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I.
Introduction
Titration is one of the most accurate and convenient analytical procedures in studying acidbase reactions quantitatively (Chang 2009). This procedure can also be applied to determine the
concentration of citric acids (H3C6H5O7) in fruits and fruit juices. Titration allows us to compare the
concentrations of different commercial fruit juices.
Titration is a type of chemical comparison. A solution of accurately known concentration,
called a standard solution, is gradually added to another solution of unknown concentration, until
the completion of the reaction of the two solutions (Chang 2009). The completion of the reaction is
called the equivalence point, signalled by chemical indicators (T. Brown et al. 2012). The amount of
the standard solution, or the titrant, needed to achieve chemical equivalence is compared to the
amount of the solution with the unknown concentration, or the analyte.
Strong acid or base titrants are generally used to achieve the highest possible equilibrium
constant for the titration reaction. Sodium hydroxide, a strong base, is one of the frequently used
bases as titrant in titration. On the other hand, solid sodium hydroxide in its pure form, therefore, a
solution of sodium hydroxide must be standardized first before it can be used in analytical
computations. The standardization of the sodium hydroxide solution can be done by titrating it
against an acid solution of accurately known concentration. A monoprotic acid called potassium
acid phthalate (KHC8H4O4), a white, soluble solid, is frequently used. It reacts with a ratio 1:1 with
NaOH in the standard solution as shown in Equation 1.1 (Chang 2009).
Equation 1.1
Indicators are substances that have particularly different colors when in acidic and basic
media. An example is phenolphthalein, which is colorless in acidic and neutral solutions but reddish
pink in basic solutions. When the reaction reaches the equivalence point, the potassium acid
phthalate will be neutralized by the added NaOH, and the solution is still colorless. However, if a
drop of NaOH solution is added, the solution will immediately turn pink because the solution is
already basic (Chang 2009). A list of other possible indicators can be found in Table 1.1.
In Acid
Red
Yellow
Orange
Red
Yellow
Yellow
Yellow
Colorless
In Base
Yellow
Bluish purple
Yellow
Yellow
Red
Blue
Red
Reddish pink
pH range
1.2-2.8
3.0-4.6
3.1-4.4
4.2-6.3
4.8-6.4
6.0-7.6
7.2-8.8
8.3-10.0
The calculated concentration of the titrant can now be used in determining the
concentration of the citric acid. The equation for the reaction between citric acid and NaOH is
shown in Equation 1.2.
H 3 C 6 H 5 O7 ( aq ) +3 NaOH ( aq ) Na C6 H 5 O7 ( aq ) +3 H 2 O(l)
Equation 1.2
Molarity and normality are the most commonly used units in describing the concentration of
solutions in titrimetry (Snelling 2012). Molarity presents the number of moles of reagent contained
in one liter of solution while normality gives the number of equivalents of reagents in the same
volume.
II.
Materials
A. Reagents
NaOH pellets
0.150 g of potassium acid phthalate
phenolpthalein
B. Apparatus and Equipment
250-mL beaker
iron stand
50-mL buret
stirring rod
10-mL pipet
buret holder
III.
Procedure
A. Preparation of the NaOH solution
In the experiment, 0.05 M of NaOH solution must be prepared to be used as the titrant.
Given the equation for molarity in Equation 1.3, an equation to determine the mass of NaOH pellets
to be used can be derived.
Equation 1.3
Figure 1.3. Addition phenolphthalein (indicator) to the analyte with white background.
C. 1
Five milliliters of the first juice sample (Apple Juice) was transferred to two 200-mL
Erlenmeyer flasks. Twenty millilitres of distilled water was used to dilute each sample. Two to three
drops of phenolphthalein was added to both Fruit Juice A samples. Each sample was titrated at the
same time using the sodium hydroxide (NaOH) solutions prepared earlier.
C. 2
Five milliliters of the second juice sample (Fruit Juice B) was transferred to two 200-mL
Erlenmeyer flasks. Twenty millilitres of distilled water was used to dilute each sample. Two to three
drops of phenolphthalein was added to both Fruit Juice B samples. Each sample was titrated at the
same time using the sodium hydroxide (NaOH) solutions in the burets.
IV.
Table 2.
84.54
85.04
0.50
Trial I
0.150
14.50
0.00
14.50
0.0507
Trial II
0.150
12.70
0.00
12.70
0.0578
0.05425
Trial I
5.00
18.30
14.50
3.80
Trial II
5.00
16.10
12.70
3.40
Trial I
5.00
24.30
18.40
5.90
Trial II
5.00
21.70
16.10
5.60
V.
