Procedure for Measuring Dissolved Oxygen Using Winkler's Method
Step 1: Collect Water Sample
- Get water from the source you're interested in.
- Store it carefully to keep the oxygen level stable until you can test it.
Step 2: Prepare the Sample
In the lab, you'll treat the water with chemicals to make the oxygen measurable. Here's how:
a. Add Manganese Sulfate (MnSO4)
- This acts as a catalyst for the reactions you'll do next.
b. Add Alkali Solution (KI)
- This changes the oxygen in the water into a form that's easier to measure.
Reaction: O2 + 2OH- → H2O2 + 2e-
c. Titrate with Iodine (I2) Solution
- This step helps you find out how much oxygen was in the water.
Reaction: I2 + 2e- → 2I-
Step 3: Use Starch Indicator
- Add starch to the water.
- The water will turn blue because of the iodine.
Step 4: Titration
- Keep adding iodine drop by drop and mix the sample.
- When the blue color vanishes, you've found what you're looking for—the 'endpoint.'
Step 5: Calculate Dissolved Oxygen
- Use the formula to find the oxygen level in mg/L:
DO (mg/L) = (Volume of iodine (mL) × 0.003 × 32,000) / Volume of water sample (mL)
Key Points:
- 0.003 is a constant related to oxygen's molar mass.
- 32,000 helps convert the result to mg/L.
Calculation for trial 1:
(18*0.003*32000)/201
= 8.59 mg/l
Calculation for trial 2:
Raw Data:
Initial Burette Final Burette
Reading (mL) ± Reading (mL) ± Volume of Titrant Dissolved Oxygen Content
Trial No. 0.05 0.05 Used (mL) ± 0.1 (mg/L) ± 0.2
1 0.00 ± 0.05 5.20 ± 0.05 5.20 ± 0.1 8.0 ± 0.2
2 0.00 ± 0.05 5.05 ± 0.05 5.05 ± 0.1 7.7 ± 0.2
3 0.00 ± 0.05 5.30 ± 0.05 5.30 ± 0.1 8.1 ± 0.2
4 0.00 ± 0.05 5.10 ± 0.05 5.10 ± 0.1 7.8 ± 0.2
5 0.00 ± 0.05 5.35 ± 0.05 5.35 ± 0.1 8.3 ± 0.2
Chemicals:
● Sample of water containing dissolved oxygen
● 10 mL of 1% potassium iodide solution
● 2 mL of sulfuric acid
● A few drops of starch solution (as an indicator)
● Sodium Thiosulfate solution
● Manganese Sulphate
Glassware:
● Burette
● Conical flask
● Pipettes
● Beakers
● Grad cylinders
● Magnetic stir bar
Prepare the Sample:
Take a sample of water containing dissolved oxygen (specified volume, e.g., 250 mL).
Add Chemicals to the Sample:
Add 10 mL of 1% potassium iodide solution to the water sample.
Add 2 mL of sulfuric acid to the sample.
Use an Indicator:
Add a few drops of starch solution to the sample. The solution turns blue.
Perform the Titration:
Use a burette to slowly add the sodium thiosulfate solution to the sample while stirring with a
magnetic stir bar.
Continue adding until the blue colour disappears. Note the volume of sodium thiosulfate solution
used (V1).
Blank Titration:
Repeat the titration steps, but this time titrate a sample without the water (just the chemicals) to
determine the blank titration volume (V0).
Calculate the Dissolved Oxygen:
Calculate the amount of dissolved oxygen (in mg/L or ppm) using the formula:
Dissolved Oxygen (mg/L) = (V0 - V1) x Normality of Sodium Thiosulfate x 8
**Chemical Reactions in Winkler's Method:**
Winkler's Method involves a redox (reduction-oxidation) reaction to determine the amount of
dissolved oxygen in water. Here's a simple explanation of the chemical reactions involved,
including the key redox reaction:
1. Oxidation of Iodide (I⁻) to Iodine (I₂):
- In the presence of oxygen, the potassium iodide (KI) in the sample undergoes oxidation.
Oxygen turns the iodide ions (I⁻) into iodine molecules (I₂).
Chemical Equation: 2I⁻ + O₂ → I₂ + 2OH⁻
2. Reaction of Iodine (I₂) with Thiosulfate (S₂O₃²⁻):**
- Iodine (I₂) produced in the first step reacts with sodium thiosulfate (Na₂S₂O₃). This reaction
reduces iodine back to iodide ions and produces tetrathionate ions (S₄O₆²⁻).
Chemical Equation: I₂ + 2S₂O₃²⁻ → 2I⁻ + S₄O₆²⁻
3. Formation of Starch-Iodine Complex:
- When iodine is present, it reacts with the starch indicator to form a blue complex. This blue
colour indicates the presence of excess iodine.
No Chemical Equation (This is a colour change reaction).
4. Titration with Sodium Thiosulfate:
- Sodium thiosulfate (Na₂S₂O₃) solution is added from the burette to the reaction mixture. It
reacts with the excess iodine (I₂) formed in step 1.
Chemical Equation: I₂ + 2S₂O₃²⁻ → 2I⁻ + S₄O₆²⁻
5. Blank Titration Reaction:**
- During the blank titration, the sodium thiosulfate reacts with any remaining iodine from step 1
in the absence of water.
Chemical Equation:** I₂ + 2S₂O₃²⁻ → 2I⁻ + S₄O₆²⁻
Redox Reaction Simplified Explanation for a 5-Year-Old:
1. At first, we have some tiny things called iodide (I⁻) in the water. When oxygen comes, it
changes these iodide things into iodine (I₂).
2. Then, the iodine meets another thing called thiosulfate (S₂O₃²⁻), and they play together. Iodine
changes back into iodide, and they create a new thing called tetrathionate (S₄O₆²⁻).
3. The blue colour we see is like a party where iodine and starch get together, like making a
painting.
4. We use a special liquid (sodium thiosulfate) from a tube to make the blue colour go away. It's
like erasing the blue painting, and the sodium thiosulfate does that job.
5. We also do this without water to see how much blue colour we can erase, and then we can
use the numbers to figure out how much oxygen was in the water. It's like counting how many
toys you have and doing some maths to find out the answer.
1. Oxygen Conversion (First Step):
2Mn^2+ + O2 -> 2Mn^3+
In the first step, dissolved oxygen (O2) in the water is converted to manganese ions in their
higher oxidation state (Mn^3+). This conversion is facilitated by the addition of manganese
sulfate (MnSO4).
2. Iodine Formation (Second Step):
2Mn^3+ + 4I^- -> 2Mn^2+ + 4I2
In the second step, the Mn^3+ ions produced in the first step react with iodide ions (I^-) to form
iodine molecules (I2). This reaction is initiated by the addition of an alkaline iodide solution.
3. Iodine Titration (Third Step):
I2 + 2S2O3^2- -> 2I^- + S4O6^2-
In the third step, the iodine (I2) produced in the second step is titrated with a standardized
solution of sodium thiosulfate (Na2S2O3). This reaction results in the conversion of iodine to
iodide ions and the formation of a complex ion called tetrathionate (S4O6^2-).