REPORT OF CHEMISTRY I LABORATORY

DETERMINATION OF DISSOLVED OXYGEN IN WATER

By :
Group : 4

Name / NRP : Cindy Suyitno / 5503017008

Name / NRP : Bary Leonard / 5503017018
Name / NRP : Clara Selin / 5503017029

ANALITICAL CHEMISTRY AND INSTRUMENT LABORATORY

CHEMICAL ENGINEERING DEPARTMENT
ENGINEERING FACULTY
WIDYA MANDALA CATHOLIC UNIVERSITY SURABAYA
2018

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 FEEDBACK FORM

DETERMINATION OF DISSOLVED OXYGEN IN WATER

Day, date of experiment: Thursday, April 26th 2018

By :
Group : 4

Name / NRP : Cindy Suyitno / 5503017008

Name / NRP : Bary Leonard / 5503017018
Name / NRP : Clara Selin / 5503017029

Assistant: Dra. Adriana A. A., M.Si

FEEDBACK RECORD

Submission Date of
Feedback Assistant signature
date return

ii
 CONTENT

REPORT COVER i

FEEDBACK FORM ii

CONTENT iii

CHAPTER I. INTRODUCTION 1

I. 1. Objective 1
I. 2. Literature review 1

CHAPTER II. EXPERIMENTAL METHOD 4

II. 1. Materials and apparatus 4

II. 2. Experimental procedure 5
II. 3. Solution preparation 6

CHAPTER III. RESULT AND DICUSSION 11

III. 1. Results 11
III. 2. Calculation 12
III. 3. Discussion 12

CHAPTER IV. CONCLUSION 15

REFERENCES 16

APPENDIX 17

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 CHAPTER I

INTRODUCTION

1.1.Objective
To be able to:
1. Determine the sample density using pycnometer
2. Calculate the oxygen percentage in water sample

1.2. Literature review

DISSOLVED OXYGEN IN WATER
The dissolved oxygen concentration of water is defined as the number of
milligrams of dioxygen gas (O2) per liter of water (mg/l). Dissolved Oxygen in a
stream may vary from 0 mg/l to 18 mg/l. Readings above 18 mg/l are physically
impossible. Dissolved oxygen gets into the water by diffusion from the atmosphere,
aeration of the water as it tumbles over falls and rapids, and as a waste product of
photosynthesis. Decreased DO levels may be indicative of too many bacteria and an
excess amount of biological oxygen demand -BOD (untreated sewage, partially treated
sewage, organic discharges, anoxic discharges) which use up DO. (Oram, 2014)

Water Quality Index Chart- Based on DO and BOD

(https://www.water-research.net/index.php/dissovled-oxygen-in-water)

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The concentration of dissolved oxygen (DO) is affected by:
 Plant activity : DO levels fluctuate throughout the day, increasing during the
morning and peaking in the afternoon. Decreases occur at night when
photosynthesis ceases and plants and animals continue to respire using oxygen.
 Temperature : it affects the ability of water to dissolve oxygen due to different
solubilities at different temperatures. Cooler water have a greater capacity to
dissolve oxygen than warmer water.
 Decaying organic matter in water: decomposition releases heat, warming water
and decreasing dissolved oxygen capacity.
 Stream flow: the faster the water moves and churns, the greater the amount of
oxygen is dissolved.
 Altitude/atmospheric pressure: high altitudes and atmospheric pressure reduce
dissolved oxygen capacity
 Human activities: removal of shade or the release of warm water used in industrial
processes can cause an increase in water temperature, resulting in lower dissolved
oxygen capacity. (Johnson, 1999)

A high DO level in a community water supply is good because it makes

drinking water taste better. However, high DO levels speed up corrosion in water
pipes. For this reason, industries use water with the least possible amount of dissolved
oxygen. Water used in very low pressure boilers have no more than 2.0 ppm of DO,
but most boiler plant operators try to keep oxygen levels to 0.007 ppm or less.
Dissolved oxygen (DO) refers to the amount of oxygen dissolved in water. The amount
of oxygen water can hold depends upon temperature (more oxygen can be dissolved
in colder water), pressure (more oxygen can be dissolved in water at greater pressure),
and salinity (more oxygen can be dissolved in water of lower salinity). Many lakes and
ponds have anoxic (oxygen deficient) bottom layers in the summer because of
decomposition processes depleting the oxygen.