Apple Juice
0.0130
1.25
0.200
Pineapple Juice
0.0208
1.00
0.400
Discussion
A. Analysis of the Results
The experiment involves the titration of two fruit juice samples. Naturally occurring citric
acid in fruit juices is a weak acid, thus, it needs to react with a strong base to produce a
neutralization reaction. Therefore, we can categorize the experiment as a Weak Acid-Strong Base
titration. The concentration of the fruit juice samples can be determined through titration using the
strong base NaOH as a titrant.
Although the concentration of NaOH solution is known, standardization was still done. In a
pre-weighed 250-mL beaker, 0.50 grams of NaOH, previously calculated, was weighed and was
dissolved using 10 mL of water. The solution was then stirred and cooled with tap water. Cooling
was done to ensure that the reaction between the NaOH and H 2O is completed, since increase in
temperature in the solution shows that there are still ongoing reactions between the NaOH
molecules and water molecules. Afterwards, the NaOH solution was quantitatively transferred to a
100-mL volumetric flask filled with 50 mL of distilled water. Quantitatively transfer means every
molecule of the NaOH solution must be transferred. This was done by washing the beaker with
water and transferring the liquid to the volumetric flask. The volumetric flask was filled with water
up to the 100-mL mark. The two burets must be cleaned before transferring the NaOH solution. In
cleaning the buret, it must be filled with distilled water and then drained afterwards. No drops of
water should be found adhering to the sides of the buret, otherwise, the buret must be cleaned
again.
In the preparation of the analyte, 0.150 grams of potassium acid phthalate was weighed in
two 200-mL Erlenmeyer flasks. Afterwards, the solid potassium acid phthalate was dissolved with
50 mL distilled water. Potassium acid phthalate was used because it exhibits the characteristics of a
good primary standard. A good primary standard has atmospheric stability, has a modest cost, has
reasonable solubility in titration medium, and has reasonable large molar mass for minimized
relative error associated with weighing the standard. It must also be available in highly pure form
and does not have hydrate water. Two to three drops of phenolphthalein must be added to the
potassium acid phthalate. Phenolphthalein is generally used as indicator in acid-base titrations. In
Table 1.1, the pH range of phenolphthalein is 8.3-10.0, meaning it will change color when the pH of
the solution reaches 8.3-10.0 or in basic medium. This also means that when a drop of the base is
added to the acid and base reaction in equivalence point, there will be a color change of
phenolphthalein, indicating that the solution is slightly basic.
A white background is used while titrating to easily see the change in color in the solution.
The titrant was added gradually to the analyte. This is to ensure that the solution will not overrun.
Overrun is when the color of the solution turns reddish pink rather than faint pink, indicating that
solution is more basic. Half-drops are also used to carefully add titrant to the analyte. Using a wash
bottle, the drop of NaOH solution still adhered to the tip of the buret was flushed with distilled
water. Subtracting the initial reading of the buret from the final reading, the volume of NaOH
solution used can be calculated. The number of moles of the NaOH solution can be calculated by
getting first the number of moles of potassium acid phthalate that reacted with it. Dividing the
mass of potassium acid phthalate used (0.150 g) with its molar mass (204.22 gr/mol), a value of
7.35 x10-4 g can be calculated. Going back to the equation, the ratio of potassium acid phthalate to
NaOH is 1:1, meaning the number of moles of potassium acid phthalate is equal to the number of
moles of NaOH in the solution. With the number of moles of NaOH and the volume of the NaOH
calculated, the molarity of NaOH can now be solved. The calculated molarities of the two samples
are not the sameThe next step is to get the average molarity that will be used for further
calculations. Adding the two calculated molarities and dividing it by two, the value would be 0.0542
M.
The titration of the first juice sample (Fruit Juice A) and the second juice sample (Fruit Juice
B) is the same with the procedure in titrating the potassium acid phthalate.
B. Errors committed in the experiment and its effect in the results
Before the experiment, the group may have forgotten to wash the buret with distilled water
and the titrant, thus, causing an increase in the volume of measured NaOH used, meaning, lower
molarity of NaOH, lower number of moles of citric acid. Unwashed burets can affect the calculated
value in a titration experiment, like a decrease in the calculated molarity of citric acid.
reaction between the solutions, thus resulting to an erroneous result. These possible errors can
be avoided by doing carefully the prepared instructions.
VI.
