Chem111E Chemistry of Engineers Activity 07.

Determination of Dissolved Oxygen Content of Water | 1

Chem111E Chemistry of Engineers

Semester 1, AY2021-2022
Activity 07 (Determination of Dissolved Oxygen Content of Water)

Instructions:

1. Divide the class into four (4) groups.

2. Watch the recorded video of the experiments on the link indicated below. DO NOT perform the experiments at home.
3. Make a laboratory report based on the experiment conducted in the video. The template can be found on pages 2 to 4
of this document.
4. Convert the laboratory report in PDF file and rename it as “Group#_CE1D/E_Chem111E”.
5. Submit the pdf file thru MS teams under Chem111E Laboratory.
Channel > Chem111E Laboratory > Activity 07 > Chem111E Activity 07 Submissions
6. All submissions must be in on/before December 17 (Friday, 9AM) the indicated deadline in the material.

Experiments:

Refer to the link indicated below to watch the series of experiments conducted to determine the amount of dissolved
oxygen in the water sample.

https://www.youtube.com/watch?v=frtln5ZoeNQ
Chem111E Chemistry of Engineers Activity 07. Determination of Dissolved Oxygen Content of Water | 2

Chem211E Organic Chemistry

Semester 1, AY2021-2022
Activity 07 (Determination of Dissolved Oxygen Content of Water)

Students

List the name of students in the group and indicate each student’s contribution in accomplishing the laboratory report.

Students ID Number Contribution

Concepcion, Diana 21-02316 Methods B
Conclusion
Editor
Del Rosario, John Guiller 21-10093 Reagent 2: Materials and Methods

Labrador, Jhon Mar 21-01275 Reagent 3: Materials and Methods

Mateo, Cherilyn 21-10005 Results and Discussion 1

Mosquito, Shaine 21-20039 Reagent 5: Materials and Methods

Rivera, Michael 21-22993 Reagent 6: Materials and Methods

Salvio, Mariel 21-20745 Reagent 1: Materials and Methods

Santiago, Keren Joy 21-21765 Reagent 8: Materials and Methods

Siriban, Dulce 21-40008 Reagent 4: Materials and Methods

Ziganay, Claire 21-40030 Reagent 7: Materials and Methods

Laboratory Report

Objectives:

The main objective of the experiment is to determine the dissolved oxygen present in the water sample. Specifically,
it aims:
1. to familiarize on the preparation of reagents needed for the test are prepared;
2. to familiarize on the experimental procedure in determining the dissolved oxygen present in the water sample;
and
3. to calculate the amount of dissolved oxygen present in the water sample.

Introduction:

Dissolved oxygen (DO) levels in environmental water depend on the physiochemical and biochemical activities in
water body and it is an important useful in pollution and waste treatment process control. Two methods are commonly used
to determine DO concentration: (1) The iodometric method which is a titration-based method and depends on oxidizing
property of DO and (2) The membrane electrode procedure, which works based on the rate of diffusion of molecular oxygen
across a membrane.

In the Iodometric method, divalent manganese solution is added to the solution, followed by addition of strong alkali
in a glass-stopper bottle. DO rapidly oxidize an equivalent amount of the dispersed divalent manganese hydroxide
precipitates to hydroxides of higher valence states. In the presence of iodide ions in an acidic solution, the oxidized
manganese reverts to the divalent state, with the liberation of iodine equivalent of the original DO content. The iodine is
Chem111E Chemistry of Engineers Activity 07. Determination of Dissolved Oxygen Content of Water | 3

then titrated with a stranded solution of thiosulfate. The titration end point can be detected visually with a starch indicator.
Some oxidizing and reducing agents present in solution can interfere with the iodometric method. Oxidizing agents liberate
iodine from iodides (positive interference) and some reducing agents reduce iodine to iodide (negative interference). Also,
organic matter present in solution can be oxidized partially in the presence of oxidized manganese precipitate, thus causing
negative errors. Thus some modification of procedure is required.

Materials:

List the compounds needed to prepare the reagents used in the experiment. In addition, enumerate the laboratory tools
and types of equipment used to perform the experiment. Follow the below table to indicate your answers in this part of the
report.