Microbes play a key role in the loss of oxygen from surface waters. Microbes
use oxygen as energy to break down long-chained organic molecules into simpler,
more stable end products such as carbon dioxide, water, phosphate and nitrate. As
microbes break down the organic molecules, oxygen is removed from the system and

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must be replaced by exchange at the air-water interface. Each step above results in
consumption of dissolved oxygen. If high levels of organic matter are present in a
water, microbes may use all available oxygen. (APEC Water, 2017)

WRINKLER METHOD TITRATION

The Winkler titration method measures the amount of dissolved oxygen in

water samples. The results of the experiments determine the health of a particular body
of water and can also predict other oxygen-related activities in the water. This method
remains in use and also serves as a basis for adaptations made to methods for testing
dissolved oxygen in both fresh and saltwater samples. The Winkler method uses a 300-
milliliter sample of water. Added to the water are two reagents: 2-milliliter manganese
sulfate and 2-milliliter alkali-iodide-azide. These reagents are added individually
under the surface of the water and slowly to prevent exposure to oxygen through
bubbles. The solution is inverted to mix the reagents together with the water, and then
2 milliliters of concentrated sulfuric acid get added from above the water surface. This
completed solution then becomes titrated with drops of sodium thiosulfate until it
produces a pale straw color. After completion, scientists add 2 milliliters starch
solution, which turns the water solution blue. Individual drops of sodium thiosulfate
are titrated into the solution until the solution becomes clear, which marks the end of
the process. Each milliliter of sodium thiosulfate equates to one milligram per liter of
dissolved oxygen. The total milliliters of sodium thiosulfate used to turn the solution
pale straw, and then clear, equates to the total amount of dissolved oxygen in the water
sample. Since gas becomes more soluble in cold water than warm water, expected
results should indicate higher levels of dissolved oxygen in colder water than in hotter
water samples. (Soden, 2017)

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 CHAPTER II

EXPERIMENTAL METHOD

2.1 Materials and Apparatus

2.1.1 Materials for the experiment:
a. Potassium Iodate
b. Sodium Thiosulfate
c. Concentrated Sulfuric Acid
d. Potassium Iodide
e. NaN3
f. Starch
g. KOH
h. MnSO4
i. Water sample
j. Aquadest
2.1.2 Apparatus for the experiment:
a. Weighing Bottle
b. Beaker Glass
c. Mixing Rod
d. Funnel
e. Volumetric Flask
f. Watch Glass
g. Measuring Cylinder
h. Pipette Volume
i. Pipette
j. Iodine Flask
k. Burette
l. Statif and Clam
m. Spray Bottle
n. Pycnometer
o. Thermometer

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2.2 Experimental Procedure
2.2.1. Standarization of Na2S2O3 solution
1. 10 mL of KIO3 was taken with pipette volume and moved it into iodine flask
2. 2 mL of diluted H2SO4 solution and 8 ml of KI 10% solution was added
3. It was titrated with Na2S2O3 solution until the color of KIO3 solution becomes
light yellow
4. adding 3 mL of starch solution
5. titrating it again with Na2S2O3 solution until the dark blue color vanished
6. recording the volume of Na2S2O3 solution needed and the changes in color
7. Repeating this procedure one again

2.2.2. Determination of oxygen content in water

1. 250 mL water sample was measured accurately and added into an iodine flask;
adding 2 mL MnSO4 solution
2. 2 mL of Alkali – Iodine – Azide solution was added, then the iodine flask was
closed carefully in order to avoid air trapped in the solution
3. The solution was shaken for few minutes
4. Coagulation was let to be formed perfectly and setting was allowed. The clear
part of the solution was removed from the iodine flask into another iodine flask
5. 2 mL of concentrated H2SO4 was added by passing it through inner iodine flask
wall to dissolve the sediment and then closing the iodine flask
6. The iodine flask was shaken carefully until all the sediment and then closing the
iodine flask
7. Iodine resulted from the reaction is then being titrated with Na2S2O3 until the
color change to light brown
8. 1 ml of starch solution was added as the indicator to the sample then it was
titrated again until the dark blue color vanished
9. Few drops of concentrated H2SO4 was added into the clear part of the solution
in step 3 and titrating with Na2S2O3 solution
10. The total volume of Na2S2O3 solution needed and the changes in color was
recorded
11. This procedure was repeated once again

