ACID – BASE TITRATIONS

Determination of Purity of Potassium Acid Phthalate

Experiment No. 2

I. Objectives
1.) To perform an acid-base titration
2.) To prepare the necessary chemicals needed for the experiment
3.) To determine the relative concentrations of the hydrochloric acid and sodium
hydroxide solutions
4.) To standardize the sodium hydroxide solution with potassium acid phthalate
5.) To determine the purity of the potassium acid phthalate

II. Results and Discussion

Table 1. Measurement of the Relative Strengths of Acid and Base

Trials I II III
Final Reading HCl (mL) 18.00 36.00 18.00
Initial Reading HCl (mL) 0.00 18.00 0.00
Volume HCl used (mL) 18.00 18.00 18.00

Final Reading NaOH (mL) 14.50 29.10 43.60

Initial Reading NaOH (mL) 0.00 14.50 29.10
Volume NaOH used (mL) 14.50 14.60 14.50

Acid to Base Ratio 1.24137931 1.232876712 1.24137931

Average Acid/Base Ratio 1.238545111

Base to Acid Ratio 0.805555555 0.811111111 0.805555555

Average Base/Acid Ratio 0.807407407

Table 1 shows the amounts of HCl used and the corresponding amounts of NaOH needed
to achieve the end point; in this case, the slight pink coloration in the solution. The acid to base
and base to acid ratios were also computed.

Table 2. Standardization of Sodium Hydroxide

Primary Standard Used: Potassium Acid Phthalate (KHP)

Formula Mass of Primary Standard: 204.2212 g/mol
% Purity of Primary Standard: 99.8%

Trials I II III
Weight of Standard KHP (g) 0.3150 0.3318 0.3325
Corrected Weight of KHP (g) 0.314370 0.3311364 0.331835

Final Reading NaOH (mL) 16.80 34.60 40.2

 Initial Reading NaOH (mL) 0.00 16.8 23.1
Volume NaOH (mL) 16.80 17.80 17.1

Normality of NaOH 0.091628587 0.091093229 0.095022238

Average Normality of NaOH 0.092581351

To determine the unknown concentration of a known reactant, titration is used. It is a

common method in chemical analysis, where in a reagent, called the titrant, of known
concentration and volume is used to react with a solution of the analyte whose concentration is
unknown. The titration setup involves the titrant placed in a calibrated burette and the analyte
placed in a flask just below the burette tip. The titrant is then ran until the experimental end point
is reached. The end point signals the end of titration. The physical indication that the end point
has been reached is the change of the color of the solution to a slightly pink hue that persists for
about a minute or more. The end point is achieved through the help of an indicator, or that which
will physically indicate the end point. In this case, phenolphthalein indicator was used. This end
point is also more or less the same with the equivalence point, where the moles of the titrant is
equal to the moles of the analyte.

Since standard solutions play an important role in titimetry, standardization was

performed in this part of the experiment to determine the concentration of NaOH. In
standardization, the concentration of a volumetric solution is determined by titrating it against a
carefully measured quantity of a primary or a secondary standard or an exactly known volume of
another solution (Skoog, 2004). In this experiment, the titrant to be standardized was used to
titrate a weighed amount of a primary standard. In this case, the volumetric solution was NaOH
while the primary standard that was used was KHP.

The average normality that was calculated from the data shows that it is approximately
near the 0.1 N NaOH that we had prepared. There could be minimal errors in this experiment,
particularly because these errors are indeterminate. For example, there is a slight difference
between the change in indicator color and the actual equivalence point of the titration. Our
inability to observe and detect little differences in the physical changes also affects our
determination of the end point.

Table 3. Analysis of KHP sample

Trials I II III
Weight of KHP sample (g) 0.3347 0.3521 0.3941
Final Reading NaOH (mL) 8.30 17.7 29.40
Initial Reading NaOH (mL) 0.00 8.30 17.70
Volume NaOH (mL) 8.30 9.40 11.70

mg KHP in sample 156.928719 177.726501 221.212772

% KHP in sample 46.88638154 50.47614343 56.13112713
Average % KHP in sample 51.1645507

This part of the experiment aims to determine the purity of the KHP and the actual
amount of KHP that there is in the samples. KHP or potassium acid phthalate is the primary
standard that was used and to which the NaOH was compared against. The results showed that
the average percent purity of KHP in the three samples was only approximately equal to 51.16%.
This result is much less than that of the stated percent purity of the primary standard which is
 99.8%. This large difference may be due to a couple of systematic, random and gross errors, all of
which affect the results.

