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Gabriel C.

Raola
Answers to Questions: Experiment 11
1. The significant regions (pre-equivalence point, equivalence point and postequivalence point) in the titration curve and relate the characteristics of each
region to the pH results obtained.
The region pre-equivalence or the acidic region exhibits pH of less than
7 where hydronium ions prevail. The instantaneous rate at which the pH
increases as more titrant is added also increases with volume of titrant
added. On the other hand the region that contains the equivalence point is
slightly basic because KHP is a weak acid, and a weak acid titrated with a
strong base results to a slightly basic solution at the equivalence point. The
instantaneous rate at which the pH increases as more titrant is added is
highest at the equivalence point. The last region, the post equivalence region
is the basic region because the pH obtained from this region is all greater
than 7. The number of moles of titrant added is more than that of the
analyte, making it the excess reagent. The instantaneous rate at which the
pH increases as more titrant is added decreases with volume after the
equivalence point.
2. Explain the differences if any in the Veq to the pH results obtained among the
three plots.
The Veq for the three trials are 11.5 mL, 9.55 mL and 9.45 mL. We can
see that the Veqs of trial 2 and 3 are quite close while the Veq of trial 1 is
slightly far from the two other trials. It is because the first trial was performed
at a constant increment of 1mL while trials 2 and 3 were performed using
varying increments which affected the precision of the volume at the
equivalence point.
3. How is the endpoint estimated using potentiometric if no chemical indicator is
added to the analyte solution?
The endpoint was estimated graphically. The 1 st and 2nd derivative plots
were obtained through plotting. The 1 st derivative plot was obtained by
plotting the change in pH vs the change in volume. Similarly, the 2 nd
derivative plot was obtained by plotting the change in the change in pH vs
the change in the average volume. The point in the 1 st derivative plot wherein
the change in pH is the highest and the point in the 2 nd derivative plot
wherein the maximum difference between a positive y value and negative y
value is obtained also known as the inflection point corresponds to the
endpoint.1
4. The importance of continuous stirring (use of stirrer and magnetic stir bar) in
potentiometric titration.
Continuous stirring was done in order to uniformly distribute the added
titrant within the solution in order to prevent the variation in concentration in

the different portions of the solution which may result to inaccurate pH


readings. 2
5. Why should the increments of addition of titrant be narrowed down as the
titration approaches the equivalence point?
Smaller increments were used upon reaching the end point in order to
stay at a close range from the equivalence point and in order to avoid going
beyond the equivalence point immediately. The increments were narrowed
down in order to obtain a sharper endpoint and make precise measurements
and more accurate plots.
6. The advantages and disadvantages of using potentiometric titration.
Some advantages of potentiometric titrations are the undoubtedly
more accurate and precise data as compared to a regular titration set-up. 3
Also, no indicator is needed for the titration, therefore removing the human
error in the judgment of whether the solution has reached its endpoint or
not.3 However, the disadvantages of using potentiometric titration include the
expensive cost of a pH meter and the tedious and time-consuming work done
primarily because the pH should be recorded per increment of the titrant
added.
7. Possible sources of error and their effect on the %purity of the KHP in the
sample.
The large deviation from the real value of the acid dissociation
constant of KHP could have occurred due to different reasons. One of which is
the failure to uniformly distribute the added titrant concentration within the
solution upon reading the pH meter which could either cause an increase in
pH and consequently cause a lower value for the acid dissociation constant or
a decrease in pH which yields a higher Ka and %purity depending on the
gradient present near the electrode. Another is the presence of a bubble in
the buret could have also affected the recorded data because a less change
in pH will be observed to the increase in the volume read but a decrease in
the amount of titrant added and would yield a higher %purity. Another
source of error is the accuracy of the observation of the titrant volume in the
buret due to parallax. Depending on whether the perceived volume is greater
or lesser than the actual volume, it can either increase of decrease the
recorded volume of titrant needed to reach equivalence point, therefore
increasing or decreasing the calculated % purity of the KHP sample. Another
reason could be due to the contamination of the glassware used in the
experiment and improper preparation of the solutions could have also been a
cause for the deviations in the percent purity.

REFERENCES
[1]Harris, D. C. Quantitative chemical analysis. (8th ed.)(2010).
[2] Skoog, D., West, D., Holler, F., & Crouch, S. (2010).. InFundamentals of
Analytical Chemistry (8th ed.). Cengage Learning Asia Pte Ltd.
[3] Harvey, D. (2000). In Modern Analytical Chemistry. The Mc-Graw hill
companies, Inc.

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