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2.2.3. Density determination
1. The pynometer was cleaned with its lid then the pycnometer is weighed (m1)
2. The pycnometer was filled with distilled water until full and there is no bubble
inside it
3. The pycnometer lid was put on and the outside wall of the pycnometer was dried
4. The pycnometer was weighed with analytic balance and the mass (m2) was
recorded
5. The pycnometer was emptied and refilled with drinking sample
6. The pycnometer was weighed with analytic balance and the mass (m3) was
recorded

2.3. Solutions Preparation

2.3.1. Preparation of KIO3 solution
Calculations
Potassium Iodate = KIO3
Normality = 0.025 N
Molecular weight = 214.02 g/mol
Volume = 0.1 L
Valence =6
𝑚𝑜𝑙𝑒
N = 𝑣𝑜𝑙𝑢𝑚𝑒 × 𝑣𝑎𝑙𝑒𝑛𝑐𝑒
𝑚𝑎𝑠𝑠
N = 𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡×𝑣𝑜𝑙𝑢𝑚𝑒 × 𝑣𝑎𝑙𝑒𝑛𝑐𝑒
𝑀𝑊 × 𝑉𝑜𝑙𝑢𝑚𝑒 × 𝑁
Mass =
𝑣𝑎𝑙𝑒𝑛𝑐𝑒
0.025 × 214 × 0.1
Mass =
6
Mass = 0.0892 gram

Tolerance ±10%
0.0892 − 0.00892 = 0.08028 ≈ 0.0803 gram
0.0892 + 0.00892 = 0.09812 ≈ 0.0981 gram
Procedures
1. 0.0906 gram of potassium iodate (KIO3) was with analytic balance.
2. The KIO3 solid was dissolved in a 100mL beaker glass using distilled water until
the volume below 100 mL.

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 3. The KIO4 solution was transferred into a 100mL volumetric flask through a
funnel.
4. The weighing bottle, glass rod, 100mL beaker, and funnel were washed with
distilled water and the washing was added to a 100mL volumetric flask.
5. The 100mL volumetric flask was topped up with distilled water until the 100mL
mark, stoppered, and shaken well.

2.3.2 Preparation of Na2S2O3

Calculation
Sodium Thiosulfate = Na2S2O3.5H2O
Normality = ± 0.01 N
Molecular weight = 248.21 g/mol
Volume =1L
𝑚𝑜𝑙𝑒
N = 𝑣𝑜𝑙𝑢𝑚𝑒 × 𝑣𝑎𝑙𝑒𝑛𝑐𝑒
𝑚𝑎𝑠𝑠
N = 𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑤𝑒𝑖𝑔ℎ𝑡×𝑣𝑜𝑙𝑢𝑚𝑒 × 𝑣𝑎𝑙𝑒𝑛𝑐𝑒
𝑀𝑤 × 𝑉𝑜𝑙𝑢𝑚𝑒 × 𝑁
Mass =
𝑣𝑎𝑙𝑒𝑛𝑐𝑒

241.21 × 0.15 × 0.025

Mass =
6
Mass = 0.9308 gram 0.9 gram
Procedures
1. 0.9 gram of Na2S2O3.5H2O powder was weighed by using hard balance.
2. Na2S2O3 powder was dissolved by using distilled water in a 1L beaker glass until
the 1L mark.

