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ATQ: Experiment #8

1. Give the pertinent chemical equations and stoichiometry in the standardization of

Na2S2O3 was first standardized using the primary standard KIO3 with starch as the indicator.
The following reaction takes place:
IO3- + 5I- + 6H+ 3I2 + 3H2O
Since iodine is a halogen, it reacted with the water produced in the first reaction:
I2 + H2O H+ + I- + HIO
A pale yellow solution would then be obtained after the first titration. Afterwards, the
presence of iodine was then implicated by the addition of starch. Another titration was made after
the addition of starch, and slowly the blue color faded:
I3- + 2S2O32- 3I- + S4O62Stoichiometric ratio of 1 mmol of IO3- is to 6 mmol of S2O32-.
2. Explain the purpose of the addition of H2SO4 and excess KI during the
standardization and why the acid was added before KI.
To produce more I2, the application of the principle of the common-ion effect was observed.
The addition of H2SO4 before the titration occurred would cause the equilibrium to shift producing
more iodine. The H2SO4 liberates the free iodine from the iodate in the sample. The excess KI that
is added helps make the free iodine soluble the and would yield a sharper titration endpoint.
3. Give the pertinent chemical equations and stoichiometry in the sample analysis.
For the sample analysis the same concepts were used to determine the amount of
dissolved oxygen.
Mn2+ + 2OH- > Mn(OH)2
4Mn(OH)2 + O2 > 4Mn(OH)3 + 2H2O
6H+ + 2MnO(OH) + 2I- > 2Mn2+ + I2 + 4H2O
Stoichiometric ratio of 1 mmol O2 is to 4 mmol S2O32-

4. Explain stepwise how I3 was produced from the dissolved O2 in the water sample.
Explain briefly why the reagents are added in a definite sequence.

The iodine has a low solubility in water making it first to be converted to a complex
consisting of Iodine. This is done by dissolving the I2 in a KI solution.
I2 + I- > I3The I2 produced in the reaction is then titrated with Na2S2O3 which yields the reaction:
I2 + 2S2O32- > 2I- + S4O62The water sample was filled to the brim and when the bottle was opened MnSO4, NaOH
with KI and NaN3 were added to the sample. Upon shaking the sample forms brown precipitate in
the form of Mn(OH)3 and the oxygen content is fixed. H3PO4 is added and the bottle is shaken to
dissolve the precipitate. Once the precipitate dissolves the solution is titrated and follows the same
procedure as the standardization.
5. Give the reason why starch was used as an indicator in the analysis and why it
was added towards the end of the titration.
Starch is used as an indicator for redox titrations where triiodide is present. Starch forms a
very dark blue-black complex with triiodide which can be made by mixing iodine with iodide which
is often from potassium iodide. The addition of starch is delayed at the point where dilute iodine
imparts a pale yellow color to the solution. Adding the starch indicator at the beginning of the
titration while the iodine concentration is high a iodine-starch complex will form and produce a
reddish brown color endpoint. The starch may hydrolyze and interfere with the reaction in acidic
6. How is this analysis (an iodometric process) different from an iodimetric one?
For an iodometric process he titrant used is sodium thiosulfate and the analyte is iodine.
On the other hand an iodometric process uses iodine as a titrant and sodium thiosulfate as
an analyte.
7. From the calculated ppm O2, identify the degree of water pollution and ability of
the water sample source to sustain aquatic life.
After computing the ppm of dissolved oxygen in the water sample the value computed was
1.7638 ppm. The results obtained indicates that the pond water in the math building is highly
polluted and is not a good source to sustain life.
8. Predict the effect, if any, of each of the following on the DO content obtained:
a. The water sample is made to stand overnight before analysis.
The effect of leaving the sample overnight to the content of dissolved oxygen is
indeterminate. The water sample may have heterotrophic or photosynthetic organisms that could
perform cellular respiration and photosynthesis. The effect on the oxygen cannot be determined.

b. MnSO4 is added and the solution made to stand for an hour before the
alkaline KI solution is added.
The amount of dissolved oxygen will decrease. Manganese is sensitive to light and
undergoes reduction. This will cause the volume of the titrant used to decrease and the calculated
dissolved oxygen concentration will decrease.
9. What are the possible sources of errors and their effect on the calculated
parameters? Rationalise.
A partially filled bottle may result in an increased calculated DO concentration due to the
additional oxygen coming from the air spaces. If the bottle is not shaken well the calculated DO will
decrease because not all of the DO is accounted for. Not using boiled distilled water the calculated
molarity of sodium thiosulfate will decrease because of the possible carbonic acid error. If the
sample is left in the locker the calculated DO content will decrease because the oxygen may be
consumed by heterotrophic organisms.