Andre Smith

October 7, 2015
FST 101A-A06, Wednesday 9 AM
RH
LAB 2 & 3 Preparing a Standard Base Solution
& Total Acidity and pH of Liquid and Solid Foods
I. Purpose/Objective
The purpose of Lab 2 was to prepare a standardized NaOH solution using the primary
standard KAP. The purpose of Lab 3 was to determine the %acidity, equivalence points, and
Brix of fruit juices and cheeses.
II. Introduction
When determining acidity and basicity by titration, you must have an accurate
standardized solution to get an accurate measurement. In this experiment, an NaOH solution
was standardized by using the primary standard Potassium Acid Pthalate (KAP). NaOH is
hygroscopic, so it absorbs water and carbon dioxide from the air. The NaOH can be
standardized after it is put in solution and its normality can be determined. Once the standard
base solution is prepared, the normality of the solution can be used to calculate the acidity
and equivalence points of acids.
In the food industry, standardized solutions are important to determine Brix/Acid ratios of
foods. Consumers will expect foods to taste a certain way, and if food chemists miscalculate
how acidic certain foods are, the foods will not taste good enough for optimal consumer
satisfaction.
III. Procedure
The procedure for Lab 2 is found in Principles of Food Composition, Laboratory Manual,
FS&T 101A (2015) pages 14 and 15.
Modifications: In the first step, the procedure directs to use approximately 30 ml of T1 water
but exactly 40 ml is used. In step 10, the procedure is modified such that the titration was
continued all the way to pH 11. The manual also instructs to use two vials of KAP with an
unknown weight to check the accuracy of the standardization. Only one vial of a KAP
unknown was used.

The procedure for Lab 3 is found in Principles of Food Composition, Laboratory Manual,
FS&T 101A (2015) pages 19 and 20. The modification for lab 3 is to use 25 ml of cheese
solution instead of 50 ml. The cheese should be put into the blender after the water.
 IV. Data
Table 1: KAP samples with weights, volumes, pH, and NaOH concentrations.
Sample # Weight (g) Start Ending pH NaOH
Volume(ml) Volume(ml) (Normality)
172 0.3641 0.00 16.25 - -
252 0.3351 16.30 31.11 7.04 0.1109
401 0.3771 3.99 20.65 6.97 0.1108
411 0.3735 20.65 37.20 7.19 0.1105
440 0.3763 24.60 41.20 0.1104
(unknown) (actual
0.3741)

Table 2: Volume of NaOH added vs. pH for fourth titration with KAP
Volume
(ml) pH 25.51 4.72 30.95 5.28 36.1 6.18
(start)20.
65 3.97 25.99 4.76 31.4 5.33 36.3 6.27
21.1 4.02 26.5 4.82 31.92 5.39 36.42 6.32
21.6 4.08 27.02 4.88 32.5 5.45 36.51 6.39
21.9 4.22 27.51 4.93 33 5.52 36.65 6.5
22.42 4.29 28.1 4.99 33.45 5.6 36.9 6.77
22.98 4.36 28.5 5.02 34.08 5.67 37 6.85
23.45 4.45 29 5.07 34.51 5.76 37.08 7.19
24.01 4.53 29.5 5.13 35 5.85 37.2 7.31
24.51 4.59 30.01 5.19 35.5 5.93 37.35 10.81
25 4.65 30.48 5.23 36.01 6.12 39 12.14

Table 3: Sensory evaluation of total acidity of liquids and solid foods

Most Sweetes Preferen
acidic t ce
AJ>GJ>
Juice OJ>GJ>AJ OJ GJ
Vineg S>2>1> 3>1>2>
ar 3 S 1
Chees Mozzarel
e Cheddar la Cheddar

