EXPERIMENT NO.

TITLE: Determination of the Amount of Dissolved Oxygen in a Water Sample

OBJECTIVES

 To determine the amount of dissolved oxygen in a water sample

 Identify the volume of Sodium Thiosulfate used during the titration.

PRINCIPLES INVOLVED

 Wrinkler method

MATERIALS

 1000 mL Beaker  1L Amber bottle w/  250 mL Volumetric

cover Flask

 Burette  Test tube rack  Wash bottle

 Iron stand  Wire gauze  25 mL Pipette

 Burette clamp  Dispirator  250 mL Erlenmeyer

 Electric stove  Stirring rod Flasks (5)

 Test tube (3)  Funnel  10 mL Graduated

cylinder

CHEMICALS

A. KI-NaOH solution (20 g of KI, 36 g NaOH and 0.5 g sodium azide dissolved in

distilled water and diluted to 100 mL mark of the volumetric flask)

B. Manganese (II) Sulfate (45 g of MnSO4.4H2) in sufficient distilled water to

make 100 mL).

PROCEDURE

A. Preparation of Approximately 0.1 M Sodium Thiosulfate Solution

1. Boil 1000 mL distilled water for at least 5 minutes.

 2. Cool and add about 25.0 g of Na2S203.5H2O and 0.2 g of Na2CO3

3. Stir until solution is complete.

4. Transfer to a clean stoppered bottle (glass or plastic)

5. Store solution in clean, tightly capped amber bottle to protect it from light and air.

B. Preparation of primary Standard Potassium Iodate (KIO3)

1. Dry 1.5 g of KIO3 (potassium iodate) for 1-2 hours at 110℃

2. Store in desiccator until cool and ready to be weighted.

3. Prepare 0.01 M standard potassium iodate solution (analytical balance).

4. Add 0.5 g of the dried solid reagent and dissolving it in distilled water in a 250 mL

volumetric flask.

5. Calculate molar concentration of the solution from the exact weight of the

reagent used.

C. Standardization of Sodium Thiosulfate Solution

1. Pipet 50 mL of KIO3 solution into a 250 mL Erlenmeyer flask.

2. Add 2 g of solid KI (potassium iodide) and 10 mL of 0.5M H2SO4

3. Titrate this solution with Na2S2O3 solution from the burette until the initial

red-brown color of the solution turns to pale yellow.

4. Add 2 mL of starch indicator and complete titration just at the disappearance

of the blue color, marking the end-point.

5. Repeat the titration with two additional 50 mL aliquots of KIO3 solution. Record the date

and calculate the molarity of the Na2S2O3 solution.

Sampling:

1. With soap and water clean thoroughly a one-liter bottle with cap. Let dry in the air.

2. Immerse the capped bottle about one foot below the surface of the pond (lake, river or any

fresh water body). Remove the cap and allow water to enter the bottle until it is completely filled.
3. Put the cap back on the bottle while still immersed below the surface. Gently lift the bottle out

of the water and avoid unnecessary agitation.

4. Analyse for D.O right away. If this is not possible, store the sample in a refrigerator and protect

from light

Analysis Dissolved Oxygen Content.

1. Clean a 50-mL burette thoroughly and rinse twice with distilled water. Then rinse the burette

three times with 10-mL portions of standard Na2S2O3 solution.

2. Fill the burette with standard Na2S2O3 solution making sure there is no air gap at the tip and

clamp it to an iron stand.

3. Measure 3 mL of 1% starch indicator into a clean test tube. Set aside.

4. Open the sample bottle with great care, avoiding aeration of the surface of the sample with

bubbles of undue agitation

5. Add8 ml of MnSO4 solution from a glass pipette; discharge the reagent well below the surface

(some overflow will occur)

6. Similarly, introduce 8 mL of the KI-NaOH solution. Place the stopper in the bottle be sure that

no air becomes entrapped. Invert the bottle several times to distribute the precipitate uniformly.

After shaking the sample, let the bottle stand for a few minutes to allow the precipitate to settle.

When the precipitate has settled leaving the supernatant clear, shake again (IMPORANT; DO

NOT PROCEED TO THE NEXT STEP UNTIL ALL THE PRECIPITATE HAS SETTLED DOWN.)

7. When the precipitate has settled at least 3 cm below the stopper, introduce 8 mL of

concentrated (18 M) H2SO4 well below to the surface. (Care should be taken to avoid exposure

to the overflow, as the solution is quite alkaline.) replace the stopper and mix until the precipitate

dissolves. Let it stand for 10 minutes.

8. When the precipitate has dissolved and the sample has become uniformly colored pipet 200

mL of the acidified sample into a 250 mL Erlenmeyer flask

9. Titrate with standard Na2S2O3 until the iodine color becomes faint (pale yellow) Add the starch

indicator and continue titration until the blue color completely disappears for the first time.

10. Analyze the triplicate samples.

11. Discard the remaining sample in your bottle and fill it to the brim with tap water. Determine

the total volume of your water sample by pouring the water into a large graduated cylinder. Record

the volume.

