Introductory Chemistry

SCHOOL OF SCIENCE AND HEALTH

A REDOX TITRATION TO DETERMINE

THE VITAMIN C CONTENT OF FOODS
AND SUPPLEMENTS

STUDENT NAME:

PRACTICAL SESSION:

DAY Start TIME PLACE

Introductory Chemistry –Determination of Vitamin C

DETERMINATION OF VITAMIN C

PRE-WORK
 Prepare your laboratory notebook for the experiment. See the vUWS site for
instructions on how to do this.
 Vitamin C. or ascorbic acid has the molecular formula C6H8O6. Whilst this
statement tells us the molar mass of vitamin C, it gives no indication of either
the usefulness of vitamin C or its reactivity. For this you need the structural
formula. In the course of this experiment we will be oxidizing L-ascorbic acid
to L-dehydroascorbic acid. Look up the structure of L-ascorbic acid and L-
dehydroascorbic acid. In your laboratory note book, write the redox half-
equation for the conversion of ascorbic acid to dehydroascorbic acid, showing
clearly the structures of both the organic compounds.
 Copy the results and data tables into your laboratory notebook.

Aims - in this experiment, you will

 Perform iodate titrations to determine the vitamin C content of a food
supplement.
 Compare the chemical amount of vitamin C and determine whether the
supplement is the good source of vitamin C.

INTRODUCTION
Vitamin C
Vitamin C, also known as L-ascorbic acid, is an essential nutrient for humans. It
cannot be synthesized by the human body and must be consumed. Fruits and
vegetables are the primary source of dietary vitamin C. Vitamin C deficiency can lead
to the disease scurvy in humans. It is an antioxidant (prevents oxidation) and is often
used as a food additive.

Our bodies need ascorbic acid in order to synthesise collagen. A protein that helps
skin, bone, hair and blood vessels stick together. Ascorbic acid also assists our
ability to absorb Fe2+ ions.

Our bodies can store about 1 month’s supply of vitamin C, but no more. Since we do
not synthesize ascorbic acid ourselves, we need a constant supply of the
compounds within our diet. Nutritional research has shown that a healthy diet
includes approximately 90 mg of ascorbic acid per day.

Further research has shown that we metabolize ascorbic acid more quickly if we are
under stress and that smoking also increases the rate of consumption of vitamin C,
potentially leading to deficiencies of the compound.

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 Introductory Chemistry –Determination of Vitamin C

It is widely believed that stresses associated with illnesses such as colds can be
alleviated by taking supplementary doses of vitamin C and that it may assist in the
avoidance of some forms of cancer.

In order to maintain health, many people take vitamin C in the form of a dietary
supplement or in pre-packaged fruit juices. This experiment is designed to test
whether these are viable sources of ascorbic acid.

Vitamin C is a water soluble vitamin found in fruit, vegetables, including citrus,

broccoli, tomatoes and green capsicums. It is widely known that vitamin C is
sensitive to heat, water and air. Food and supplement preparation methods may
therefore lead to a loss of this vital vitamin. A Danish study, for instance, showed that
boiling food for just five minutes led to the loss of between 45 to 64 percent of the
vitamin C content.

The recommended daily intake by the U.S. Food and Nutrition Board of the Institute
of Medicine for men more than 18 years old is 90 milligrams of vitamin C daily; for
women more than 18 years old, it is 75 milligrams daily; for pregnant women more
than 18 years old, it is 85 milligrams daily; and for breastfeeding women more than
18 years old, it is 120 milligrams daily. Recently, some experts have questioned
whether the recommended daily intake should be raised. Others have recommended
an additional 35 milligrams daily intake in some individuals, such as smokers.
The upper limit of intake (UL) should avoid exceeding 2,000 milligrams daily in men
or women more than 18 years old (including pregnant or breastfeeding women).

Titration

This form of titration is a special case of volumetric analysis, in which the chemical
amount (moles) of substance present in a solution is determined from
measurements of volume and concentration. As before, in a titration the titrant is
added gradually to the analyte until the reaction is just completed. This point is the
stoichiometric (or equivalence) point, the stage at which the volume of titrant
added to the analyte is exactly that required to react with all the analyte. However,
whereas in most acid-base titrations an indicator is needed to detect the
stoichiometric point (for example, phenolphthalein is colourless in acidic solution but
purple-pink in basic solution) in this case the colour change occurs within the titrant
solution. In this form of ‘oxidative’ titration the stoichiometric relation is obtained from
the chemical equation for the reaction. This is used to obtain the mole ratio, and the
molarities of the solutions are used to convert between the moles of reactants and
the masses of ascorbic acid in the analytes.

