REPORT

EXPERIMENT 3: REDOX TITRATION OF

VITAMIN C

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Instructor: Dr. Nguyen Thao Trang Summer SemesterI: 2014-2015

 1. Standardization of Na2S2O3 solution

IO3− + 8I− + 6H+ → 3I3− + 3H2O (1)

0.0001 0.0003
–
2S2O3 2- + I3 → S4O6 2- + 3I (2)
0.0006 0.0003
Molar concentration of standard KIO3 solution = 0.01 M
# moles of KIO3 = 0.01 x 10 x 10-3 = 0.0001 mol
-
# moles of iodine I2 (in the form of I3-) generated = 1/3 # moles of iodine I2 (in the form of I3 )
generated
# moles of S2O32- = 0.0006 mol

Burette reading Molar

Volume of Na2S2O3
Trial # concentration of
Initial Final (mL)
S2O32- (M)
1 23.9 37.0 13.1 0.0458
2 22.2 36.5 14.3 0.0420
3 36.0 49.7 13.7 0.0438

0.0458+0.0420+0.0438
Mean of molar concentration of Na2S2O3 solution = = 0.0439
3
∑𝐍 ̅)𝟐
𝐢=𝟏(𝐱𝐢 − 𝐱 (𝟎.𝟎𝟒𝟓𝟖−𝟎.𝟎𝟒𝟑𝟖)𝟐 + (𝟎.𝟎𝟒𝟐𝟎−𝟎.𝟎𝟒𝟑𝟗)𝟐 + (𝟎.𝟎𝟒𝟑𝟖−𝟎.𝟎𝟒𝟑𝟗)𝟐
Standard deviation =√ = =√ = 1.952 x 10-3
𝐍−𝟏 𝟑−𝟏
** Note: xi means [NaOH]

2 Analysis of vitamin C
Weight of a vitamin C capsule (only count the powder) = 0.5

IO3− + 8I− + 6H+→ 3I3− + 3H2O (1)

Ascorbic acid (vitamin C) + I3− → Dehydroascorbic acid + 3I− (2)

2S2O32- + I3− → S4O62- + 3I− (3)

# mole of S2O32- = 𝑉𝑁𝑎2 𝑆2 𝑂3 x 𝐶𝑚𝑒𝑎𝑛 = 20.6 * 0.0439 = 0.9033 x10-3 ( mol)

#mole of I3- excess = 0.5 x 𝑛𝑆2 𝑂3 2− = 0.5 * 0.9003 = 0.4517 x10-3 ( mol)

#total mole of I3- = 3 x 𝑛𝐾𝐼𝑂3 = 3 * 20* 0.01= 0.6 x10-3 ( mol)

#mole of Vitamin C = #total mole of I3- - #mole of I3- excess

= 0.6 - 0.4517 = 0.1483 x10-3 ( mol)

Instructor: Dr. Nguyen Thao Trang Summer SemesterI: 2014-2015

 # Trial Burette reading Volume of Na2S2O3
(mL) Moles of S2O32-
Initial Final
1. 9.6 30.2 20.6 0.9033 x10-3
2. 26.7 49.6 22.9 0.1004 x10-3
3. 16.5 37.5 21 0.9209 x10-3

Mass of vitamin C % by mass of

# Trial Moles of I3- excess Mole of
vitamin C /capsule (g) vitamin C/capsule
1. 0.4517 x10-3 0.1483x10-3 0.0261
52.21
2. 0.5012 x10-3 0.0979 x10-3 0.0172 34.46
3. 0.4604 x10-3 0.1396 x10-3 0.0246 49.12

500
Mass of vitamin C in 1mL: 𝑚𝑣𝑖𝑡𝑎𝑚𝑖𝑛 𝐶/1𝑚𝐿 = 200 = 2.5 (mg/mL)

Mass of vitamin C in 20mL = 20 x 𝑚𝑣𝑖𝑡𝑎𝑚𝑖𝑛 𝐶/1𝑚𝐿 = 20 x 2.5 = 50 (mg)

Mass of vitamin C/capsule : 176 x 𝑛𝑣𝑖𝑡𝑎𝑚𝑖𝑛 𝐶 = 176 x 0.1483 ( g )

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑣𝑖𝑡𝑎𝑚𝑖𝑛 𝐶 (𝑚𝑔) 0.0261 𝑥 103

 % 𝑏𝑦 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑣𝑖𝑡𝑎𝑚𝑖𝑛 𝐶/𝑐𝑎𝑝𝑠𝑢𝑙𝑒 = x 100 = x 100 = 52.21
50 (𝑚𝑔) 50

0.0261+ 0.0172+0.0246
Mean of mass of 1 vitamin C in 1 capsule = = 0.0226
3
∑𝐍 ̅)𝟐
𝐢=𝟏(𝐱𝐢 − 𝐱 (𝟎.𝟎𝟐𝟔𝟏−𝟎.𝟎𝟐𝟐𝟔)𝟐 + (𝟎.𝟎𝟏𝟕𝟐−𝟎.𝟎𝟐𝟐𝟔)𝟐 + (𝟎.𝟎𝟐𝟒𝟔−𝟎.𝟎𝟐𝟐𝟔)𝟐
Standard deviation = √ =√ = 0.0047
𝐍−𝟏 𝟑−𝟏

