FACULTY OF RESOURCE SCIENCE AND TECHNOLOGY

DEPARTMENT OF CHEMISTRY

STK1211- PRACTICAL ANALYTICAL CHEMISTRY

PRACTICAL 4

REDOX TITRATION- ASCORBIC ACID

DATE OF EXPERIMENT : 16th June 2020

GROUP MEMBERS AND MATRIC :  Nur Syahirah binti Mohd Sahril

NUMBERS (71045)- Leader of introduction,
apparatus and conclusion section

 Putri Iman Basysyasy binti Ariffin

(71348)- Leader of methods section

 Farah Adha binti Rohani (69671)-

Leader of discussion section

 Xelarine Desslor Anak Behal (71987)-

Leader of results and post-lab questions

LAB FACILITATOR : Dr. Showkat Ahmad

REPORT DUE DATE : 22nd June 2020

INTRODUCTION

The human body does not synthesize vitamins; therefore the vitamin that we need for

catalyzing specific biochemical reactions are gained only from the food that we can eat. We

are generally aware that vitamin C can be obtained from citrus fruits, but it can also be

obtained from a variety of fresh fruits and vegetables. However, storage and processing

causes vegetables to lose a part of their vitamin C content. Cooking leaches the water-soluble

vitamin C from the vegetables; in addition, the high temperatures accelerate its degradation

by air oxidation. Therefore to maximize the intake of vitamin C, only fresh fruits or

vegetables should be consumed.

Vitamin C, also called ascorbic acid, is one of the more abundant and easily obtained

vitamins in nature. It is a colourless, water-soluble acid that, in addition to its acidic

properties, is a powerful biochemical reducing agent, meaning it readily undergoes oxidation,

even from the oxygen of the air.

Even though ascorbic acid is an acid, its reducing properties are used in this experiment to

analyze its concentration in various samples. There are many other acids presents in foods

that would interfere with an acid analysis and not permit us to selectively determine the

ascorbic acid content. The equation for the oxidation of ascorbic acid is

C6H8O6(aq) + H2O(l) C6H8O7(aq) + 2H+ +2e-

In analysing for ascorbic acid, the sample is dissolved in water and treated with a measured

excess of iodate ion, IO3- , a strong oxidizing agent; in an acidic solution containing an excess

of iodide ion, I-, IO3-, converts to I3- (red-brown),a milder oxidizing agent ( Equation 1).

IO3- (aq) + 8I- (aq) + 6H+ (aq) 3I3- (aq) + 3H2O (l) ….. (Equation 1)

Some of the I3- then oxidizes the ascorbic acid (equation 2) present in the sample.
I3- (aq) + C6H8O6 (aq) + H2O(l) C6H8O7(aq) + 3I-(aq) + S4O62- (aq) …..(Equation 2)

The remaining I3- (the excess, ‘xs’) is titrated with a standard thiosulfate, S2O32-, solution,

producing the colourless I- and S4O62- ions. (Equation 3) .

(xs) I3- (aq)+ 2S2O32-( aq) 3I-(aq) + S4O62- (aq)..... (Equation 3)

Therefore the difference between the I3- generated initially and that which is titrated in excess

is a measure of the ascorbic acid content of the sample. The stoichiometric point is detected

using starch as an indicator. Just prior to the disappearance of the red-brown I3- in the

titration, starch solution is added; this forms the deep-blue ion, [I3.starch]-. The addition of

the S2O32- titrant is continued until the [I3.starch]- has been reduced to I- , the solution appears

colourless at the end point.

In this experiment, we are required to prepare and standardize a Na2S2O3 solution using solid

KIO3 as a primary standard. The standard solution is then used to analyze for ascorbic acid in

the sample provided.

In this experiment, the results were calculated using the titration formula. If the titrant and

analyte have a 1:1 mole ratio, the formula is molarity (M) of the acid x volume (V) of the

acid = molarity (M) and base × volume (V) of the base.

METHODOLOGY

Part A: A Primary Standard 0.01M Potassium Iodate, KIO3, Solution

1. About 0.5g (±0.001 g) of KIO3 was measured on weighing paper, the solid was then

transferred to a 250mL volumetric flask, it was dissolved and diluted to the mark.

