TABLE OF CONTENT

CONTENT
1. Abstract / summary
2. Introduction
3. Aims / objectives
4. Theory

PAGE
2
2-4
4
4-6

5. Apparatus and Materials

6. Experimental procedure

6-7

7. Result

7-10

8. Sample calculation

11

9. Discussion

11-12

10. Conclusion

13

11. Recommendation
12. References
13. Appendix

13-14
14
14-16

1.0 ABSTRACT
In this experiment, we have determined the amount of dissolved oxygen (DO) in the
water that was collected in the lake. Through observation, we know that the water
sample contained the oxygen by having colour of orange-brown with precipitate when
added with ManganousSulphate Powder Pillow with Alkali Iodide Azide Reagent Powder
Pillow and it have a colour of yellow when added with Sulfonic Acid Powder. Both of
these proves the existence of oxygen in this water sample.
Besides, there are many factors that affect the level of DO in water systems. The major
source of DO in lake is atmosphere. Waves and tumbling of water will mix the
atmospheric oxygen into the river. DO concentrations in water also increase due to the
oxygen produced by the roots of aquatic plants and algae as a product of
photosynthesis.
The amount of DO can be decreased due to several factors. There are high
temperature and the amount of bacteria and microorganism in a particular water
system. The factor of temperature may result from high turbidity, the return of industrially
used water to the riveror from drought. While, the second factor that can decrease the
amount of DO is bacteria which decompose plant material and animal waste will
consume DO that is present in the water, thus decreasing the quantity available to
support life.

2.0 INTRODUCTION
Comprising over 70% of the Earths surface, water is undoubtedly the most
precious natural resource that exists on our planet. Without the seemingly invaluable
compound comprised of hydrogen and oxygen, life on Earth would be non-existent: it is
essential for everything on our planet to grow and prosper. Although we as humans
recognize this fact, we disregard it by polluting our rivers, lakes, and oceans.
Subsequently, we are slowly but steadily harming our planet to the point where
organisms are dying at a very alarming rate. In addition to innocent organisms dying
off, our drinking water has become greatly affected as is our ability to use water for
recreational purposes. In order to combat water pollution, we must understand the
problems and become part of the solution.The complexity of water quality as a subject
is reflected in the many types of measurements of water and waste water quality.
The physical, chemical, and biological characteristics are the main criteria to
determine the quality of water. Basically, natural water contains impurities; whereas,
pure distilled water is composed of only oxygen (O 2) and hydrogen (H2). The treatment
of waste water requires us to determine the quality of water. The treatment depends
upon the quality of the raw water and the desired quality of treated water.
For this experiment, we are going to study about the dissolved oxygen in water.
Dissolved oxygen (DO) level is refers to the amount of oxygen dissolve in water and is
particularly important in aquatic ecology.Dissolved oxygen is a very important part in
determining the quality of a drinking. A high level of DO in water can be a sign that the
water is of a very good quality. For example, most of mineral water that had undergone
the reverse osmosis process had a very high level of DO.

3.0 OBJECTIVES
1. To learn the specific sampling technique in determining dissolved oxygen
concentration in a sample of water.
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2. To determine the concentration of dissolved oxygen in water sample.

3. To identify the factors affecting the concentration of dissolved oxygen in water
sample.

4.0 THEORY
The term Dissolved Oxygen is used to described the amount of oxygen dissolved in a
unit volume of water . Dissolved oxygen (DO) is essential for the maintenance of
healthy lakes and rivers. It is a measure of the ability of water to sustain aquatic life .The
dissolved oxygen content of water is influenced by the sources , raw water temperature
, treatment and chemical or biological processes taking place in the distribution
system .The presence of oxygen in water is a good sign. Depletion of dissolved water
supplies can encourage the microbial reduction of nitrate to nitrite and sulfate to sulfide.
It can also cause an increase in the concentration of ferrous iron in solution , with
subsequent discoloration at the tap when the water is aerated. Hence ,analysis of
dissolved oxygen is an important step in water pollution control and wastewater
treatment process control . there are various methods available to measure DO. In a
healthy body of water such as lake , river , or stream , the dissolved oxygen is about 8
parts per million. The minimum DO level of 4 to 5 mg/L is desirable for survival of
aquatic life .If that a source of oxygen demanding wastes , such as feed a lot , a paper
mill or a food processing plant , is built besides the river. The facility begins operating
and discharging wastes into the river. This increases the BOD and effects the
concentration of DO in the waters downstream. The wastes serve as the food for certain
aerobic bacteria as it moves downstreams , the concentration of bacteria increases.
Because these bacteria remove oxygen from water , their population increase causes a
4

decline in the amount of DO. Beyond certain point , most of the wastes break down. The
concentration of DO rises as the river recovers oxygen from the atmosphere and
aquatic plants. Thus , DO test is the basis for BOD test which is an important parameter
to evaluate organic pollution of a waste. It is necessary for all aerobic biological
wastewater treatment processes to control the rate of aeration.