3. Conclusion (briefly discuss your observation and conclusion about this experiment, discussion of
the reproducibility must be included)
 Starch is a viable indicator in the titration process because starch forms a complex with triiodide ion
that displays an intense dark purple color. This change of color due to the end point of
standardization of Na2S2O3 solution.
 Vitamin C and S2O32- converts I3- to I-, so the starch mixture turns from blue to colorless until all
the excess iodine is used up, and this change of color marks the end point of titration.
 The first experiment: standardization of Na2S2O3 solution
+ The solution for titration contains 10 mL of KIO3 0.01M; 5 mL of KI 1M and 0.5 mL of H2SO4 solution.
At the beginning, brownish color appeared due to forming of I3-, and it turns to pale yellow at the end point
of standardization until 11.3 mL of Na2S2O3 were dropped to the Erlenmeyer for 1st, 2nd trial and 11.0 mL
for the 3rd trial. Then add 2 mL of starch indicator, the solution turns to dark blue. The solution became
colorless at the end point of titration when the total volume of Na2S2O3 added is 13.1 mL for 1st trial; 14.3
for 2nd trial and 13.7 mL for the 3rd trial, this change of color marks that the titration was stopped.
 The second experiment: titration of excess I3- with Na2S2O3
+ The solution for titration contains 10 mL of KIO3 0.01M; 5 mL of KI 1M and 20 mL of ascorbic solution
(prepared with vitamin C and 0.3M H2SO4). At the beginning, brownish color appeared due to forming of
I3-, and it turns to pale yellow at the end point of standardization until 10 mL of Na2S2O3 were dropped to
the Erlenmeyer for 1st, 3rd trial and 10.8 mL for the 2nd trial. Then add 2 mL of starch indicator, the
solution turns to dark blue. The solution became colorless at the end point of titration when the total volume

Instructor: Dr. Nguyen Thao Trang Summer SemesterI: 2014-2015

of Na2S2O3 added is 20.6 mL for 1st trial; 22.3 for 2nd trial and 21.0 mL for the 3rd trial, this change of
color marks that the titration was stopped.

 Conclusion: Redox titration use to determine the concentration of an unknown solution. The
experiment obtained the titration for Na2S2O3, and I3- excess that use to determine the mass of
vitamin C. Although the mass of vitamin C is known, after titration, the mass has a bit difference
(will be proofed by T-test). It can made by missing the end point.
 We use the T-test to demonstrate the result of titration with the mass of capsule (vitamin C) = 0.5g:
+ We take the confidence interval at 95% with 2 degrees of freedom t = 4.30
+ The null hypothesis: H0: μ = μ0 = 0.5 g ; Alternative hypothesis is: Ha: μ ≠ 0.5 g
t = (x ̅ - μ)/(s/√N) = (0.247067 -0.5)/(0.0048303/√3) = - 90.69
+ From the table 7-3, the critical value t for 2 degrees of freedom and 95% confidence interval is 4.30. Since
t ≤ -4.30, the null hypothesis is rejected. Therefore, the mass of known vitamin C has a significantly
difference from the vitamin C titration and thus bias in the method.
 Reproducibility is the closeness of the agreement between the result of measurements of the same
measured carried out with the same methodology described in the corresponding scientific evidence.
+ RSD in percent (coefficient of variation): CV = S/x ̅ x 100% = 0.0048303/0.237067 x 100% = 2.04%
<5%
can be repeatable. Thus, it can be reproducible.

4.Questions

1/ Why is H2SO4 added for the titration?

- Sulphuric Acid (H2SO4) is used in the redox titration process because it provides the H(+) ions
necessary for the reaction to occur more quickly while the sulphate(-) ions barely react during the
reaction.

- IO3- + 8I- + 6H+ —> 3I3- + H2O

+ I3- (brownish color)

- It is difficult to store and prepare iodine (I3-). In the laboratory, iodine was obtained by mixing known
concentration of potassium iodate (IO3- ion) and potassium iodine (I- ion). Adding H2SO4 have an
important role in increasing the rate of the reaction while sulphate ions (SO4 2-) does not have any effect.

2/ What gives the blue color of the titration?

- Starch is often used in chemistry as an indicator for redox titrations where triiodide ion is present

- The resulting complex with starch produces an intense "blue-black" color.

- During iodine titrations, concentrated iodine solutions must be reacted with thiosulfate, in order to
remove most of the iodine before the starch is added. This is due to the insolubility of the starch-triiodide
complex which may prevent some of the iodine reacting with the thiosulfate. Close to the end-point, the
starch is added, and the titration process is resumed taking into account the amount of thiosulfate added
before adding the starch.

Instructor: Dr. Nguyen Thao Trang Summer SemesterI: 2014-2015