School of Chemical, Biological and Materials Engineering and Sciences

BE121L Chemical Analysis in Biological Engineering Laboratory

2nd Quarter SY 2019-2020

Preparation of Standard Solutions and Acid-Base Titration

Apan, Jhon Jasper D 1; Carpena, Ferdinand Lauren F 2; Sy, Ellah Mae B 3

1,2,3
Students, BE121L/B10, School of Chemical Engineering and Chemistry, Mapúa University

ABSTRACT
Titration is a means of chemical analysis employed to determine the concentration of a substance by adding a solution of known
concentration. The objectives of this experiment are (1) to learn how to prepare acid and base titrant solutions; (2) to learn how to
standardize titrant solution using primary standard; and (3) to determine the purity of sample through acid base-titration. In preparing the
solution, 0.4mL of 50% (w/w) NaOH was added to 200mL of distilled water. The solution is then standardized by titrating it 20mg of
potassium hydrogen phthalate (KHP). Across three trials, the average concentration of the titrant was 0.0131 mmol/mL with a ±0.00143
mmol/mL margin of error and 11.75% relative standard deviation. The standardized NaOH solution was then used to analyze three
tablets of aspirin with a brand of Bayer. The average percent purity of the aspirin tablets was 66.87% with a ±5.96% margin of error and
a relative standard deviation of 9.61%. Errors that were observed in this experiment may have been caused by impaired color vision of
one of the students and the inaccurate standardization of the titrant that resulted to the incorrect concentration of the NaOH solution
used in the calculations.
Keywords: acid-base titration, standardization, aspirin, purity

INTRODUCTION

Titration is a means of chemical analysis employed to
determine the concentration of a substance (called an
analyte) by adding a solution of known concentration (called
titrant) until the reaction reaches neutralization, known as th
end point of titration [1]. After the titration process, the
concentration of the titrant, the volume of the titrant used,
and information from the balanced chemical reaction of the
titrant and analyte are used for stoichiometric computations
for the concentration of the analyte [2].
Since the concentration of the titrant is important for a
reliant analysis, it is therefore necessary to determine the
exact concentration of the titrant. This is accomplished by
standardization of the titrant. To standardize the titrant, it is
titrated against a well-characterized analyte [3]. This
analyte must be a primary standard for accurate results.
Primary standards are substances which must have high
level purity, must be stable, must have high equivalent
weight, must not absorb moisture from air, and must be
inexpensive and readily available [4]. In this experiment,
the primary standard used was potassium hydrogen
phthalate (KHP).
titrant results to excess, unreacted molecules. This excess
molecules will react with the indicator, which in turn,
changes the structure of the indicator molecules, resulting
in a change in color [5].
The end point for the indicator depends on its pKa value.
However, indicators do not change color at an exact pH or
pKa value. Rather, their colors change within a range of pH
values. In choosing the indicator to be used for titration, the
endpoint must first be predicted using titration curves. The
indicator to be used must change color within the same pH
where the endpoint of titration is expected [5][6]. In this
experiment, the indicator used was phenolphthalein whose
pH range is 8.3 to 10.
Although titration is a reliable process, it is an error prone
process. Some of the errors that can arise from titration are
(1) end point error which can be caused by addition of
excess titrants or by the difference of color perception of
individuals; (2) volumetric error which can be caused by not
reading the burette from eye level; bubbles formed in the
burette, or by small leaks in the burette; and (3) incorrect
concentration of the titrant used in the calculation [7].

Another important component of acid-base titration process

are indicators. Upon reaching the endpoint of titration, the
titrant will neutralize the analyte. Further addition of the

Experiment 2│ Group MEBE │ November 25, 2019 1 of 4

 School of Chemical, Biological and Materials Engineering and Sciences
BE121L Chemical Analysis in Biological Engineering Laboratory
2nd Quarter SY 2019-2020