In the procedure, you will initially weigh a sample of unknown ascorbic acid from a
vitamin C supplement and dissolve this sample to prepare a solution of unknown.
You will then measure an aliquot of this unknown acid solution with a pipette,
and titrate this aliquot with a sodium iodate solution of known concentration. The
vitamin C content of different substances is determined using iodate, IO3-, as an

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 Introductory Chemistry –Determination of Vitamin C

oxidising agent, in the presence of iodide (I-) in a redox titration according to the
following stoichiometry:

IO3-(aq) + 6H+(aq) + 5I−(aq) → 3I2(aq) + 3H2O(l)

The iodine produced by this reaction will (for as long as any of it remains in the
solution) cause the ascorbic acid to oxidize to dehydroascorbic acid according to the
following stoichiometry:

C6H8O6(aq) + I2(aq) + H2O(l) → C6H6O6(aq) + 2I-(aq) + 2H+(aq)

Since I2 is reduced to I- (aq) this makes the solution go clear again. This process will
continue until all of the ascorbic acid is used up, at which time the solution will
remain purple.

Strictly speaking, iodine is not soluble in water and what really forms in solution is I3-
(aq) rather than I2 (aq). These reactions should therefore be:

IO3-(aq) + 8H+(aq) + 6I−(aq) → 3I3-(aq) + 3H2O(l)

and

C6H8O6(aq) + I3-(aq) + H2O(l) → C6H6O6(aq) + 3I-(aq) + 2H+(aq)

However, since this makes no difference to the stoichiometric ratios, it is more

common to write the reactions in terms of iodine (I2).

Once the end point is reached, the free iodine combines with the starch indicator
to form a blue-black starch-iodine complex. This is the end point of the titration.

PROCEDURE

Part1: Determination of the vitamin C content of a food

supplement tablet
1. Record the mass of one ‘half’ of a soluble vitamin C tablet on the electronic
balance.
2. Carefully grind the tablet to a powder in a beaker (taking care not to lose
any of the tablet or break the beaker!). Add a small volume of deionized
water to dissolve the powdered tablet.
3. Quantitatively transfer the solution into a 250 mL volumetric flask. Make
up to the mark with deionized water.
4. Pipette 20.00 mL of this standard solution into a 250 mL conical flask.
5. To the conical flask, also add:

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 Introductory Chemistry –Determination of Vitamin C

- 150 mL of deionized water.

- 5 mL of potassium iodide solution (0.6 M).
- 5 mL of hydrochloric acid (2 M).
- 5 mL of starch indicator.
Swirl the contents of the flask well.
6. Collect 80 mL of the titrant KIO3 (approximately 0.002 M) into a
stoppered flask.
7. Rinse the burette with a small amount of the solution and then fill the
with the KIO3 solution, ensuring that there are no air bubbles in the
burette. Record the initial burette reading to 2 decimal places.
8. Titrate the analyte with the KIO3 solution until a blue-black colour appears
indicating the end point. Record the final burette reading to 2 decimal places
and determine the titre volume.
Repeat until 3 titre readings are concordant. The differences between the initial
and final burette readings should be within 0.15 mL (each drop is about
0.05 mL). Good students often get within 0.10 mL routinely. These titres are
then said to be concordant.

It may be necessary to refill the burette each time, though note that the titrant
solution does not have to be filled to the 0.00 mL mark each time as the titre is
calculated by difference.

Calculation
1. Calculate %m/m concentration of vitamin C present in the tablet. Use
the errors from the glassware and equipment to determine the
uncertainty in your answer and quote this uncertainty to the appropriate
degree of precision.
2. Place your results onto the whiteboard. The supervisor will discuss the
results of each of the experiments with the class.
3. In your lab book, comment on how this value compares to the reported
vitamin C content shown on the vitamin C supplement container.