RESULTS

Data

Table A. Determination of volume of sodium thiosulfate for two trials

Initial Reading Final Reading

Trial 1 0.0 mL 34.7 mL

Trial 2 0.0 mL 35.9 mL

Table B. Determination of D.O. in Water Sample

Trial 1 Trial 2 Trial 3

Volume of the sample 250mL 250mL 250mL

Initial Reading of
0.1 mL 0 mL 0 mL
Na2S2O3

Final Reading of
3 mL 2.5 mL 2.6 mL
Na2S2O3

Volume of Na2S2O3
3 mL 2.5 mL 2.6 mL
used

Ppm D.O. 18.113088 15.094240 15.698009 Average D.O.

ppm D.O. ppm D.O. ppm D.O. 16.301779 ppm D.O.

Total volume of water

sample 1009. 2 mL
Calculations:

106
ppm D.O.  mL Na2 S 2O3 X N Na2 S 2O3 X 0.008 X
mL sample

A. Dissolved Oxygen Content Determination

Trial 1:

106
ppm D.O.  mL Na2 S 2O3 X N Na2 S 2O3 X 0.008 X
mL sample

10 6
ppm D.O.  3mL Na2 S 2O3 X 0.188678Na2 S 2O3 X 0.008 X
250 mL sample

ppm DO  18.113088 ppm DO

Trial 2:

106
ppm D.O.  mL Na2 S 2O3 X N Na2 S 2O3 X 0.008 X
mL sample

10 6
ppm D.O.  2.5mL Na2 S 2O3 X 0.188678 Na2 S 2O3 X 0.008 X
250 mL sample

ppm DO  15.09424 ppm DO

Trial 3:

106
ppm D.O.  mL Na2 S 2O3 X N Na2 S 2O3 X 0.008 X
mL sample

106
ppm D.O.  2.6mL Na2 S 2O3 X 0.188678Na2 S 2O3 X 0.008 X
250 mL sample

ppm DO  15.698009 ppm DO

Average D.O =16.301779 ppm DO

DISCUSSION
 In this experiment, students are task to find the amount of dissolved oxygen in a water

sample. In order to find the result, student began to put a 200 mL of the acidified sample into a

250 mL Erlenmeyer flask. Then, started the titration using Na2S2O3. The sample in an Erlenmeyer

flask was noticeable turning into a pale yellow as every drop of Na2S2O3 is added onto it. Then,

students add 8 mL of starch solution onto the Erlenmeyer flask in which the solution turned to

green as soon as the starch was added. The green color in the Erlenmeyer flask slowly turns to

become clear. As the solution became clear students stopped the titration and repeat the

procedure for a second trial and third trial. Then, the students record the Na2S2O3 used that can

be used to identify or calculate the ppm dissolved oxygen. Then, the students calculated an

average dissolved oxygen in ppm which is 16.301779 ppm D.O.

The sample was taken in the Pangi River in Matina Pangi, Davao City. Within the coordinates

of 7o4’37.8 N, 125o33’48.09 E.

CONCLUSION

The students found out that the sample gathered in the river water in Pangi River could be

slightly fit for fishes to live since the ppm dissolved oxygen of the water sample is 16.301779 ppm.

A dissolved oxygen level that is too high or too low can harm aquatic life and affect the water

quality. Organisms in the shallow water need a 4-15 ppm of dissolved oxygen in order to survive.

Where the water sample in Pangi River is just near to the needed ppm dissolved oxygen of the

organisms. According to USEPA, the fishes do well when the dissolved oxygen is five parts per

million (ppm) (= 5/1,000,000) or higher. Therefore, the Pangi River would be fit for fishes and

other organisms.

Guide Questions:
Comment on the various uncertainties and biases involved in this analysis. What do you
think the limit of accuracy is in this experiment (that is, estimate the cumulative value of
the random and determinant errors)?
 Some errors on this experiment might came from small details from the procedure like the
entrapment of air during the process and the accuracy of the measurements using the apparatus.
Errors might also include, even from the start of the sampling, while getting water from the river.
Some procedures might not been followed.
How is the chemical oxygen demand of Chemical Oxygen Demand (COD) different from
Biochemical Oxygen Demand (BOD)?
Biochemical Oxygen Demand, is the amount of oxygen in mg/l that microorganisms need to
consume the organic pollutants (sugars, fat, proteins). Biochemical Oxygen Demand can be
normally higher in polluted water than freshwater.
Chemical Oxygen Demand on the other hand is the amount of oxygen required to degenerate
all pollution chemically. It refers to the required amount of dissolved oxygen for the oxidation of
organic matter and inorganic constituents.

Give the effect of adding sulfuric acid prior to the addition of NaOH-KI solution.
Adding sulfuric acid to sodium hydroxide-potassium iodide will produce Sodium sulphate and
water. It is a neutralization reaction since sulfuric acid is an acidic solution and NaOH-KI is a basic
solution.