A mole ratio of 3:1 can be found, meaning that there are 3 moles of NaOH solution reacting with 1 mole of
citric acid. This mole ration is then used to calculate for the number of moles of citric acid present in the pineapple
and apple juice. In this part of the experiment, two trials were also done with each kind of fruit juices. The
concentration of the fruit juices was determined through acid-base titration. With the definite volume of the titrant
and the average molarity of the standardized solution, it is now easy to calculate for the number of moles of Citric
Acid present in the fruit juices.
The numbers of moles of citric acid obtained in the apple juice are 2.06 x 10-4 mol. in 0.0137 M citric acid
in the first trial and 1.84 x 10-4 mol.in 0.0123 M citric acid in the second trial. Thus, the average
molarity of the apple juice is 0.0130 M. Next is the determination of the concentration of citric acid
in the pineapple juice, with a definite volume of NaOH used during the titration, average molarity of
NaOH and the balanced chemical equation, the number of moles obtained in the first trial is 1.07 x
10-4mol Citric Acid with the concentration of 0.0214 M and 1.01 x 10-4mol of citric acid with the
concentration of 0.0202 M in the second trial with an average molarity of 0.0208 M of pineapple
juice.
This information suggest that 0.624 g of citric acid of pineapple juice from the volume of the citric
acid assuming that the density of citric acid is 1g/mL constitutes 0.250% of citric acid is present in
250 mL of apple juice.
Calculations is also done with the 250 mL of pineapple juice which suggests that a given volume of
citric acid present in pineapple juice, 1.00 mL from 1.00 g assuming that 1g/ml is the density of
citric acid, constitutes 0.400% of citric acid present per 250 mL of pineapple juice or per pack.
This also reflects that the citric acid of pineapple juice is more concentrated than the citric acid of
apple juice. Therefore, citric acid of the pineapple juice constitutes lesser part in the 250 mL
solution than that of the citric acid of apple juice in 250 mL.
VII.
Sample Calculations
A. Mass of NaOH used
Molarity= no. of moles solute
volume of solution in liters
= mass/molar mass
volume of the solution in liters
Mass= (Molarity) (Volume of solution in Liters) (molar mass)
Given that the molar mass of NaOH is 40.00 g/mol:
Mass= (0.05 M) (0.250L) (40.00 g/mol)
= 0.50 g NaOH pellets to be used
Trial 2
0.0127 L
= 0.0578 M
E. Average Molarity of NaOH Solution
Average Molarity of NaOH Solution= Molaritytrial 1 + Molaritytrial2
2
= 0.0507 M +0.0578 M
2
= 0.05425 M
F.
Trial 2
Volume of NaOH= 3.40 mL
Average molarity of NaOH= 0.05425 M
= (M NaOH) (V NaOH)
= (0.05425 M) (0.00340 L)
=1.84 x 10-4 mol.
Trial 1
0.0137 M + 0.0123 M
2
= 0.0130 M
I.
=3.20 x 10 molNaOH
J.
Trial 1
Trial 2
0.0214 M + 0.0202 M
2
= 0.0208 M
M. Mass of Citric Acid per pack of Apple Juice and the percent Citric Acid
Mass of Citric Acid per pack Apple juice= (Molarity) (Volume) (molar mass)
= (0.0130 M) (0.250 L) (192.124 g/mol)
=0.624 g of Citric Acid per pack of Apple Juice
N. Mass of Citric Acid present in Pineapple juice and the percent Citric Acid
Mass of Citric Acid per pack Pineapple juice= (Molarity) (Volume) (molar mass)
= (0.0208 M) (0.250 L) (192.124 g/mol)
=1.00 g of Citric Acid per pack of Pineapple Juice
VIII.
References
Books:
Brown, Lemay, and et al. (2012). Chemistry: The Central Science, Twelfth Edition. Pearson Prentice Hall.
United State of America. pp. 714-718.
Chang, R. (2008). General Chemistry: The Essential Concepts, Fifth Edition. McGraw-Hill. 1221 Avenue
of the Americas, New York, NY 10020. pp. 120-123, 575-589.
Ebbing and Gammon. (2009). General Chemistry: Ninth Edition. Houghton Mifflin Company. United
States of America. pp. 682-689.
Mcmurry and Fay. (2003). Chemistry, Fourth Edition. Pearson. pps. 95-97.
Internet:
C.R. Snelling. Titration: Determining the Acidity of an Unknown Acid. Retrieved (October 4, 2012).
http://www2.volstate.edu/chem/1110/Titration.htm