You are on page 1of 3

Research Project

Dissolved Oxygen Determination


“If we knew what it was we were doing, it would not be called research,
would it?”
—Albert Einstein
Physicist

Abstract
This experiment will use a redox (reduction-oxidation) titration to determine the amount of dissolved
oxygen in water samples. It is often done in conjunction with a precipitation titration to determine the
amount of chloride. For both titrations, the reactions occurring with the dissolved oxygen and chloride
will result in color changes, therefore providing a natural end point indicator.

Application
The EPA recommends a minimum of 5 ppm dissolved oxygen content for water to maintain healthy fish
live. The amount of dissolved oxygen will obviously vary from location to location, but it will also vary
with temperature, pressure, and chloride concentration i. It is the students’ objective to determine the
relationship between chloride concentration and the ppm of dissolved oxygen in water.

Sample Issues
The titration is straight-forward, however, as with all color changing reactions, a deeply colored sample
makes end point determination difficult. Water samples should be mostly colorless and free of any solid
contaminates.

Background
Dissolved oxygen in water is essential for plant and fish survival. The EPA recommends a minimum of 5
ppm oxygen in water; however, many bodies of water contain a larger concentration of oxygen. The EPA
also believes that the concentration of dissolved oxygen is affected by the amount of chloride in the water.
It is up to the student to determine if in fact the dissolved oxygen concentration is affected by the amount
of chloride in the water and the relationship between the two.

For the determination of dissolved oxygen, a series of reactions are necessary in order for a color
changing reaction to occur. First, manganese(II) hydroxide and potassium iodide are added to the water
sample. The manganese(II) hydroxide oxidizes the dissolved oxygen in the solution and forms
manganese(III) hydroxide. The manganese(III) hydroxide is then reacted with added sulfuric acid to form
manganese(III) sulfate. The manganese sulfate immediately reacts with the potassium iodide to oxidize
the iodide to iodine (I3-). The iodine complexes starch to form a blue color. The iodine is the titrated
with sodium thiosulfate. Once all the iodine is titrated the blue color disappears indicating the end point
of the titration. The following reaction scheme depicts what occurs in the water sample:
4Mn(OH)2 + O2 + H20 4Mn(OH)3

2Mn(OH)3 + 3H3SO4 2Mn3+ + 3SO42- + 6H2O

2Mn3+ + 2I- 2Mn2+ + I2

I2 + I- I3-

2S2O32- + I3- (blue) 3I- + S4O62- (colorless)

Procedure
Although this is primarily a measurement lab, there are many observations you can make to help you with
your analysis. In particular, you should be noting what changes occur in your samples every time you
perform an operation. Unusual observations often explain unusual numbers. Remember that to be able to
describe any changes that occur, you will need to have accurate descriptions of the starting conditions as
well as the ending conditions.

Reagents & Other Materials. All chemicals are provided as solids. The water samples will
have to be prepared for titration and the titrants will have to be prepared. No indicator is required as the
starch solution also fulfills this function. The procedure requires a 3% starch solution.

In addition to the normal lab items found in your locker and in the room, the materials that will be
provided by the preproom are detailed in the Research Project Materials List,

You are responsible for providing your own samples to evaluate. Additional, non-sample materials may
be requested of the preproom. Such requests must be submitted by your TA.

Design Issues The titration is very straight forward and easy to perform. Design issues relate to
sample preparation. Solid reagents need to be dissolved to form aqueous solutions.

Procedure Outline
The following is a description of the steps required to obtain results for a generic sample containing
glucose. This procedure will need to be modified, and more detail added, based on the nature and number
of samples to be evaluated.

Dissolved Oxygen Titration This titration will require the preparation of the following
solutions. Recommended amounts for most applications are given in parenthesis.

1.25x10-3 M solution of Na2S2O3 (250ml)


6.6x10-2 M solution of MnSO4 (10ml)
0.24 M solution of KI (5ml)
0.24 M solution of KOH (5ml)
3% by weight Starch Solution (100ml)
Dissolved Oxygen Procedure. Place 50 ml of water sample into a 150 ml beaker. While
stirring, add 2 ml of the MnSO4 solution 1 ml each of the KI and KOH solution and 4 drops of
concentrated sulfuric acid (WARNING CORRESIVE). Once all reagents are thoroughly mixed
place 20 ml of prepared water sample into a separate beaker and add starch solution drop wise
until the water sample turns to a blue color. Titrate the sample with the Na2S2O3 solution until
blue color disappears.

i
Crosson, M.; Gibb, R. J. Chem. Ed. 1992, 69, 830.

You might also like