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 Introductory Chemistry –Determination of Vitamin C

DATA (the following tables must be copied into your lab notebook prior to the lab):

Ascorbic acid in vitamin C supplement

Mass of beaker
+/- g

Mass of beaker
plus unknown
+/- g
‘½’ vitamin C
tablet

Mass of vitamin
‘½’ C tablet
+/- g

Mass of a whole 0.9401 + 0.00005g

Vitamin C tablet

Volume of volumetric flask 250.0 ± 0.20 mL

Volume of pipette 20.00 ± 0.06 mL

Concentration of KIO3 solution

(value provided by supervisor) ± 0.00008 M

KIO3 solution (in burette) Trial 1 Trial 2 Trial 3 Trial 4 Trial 5

Initial burette reading (mL)

Final burette reading (mL)

Titre (mL)

NOTE: uncertainty in each burette reading is 0.03 mL, hence the uncertainty in the titre value is
0.06 mL.

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 Introductory Chemistry –Determination of Vitamin C

Average titre of KIO3 solution

(of three concordant titres) ± mL

NOTE: uncertainty in average titre is half of the range or 0.06 mL, whichever is the larger.
Example - if the titres were 22.30, 22.25, and 22.40 mL,
Average is 22.32 mL. Range is 22.25 to 22.40 = 0.15 mL  uncertainty = 0.08 mL.
Hence 22.32 ± 0.08 mL. Note: values rounded to 2 decimal places.

Volume of unknown ascorbic acid solution used in each

20.00 ± 0.06 mL
titration

Study the following sample calculation on how the working should be set out and
how the uncertainty is calculated in a titration analysis.

SAMPLE CALCULATION -
A student weighed 0.4245 g ‘½’ tablet of a vitamin C tablet and dissolved this solid
into a 250 mL volumetric flask.

Mass of the unknown = 0.4245 + 0.0002 g

The student titrated 20.00 mL aliquots of this unknown acid solution with a 0.0002 ±
0.00008 M KIO3 (aq) solution four times, giving the following data:

KIO3 solution Trial 1 Trial 2 Trial 3 Trial 4 Trial 5

Initial burette reading (mL) 0.00 10.08 20.15 35.13

Final burette reading (mL) 9.65 19.48 29.65 44.55

Titre (mL) 9.65 9.40 9.50 9.42

These three titres are ‘good’ i.e.

Put a line through the ‘worst’ titre; within 0.10 mL, so another titration
this is rejected from the average. was not necessary.

CALCULATE THE CHEMICAL AMOUNT OF ASCORBIC ACID

Step 1: The average titre of KIO3 solution is calculated to be 9.44 mL. The range of titres is
9.40 to 9.50 = 0.10 mL  range uncertainty = 0.05 mL < 0.06 mL  uncertainty is ±
0.06 mL.
Titre = 9.44 ± 0.06 mL

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 Introductory Chemistry –Determination of Vitamin C

Step 2: Write down the balanced equation for the reaction.

The balanced equation for the reaction is

IO3-(aq) + 6H+(aq) + 6I−(aq) → 3I2(aq) + 3H2O(l)

Calculate the moles of ‘known’ reactant.

Since concentration and volume are known for KIO3, calculate moles of KIO3. That
is, known c, V of KIO3 calculate moles of KIO3

convert mL to L usually 4 sig. figures

n = c  V becomes

- 9.44 -4
moles of KIO3 = cV = 0.002 mol L 1 L = 0.1888 10 mol
1000

Step 3: Calculate the moles of ascorbic acid using the moles of ‘known’ reactant and
the stoichiometric ratio from the balanced equation.

C6H8O6(aq) + I2(aq) + H2O(l) → C6H6O6(aq) + 2I-(aq) + 2H+(aq)

moles of ascorbic acid = moles of I2

Since 1 mole IO3-(aq) produces three moles of I2,

-4
moles of I2 = moles ascorbic acid = 0.1888x 10 x 3 = 0.5664 x 10-4 mol.

Step 4: Calculate the moles of unknown acid in volumetric flask from number of
moles in the 20 mL aliquot.

volume volumetric flask

moles of HA in volumetric flask =  moles of HA in titration =
volume pipette

250 ml
0.00005664 mol = 0.000708 mol
20 ml

(Mass of whole tablet/mass of ‘1/2’ tablet)

Step 5: Calculate the mass of ascorbic acid in a whole tablet. round to 4 sig. figures
m = nM x (0.9401/0.4245)
mass of ascorbic acid =
0.000708 mol x 176.12 x (0.9401/0.4245) g mol-1 = 0.2761 g

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 Introductory Chemistry –Determination of Vitamin C

Step 6: Calculate the mass % of ascorbic acid in a tablet.