2. The molar concentration of the KIO3 solution was calculated and recorded.

Part B: A Standard 0.1 M Na2S2O3 Solution

1. About 6g (±0.001 g) of Na2S2O3.5H2O was dissolved with distilled water and diluted

to 250mL. The solution then stirred until the salt dissolved.

2. A clean 50mL burette was prepared properly and filled with the Na2S2O3 solution, tip

of the air bubble was drained, and the initial volume (±0.02mL) was recorded.

3. 25 mL of the standard KIO3 solution was pipetted into a 250 mL Erlenmeyer flask

and about 1g (±0.01 g) of solid KI was added. About 5 mL of 0.5M H2SO4 and 0.1 g

of NaHCO3 was added.

4. The Na2S2O3 solution was titrated immediately. 2 mL of starch solution was added

when the red-brown solution changes to pale yellow colour. The solution was

constantly stirred and titrated slowly until the blue colour disappears.

5. Before the endpoint point, the procedure was repeated twice by rapidly adding the

Na2S2O3 solution until 1 mL.

6. The molar concentration of the Na2S2O3 solution was calculated and recorded.
Part C: Sample Preparation

(a) Vitamin C tablet

1. To determine the approximate mass of vitamin C in each tablet, read the label. The

fraction of the total mass of a tablet that corresponds to 100 mg of ascorbic acid was

measured (±0.001 g).

2. Dissolved it in a 250 mL Erlenmeyer flask with 40 mL of 0.5 M H2SO4. About 0.5 g

NaHCO3 was added.

3. Immediately proceed to part D.

(b) Fresh fruit sample

1. About 120 mL of freshly squeezed juice was filtered through several layers of muslin.

2. The mass (±0.01 g) of a clean, dry 250 mL Erlenmeyer flask was measured. About

100 mL of the filtered juice was added and the mass was determined again.

3. 40 mL of 0.5M H2SO4 and 0.5 g NaHCO3 was added, part D was proceed

immediately.
Part D: Vitamin C analysis

1. 25.0 mL of the standard KIO3 solution (from part A) was pipetted into the sample

solution from part C and 1 g of KI was added.

2. About 5 mL of 0.5 M H2SO4 and 0.1 g NaHCO3 was added. The excess I3- was

titrated in the sample with the standard Na2S2O3 solution as described in Part B.4. The

final burette reading was recorded (±0.02 mL).

3. In order to complete the three trials, the analysis was repeated twice.

4. The percent of the ascorbic acid in the sample was calculated.

APPARATUS

 250 ml volumetric flask

 250-ml Erlenmeyer flask

 50-ml burette with stand

 Glass stirring rod

 Beaker

 Muslin

 Filter funnel

REAGENTS

 Potassium iodate, KIO3

 Sodium thiosulfate, Na2S2O3

 Potassium iodide, KI

 Starch solution

 0.5 M H2SO4
  Sodium hydrogen carbonate, NaHCO3

 Vitamin C tablets

 Fresh fruit juices

RESULTS

Part A: A Primary Standard 0.01 M Potassium Iodate, KIO3, Solution

Mass of KIO3 (g) 0.50

Moles of KIO3 (mol) 2.336 × 10-3

Molarity of standard KIO3 solution (M) 9.344 × 10-3

Table 1: A primary standard 0.01 M Potassium Iodate, KIO3 solution

Part B: A Standard 0.1 M Na2S2O3 Solution

Particular Trial 1 Trial 2 Trial 3

Volume of KIO3 solution (mL) 25.00 25.00 25.00

Moles of KIO3 titrated (mol) 2.336 × 10-3 2.336 × 10-3 2.336 × 10-3

Moles of I3- generated (mol) 7.008 × 10-3 7.008 × 10-3 7.008 × 10-3

Volume of Na2S2O3 added (mL) 14.40 14.80 14.50

Moles of Na2S2O3 added (mol) 0.0379 0.0379 0.0379

 Molarity of Na2S2O3 solution (M) 0.016 0.016 0.016

Average molarity of Na2S2O3 0.016

solution (M)