The objectives of this experiment are (1) to learn how to Table 1. Standardization of NaOH solution against KHP
prepare acid and base titrant solutions; (2) to learn how to Trial 1 Trial 2 Trial 3
standardize titrant solution using primary standard; and (3) Weight of KHP (g) 0.019 0.021 0.019
to determine the purity of sample through acid base- Moles of KHP (mmol) .093037 .10283 .093037
titration. Volume of NaOH used
6.3 8.7 7.3
(in mL)
MATERIALS AND METHODS Molarity of NaOH
0.0148 0.0118 0.0127
solution (mmol/mL)
The first part of the experiment was dedicated in preparing Average molarity of
the titrant. Using a 1mL measuring pipette, 0.4mL of 50% NaOH solution 0.0131
weight by weight (w/w) sodium hydroxide (NaOH) was (mmol/mL)
placed in 200mL of distilled water in a volumetric flask. The Relative standard
11.75%
volumetric flask was covered, and the solution was mixed deviation
thoroughly.
The weight of KHP used for the three trials were 0.019g,
In the next part, the NaOH solution was standardized 0.021g and 0.019, and their moles were 0.093037mmol,
against potassium hydrogen phthalate (KHP). Using an 1.0283mmol, and 0.093037mmol, respectively. The volume
analytical balance, three 0.02g of KHP samples were of the titrant used for the three samples were 6.3mL, 8.7mL,
obtained. These samples were separately placed into three and 7.3mL respectively. The molarity of the NaOH solution
250mL Erlenmeyer flasks. Fifty (50) mL of distilled water was then computed to be 0.0148 mmol/mL, 0.0118
were used to dissolve each sample of KHP, and three mmol/mL, and 0.0127 mmol/mL. The average molarity was
drops of the indicator phenolphthalein were added to each. 0.0131mmol/mL with a relative standard deviation of
Then, the titration set-up was made. The NaOH solution 11.75%
from the first part of the experiment was placed in the
burette which was then clamped on the iron stand. Each 0.02
sample of KHP was then titrated until the colorless solution 0.01
turned into light pink. The volume of NaOH used for each 0.01
sample were recorded.
0.01
0.01 Average Molarity
After the titrant has been standardized, it was used to Molarity per trial
analyze the percent purity of acetylsalicylic acid in Bayer, a 0.01
brand of aspirin. The aspirin was crushed using mortar and 0.01
pestle and was placed in an Erlenmeyer flask. Then, 25mL 0.01
of 50% ethanol solution were added into the Erlenmeyer 0.01
flask. The flask was swirled until the aspirin has dissolved. 0.5 1 1.5 2 2.5 3 3.5
Three drops of the phenolphthalein indicator were then
added to the solution. The solution was titrated until the Figure 1. 95% confidence interval for molarity of NaOH solution
solution turned light pink. Similarly, the initial and final
burette readings were recorded. Three trials of titration Figure 1 shows the values of the computed molarity of
were conducted. NaOH solution plotted against a 95% confidence interval of
the mean molarity 0.0131mmol/mL. With 95% confidence,
RESULTS the mean value for the molarity fell within the range 0.01167
mmol/mL to 0.01453 mmol/mL. The margin of error was
Using KHP as the primary standard, the NaOH solution was ±0.00143 mmol/mL.
titrated and standardized. Table 1 shows the values
obtained and calculated when standardizing the NaOH After standardizing the NaOH solution, it was used to titrate
solution across three trials. three tablets of aspirin. Table 2 summarizes the values
obtained and calculated for the analysis of analysis.

Experiment 2│ Group MEBE │ November 25, 2019 2 of 4

 School of Chemical, Biological and Materials Engineering and Sciences
BE121L Chemical Analysis in Biological Engineering Laboratory
2nd Quarter SY 2019-2020

