein it was found out that the actual molarity of these solutions were 0.086 M
NaOH and 0.126 M HCl; 0.086 M NaOH being lesser than 0.1 M NaOH while 0.126 M HCl being
greater than 0.1 M HCl. Amongst many sources of error committed in performing this experiment,
the greatest factor that affected the calculated percent content by mass of acetylsalicylic acid (%
ASA) in the aspirin tablet was having standardized solutions with deviated molarity from the
expected values and also with huge difference from each other. % ASA in an aspirin tablet was
expected to be at approximately 70% ASA, yet only 21.29% ASA or C9H8O4 was calculated from
the group’s recorded and analyzed data. Thus, the group believes that the experiment was more
likely a failure due to major errors and inaccuracies that occurred during the experiment, leading
to erroneous calculations and results from the expected.
Basing from the possible error sources listed in the questions portion, the experiment must
be repeated with lesser or better yet, no errors at all, in order to obtain very accurate and precise
data from the experiment, which will then correspond to the expected standard values.
Appendix
A. Answers to Questions
1. What would be the effect of a more dilute solution of NaOH on the titration?
The pH level of a more dilute NaOH solution is lower, which then causes more amount
of titrant to be used and longer time of titration to show the indicator color to signal that the
equivalence point of the titration has already been achieved. Since the indicator is used to
determine the titration endpoint, this will lead the entire result of the titration to be afflicted
with error. Using a more dilute NaOH solution will affect the calculated percent content by
mass of acetylsalicylic acid in the aspirin tablet (% ASA). Since more dilute NaOH solution
means decreased molar concentration of the NaOH solution, there will be less moles NaOH
to react with HCl, which will lower also the moles C9H8O4 and eventually leading to lower
% ASA.
2. Given four 250-mg tablets of aspirin (90% pure acetylsalicylic acid) what volume of 1.000
M NaOH is used in the hydrolysis reaction if 10.00 ml of 0.500 M HCl is consumed in the
back titration?
Given:
Molarity of acid (HCl) (MA) = 0.500 M
1L
Volume of acid (HCl) (VA) = 10.00 mL x = 0.01 L
1000 mL
Solution:
MA x VA = MB x VB
8. Record the titres of acid and determine the molarity of the original NaOH solution, showing
all steps in your calculation.
Moles of NaOH
mol NaOH = mol HCl x mol NaOH
mol HCl
mol HCl = 0.003591 mol HCl x 1 mol NaOH = 0.003591 mol NaOH
1 mol HCl
Molarity of NaOH
mol NaOH 0.003591 mol NaOH
M NaOH = = = 0.3591 or 0.36 M NaOH
L NaOH 0.01 L NaOH
9. Determine the number of moles of NaOH originally added to the aspirin sample and the
number of moles of NaOH used in the hydrolysis step.
Solution:
Moles of NaOH
mol NaOH
mol NaOH = mol HCl x
mol HCl
mol HCl = 0.0036 mol HCl x 1 mol NaOH = 0.0036 mol NaOH
1 mol HCl
10. Calculate the number of moles of acetylsalicylic acid present in the titre sample.
Solution:
excess moles NaOH = 0.003591 mol HCl x 1 mol NaOH = 0.003591 mol NaOH
1 mol HCl
11. Calculate the mass of acetylsalicylic acid in each tablet and compare this with the
specification shown on the package.
From the previously calculated moles of ASA (0.0003545 mol C9H8O4), the mass of ASA
(mass C9H8O4) can be calculated:
mass C9H8O4 (g) = 0.0003545 mol C9H8O4 x 180.158 g C9H8O4 = 0.063866011 g C9H8O4
1 mol C9H8O4
1000 mg C9H8O4
mass C9H8O4 (mg) = 0.063866011 g C9H8O4 x = 63.866011 mg
1 g C9H8O4
mass C9H8O4 (mg) ≈ 64 mg
The mass of acetylsalicylic acid specified in the aspirin tablet package is 325 mg.
However, the calculated average mass of acetylsalicylic acid in each tablet was lesser at only
64 mg, having a difference of 261 mg (80.31%) from the indicated specification on the
package.
