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CHAPTER III

Results and Discussion

Table 1. Masses

Name of compound Mass, g


NaOH 1.92
KHP (T1) 0.25
KHP (T2) 0.24
KHP (T3) 0.24

Table 2. Volume of NaOH

Trial Initial Reading, mL Final Reading, mL Total Volume Used,


mL
1 0 12.9 12.9
2 12.9 26.09 13.9
3 26.09 40.29 14.2

In the standardization of NaOH, the primary standard used for the titration with the NaOH
solution is the potassium acid phthalate (KHP), with phenolphthalein as the indicator. The mass
of NaOH measured using the analytical balance was 1.92g. On the other hand, the mass of KHP
recorded are as follows: T1, 0.25g; T2, 0.24g; and T3, 0.24g.
Shown in table 2 is the volume of NaOH recorded by subtracting the initial reading from the
final reading – 12.9 mL for trial 1; 13.9 mL for trial 2; and 14.2 mL for trial 3.
Based on the calculations, the mass of NaOH used to prepare a 0.1 M NaOH solution is
1.99985g NaOH. The average volume of NaOH required to react with KHP is 13.43 mL. Using
those data and the mass of KHP which was initially recorded, the concentration of Standard
NaOH was calculated; M1= 0.09489 M, M2=0.08909 M, M3= 0.08276 M – giving an average
concentration of 0.08891 M. Through the process of standardization, we were able to determine
the exact concentration of the solution which is 0.08891 M, allowing us to move forward
towards the next analysis.

Table 3. Titration Data

Volume pH
of Vol NaOH vs pH
NaOH 14.00
0.00 2.96 12.00
2.00 3.18 10.00
4.00 3.40 8.00
6.00 3.58
pH

6.00
7.98 3.73 4.00 30.48
10.01 3.86 2.00
10.98 3.92 0.00
-1.00 3.50 8.00 12.50 17.00 21.50 26.00 30.50 35.00 39.50 44.00 48.50
12.05 3.98
Volume of NaOH
13.01 4.03
14.03 4.09
15.08 4.15
16.05 4.21
17.00 4.27
Figure 1. Volume vs pH
18.05 4.33
19.01 4.39
20.10 4.45
21.04 4.52
At Half Equiv. pt. pH vs. V(NaOH)
4.35

4.25
4.05

3.95
11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00 19.00

22.00 4.59 Volume of NaOH


23.08 4.67
24.05 4.76
25.05 4.86
26.06 4.97
27.02 5.11
28.00 5.30
29.01 5.60
30.02 6.40
31.00 10.76
32.01 11.26
33.00 11.49
34.04 11.63
36.09 11.83
38.01 11.97
40.00 12.06
42.00 12.13
44.05 12.20
46.00 12.25
48.09 12.30
50.00 12.33

Table 4. First Derivative Data

Vol NaOH pH pH V Vavg pH/V


27.02 5.11
28.00 5.30 0.19 0.98 27.51 0.19
29.01 5.60 0.30 1.01 28.51 0.30
30.02 6.40 0.80 1.01 29.52 0.79
31.00 10.76 4.36 0.98 30.51 4.45
32.01 11.26 0.50 1.01 31.51 0.50
33.00 11.49 0.23 0.99 32.51 0.23
First Derivative Plot
5.00
4.50
4.00
3.50
3.00
DpH/DV

2.50
2.00
1.50
1.00
0.50
0.00
27.00 28.00 29.00 30.00 31.00 32.00 33.00
Vavg

Figure 3. First Derivative Plot

Table 5. Second Derivative Data

Vavg pH/V (V) (pH/V) Vavg (pH/V)/(V)

27.51 0.19

28.51 0.30 1.00 0.10 28.01 0.10

29.52 0.79 1.01 0.50 29.01 0.49

30.51 4.45 0.99 3.66 30.01 3.68

31.51 0.50 1.00 -3.95 31.01 -3.97

32.51 0.23 1.00 -0.26 32.01 -0.26

Second Derivative Plot


5.00
4.00
3.00
2.00
D(DpH/DV/V/DV)

1.00
0.00
27.50 28.00 28.50 29.00 29.50 30.00 30.50 31.00 31.50 32.00 32.50
-1.00
-2.00
-3.00
-4.00
-5.00
VNaOH avg

Figure 4. Second Derivative Plot


Table 6. Physical Data for Organic Acids

Shown in figure 1 is the plot of the first titration curve. With the volume of NaOH on the x-
axis and the pH on the y-axis, we determined the approximate location of the equivalence point which is
30.48; this specific point of the curve is the point of maximum slope in the titration. After identifying the
equivalence point’s location, we then calculated the volume of sodium hydroxide at the equivalence point
in the titration and therefore the volume at which exactly half of the acid had been neutralized.
Shown in figure 2 is the point of the curve, known as the buffer point, which visualizes an
estimate of the acid dissociation constant of the acid being titrated. The equivalence point in this titration
is at 30.02 mL, the buffer point at 15.08 mL, and the pKa is approximately 4.15. These information are
significant in identifying the given unknown acid.
After getting the equivalence point and the buffer point, we now head towards attaining the
first derivative plot which is another valuable information that could give us a better approximation of the
volume at equivalence point. Shown in figure 3 is the plot of the rate of change with change in volume
versus volume as calculated in table 2. As a result, a “spiked” curve should appear and its peak should be
at the equivalence point.
Shown in figure 4 is the plot of the second derivative. Getting the second derivative plot gives
us a more precise and a clearer view in determining the volume of the titrant. Visually, the second
derivative should pass through x-axis at equivalence point, and in this case, the equivalence point is at
30.39 mL.
After determining the equivalence volumes and the pKa, using the reference table, table 4, we
can determine the unknown acid’s identity. The pKa of our unknown acid which was determined in the
half-equivalence point was 4.15, we ought to refer on table 4 and find the closest pKa value which will
help us determine the identity of our unknown acid, which in this case, is the benzoic acid.

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