% m/m = 100 x (mass ascorbic acid)/mass of tablet
= 100 x 0.2761/0.9401 = 29.37%

Step 7: Put this value onto the white board so that the class average can be
calculated.

UNCERTAINTY ANALYSIS
An important part of the analysis is to consider uncertainties - how much and where
it arises. It is essential for you to become familiar with statistical analysis.
The uncertainty in the final value is determined by the uncertainty in each
measurement in the calculation. Since all the calculations involve
multiplication/division, the total percentage uncertainty on the final value is
the sum of the percentage uncertainties of the values used to calculate the final
value. Hence, for the above example,

0.00008
% uncertainty in concentration of KIO3 =  100 = 4%
0.002

0.06
% uncertainty in titre (burette) of KIO3 =  100 = 0.62%
9.44

0.06
% uncertainty in pipette volume of ascorbic acid=  100 = 0.3%
20.00

0.15
% uncertainty in volumetric flask of ascorbic acid = ×100 = 0.06%
250.00

0.0002
% uncertainty in mass of ‘½’ tablet ascorbic acid =  100 = 0.047%
0.4245

0.0005
% uncertainty in mass of whole tablet ascorbic acid =  100 = 0.053%
0.9401

Total % uncertainty = 4 + 0.62 + 0.3 + 0.06 + 0.047 + 0.053 = 5.1%

Hence the absolute (or actual) uncertainty in the mass ascorbic acid =

5 .1
 29.4 %m/m = 1.50 %m/m
100
rounded to 1 significant figure, uncertainty in molecular weight is 2 %m/m
divide answer by two to give +

% Mass of ascorbic acid = 29.4 ± 1

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 Introductory Chemistry –Determination of Vitamin C

After the Laboratory session is complete, there is no need

to complete the results analysis. This will be done by the
supervisors and demonstrators in class.
However, postwork must be completed prior to your next
laboratory session.

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 Introductory Chemistry –Determination of Vitamin C

Marking Sheet
TOTAL: 22 MARKS
Pre-work Laboratory book 2 marks
No laboratory book Experiment title, aim Experimental title aim &
Tables completed
0 1 2

Technique 4 marks
Did not complete Many errors in Several errors in Single error in No errors in
experiment technique technique technique technique
0 1 2 3 4

Concordant results 3 marks

No concordant results 3 titrations within 0.25 3 titrations within 0.15 3 titrations within 0.10
ml ml at only 4 attempts ml at only 4 attempts
Or
3 titrations within 0.10
ml at only 5 attempts
0 1 2 3

Laboratory Book 3 marks

No laboratory book little data not recorded Not all data recorded Correct and legible
in lab book or incorrect corrected and legibly recordings of all data
and illegible records (procedure,
appearance, mass,
melting point)
0 1 2 3

Correct calculation of mass percent 3 marks

Could not do Several errors in Single error in No errors
calculation calculation calculation
0 1 2 3

Correct calculation of uncertainty and representation of result

3 marks
Could not do Several errors in Single error in No errors
calculation calculation calculation or
representation of result
0 1 2 3

Accuracy 4 marks
> 10% of correct Within 10% of Within 6% of Within 5% of
value correct value correct value correct value
1 2 3 4

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 Introductory Chemistry –Determination of Vitamin C

GENERIC LAB SKILLS (Part Three)

As part of the practical component of the Unit you are required to demonstrate
competency in a number of generic laboratory skills. These are assessed by the
demonstrators on an individual basis. The demonstrators will tick the appropriate
boxes when they have verified that you have completed the named tasks correctly.

You should separate this sheet from the laboratory notes and stick it into you
laboratory book as a record that you have completed the tasks. You are required to
complete all of the tasks before the end of the Unit. Failure to complete ALL the
tasks will result in you having to attend and complete a ‘repechage’ event at the end
of the semester, else you will receive a compulsory fail for the Unit.

For this Practical the tasks are:

Generic Skill Complete

Using analytical balance correctly

Making up a solution using a volumetric flask

Transferring measured volumes using pipette

Using burette to deliver measured volumes

Determining end point of titration using iodate

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