5.0 APPARATUS AND MATERIALS

Figure1
1-Digital Titrator
3- J Delivery Tube

2- Sodium Thiosulfate Titration Cartridge

4. BOD bottle

5. Conical flask

Figure 3
6. Reagent Compartment

7. Starch Indicator Solution

Manganous Sulfate Powder Pillow

Alkaline Iodide Azide Powder Pillow
Sulfamic Acid Powder Pillow

6.0 PROCEDURES
OXYGEN DISSOLVED: Azide Modification of Winkler Method
1. A water sample was collected in a clean 100 mLBOD bottle.
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2. The contents of one Manganous Sulfate Powder Pillow and one Alkaline Iodide
Azide Reagent Powder Pillow were added.
3. The stopper was inserted immediately so that air does not trap in the bottle. The
bottle was inverted for several times to mix. A flocculent precipitate which was
orange brown(

O2

present ) or white (

O2

absent ) formed in the bottle. The

floc settled slowly in salt water. Step 4 was preceded when the floc settled.
4. The bottle was inverted for 5 minutes to ensure that the sample and reagents
reaction is complete. When the floc settled and the top half of the solution had
cleared, Step 5 was preceded.
5. The stopper was removed and the content of one Sulfamic Acid Powder Pillow
was added. The stopper was replaced without trapping air in the bottle. The
sample was inverted several times to mix. The floc dissolved and left a yellow
coloursolution (

O2

present ).

6. A sample volume and Sodium Thiosulfate Titration Cartridge were selected

corresponding with expected dissolved oxygen ( DO ) concentration.
7. Then a clean delivery tube was inserted into the titration cartridge to the titrator
body. After that, the delivery knob was turned to inject a few drops of titrant. The
counter is resetted to zero and the tip was wiped.
8. A graduate cylinder was used to measure the sample volume and the sample
was transferred to 250 mL Enrienmeyer flask.
9. The delivery tube was placed into the solution and the flask is swirled while the
solution was titrated with sodium thiosulfate to a pale yellow colour.
10. Next, to 1 mL dropper of starch indicator solution were added and the mixture
was swirled.
11. The titration was continued to get a colorless end point. The number of digits
required were recorded.
12. Finally, dissolved oxygen were calculated and being tabulated in a table.

7.0 RESULT
7

(I)

To determine the amount of dissolved oxygen in the water sample 100

mL BOD bottle

Reagent
ManganousSulphate

Observation
Powder Orang-Brown

Conclusion
with Oxygen is present

Pillow + Alkaline Iodide Azide precipitate

Powder Pillow
Sulfonic Acid Powder

Yellow colour

Oxygen is present

Digit required : 113

Digit multiplier : 0.02
Range dissolver oxygen : 2.26
(II)

20 mL BOD bottle

Reagent
(Dissolved

Oxygen

Observation
+ Orange-Brown

Conclusion
Oxygen is present

Dissolved Oxygen 2 + Dissolved

Oxygen 3 ) Reagent Powder
Pillow

Digit Required : 22
Digit Multiplier : 0.1
Range dissolver oxygen : 2.2

8.0 CALCULATIONS
Oxygen Dissolved (Azide Modification Of Winkler)
Using BOD bottle
8

Sample of calculation:
Digit Multiplier Digit Required = mg/L Dissolved Oxygen
100 mL (titration cartridge Na2S2O3, 0.2M)
0.02 x 113 = 2.26 mg/L as Dissolved Oxygen
20 mL (titration cartridge Na2S2O3, 0.2M)
0.1 x 22 = 2.2 mg/L as Dissolved Oxygen
9.0 DISCUSSION
This Basic Water Properties 1 experiment was carried out to:
1. Study the method used to detect the concentration of dissolved oxygen in water
sample.
2. Determine the concentration of dissolved oxygen in water sample.
3. Identify the factors affecting the concentration of dissolved oxygen in water
sample.
The water sample that we used in this experiment was from Tasik Shah Alam
Seksyen 7. From the experiment, the concentration of dissolved oxygen in water can be
detected using the Hach Dissolved Oxygen Kit. There were 3 types of powder pillow
used to detect the dissolved. The first one was the Manganous Sulfate Powder Pillow.
The Manganous Sulphate Powder Pillow was added into water sample together with the
Alkaline Iodide-Azide Powder Pillow.
What is going on in this step:

Reagent Powder Pillow #1 (Manganous Sulfate) MnSO4

This powder packet contains a powdered chemical called Manganous Sulfate
which reacts with the oxygen present in the water. During the reaction, the
9

oxygen is bound to the manganese (chemical element Mn), forming a brownish

solid which settles to the bottom of the bottle (MnO 2). This process is called
fixing the oxygen. In order for this fixation process to work however, the solution
must be at high pH, so we need another reagent to make this occur...
MnSO4 + O2

MnO2 (brown)

Reagent Powder Pillow #2 (Alkaline Iodide Azide)