76
Table 2. Titration of acetylsalicylic acid in Bayer aspirin 74
Trial 1 Trial 2 Trial 3 72
Weight of aspirin tablet 70 Average Percent
0.122 0.122 0.122
(g) 68 Purity
Volume of NaOH used 66 Percent purity per
38.4 32.3 33 trial
(in mL) 64
Moles of NaOH used 62
0.503 0.423 0.432
(mmol) 60
0.5 1 1.5 2 2.5 3 3.5
Actual moles of aspirin
0.503 0.423 0.432 Figure 2. 95% confidence interval for the percent purity of Bayer
(mmol)
aspirin
Theoretical moles of
0.6772 0.6772 0.6772
aspirin (mmol)
Figure 2 shows the percent purity of Bayer aspirin for each
Percent purity of aspirin 74.22% 62.48% 63.84%
trial plotted against a 95% confidence interval of the
Average percent purity
66.87% average percent purity of the sample. With 95% confidence,
of aspirin
the average percent purity was between 60.91% and
Standard deviation 5.27% 72.83%. The margin of error was ±5.96%.
Relative standard
9.61%
deviation
DISCUSSION
The weight of the three tablets used were 0.122g each.
From Table 1 and Figure 1, it can be seen that the results
Across the three trials, the volume of the NaOH used were
contained errors that decreased the accuracy and precision
38.4mL, 32.3mL, and 33mL. Using the concentration
of the results of the standardization of the NaOH. The high
obtained from the standardization of NaOH, the moles of
relative standard deviation implies that the results were
NaOH used in titrating the aspirin were 0.503 mmol, 0.423
unprecise. The result for Trial 1 also did not fall within the
mmol, and 0.432 mmol. Since the stoichiometric ratio of
95% confidence interval which means that the result
NaOH and aspirin is 1:1, then, it follows that the actual
obtained was not accurate.
moles of aspirin is equal to the moles of NaOH used.
Meanwhile, using the molecular weight of aspirin, the As described, using an incorrect concentration of the titrant
theoretical moles of aspirin was computed to be 0.6772 in the calculations would lead to inaccurate results [7].
mmol each. Because of the errors in the concentration of the NaOH
solution, it was also expected that the results for the
The percent purity for the three trials were then computed analysis of the aspirin would also be erroneous. The
to be 74.22%, 62.48%, and 63.84%, respectively. The relative standard deviation was also high at 9.61%.
average purity was 66.87% with a standard deviation of Similarly, the results for Trial 1 was also out of the
5.27% and a relative standard deviation of 9.61%. confidence interval
The errors in first trials of the first and second part of the
experiment may have been endpoint errors which may have
been caused by the impaired color vision (color blindness)
of the student who performed the said trials. As described,
the difference in color perception of individuals will affect
the outcome of the experiment [7].

CONCLUSIONS AND RECOMMENDATIONS

The objectives of this experiment are (1) to learn how to

prepare acid and base titrant solutions; (2) to learn how to
standardize titrant solution using primary standard; and (3)

Experiment 2│ Group MEBE │ November 25, 2019 3 of 4

 School of Chemical, Biological and Materials Engineering and Sciences
BE121L Chemical Analysis in Biological Engineering Laboratory
2nd Quarter SY 2019-2020

to determine the purity of sample through acid base-
titration.
The first objective was met. The students were able to
prepare acid-base titrant solution. The students prepared a
titrant from 50% NaOH solution which was used throughout
the experiment.
The students also learned how to standardize the titrant
they have prepared. Using KHP as the primary standard,
the students were able to determine the concentration of
the NaOH titrant they have prepared which was found out
to be 0.0131 mmol/mL.
Finally, the students have also been able to determine the
purity of sample. The students determined the purity of
Bayer aspirin to be 66.87% using the standardized NaOH
solution they prepared.
December 15, 2019).
[5] B. Yool, What Is an Indicator for a Titration?,
(2017). https://sciencing.com/indicator-titration-
6549531.html (accessed December 15, 2019).
[6] J. Clark, Acid-Base Indicators, (2019).
https://chem.libretexts.org/Bookshelves/Physical_a
nd_Theoretical_Chemistry_Textbook_Maps/Supple
mental_Modules_(Physical_and_Theoretical_Chem
istry)/Equilibria/Acid-Base_Equilibria/6._Acid-
Base_Indicators (accessed December 15, 2019).
[7] M. Carpenter, Errors in Titration Experiments,
(2018). https://sciencing.com/errors-titration-
experiments-8557973.html (accessed December
15, 2019).

Titration is prone to errors. It is therefore recommended to

be sensitive and careful in performing the experiment.
Performers of the experiment also need to have good color
vision to avoid errors that have been observed in this
experiment. Furthermore, since titration is prone to errors, it
is recommended that if the analysis requires high level of
accuracy and precision, other methods of analysis shall be
employed.

REFERENCES

[1] LibreTexts, Titration, (2019).

https://chem.libretexts.org/Bookshelves/Ancillary_M
aterials/Demos%2C_Techniques
%2C_and_Experiments/General_Lab_Techniques/
Titration (accessed December 15, 2019).
[2] J. Brubaker, How to Determine the Concentration of
a Titration, (2017). https://sciencing.com/determine-
concentration-titration-6391245.html (accessed
December 15, 2019).
[3] Chromacademy, Titrant Standardization, (n.d.).
https://www.chromacademy.com/lms/sco735/03-
Titrant-Standardization.html?
fChannel=22&fCourse=97&fSco=735&fPath=sco73
5/03-Titrant-Standardization.html (accessed
December 15, 2019).
[4] A.M. Helmenstine, Primary Standards in Chemistry,
(2018). https://www.thoughtco.com/definition-of-
primary-standard-and-examples-605556 (accessed

Experiment 2│ Group MEBE │ November 25, 2019 4 of 4