12. Analyze your own technique and assumptions in the experiment. List, in estimated order of
importance, various sources of error which could arise in this analysis.
Huge difference in molarity of standardized solutions used in the analysis
Using very concentrated or very diluted solutions
Faulty weighing and measuring of sample solutions
Inaccurate data recording
Incomplete hydrolysis of the solutions
Incomplete mixing of the solutions
Using inappropriate chemicals/solutions for rinsing the pipette and flasks, leading to
contamination of solutions involved in the titration
Not letting the reaction mixture cool down to room temperature
13. How will the percentage of acetylsalicylic acid in the aspirin tablet be affected if you forget
to fill the tip of the buret with sodium hydroxide solution before you started the titration?
The purpose of filling the buret tip with NaOH solution is to leave no air bubbles in it.
If this step is forgotten before starting the titration, these air bubbles will prevent the NaOH
solution from filling up the entire tip that will cause errors in reading the initial and final
volumes of the NaOH solution to be greater than its actual volume, which will cause the
calculated percentage of acetylsalicylic acid (% ASA) to be also greater and inaccurate.
14. If your lab partner "overshot" the endpoint in the second titration, would you be able to
salvage the lab without compromising results? Explain.
No. Unfortunately, the results will already be compromised even if the lab can be
salvaged. Adding more of the base (NaOH) needed to reverse the overshooting of the
equivalence point means that there is already higher volume of NaOH, which will affect the
moles NaOH present in the titration, thus leading to a higher calculated % ASA than the
actual result. Furthermore, it will lead to multiple errors in the calculations and inaccurate
results.
B. Calculations
Data:
Weight of KHP Volume of 0.1M prepared NaOH
Trial 1 Trial 2 Trial 3
0.5740g
34.0 mL 32.0 mL 32.0 mL
Moles of NaOH
MW KHP = (8 x MM C) + (5 x MM H) + MM K + (4 x MM O)
MW KHP = (8 x 12.011 g/mol) + (5 x 1.008 g/mol) + 39.098 g/mol + (4 x 15.999 g/mol)
MW KHP = 96.088 g + 5.04 g + 39.098 g + 63.996 g = 204.22 g KHP
Molarity of NaOH
0.0028 mol NaOH
M NaOH = mol NaOH = = 0.08562691131 or 0.086 M NaOH
L NaOH 0.0327 L NaOH
b. Standardization of 0.1000 M HCl solution against a standardized NaOH
Data:
Volume of HCl Volume of NaOH used
Trial 1 Trial 2 Trial 3
25.0 mL
30.9ml 31.5ml 32.2ml
Average Volume of 0.1000 M standardized NaOH solution used in all three trials
V1 + V2 + V3
Vave 0.1 M NaOH =
3
30.9 mL + 31.5 mL + 32.2 mL 94.6 mL
Vave 0.1 M NaOH = = = 31.5 mL NaOH
3 3
Moles of NaOH
mol NaOH = L NaOH x M NaOH
mol NaOH = 0.0315 L NaOH x 0.1000 mol NaOH = 0.00315 mol NaOH
1 L NaOH
Moles of HCl
mol HCl = mol NaOH x mol HCl
mol NaOH
mol HCl = 0.00315 mol NaOH x 1 mol HCl = 0.00315 mol HCl
1 mol NaOH
Molarity of HCl
0.00315 mol HCl
M HCl = mol HCl = = 0.126 M HCl
L HCl 0.025 L HCl
c. Analysis of Acetylsalicylic Acid in Aspirin Tablet Sample
Data:
Volume of aliquot Volume of 0.1M standard HCl solution
Trial 1 Trial 2 Trial 3
50.0mL
28.0ml 28.5ml 29.0ml
Given:
V aliquot = 50 mL x 1L = 0.05 L aliquot
1000 mL
28.0 mL + 28.5 mL + 29.0 mL 85.5 mL 1 L = 0.0285 L HCl
Vave HCl = = = 28.5 mL x
3 3 1000 mL
Solution:
excess moles NaOH = 0.003591 mol HCl x 1 mol NaOH = 0.003591 mol NaOH
1 mol HCl