Table 4: Volume of NaOH added vs. pH of grape juice for Group 9

Volume
(ml) pH 14 4.69 21.82 6.82 26.1 8.48
(start )1 3.42 14.52 4.77 22 6.86 26.2 8.54
1.45 3.45 15.12 4.85 22.18 6.92 26.3 8.6
 1.98 3.49 15.55 4.92 22.3 6.96 26.45 8.64
2.5 3.53 16 4.98 22.6 7.13 26.58 8.69
3 3.57 16.5 5.08 22.75 7.18 26.72 8.73
3.45 3.6 17.05 5.23 22.9 7.24 26.9 8.78
3.92 3.65 17.5 5.3 23 7.32 27 8.81
4.5 3.7 18 5.45 23.21 7.39 27.12 8.85
5.03 3.75 18.51 5.53 23.5 7.46 27.28 8.91
5.52 3.79 19 5.68 23.6 7.53 27.4 9
6 3.83 19.5 6.07 23.7 7.6 29.35 9.09
6.45 3.87 19.65 6.12 23.85 7.71 31 9.14
7 3.92 19.7 6.15 24 7.76 33 9.2
7.51 3.97 19.8 6.21 24.2 7.8 35 9.3
8 4.01 20 6.28 24.3 7.86 37 9.42
8.5 4.06 20.12 6.31 24.5 7.88 39 9.52
9 4.11 20.23 6.36 24.7 7.92 41 9.64
9.52 4.16 20.3 6.42 24.85 8.01 43 9.84
10.12 4.23 20.5 6.46 25 8.08 45 10.03
10.51 4.28 20.6 6.49 25.15 8.15 47 10.1
11 4.32 20.68 6.53 25.28 8.21 49 10.26
11.47 4.38 20.8 6.58 25.35 8.25 50 10.43
12 4.44 21 6.6 25.5 8.29
12.5 4.49 21.15 6.65 25.65 8.34
13.11 4.56 21.3 6.7 25.8 8.4
13.5 4.63 21.5 6.75 25.95 8.45

Table 5: Volume of NaOH added vs. pH of mozzarella cheese for Group 9

Volume
(ml) pH 1.14 6.5 2.42 7.13 3.5 8.58
(start)
0.1 6.32 1.25 6.53 2.5 7.2 3.65 8.78
0.3 6.25 1.3 6.58 2.65 8 3.8 9.05
0.42 6.3 1.45 6.63 2.8 8.11 3.9 9.3
0.51 6.33 1.62 6.66 2.93 8.21 5.9 9.53
0.6 6.35 1.78 6.74 3.01 8.28 7.98 9.75
0.7 6.38 1.9 6.81 3.13 8.35 10 10.04
0.8 6.4 2 6.88 3.21 8.48 12 10.4
0.9 6.41 2.1 6.94 3.3 8.57 13.99 10.73
1.03 6.44 2.3 7.04 3.44 8.57 16 11.04

Table 6: Section A06 class data for juice and cheese titrations
 Juice Cheese
Juice/ [NaOH]N
Group # NaOH at Mass NaOH at
Cheese Eq. pH Brix Initial pH Eq. pH Brix (eq/L)
eq. (mL) (g) eq. (mL)
1 O/M 26.53 7.36 11.9 12.04 2.5 5.99 7.51 1.1 0.107
2 O/C 25.7 7.14 11.8 12 5.2 5.21 7.5 1.6 0.107
3 O/M 30.55 9.41 11.8 12 4.15 5.91 7.32 1 0.108
4 O/C 27.9 7.57 12.5 12 6 5.78 6.7 1.7 0.108
5 A/M 15.65 8.7 12.6 12 3.15 6.11 8.2 1.1 0.11
6 A/C 15.6 8.43 12.5 12.2 9.1 5.52 8.62 1.7 0.107
7 A/M 9.75 5.99 12.5 11.9 1.95 5.9 8.53 1.3 0.11
8 A/C 15.95 7.24 12.5 12.05 9.15 5.55 7.41 1.7 0.106
9 G/M 22.78 7.66 16 12.1 2.57 6.32 7.5 1.1 0.111
10 G/C 19.05 6.17 15.9 12 6.55 5.62 8.11 1.5 0.108
11 G/M 21.35 8.02 15.1 12.01 1.35 7 8.36 1.1 0.111
12 G/C 25.5 6.4 15.1 12 - - - 1.8 0.111

Table 7: % Acidity, pH, Brix, Brix:Acid, Sensory Ranking, starting pH, and food label values
for class data.
% Starting
Acidi Brix/Titratable Taste Test Juice Labeled %
Sample ty pH Brix Acidity Ranking pH Sugar
Orange 0.76 1st acidic,
Juice 2 7.87 12.0 15.7 3rd sweet 3.9 10.0
3rd acidic,
Apple 0.41 1st
Juice 3 7.59 12.5 30.3 sweetest 3.79 11.3
2nd acidic,
Grape 0.73 2nd
Juice 3 7.06 15.5 21.2 sweetest 3.2 16.3
1.16
Cheddar 2 7.67 1.7 1.4 Most acidic - -
0.42
Mozzarella 9 7.90 1.1 2.6 Sweetest - -
 KAP pH vs. volume NaOH added
25

20

15
pH/ ( pH/ V)
10

0
0 2 4 6 8 10 12 14 16 18 20

Volume NaOH added (ml)

KAP pH pH/ V

Fig. 1: Titration curve of KAP with 0.111N NaOH vs. first derivative.