If the Manganous Sulfate fixes the oxygen dissolved in the water, why do we need more
chemicals? There are three specific chemicals present in packet #2 which are important
to the fixation of the oxygen.
o LiOH (Lithium Hydroxide) is a base, which means that in water it breaks
up to form the OH- ion, and the Li+ ion. In this reaction, LiOH basically just
functions as a catalyst to activate the binding process. The binding
process involved with Manganous Sulfate requires a high pH to proceed.
The addition of LiOH does just that.
o KI (Potassium Iodide) is added to function as a dye, and will react with
the sulfamic acid added, as explained below.
o NaN3 (Sodium Azide) is an agent added which will not come into play
until later in the reaction sequence. Because we will not come back to it, a
quick explanation is appropriate. (For a more in-depth explanation, see the
Winkler method titration page.) Basically during the final titration, Sodium
Thiosulfate produces some nitrite (NO2-) which conflicts with the intended
reaction. The addition of Sodium Azide prevents this conflictual reaction
from occuring.
After that the third powder pillow, Sulfamic Acid Powder Pillow was added into the
water sample.
10

What is this mysterious Sulfamic Acid Powder Pillow?

Reagent Powder Pillow #3 (Sulfamic Acid C 6H13O3NS) Upon addition of the

Sulfamic Acid, the MnO2 from above is reduced to Mn 2+, and the Iodine from the
Potassium Iodide above is oxidized by the MnO 2 from I- to I2. This reaction step
effectively causes the solution to take on a yellow-ish brown color proportional to
the number of I2 molecules present which in turn is proportional to the original
amount of O2 molecules in the water.
MnO2 + 4H+ + 2I- = Mn2+ + I2 + 2H2O (yellow)

We say at this point, that the oxygen is fixed. This means that all of the oxygen from the
original sample which was in solution has now been chemically modified to a form which
won't change when exposed to the air. It is now in a stable form, and can be transported
back to a classroom for analysis if necessary.
The water sample was titrated with 0.2 M Sodium Thiosulfate to a pale yellow
colour. A dark blue solution was formed when Starch Indicator solution was added. The
titration was continued until a colourless solution was obtained.
From the Digital Titrator, the value obtained was 113. So by multiplying it with the
digital multiplier, we got the concentration of dissolved oxygen in water sample to be
2.26 mg/L. The value of dissolved oxygen was quite high, so this water was suitable for
aquatic organism. This high concentration of dissolved oxygen was mainly due to the
high density of algae surrounding the sewage system. On a bright day, these algae will
carry out photosynthesis and oxygen will be produced. This oxygen will easily dissolve
in the water as the sewage run continuously.

10.0 CONCLUSION
This experiment was a big success. All of the objectives in this experiment had been
achieved. The result was:

11

1 To study the method used to detect the concentration of dissolved oxygen in

water sample by using the Hach Dissolve Oxygen Kit.
2 To determine the concentration of dissolved oxygen in water sample 2.26 mg/L
3 To identify the factors affecting the concentration of dissolved oxygen in water
sample large population of algae surrounding the lake, the continuous
movement of water in the lake had encourage the oxygen to dissolve into the
water.
11.0 RECOMMENDATIONS
These are the steps to obtain better results of the experiment.

Firstly , if the sample was obtained by a sampling device of some kind , the water
cannot be simply poured into a BOD bottle, since this would cause aeration of

the sample .
Instead , the sample must be drawn off from a tube located near the bottom of
the sampling device. Place the rubber tube into the bottom of the BOD bottle and
fill the bottle , again allowing the bottle to overflow. For shallow depth use normal

water samplers .
However for depth greater than 150 cm use Kemmerer Sample Bottles.

12.0 REFERENCES
http://www.kimia.um.edu.my/images/kimia/lab%20manual/level%202/Experiment
%20SCES2441-AnalisisLevel2.pdf
http://www.uic.edu/classes/cemm/cemmlab/Experiment%201-Water%20Content.pdf
http://nitttrc.ac.in/Four%20quadrant/eel/Quadrant%20-%201/exp10_pdf.pdf
http://intro.chem.okstate.edu/1515SP01/Laboratory/Propertiesofwater.pdf

12

13.0 APPENDIX
PROPOSED NATIONAL WATER QUALITY STANDARDS FOR MALAYSIA

Classes
Parameters
Unit

IIA

IIB

III

IV

Ammoniacal-N

mg/L

0.1

0.3

0.3

0.9

2.7

>2.7

BOD

mg/L

12

>12

COD

mg/L

10

25

25

50

100

>100

DO

mg/L

5-7

5-7

3-5

<3

<1

6.5-8.5

6-9

6-9

5-9

5-9

Ph
Colour

TCU

15

150

150

Elec. Cond

mhos

1000

1000

6000

Floatables

Odour

0.5

500

1000

4000

Salinity*

Taste
Tot. Diss. Sol.*

mg/L

13

Tot. Susp. Sol.

mg/L

Temperature

25

50

Normal

50

NTU

counts/100

10 -

F. Coliform**

300

>300

Normal
-

Turbidity

150

50

50

100

400

5000

5000

ml
(20000)

(20000)

e
counts/100
Total Coliform

100

5000

5000

50000

50000

>50000

ml

Before adding sulfarnic acid, flocculation

happen
14

After adding of sulfarnic acid

Digital Titrator with Sodium Thiosulfate

Cartridge

15