III. Conclusion

It has already been said that chemical analysis is extremely important and useful in many
ways. Titration allows us to analyze the samples which are actually representatives of the bulk
quantity. This particular technique allows us to compare the samples on standard materials of
accurately known composition (Skoog, 2004). Through titration, we have standardized NaOH
and determined the actual amount of KHP in the given samples. Titration is a very important
procedure where we can verify the quality and quantity of the components of the samples. Errors
and large differences may occur, but these errors are always present and usually unavoidable.

IV. Questions and Problems

1.) In the preparation of 0.1N NaOH, why is it necessary to use carbonate-free base?
It is necessary that the NaOH solution is carbonate-free so that the carbonate ions
will not react with HCl or with the KHP.

2.) What will be the resulting concentration of sodium hydroxide when the tip of the burette
is not filled completely? Is it higher, lower or no change? Explain your answer.
If the tip of the burette is not filled completely (ie. has bubbles), then the volume
you have measured is larger than the actual volume that has been ran in the analyte
because the bubbles take up a space which has been included in your reading. So if you
remove the bubbles, you will see that the volume decreases. In effect, if you have a
volume that is actually larger than the actual, you will get wrong answers in the
molarities of NaOH and amount of KHP present in the samples.

3.) Write the net ionic reaction of titrant and the secondary standard used in the experiment.
NaOH + HCl  NaCl + H2O

4.) Why is potassium acid phthalate used as a primary standard? What are its properties
which are considered to be important?
KHP was used as primary standard because it has the following properties: high
purity where established methods for confirming its purity is available; atmospheric
stability; absence of hydrate water so that the composition of the solid does not change
with variations in humidity; modest cost; reasonable solubility in the titration medium;
reasonably large molar mass so that the relative error associated with weighing the
standard is minimized.

5.) Calculate the concentration (molarity) of NaOH given that 0.5123 g of KHP requires
21.06 mL of NaOH.
0.5123 g KHP x 1 mol KHP x 1mol NaOH = 2.509 x 10-3 mol NaOH
204.2212 g 1 mol KHP

2.509 x 10-3 mol NaOH = 0.119 M NaOH

0.02106 L NaOH
V. References
 [1] Skoog DA, West DM, Holler, FJ, Crouch SR.2004.Fundamentals of Analytical
Chemistry.Singapore.Brooks/Cole.pp91-170.
[2] Kelley MT.1959.Analytical Chemistry.New York.Ergmon Press.pp14-36.
[3] http://www.wikipedia.com/

VI. Sample Calculations

1.) Acid to Base Ratio

= vol acid = 18.00 mL = 1.24137931
vol base 14.50 mL

2.) Average Acid to Base Ratio

= 1.24137931 + 1.232876712 + 1.24137931 = 1.238545111
3

3.) Base to Acid Ratio

= vol base = 14.50 mL = 0.805555555
vol acid 18.0 mL

4.) Average Base to Acid Ratio

= 0.805555555 + 0.811111111 + 0.805555555 = 0.807407407
3

5.) Corrected Weight of KHP

= weight KHP x % purity = 0.3158 x 0.998 = 0.31437 g

6.) Normality of NaOH

= corrected weight KHP x n = 0.31437 g x 1 . = 0.091628587 N NaOH
MW KHP x Vol NaOH 204.22 g/mol x 0.0168 L

7.) mg KHP in sample

= average [NaOH] x Vol NaOH used x MW KHP
= 0.092581351 mol x 0.0083 L x 204,221.2 mg . = 156.9287192 mg KHP
L mol

8.) % KHP in sample

= weight above . x 100 = 156.9287192 mg KHP x 100 = 46.8863816
Weight measured KHP 334. 7 mg