Reagent 1. Manganese sulfate solution

Compounds Laboratory tools and Equipments
48g Manganese Tetrahydrate/
40g Manganese Sulfate /
100 ml beaker
36.4g Manganese Sulfate
Monohydrate
Deionized water Stirring rod
Dilute Sulfuric acid Volumetric flask (100ml)
Funnel

Reagent 2. Alkaline-iodide-azide reagent

Compounds Laboratory tools and Equipments
50g Sodium Hydroxide/
250ml beaker; 10ml beaker
70g Potassium Hydroxide
13.5 Sodium iodide/
Stirring rod
15g Potassium iodide
Deionized water Volumetric flask (100ml)
1g Sodium azide Funnel
Salt Pipette

Reagent 3. Concentrated sulfuric acid

Compounds Laboratory tools and Equipments

Reagent 4. Starch indicator solution

Compounds Laboratory tools and Equipments
Soluble starch powder Beakers
Deionized water Stirring rod
Salicylic acid Droppers
Formaldehyde Gloves and goggles

Reagent 5. Standard sodium thiosulfate titrant

Compounds Laboratory tools and Equipments
3.1025g sodium thiosulfate 100mL/250mL beaker
Deionized water 1000mL volumetric flask
Chem111E Chemistry of Engineers Activity 07. Determination of Dissolved Oxygen Content of Water | 4

0.4g solid sodium hydroxide Funnel

Stirring rod
Gloves and goggles

Reagent 6. Standard potassium dichromate solution

Compounds Laboratory tools and Equipments
0.613g dry potassium
100/250ml Beaker
dichromate
Deionized water Droppers
1000 ml Volumetric flask
Funnel bottle
Stirring rod

Reagent 7. Potassium iodide crystals

Compounds Laboratory tools and Equipments

Reagent 8. 10% sulfuric acid

Compounds Laboratory tools and Equipments
Concentrated sulfuric acid Pipette
Deionized water Burette and burette stand
Starch 1000ml Erlenmeyer flask
Standard thiosulfate solution Stirring rod
10% dilute sulfuric acid 250ml Beaker

Potassium dichromate 10ml Beaker

Potassium Iodide

Methods:

Discuss the procedure done in each reagent preparation and dissolved oxygen determination based on the video
presented. Describe the methods as completely as possible. Indicate concentration of each reagent prepared.

A. Reagent Preparation

A.1 Manganese sulfate solution

1. Prepare a beaker for manganese sulfate and deionized water.
2. Weigh 48 grams of manganese sulfate tetrahydrate in a 100 ml beaker.
3. Add about 30 ml of deionized water to the reagent.
4. Stir it using a steering rod until it dissolves completely.
5. Once dissolved, transfer the solution into a 100 ml of volumetric flask.
6. Rinse the flannel with deionized water.
7. Add some ml of deionized water for the complete a 100ml final volume.
Chem111E Chemistry of Engineers Activity 07. Determination of Dissolved Oxygen Content of Water | 5

A.2 Alkaline-iodide-azide reagent

1. Prepare all needed materials

2. In a 250mL beaker, mix 50g of sodium hydroxide or 70g of potassium hydroxide along with 13.5g of
sodium iodide or 15g of potassium iodide.
3. Add 30mL of deionized water to the mixture and and stir until it dissolves.
4. Cool the mixture and transfer it to a hundred mL volumetric flask using a funnel.
5. In a separate container, 10mL beaker, mix 1g of sodium azide along with 4mL of deionized water using
a Pipette. Stir until the salt is dissolved.
6. Add the mixture (on method 5) into the volumetric flask, arriving at a 200mL volume.
7. Wash the used materials.

A.3 Concentrated sulfuric acid

A.4 Starch indicator solution

1. Weigh 1 gram of soluble starch powder in a small beaker

2. Add 5 ml of deionized water
3. Mix the contents to form a paste
4. Carefully add this paste 200 ml of boiling hot deionized water in a 250 ml beaker
5. You may also add 0.5 grams of salicylic acid or.0.5 ml of formaldehyde as a preservative into the starch
solution
6. Stir the content to dissolve the salicylic acid completely
7. Let the solution cool.

A.5 Standard sodium thiosulfate titrant

1. Prepare the 3.1025g of sodium thiosulfate in a 100mL/250mL beaker.
2. Add some amount of deionized water to the beaker, the stir using the stirring rod to completely dissolve
the thiosulfate.
3. After dissolving the sodium thiosulfate in the beaker, transfer it into a 1000mL volumetric flask using a
funnel.
4. As you transfer the contents of the beaker, wash down the funnel, stirring rod, and the beaker with
deionized water.
5. Lastly, add 0.4g or 5mL of chloroform to prevent thiosulfate deterioration.

