YACHAY TECH

School of Chemical Sciences and Engineering

Practice #4: DETERMINATION OF PHOSPORIC

ACID IN GASEOUS BEVERAGES BY
POTENCIOMETRY
Chemical Analysis II Laboratory - Report

Michelle Beatriz Chicaiza Lema |José E.Andino, Jorge Castro, Johana Gómez

November 23, 2017|November 30, 2017

OBJECTIVES:

 Analysis of a base acid-base system by potentiometric titrations.

 Evaluation of the equivalence point using the direct a first derivative
 Quantitatively determine phosphorus and phosphoric acid concentration, in soft
drinks beverages

INTRODUCTION:
The advent of instrumental analysis techniques allowed the incorporation of new forms of
equivalent point detection, which are more accurate than those using indicator substances.
The change color of indicator will determine the end point of the valuation. The objective of
a potentiometric measurement is to obtain information about the composition of a solution
by determining the potential. The potential is measured with Potentiometer. Types of
potentiometric measurements: potentiometric titrations and direct potentiometric.

Direct potentiometric: two electrodes, indicator and reference, are introduced in a solution
to be analyzed and whose activity is calculated by a reading of this solution potential.
Potentiometric Titrations: this technique consist of an assessment based on measurements
of potentials of a suitable indicator electrode depending on the volume of added titration
agent. The value of the potential measured by the indicator electrode varies throughout the
titration, with the equivalence point being reached by the appearance of a singular point on
the curve: potential vs. quantity of added reagent. The detection of this point, can be
established as:

 Direct method: it consists of plotting the potential data according to the volume of
reagent.
 First derivative: implies calculating the change of potential per unit volume of titrant
(ΔE/ΔV). The graph of these data as a function of the average volume V produces a curve
with a maximum corresponding to the inflection point. If the curve is symmetric, the
maximum point of the slope coincides with that of equivalence. Asymmetric curves give
a small titration error if the maximum point is taken as the end.

Intensive efforts are being made as the evaluation of the erosive potential adverse side effects
due the ingestion of high volume of phosphoric acid present in beverages, which might
extract part of calcium necessary for the body. The concentration of H3PO4 can be
determined by titration with a normal base, such as KOH or NaOH (0.01 or 0.02N). It is
advisable to degas these drinks.

MATERIALS: REAGENTS:

 Analytical balance  Monobasic potassium phosphate

 Hot plate, spatula (100ml, 0.02N)
 Magnetic stirring system.  Sodium hydroxide (250ml, 0.02N),
 pH meter 250ml
 burettes,  bottles of commercial drinks
 volumetric flasks (Example: Pepsi-Cola®, Coca-

 Erlenmeyer Cola®)

 Pipettes, thermometer
PROCEDURE:
RESULTS

For the neutralization of the NaOH, 𝐶1 and 𝑉1 are the concentration and volume of the
𝐾𝐻2𝑃𝑂4 respectively, 𝐶2 and 𝑉2 are the initial concentration and volume of NaOH.

𝐶1 𝑉1 = 𝐶2 𝑉2

0,02𝑀 ∗ 25𝑚𝑙 = 𝐶2 ∗ 15𝑚𝑙

𝐶2 = 0,03𝑀

Now, the concentration of NaOH was known, the concentration of phosphoric acid can be
determined by using the same relationship:

NaOH (C2), H3PO4 (C3) (unknown)

𝐶3 𝑉3 = 𝐶2 𝑉2

The volume at which the equivalence point is reached need to be obtained from the titration
graph. The data of the titration are plotted on figure 1, and show two end point before the
saturation of the solution. The phosphoric acid is polyprotic and there should be three
different equivalence points on the graph due to the three protons oh the phosphoric acid
which can be dissociated. However, the third one is almost impossible to find due to the
saturation of the solution. Probably, more additions of volume had allowed to see the third
equivalence point.

