Chemistry 153

Clark College

BALLENTINE'S ASSAY OF ASCORBIC ACID

(A Titrimetric Redox Analysis of Commercial Vitamin C)
For this experiment:
1. Complete the Prelab and obtain a stamp before you begin the experiment.
2. Write your lab notebook prelab and get it initialed/signed before you begin the
experiment. You should include the pertinent chemical/redox equations.
3. Weigh out 10 ascorbic acid tablets to obtain the mass of one tablet by taking an
average!
4. You may grind more than one tablet for the experiment, based on your required
amount needed (from the prelab).
5. Titrate 4 samples of the Vitamin C solution with the prepared KIO 3 solution. You
may do NO MORE than 5 titrations total. Perform 4 titrations, and then do your
calculations before determining if you need to do a 5 th.
6. Your titrations must all be done on the same day.
7. Determine the %Vitamin C in the tablet for the four titrations, and determine the
Average % Vitamin C, the standard deviation and the RSD. The RSD must be less
than or equal to 10.
8. Enter your % Vitamin C data into the computer in the front of the lab.
9. Using your average % Vitamin C, calculate the amount of vitamin C (in mg, to ppth
precision) in one tablet.

Turn in only the Data Report Sheet, your Notebook Sheets and the Stamped Prelab!!
Introduction
Ascorbic acid (Vitamin C) is readily oxidized to dehydroxyascorbic acid:

HO

OH
H

O
2 e- + 2 H + +

OH
OH
Ascorbic Acid
MW =176.12 g/ mol

O
(Eq. 1)

H
O

OH
OH
Dehydroxyascorbic Acid
MW =174.11 g/ mol

This reaction is reversible but dehydroxyascorbic acid can be further irreversibly oxidized
to oxalic acid and 1-threonic acid. In the following analysis only partial oxidation
according to Equation 1 is utilized. Even atmospheric oxygen causes slow oxidation of
ascorbic acid so the sample must not be dried and solutions of ascorbic acid must be
protected from oxidation by adding oxalic acid or metaphosphoric acid (HPO 3).
In this analysis the ascorbic acid is titrated with standard potassium iodate (KIO 3) in the
presence of excess potassium iodide. The iodate ion oxidizes iodide ion to I 2 and is itself
reduced to I2 according to the reaction:
IO3- + 5 I- + 6 H+ 3 I2 + 3 H2O

Ascorbic Acid Titration

Revised Spring 2008 NF

(Eq. 2)

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The ascorbic acid is quantitatively oxidized by the liberated iodine:

HO

OH

O
+ I2

2 I- + 2 H + +

O
OH

O
(Eq. 3)

OH

OH

OH

The net reaction is:

HO

OH
H

O
+ IO3-

I - + 3 H 2O +

O
OH

OH

(Eq. 4)

H
O
OH

OH

When all of the ascorbic acid is consumed, the iodine reacts with a starch indicator to form
a deep blue starch-iodine complex.
Note that in the overall reaction, iodate is reduced to iodide, which is a gain of six
electrons, so the equivalent weight of iodate is 1/6 of the formula weight. Each
ascorbic acid molecule loses two electrons so the equivalent weight of ascorbic acid
is 1/2 of the formula weight.
Analysis of Vitamin C Tablets
Pharmaceutical grade Vitamin C is generally compounded into tablets for ease of
administering, although U.S.P. grade ascorbic acid crystals can be obtained.
In
compounding, the ascorbic acid is usually mixed with various resins or gels to form into
granules for ease in blending. Fillers, such as dextrose, lactose and sucrose, are added to
make the tablet a convenient size. Binders, such as acacia gum, are added to reduce the
tendency of the tablet to crumble into powder, and finally, lubricants, such as magnesium
or zinc stearate and talcum powder, are added to aid the blending of the components into
an homogeneous powder before pressing into a pellet.
The assay of pharmaceutical Vitamin C tablets will depend upon the amounts of the
various components added in the compounding. For example, a nominal "100-mg" tablet
may actually weigh about 400 mg (corresponding to a 25% assay) and a "250-mg" tablet
may weigh about 500 mg (corresponding to a 50% assay). Your laboratory instructor may
inform you of the approximate assay to expect or you can calculate it based on the mass
of your tablets and the mass of Vitamin C listed on the bottle.
Because of the gels used in granulating the ascorbic acid, and the gums as binders,
Vitamin C tablets do not dissolve readily, and the tablets must be powdered before
analysis. Once powdered, the ascorbic acid dissolves very readily; the solution may
remain cloudy if insoluble fillers and lubricants have been used, but the ascorbic acid
will all be in solution. The binders and fillers will typically settle to the bottom of the
solution, and can be avoided.