A.6 Standard potassium dichromate solution

1. To prepare this way place the 0.613 grams of dry potassium dichromate in a 100 or 250ml beaker.
2. add some amount of deionized water and stir to completely dissolve the dichromate salt.
3. transfer the solution into a 1000 ml volumetric flask using a funnel.
4. Wash down the funnel the stirring rod and the beaker using deionized water.
5. Make up the final volume to 1000ml using the deionized water.

A.7 Potassium iodide crystals

A.8 10% sulfuric acid

1. Pipette out 10 ml of concentrated sulfuric acid into a small beaker.
2. Transfer 90 ml of deionized water into a 250 ml beaker.
3. Then slowly and carefully add the sulfuric acid into the deionized water with constant stirring
4. Allow the solution to cool down.
5. Begin the testing of the water sample for its dissolve oxygen content.
6. Standardize first the sodium thiosulfate solution if it was prepared a few weeks prior to the experiment
the standardization step may be avoided if you're using a freshly prepared thiosulfate solution
standardization can be done using either sodium by iodate or potassium dichromate.
7. In this video, we'll be following the dichromate method for the standardization procedure using
potassium dichromate way 2 grams of potassium iodide in a small beaker and introduced into a 1000
ml Erlenmeyer flask.
8. Wash it down and dissolve in it about 150 ml of deionized water.
9. Add to this 10 ml of 10% dilute sulfuric acid using a 10 ml pipette.
Chem111E Chemistry of Engineers Activity 07. Determination of Dissolved Oxygen Content of Water | 6

10. Then using a 10 ml or a 20 ml pipette introduce exactly 20 ml of standard potassium dichromate into
the flask.
11. Place the flask in the dark for about 5 mins.
12. Then add about 220 ml of deionized water to make up the final volume to 400 ml.
13. Meanwhile, fix the burette and the burette stand and fill it with standard thiosulfate solution prepared
previously.
14. Adjust the level of the lower meniscus to the zero mark.
15. Then titrate the dichromate solution in the flask with a thiosulfate solution in the burette drop wise till
the solution in the flask becomes pale yellow.
16. Then add about 5 drops of the starch indicator solution to the flask, a blue color is produced.
17. Continue adding the thiosulfate drop wise into the flask until the first disappearance of the blue color.
18. If exactly 20 ml of the thiosulfate in the burette was used up to bring about the titration endpoint it
means that the thiosulfate is indeed of exactly 0.0125 normal concentration.

B. Dissolved oxygen Determination

On determining the dissolved oxygen of a water using Modified Winkler’s Method (Azide), the following are the
methods that has been done base on the video experiment:

1. Prepare the needed materials and laboratory tools such as:

 1ml Manganese sulfate  3-5 drops Starch indicator
solution solution
 Water sample  Pippettes
 1 ml Alkaline-iodide azide  BOD bottle
reagent  Waste beakers
 Sodium thiosulfate solution  Burette
 1ml concentrated sulfuric  Funnel
acid  Cylinder
 Standard thiosulfate solution  200/250ml Erlenmeyer flask

Since there are three main steps on Dissolved Oxygen Determination, we will perform first the fixation of the
oxygen, dissolving the precipitate, and titration respectively.

2. Fill the BOD bottle with the sample water through submerging the bottle into the water with its stopper.
Carefully remove the stopper under the water and fill the bottle until there’s no oxygen inside it, and
close the bottle while it is submerged in the water.
3. Next is the fixation step, you can perform it in the field or laboratory.
a) Carefully remove the stopper, and add 1ml of Manganese sulfate solution using a 1ml pipette
in the water sample.
b) Using another pipette, add 1 ml alkaline azide reagent. Make sure that the pipette is below the
water surface while adding the reagents.
c) Put the stopper on the bottle. Make sure that there are no air bubbles formed. After that you’ll
observe a brownish precipitate of Manganese hydroxide that begins to form in the bottle.
Note: The intensity of the brown color is directly proportional to the dissolved oxygen
content in the water sample. Pale yellow means low DO, while dark brown means high DO.
d) Pour the excess water sample into the waste beaker. And mix the reagents in the bottle by
inverting the bottle several times.
e) Allow the precipitate to settle down. And now the oxygen is already fixed into as more stable
form. If the situation permits, you can now move onto the next step, if not, you can wait for up
to 8 hours.
4. Before moving in dissolving the precipitate, fill the burette up to the 0 mark with the standard thiosulfate
solution using a funnel. Let it aside.
5. Next is the dissolving of precipitate.
a) Using 1ml pipette, add 1ml of concentrated sulfuric acid by letting it flow down along the neck
of the bottle. Make sure that the pipette is just beneath the water surface. And carefully put the
stopper.
b) Remove the excess and place it in the waste beaker.
c) Dissolve the precipitate by inverting the bottle several times.
d) Take a 100ml of the sample using a 100ml pipette or cylinder. Place it in a 200 or 250ml
Erlenmeyer flask.
6. For the last step, titration.
Chem111E Chemistry of Engineers Activity 07. Determination of Dissolved Oxygen Content of Water | 7