Figure 1: Titration of phosphoric acid

To analyze the ends points can be measured by direct method or the first derivative.
In this case we can analyze this end point using the direct derivative. It consists of
plotting the potential data according to the volume of reagent. The inflection point in
the ascending part of the curve is estimated visually and is taken as the end point. The
end point occurs in a region near to 6.5 mL of reagent and at pH ~4.4. It means the
point at which a 1: 1 equilibrium will occur between the titrant and the acid in the
sample, in the figure 2.

Figure 2 End point direct derivative OF PEPSI SODA

In other hand, the graph of first derivative method of pH as a function of the average volume V
produces a curve with a maximum corresponding to the inflection point. If the curve is
symmetric, the maximum point of the slope coincides with that of equivalence. A maximum
value at a volume of 6 mL or pH=3,88.

Figure 3 Determination of equivalence point OF PEPSI SODA

In origin program the two equivalence points are determined. Where X is the volume and Y
is the derivative of pH to obtain a equivalence point.

Figure 4 fist pick of the end point of the titration

Figure 5 second pick of the end point of the titration

Two equivalence points can be clearly seen in the titration curve for pure phosphoric acid.
They correspond to the following dissociation equilibria:

H3PO4 + Na+ + OH- —> H2PO4- + Na+ + H2O

H2PO4- + Na+ + OH- —> HPO42- + Na+ + H2O

The second equivalence point is only weakly shown in the titration curve for the soft drink.
This is because, in addition to phosphoric acid, further acids are present here which also take
part in the titration with sodium hydroxide solution and exert a buffering effect in the region
of the second equivalence point. A knowledge of the first equivalence point suffices for the
calculation of the quantity of phosphoric acid contained in the soft drink.

The calculation of the phosphoric acid concentration, only the first equivalence point (from
the first derivative) is taken to make the calculations.

NaOH (C2), H3PO4 (C3) (unknown)

𝐶3 𝑉3 = 𝐶2 𝑉2

𝐶3 ∗ 25𝑚𝑙 = 0,03𝑀 ∗ 6𝑚𝑙

𝐶3 = 0,0072𝑀

In this practice is important to recognize the possible errors like when we try to determine
the equivalence point using phenolphthalein to do the neutralization of NaOH with 𝐾𝐻2𝑃𝑂4.
This error can cause the confusion on the calculus on the concentration of the sodium
hydroxide and later calculations for the concentration of phosphoric acid. Also, the pH meter
it could not have been properly calibrated. Finally, the errors on visualizing the quantity of
NaOH added when titrating, because we try to put every milliliter to measure the pH meter.

CONCLUSIONS:

 Potentiometric is a technique of multiple applications in the main areas of analysis.

Also, it is considered an easy, fast, versatile, very economical method and a simple
technique to perform.
  The phosphoric acid concentration is higher than other acids present in a soft drink.
This concentration can be determined by acid-base titration. In this case we use NaOH
like a base.
 In the graph of pH vs volume of the titrant is very clear the two equivalence points.
The phosphoric acid is polyprotic and the third equivalent point is not observed due
to the saturation of the system.
 In the graph the two equivalence points are far It can explain due to in the large
difference between their dissociation constants.
 Soft drinks contain carbonic acid (gas from the soda) and phosphoric acid and other
components. This is why in the first step of the protocol we decarbonized the drink.
It allows to avoid the secondary reactions in the experimental procedure.
 To obtain an exact data of the equivalence point we can use the direct method or the
first derivative method. The second method allows us to have more accurate data to
calculate the concentration of phosphoric acid.
 The concentration of phosphoric acid present in the Pepsi is0,0072𝑀. Although the
concentration is not very high we should consider their daily intake would cause
diseases. Because it can be related to the loss of calcium in the bones and future
complications in health.

REFERENCES:
Díaz, A. (2017). Experiment 5: POTENTIOMETRY AND VOLTAMMETRY. [Pdf].

658-730). Chemistry. Belmont: Mary Finch.