Nielsen 2007
Reaction 1a :
Reaction 1b :
O 2 + Mn(OH) 2 MnO(OH) 2
Reaction 2 :
Reaction 3 :
formed and no iodine (I2) is produced. We then add a well-known quantity of KIO3 (8 ml 0.0017M)
and I2 is produced by the reaction:
KIO3 + 5 I- + 6 H + 3 I 2 + 3 H 2O + K +
We can then determine the molarity of the thiosulfate by titration (reaction 3).
Preparation of reagents
Solution 1
Solution 2
MnCl2:4H2O
Dissolve 60g MnCl2:4H2O in 100 ml deionized water
Concentrated H2SO4
Dissolve 1 g of Na2S2O3:5H2O in deionized water. Add 10 ml of a solution of Na2CO3 (10 g/l) for
conservation. Fill until a total volume of 1000 ml.
Starch indicator
Prepare a thin paste of 1 g soluble starch in a few mL deionized water. Bring 100 mL deionized
water to a boil, remove from heat and stir in the starch paste.
Dissolved 0,3567 of dried K(IO3) in 200-300 ml deionized water in a 1L volumetric flask. Fill the
volumetric flask to 1L with deionized water. The molarity is 0.0017 M KIO3.
1. Transfer sufficient sample to the Winkler bottle (approximately 50 or 100 mL) for Winkler
determination of dissolved O2.
2. Fill the Winkler bottle completely.
3. Add 250 L MnCl2 solution and 250 L (NaI 3 M + NaOH 8 M) solution to 50 mL Winkler
bottles (twice the volume to 100 mL Winkler bottles), close and mix. Make sure that no air
bubbles are trapped inside the Winkler bottle.
4. Let the precipitate settle.
5. Add 250 L concentrated sulfuric acid (H2SO4) to 50 mL Winkler bottles (500 L to 100 mL
Winkler bottles). Close and mix until all precipitate has dissolved. At this point, the sample can
be stored for a few hours for later titration.
6. Transfer 50.0 mL to a titration beaker with a glass pipette.
7. Begin titration with the thiosulfate solution.
8. Continue titration until a pale yellow color is obtained. Then add 1-2 drops of starch.
9. Continue titration until the first disappearance of the blue color.
10. Calculate the concentration of dissolved oxygen based on the titrated volume of thiosulfate.
Standardization of Thiosulfate
KIO3 stock
t k solution
l ti 0.0017
0 0017 M
Titration of 8 mL KIO3 solution:
KIO 3 + 5 I- + 6 H+ 3 I2 + 3 H2O + K +
Standardization of Thiosulfate
Thi
Thiosulfate
lf t and
d iodine
i di reacts
t 2:1:
21
I2 + 2 Na 2 S 2 O 3 Na 2 S 4 O 6 + 2 NaI
Thiosulfate concentration =
Thiosulfate concentration =
Contains
0.0408 mmol I2
Titrate with
x mL Na2S2O3 solution
If 21.1
21 1 mLL Thi
Thiosulfate
lf t was added
dd d during
d i the
th standardization,
t d di ti
the
th
concentration of the Thiosulfate solution is:
Thiosulfate concentration =
0.0816
M = 0.0039 M = 3.9 mM
21.1
=?M
= ? mL
2 /L)
(I M
(I.e.,
Moll S2O32-
O2 Concentration =