Table 2: A Standard 0.1 M Na2S2O3 Solution

Part C & D: Sample Preparation & Vitamin C analysis

Sample name: Vitamin C Tablet

Particular Trial 1 Trial 2 Trial 3

Mass of sample (g) 0.31 0.32 0.30

Volume of KIO3 solution (mL) 25.00 25.00 25.00

Moles of KIO3 titrated (mol) 2.336 × 10-3 2.336 × 10-3 2.336 × 10-3

Moles of I3- generated (mol) 7.008 × 10-3 7.008 × 10-3 7.008 × 10-3

Volume of Na2S2O3 added (mL) 2.90 3.10 3.40

Moles of Na2S2O3 added (mol) 0.0379 0.0379 0.0379

Moles of I3- titrated with S2O32- 7.008 × 10-3 7.008 × 10-3 7.008 × 10-3
(mol)

Moles of I3- reduced by C6H8O6 0.021 0.021 0.021

(mol)

Moles of C6H8O6 in sample (mol) 2.044 × 10-4 2.254 × 10-4 2.317 × 10-4
 Mass of C6H8O6 in sample (g) 0.036 0.0397 0.0408

Percent of C6H8O6 in sample (%) 11.61 12.41 13.6

Average percent of C6H8O6 in 12.54

sample (%)

Table 3: Sample Preparation & Vitamin C analysis of vitamin C tablet

Part C & D: Sample Preparation & Vitamin C analysis

Sample name: Fresh Fruit sample

Particular Trial 1 Trial 2 Trial 3

Volume of sample (mL) 5.00 5.00 5.00

Volume of KIO3 solution (mL) 25.00 25.00 25.00

Moles of KIO3 titrated (mol) 2.336 × 10-3 2.336 × 10-3 2.336 × 10-3

Moles of I3- generated (mol) 7.008 × 10-3 7.008 × 10-3 7.008 × 10-3

Volume of Na2S2O3 added (mL) 2.20 2.50 2.40

Moles of Na2S2O3 added (mol) 0.0379 0.0379 0.0379

Moles of I3- titrated with S2O32- 7.008 × 10-3 7.008 × 10-3 7.008 × 10-3
(mol)

Moles of I3- reduced by C6H8O6 0.021 0.021 0.021

(mol)
 Moles of C6H8O6 in sample (mol) 2.648 × 10-3 3.009 × 10-3 2.889 × 10-3

Mass of C6H8O6 in sample (g) 0.4664 0.53 0.5088

Percent of C6H8O6 in sample (%) 8.8 10 9.6

Average percent of C6H8O6 in 9.47

sample (%)

Table 4: Sample Preparation & Vitamin C analysis of fresh fruit sample

CALCULATIONS

Part A: A Primary Standard 0.01 M Potassium Iodate, KIO3, Solution

Part B: A Standard 0.1 M Na2S2O3 Solution
Part C & D: Sample Preparation & Vitamin C analysis

Sample name: Vitamin C Tablet

Part C & D: Sample Preparation & Vitamin C analysis
Sample name: Fresh Fruit sample
DISCUSSION

To study and apply the concept of redox reaction we had a performed an experiment which

follow this concept which is the iodometric titration. We had started our experiment in part A

by preparing a primary standard 0.01M potassium iodate, KIO3 solution by weighing the

mass KIO3 on weighing paper then transfer and dilute it. Weighing paper is used to improve

the measurement accuracy by preventing the solid from being blocked because it has a

slippery or waxy feel. Then we had calculated and recorded the molar concentration of the

KIO3 solution with the given molecular weight of KIO3 is 214.001 g/mol. Therefore the

molar concentration of KIO3 is 9.344 x 10 -3

In part B, we had started the titration by using standard 0.1 M Na2S2O3 solution. We had

diluted the salt and stirred until it dissolved in distilled water. After that, we had prepared the

burette and filled it with Na2S2O3 solution and recorder the initial volume of the Na2S2O3

solution. Then, we had pipette about 25ml of standard KIO3 and added about 1 g of solid KI

into the Erlenmeyer flask. KI is added to help solubilize the free iodine, which is quite

insoluble in pure water under normal conditions. 5ml of 0.5 H2SO4 and 0.1 g of NaHCO3 was

added to the Erlenmeyer flask to produce CO2 which minimizing the possibility of the air

oxidation of I- ions. We had added 2ml of starch which is act as the indicator. When titration

is reach the endpoint the blue colour of the starch will change into colourless solution. This is

because all of the I3- ions is reduce into I- ions. Starch is a viable indicator in

the titration process because it turns deep dark blue when iodine is present in a solution.