a) Titrate the sample using the standard thiosulfate solution in the burette.
b) Run the thiosulfate drop-wise from the burette until the brown color of the sample turns pale
yellow or straw yellow.
c) Add 3-5 drops of starch indicator solution in the sample and mix well.
d) If the sample turned blue, immediately continue the titration until the sample becomes clear.
7. For better results or accuracy, repeat titration procedure three times.

Results and Discussion:

1. Summarize, analyze, and discuss the result of the experiments. Discussion must NOT be more than 3 sentences.
Follow the below table to indicate your answers in this part of the report.

Table 1. Experiment Observations

Steps in Determination of DO Observation Reaction/s

Based on the oxygen
fixation in the
experiments, the
dissolved oxygen in the Based on the experiment,
sample is then fixed by as it adds different
adding a series of reagents concentration its
reagents that form an acid color changes and turn it
compound that is then back to its original color.
titrated with a neutralizing As it undergo oxygen
Oxygen fixation
compound that results in a fixation, Oxygen
color change. Moreover, saturation is more soluble
the oxygen content of the in cold waters, hence
water sample also has cold waters generally
been fixed to a more have higher dissolved
stable form and DO in oxygen concentration.
water is affected by the
water temperature and
salinity.
Dissolve precipitate In our observation, DO
rapidly oxidize an
equivalent amount of Based on the experiment,
the dispersed divalent as the sample adds
manganese hydroxide concentrated sulphuric
precipitates to hydroxides acid there are tiny
of higher valence states. particles that appears but
In the presence of iodide as it shakes the bottle all
ions in an acidic solution, the precipitate were
the oxidized manganese dissolved. No bubbles
reverts to the can be seen in the
divalent state, with the dissolve precipitate of the
liberation of iodine solution.
equivalent of the original
DO content
Titration We observed, that the As the sample adds a
titration end point can be starch indicator the color
detected visually with a of the sample becomes
starch indicator. Some colorless and with the use
oxidizing and reducing of titration we can
agents present in solution determine the dissolved
can interfere with the oxygen in the water
iodometric method. sample.
Chem111E Chemistry of Engineers Activity 07. Determination of Dissolved Oxygen Content of Water | 8

2. Based from the experiment using the reagents prepared, show an empirical formula to calculate the dissolved
oxygen (DO).

MnSO4 + 2H2O + (2NaOH + 2KI ) + NaN3 + sample  Mn (OH)2 + sample + K2SO4 + Na2O2 + NaOH + NH3
+ N2I2

Empirical Formula of the Dissolved Oxygen: Mn(OH)2

3. Show an empirical formula to relate the dissolved oxygen (DO) to biological oxygen demand (BOD).

Conclusion:

Reiterate general observations on the dissolved oxygen and its relation to biological oxygen demand. Integrate
concepts of chemistry in the results of the experiments. The conclusion must NOT be more than 200 words.

Dissolved oxygen (DO) is the amount of oxygen present in water, while biological oxygen demand (BOD) is the
amount of oxygen consumed by the organisms in the water. These two are inversely proportional to each other, which
means that a high DO results low BOD and vice versa. Dissolved oxygen can be affected by several factors like pressure
of the water, salinity, and level of organic activities in it. These factors determine the range of the oxygen dissolved in the
water wherein 5-8mg/L is the ideal range of DO, while lower than 5mg/L will be fatal to the living organisms present in
the water.
There are different methods on measuring DO, one of it is the titrimetric method, where traditional Winkler’s method,
and the modified version are used. These ways are similar in the final volume, it is just that the modified adds azide reagent
in the solution to eliminate nitrites. Also, determining DO using Winkler’s method has three steps oxygen fixation,
dissolving precipitate, and titration. The amount of DO can be calculated by N/80 (0.0125N) as long as sodium thiosulfate
is used as titrant. Note that 1ml of consumed titrant is equal to 1mg/L of DO in the sample.

References:

List down the references used to accomplish this laboratory report.

https://archive.epa.gov/water/archive/web/html/vms52.html

https://www.vedantu.com/question-answer/relationship-between-do-and-bod-is-that-they-a-class-12-biology-cbse-
5fbbe1a9896fdc2ad9622ac6