Grape juice pH vs. volume NaOH added

12
10
8

pH / (pH/V) 6
4
2
0
0 10 20 30 40 50 60

Volume NaOH added (ml)

Juice pH pH/V

Fig. 2: Titration curve of tartaric acid in grape juice with 0.111N NaOH vs. first derivative.
 Mozzarella cheese pH vs. volume NaOH added
12

10

6
pH/(pH/V)
4

0
0 2 4 6 8 10 12 14 16 18
-2

Volume NaOH added (mL)

Cheese pH pH/V

Fig. 3: Titration curve of lactic acid from mozzarella cheese with 0.111N NaOH vs. first
derivative.

Acetic acid pH vs. volume NaOH added

35
30
25
20
pH/(pH/V) 15
10
5
0
0.00 5.00 10.00 15.00 20.00 25.00

Volume NaOH added (ml)

Titration Curve First Derivative

Fig. 4: Titration curve of acetic acid with 0.1N NaOH vs. first derivative.
 Phosphoric acid pH vs. volume NaOH added
12.00
10.00
8.00

pH/(pH/V) 6.00
4.00
2.00
0.00
10.00 20.00 30.00 40.00 50.00 60.00

Volume NaOH added (ml)

Titration Curve First Derivative

Fig. 5: Titration curve of phosphoric acid with 0.1N NaOH vs. first derivative.

V. Calculations
Calculating NaOH Normality:
NNaOH = (grams of KAP/ Molar Mass of KAP)
(Volume of NaOH used/1000ml/1L)
Using Group Nines data for vial # 401:
NNaOH = (0.3771g/204.22 g/mol) = 0.1108 N
(16.66 ml/1000ml/1L)

Finding the unknown KAP weight:

Rearrange the formula above to solve for grams of KAP.
Grams of KAP= (NNaOH)(Molar Mass of KAP)(Volume of NaOH used/1000 ml/1L)
Grams of KAP= (0.111)(204.22 g/mol)(16.60 ml/1000ml/1L)= 0.3763 g

pKa determination:
pKa can be determined by using titration data and plugging it into the Henderson-Hasselbach
equation. pH = pKa + log([A-]/[HA])
At the mid point, the concentration of acid is equal to the concentration of conjugate base, and
therefore, pH=pKa at the midpoint.
Figure 1 shows that 16.70 ml of NaOH was used to get to the equivalence point, so only 8.35 ml
was used to get to the midpoint. Looking at table 2, the starting volume was 20.65 ml. Adding
8.35 ml brings the volume to 29.00 ml and the corresponding pH is 5.07. Since pH=pKa at the
midpoint, the pKa for KAP is also 5.07.

%Acidity:
%Acidity = N2 x V2 x E1
(10 x V1)
Using the average class data for the titration of tartaric acid in grape juice:
N2 is the Normality of the NaOH used = 0.1102 eq/mol
V2 is how much NaOH was used to get to the equivalence point = 22.17 ml
E2 is the equivalence weight of the acid. In this case, tartaric acid is used.
(150.09 g/mol) / (2 eq/mol) = 75.02 g/eq
V1 is the volume of grape juice used = 25.0 ml
%Acidity = 0.1102 N x 22.17 ml x 75.02 g/eq = 0.733%
(10 x 25.0 ml)

Bx/Titratable acidity:
To find the value for Bx/Titratable acidity, divide the value for Brix by the value for %acidity.
Using the average class data for mozzarella cheese:
Bx= 1.1
%acidity= 0.429%
1.1 Bx/0.429 = 2.56

Calculating the Normality of acetic acid:

N1V1=N2V2
N1 is the normality of the NaOH used = 0.1 eq/L NaOH
V1 is how much NaOH was used to get to the equivalence point = 0.01962 L
N2 is the normality of acetic acid = ?
V2 is 0.050L of acetic acid.
N2= 0.1N x 0.01962L = 0.03924 N acetic acid.
0.050 L
VI. Results/Discussion
In lab 2, the fifth vial of KAP had an unknown weight. Through calculation, group nines
unknown vial (440) was calculated to be 0.3763 g, but the actual weight of the KAP in the
vial was 0.3741 g. This is a %error of 0.59%. This is a small error, so small experimental
mistakes such as titrating slightly past the endpoint or slightly misreading the volume in the
burette could have caused this error.
For lab 3, the % acidity and Brix were measured for apple juice, orange juice, grape juice,
cheddar and mozzarella. Brix is a measure of sugar content and doesnt necessarily indicate
how sweet something will be. For example, in the sensory evaluation, grape juice was rated
the preferred juice but was not rated the sweetest, despite the fact that it had the largest Brix
value and highest % sugar on the label. Although it was a sensory evaluation, the %acidity
did relate to perceived acidity or sourness. The orange juice was rated the most acidic and
actually did have the highest %acidity, then grape juice, then apple juice. For the cheeses,
cheddar had a larger %acidity and a higher Brix value and was rated to be the most acidic.
Mozzarella was rated to be sweeter despite having a lower Brix value.
When comparing the titration curve of grape juice (Figure 2) with the titration curve of
mozzarella (Figure 3) it can be noted that the equivalence point in the mozzarella solution can
be spotted much more easily than the equivalence point of the grape juice solution. This
could be because fewer data points were recorded for the cheese titration as less NaOH was
required to find the equivalence point than was needed for the grape juice titration. Moreover,
it was recommended to wait ten minutes for the pH of the cheese solution to reach ~5, but
after almost twenty minutes, the pH would not go below ~6.3. Less NaOH was required for
the cheese titration because the pH of the solution was already close to the equivalence point,
whereas the pH for the juice titration started at 3.42.
Another factor affecting pH readings was the efficiency of the stir bar to make the
solution more uniform so that the pH meter could get more accurate readings. During the
cheese titration, group nine waited for the pH to drop for about twenty minutes, after starting
the titration, the pH meter gave readings of both raised and lowered pH, attributing to the
negative value data point for group nines mozzarella titration.
Looking at the class data in Table 6, there is about a 5 ml range of variation between
groups for each individual group to reach the equivalence points. As mentioned before, the
variation could be a product of the efficiency of the stir bar to make the pH of the solution
easier to read for the pH meter. A small amount of error could also come from different
perceptions of what volume the burette actually reads. There is also variation in pH reported
from group to group for each of the individual juices. For example, most of the orange juice
groups reported an equivalence pH of ~7, but one group reported 9.41. The same story holds
true for the cheeses. There is a variation in the amount of NaOH each group used to reach the
equivalence point and there is variation in what pH was recorded at the equivalence point.
While the same errors that occurred with the juices may also apply to the cheese, it is also
possible that there was a loss when transferring the cheese solution from one piece of
glassware to the next.

VII. Conclusion
 This experiment showed the importance of standardizing solutions and how the Brix/Acid
ratio is important for the food industry and finding optimal customer satisfaction. Brix
measures the sugar content of the food but not the sweetness, so it is important to understand
how the Brix/Acid ratio relates to the customer satisfaction of your product. Without
standardizing a solution and knowing the accurate concentration you cannot find an accurate
Brix/Acid ratio.

VIII. Questions
Lab 2:
1. Why would CO2 contamination be a problem with standardized base solutions?
Carbon dioxide contamination within a standardized base solution would deviate the
actual concentration of the solution from the calculated concentration. CO 2 can react with
the NaOH to change the concentration.
2. What is the pH of the sample when the phenolphthalein indicator changes color? Explain
why this pH provides a good estimate for endpoint of a titration of a weak acid by a
strong base.
For a weak acid and strong base, the equivalence pH is usually above 7. Phenolpthalein is
a good indicator dye to use for the titration of a weak acid with a strong base because it
begins to change color at a pH above 7. Selecting an appropriate indicator is important
because although it does not show the equivalence point, it does indicate a good place to
stop the titration.
3. Plot the titration curve and first derivative of acetic acid and phosphoric acid.
Figure 4 shows the titration curve for acetic acid and Figure 5 shows the titration curve of
phosphoric acid. The equivalence point for the monoprotic acetic acid is 19.6 ml. The
first equivalence point for the polyprotic phosphoric acid is 31.5 ml and the second
equivalence point is at 48.0 ml.

Lab 3:

1. Do the titratable acidity and Brix/Acid ratio you have examined fall within the accepted
limits?
Fruit Experimental Table 2-3 Within Experimental Table 2-3 Within
%Acid % acid
Range? Brix Brix Range?
Orange 0.762 0.68-1.2 YES 12 9-14 YES
 Apple 0.413 0.27-1.02 YES 12.5 9.1- YES
13.5
Grape 0.733 0.84-1.16 NO 15.5 13.3-14.4 NO

2. Do you expect the pH and titratable acidity to be related or not? Give reasons for your
answer.
There is no direct relationship. A lower pH does not mean a larger titratable acidity. pH
measures hydrogen ion concentration within the solution and titratable acidity represents
how much base is required to neutralize the solution.