Ascorbic Acid Titration

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PROCEDURE:
Note: The ascorbic acid must be titrated within a few hours after the solution
has been prepared.
Note: Sufficient mixing is the name of the game here. It will take about 30 minutes of
near constant shaking and swirling to get the ascorbic acid dissolved away from
binders and fillers. In addition, after the sample is diluted to the mark, you must upend (flip it upside down and right-side up) the volumetric flask at least 25 times, at
the absolute minimum, to ensure a homogeneous solution of ascorbic acid for
analysis.
1. Weigh out 10 Vitamin C tablets, and use this mass to determine the mass of one tablet
(you can put the others back in the bottle). Write this in your notebook!
2. Calculate the amount of powdered vitamin C tablet needed for a 35 mL titration with
0.01 N KIO3 assuming each tablet is approximately 75% vitamin C (you have already
done this in the prelab). See the paragraphs above and the example calculations at
the end of the experiment for guidance. If you need to use more than one tablet
to get enough ascorbic acid for the titration, you may do so!
3. Now that you know how many tablets you need, grind your Vitamin C tablet(s) with a
clean mortar and pestle. Transfer the sample to a clean 100-ml volumetric flask, and fill
the flask approximately one-third full with distilled water.
4. With a graduated cylinder, add 10.0 ml of 2.0% oxalic acid to the volumetric flask.
Shake the solution occasionally (every few minutes) for about 30 minutes until all the
powder dissolves except for the residual binder and lubricants. This will ensure that all
of the ascorbic acid will dissolve from the sample. Correct technique: add solvent, add
ground tablet, shake, add more solvent, shake, add more solvent, shake and so on.
When the flask is filled to the mark, make sure to invert the flask several times for
complete mixing.
5. Fill the flask to the mark with distilled water, rinsing down the neck and stopper, to
form a solution of ascorbic acid in 0.20% oxalic acid. Mix thoroughly shaking
periodically over 30 minutes (See note). Allow the insoluble material to settle for
about an additional 15 minutes. Some binder may remain floating on the surface.
6. While the ascorbic acid solution is settling, prepare a standard ~0.01 N potassium
iodate solution by pipeting 10.00 ml of a standard 0.2500 N KIO 3 solution into a clean
250-ml volumetric flask. Do not pipet directly from the reagent bottle! Add
distilled water, swirl the solution thoroughly, and dilute to the mark with additional
distilled water to make the solution. Calculate the exact normality of your standard
potassium iodate solution to ppth precision.
7. Pipet 10.00 ml aliquots of the clear, upper portion of the prepared ascorbic acid
solution into each of four 250-ml Erlenmeyer flasks. To each sample, add 25 ml of
distilled water, 1 ml of 10% potassium iodide solution, 2 ml of 2 N sulfuric acid, and 2
ml of 1% starch indicator solution. The volumes of water, KI, H 2SO4 and starch can be
measured with a graduated cylinder, or with a marked beral (plastic) pipet.
8. Titrate the ascorbic acid solutions with your prepared, standard 0.01 N potassium
iodate solution (from step 5). The end point is the appearance of the first permanent
blue color due to the formation of the starch-iodine complex.
9. Calculate the assay (or percent) of the Vitamin C tablet and report the average assay
with a relative error of 10 parts per thousand or less. In this experiment we are not
using calibrated volumetric flasks and the oxidation of Vit.C will make our RSD less
precise than in previous experiments. If the assay is 50% or greater, round to 0.1%
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and if it is less than 50%, round to 0.01%.

10.Use your average % vitamin C to determine the amount of vitamin C in one tablet (in
mg, to ppth precision).
Sample Calculations
Ballentine's Assay of Ascorbic Acid
1. Calculate the sample weight that would be required for a sample of approximately 25%
assay. (Remember...40mL titration, impure sample, 10 mL aliquot diluted to 100 mL)
USING NORMALITY:
Equiv Wt. Ascorbic Acid =

176.12 g
mol

mol
-

2 equiv e

88.06 g
equiv

Equiv Acid =Equiv KIO 3

0.01 equiv KIO 3
L

x 0.035 L =X g tablet x

25 g Asc. Acid
100 g tablet

equiv
88.06 g Asc. Acid

10 mL sample
100 mL tablet soln

Sample Weight =1.2 g tablet Note: The sig figs are incorrect, based on the values given.
This is just an estimate!

2. Prepare a solution of KIO 3 from a 0.2500 N primary standard solution, using a 10-mL
volumetric pipet and a calibrated 250-mL volumetric flask.
N 1V1 =N 2 V2
(0.2500 N)(10.00 mL) =N 2 (250.00 mL)
N 2 =0.01000 N
3. A 1.4971 gram sample of ascorbic acid was dissolved in a 100-mL calibrated
volumetric flask. A 10.00 mL aliquot was taken with a calibrated pipet and required
39.43 mL of a 0.00992 N KIO3 solution. Calculate the % assay of the sample.
USING NORMALITY:
0.00992 eq KIO 3
L

x 0.03943 L x

1 eq Asc. A
1 eq KIO 3

88.06 g Asc. A
equic

1.4971 g tablet

Ascorbic Acid Titration

Revised Spring 2008 NF

100.00 mL tablet soln

10.00 mL sample

x 100% =23.01%

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Chem 135

Vitamin C Analysis

DATA REPORT SHEET

NAME ____________________________
Enter your data into spread sheet at the front of the lab. Dont forget to include the
sample calcs!
Normality of
KIO3 (N)
Mass of
Vitamin
Sample
Titration:
Volume
KIO3

of

% Vitamin C

Average %
Vitamin C

Mass Vitamin C in 1 tablet

Standard
Deviation

Class Average
(Instructor will fill this in)

RSD

ppth difference from

Class Average
(instructor will fill this in)

NOTE: Circle Q-test/5ppth test rejected data.

SHOW: Calculation for Normality of KIO 3:

SHOW: Sample Calculation of Ascorbic Acid Assay:

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SHOW: Statistics Calculations: Q-test, 5ppth test (if applicable), calculations

for SD and RSD that you reported in the data table.

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CHEM 135
Stamphere:

Vitamin C Analysis

PRELAB

1. Determine the sample weight needed for a 35-mL titration with 0.01 N KIO 3. For this
calculation, you may approximate the % assay at 75%

This is the amount of ascorbic acid to use for the lab!

Sample Weight =

2. A 1.236 gram sample of ascorbic acid tablet was dissolved in a 100.0 mL calibrated
volumetric flask. A 10.00 mL aliquot was taken with a calibrated pipet and required
37.51 mL of a 0.00998 N KIO 3 solution. Calculate the % assay of the sample, and
report your answer to ppth precision.

% Assay =

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Revised Spring 2008 NF

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