Therefore, we had determined the final volume of the Na2S2O3 and calculated the volume of

Na2S2O3 added. From this, we can calculated the moles, molarity and the average molarity of

the Na2S2O3 solution which is 0.016 M.

In part C, we had prepared two samples for sample preparation which are vitamin C tablet

and fresh fruit sample. We had prepared vitamin C tablet by determining the approximate

mass of the vitamin C and measuring the fraction of the total mass of the tablet. After that, we

had dissolved it into Erlenmeyer flask and added about 0.5g of NaHCO3 before we proceed

immediately to part D.

For fresh fruit sample we had filtered about 120ml of juice through several layers of muslin.

Then, we had pipetted 5ml of concentrated juice and diluted it. We had determined the mass

of filtered juice by measuring the mass of empty Erlenmeyer flask and the mass of

Erlenmeyer flask with the 50ml of filtered juice. After that, we had added 20ml of 0.5 M

H2SO4 and 0.25g NaHCO3 and immediately proceed to part D.

In part D, we had pipetted the standard KIO3 solution which is from the part A into the

sample solution from part C which are vitamin C tablet and fresh fruit sample. Then we had

added about 1g of KI. After that, we had added about 2ml of starch solution as an the

indicator and began the titration. We had titrated the excess I3- which is in the sample with

standard Na2S2O3 solution. Then, we had red, recorded the final reading and repeated the

analysis twice. From this, we had calculated the percent of ascorbic acid in vitamin C tablet

which are 11.61 %, 12.41 %, 13.6 % and the average percent of the ascorbic acid is 12.54 %.

We had performed this part twice for vitamin C tablet first and then continue for fresh fruit

sample. The percent of ascorbic acid in fresh fruit samples are 8.8 %, 10.0 %, 9.6 % and the

average percent of the ascorbic acid in fresh fruit samples is 9.47 %.

CONCLUSION

After the experiment, we have learnt the method of redox titration. This is indicated by the sample of

ascorbic acid from the fresh fruits. From part A of the experiment, we calculated the molarity of

standard KIO3 solution which turns out to be 9.344× 10-3. For part B, in preparation of a standard 0.1

M NA2S2O3 solution, the average molarity is 0.016 M. For part C&D, the average percent of

C6H8O6 in the sample of vitamin C tablet is 12.54%. The average percent of C 6H8O6 in the

sample of fresh fruit sample is 9.47%.

QUESTIONS

1. Explain why cooked fruits and vegetables have lower vitamin C content than fresh
fruits and vegetables.
 Because the high temperatures during cooking results in a loss of vitamin
C content over time.

2. If the blue color does not appear when the starch solution is added during the titration,
should you continue titrating or discard the sample? Explain.
 The sample should be discarded as this could be an indication of a high
concentration of I2 in the solution, causing the blue color to not appear.

3. 177.42 mL of a fruit juice contains 32% of the recommended daily allowance of

vitamin C (equal to 60 mg). How many mL of the fruit juice will provide 100% of the
recommended daily allowance?

𝒙 𝟏𝟎𝟎%
=
𝟏𝟕𝟕. 𝟒𝟐 𝟑𝟐%

𝟏𝟎𝟎%
𝒙= × 𝟏𝟕𝟕. 𝟒𝟐 𝒎𝑳
𝟑𝟐%

𝒙 = 𝟓𝟓𝟒. 𝟒𝟒 𝒎𝑳
REFERENCE

Tan, Y.T., Loh, W.L., Kathirasan Muniandy. (2010).Ace ahead chemistry volume

1.Selangor,

Malaysia : Oxford Fajar.

Christian,G.D., Purnendu K.,Dasgupta., Schug,K.A.(2013).Seventh edition analytical

chemistry.United States,US :Wiley.

Kotz, J. C., Treichel, P. M., Townsend, J. R.,Treichel, D. A. (2015). Stoichiometry:

Quantitative Information about Chemical Reactions. In Chemistry and Chemical

Reactivity, Instructor's Edition (pp. 139-149). Stamford, CT: Cengage Learning