2.3.3 Preparation of sulfuric acid

Calculations
Sulfuric Acid = H2SO4
Normality =±2N
Volume = 30 mL = 0.03 L
Molecular weight = 98.08 g/mol
Density (𝜌) = 1.83 g/mL
Percent concentration = 96%

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 N = M x valence
2=Mx2
M = 1 mol/L (diluted H2SO4)
ρ x % x 10
M=
𝑀𝑊
1.84 x 96 x 10
M=
98.08
M = 18.01 mol/L (comcentrated H2SO4)

(M1 x V1) concentrated H2SO4 = (M2 x V2) diluted H2SO4

18.01 x Vconcentrated H2SO4 = 1 x 30
Vconcentrated H2SO4 = 1.6657 ml
= 1.7 mL
Procedures
1. 1.7 mL of concentrated H2SO4 was taken by using a 10mL measuring cylinder.
2. The concentrated H2SO4 was dissolved in a 50 mL beaker glass with distilled
water until 50 mL.

2.3.4 Preparation of KI solution

Calculations
Volume of KI = 30 mL
% KI = 10%
Assume that :  solution =  water = 1 gram/mL
Mass of solution =  solution × Volume of solution
= 1 gram/mL × 30 mL
= 30 gram
𝑚𝑎𝑠𝑠 𝑜𝑓 𝐾𝐼
% KI = 𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 × 100%
𝑚𝑎𝑠𝑠 𝑜𝑓 𝐾𝐼
10% = × 100%
30 𝑔𝑟𝑎𝑚

Mass of KI = 30 gram

% KI = 10%
Mass of KI = 3 gram

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 Procedures
1. KI powder was weighed around 3 gram using hard balance.
2. The KI powder was dissolved in a 400 mL beaker glass using distilled water until
30 mL.

2.3.5 Preparation of MnSO4 solution

Mormality = 215 M
Volume = 30 mL
Molecular Weight = 169.02 g/mol
𝑚𝑎𝑠𝑠 1
M= x𝑣
𝑀𝑊

Mass = M x MW x V
Mass = 2.15 x 169.02 x 0.03
Mass = 10.9 gram

Preparing MnSO4 solution :

1. MnSO4 powder was weighed 10.9 gram by using a hard balance.
2. Dissolving it in the beaker glass until 30L mark with distilled water.

2.3.6. Starch solution 1% 150mL

ρ solution = ρ water
ρ solution = 1 gr/mL
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛
= 1 gr/mL
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛

Mass of solution = 1 x 150

= 150 gr

% starch solution =1%

𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑡𝑎𝑟𝑐ℎ
x 100% = 1%
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛

1% 𝑥 150
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑡𝑎𝑟𝑐ℎ = = 1.5 𝑔𝑟𝑎𝑚
100%

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 Preparing starch solution :
1. 1.5 gram of starch powder was weighed using hard balance
2. The starch powder was dissolved in beaker glass with distilled water until 150
mL
3. The solution was heated while being stirred

2.3.7. Alkali – Iodine – Azide

1. 35 gram of KOH powder and 7.5 gram of KI powder was weighed using hard
balance
2. They are dissolved in beaker glass with distilled water until 50mL
3. 0.5 gram of NaN3 powder was weighed with hard balance
4. Both solution was mixed until homogeny

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 CHAPTER III

RESULT AND DISCUSSION

3.1. Experimental result

3.1.1. Standardization of Na2S2O3 solution with standard solution of KIO3
Standard solution was prepared by weighing 0.0906 g potassium iodate then
dissolved and diluted with distilled water until 100 ml.
Chemical formula of potassium iodate : KIO3
Molecular weight of potassium iodate : 214 g/mol
Indicator : starch

V of KIO3 solution (ml) V of Na2S2O3 solution (ml) Color change

10 9.9
Dark blue –
10 9.7
colorless
Average: 10 9.8

3.1.2. Determination of dissolved oxygen in water

Name of sample : Clear Indiana O2
DO according to nutrition fact : 20 mg/L
Indicator : Starch

V sample water (ml) V of Na2S2O3 solution (ml) Color change

250 20.1
Dark blue –
250 15.3
colorless
Average: 250 17.7

3.1.3. Density determination

Aquadest temperature : 32oC
Volume of pycnometer : 10.060 ml
Mass of pycnometer (m1) : 17.4173 gram
Mass of pycnometer + aquadest (m2) : 27.4814 gram
Mass of pycnometer + sample (m3) : 27.4818 gram

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3.2.Calculation
3.2.1. Normality of Na2S2O3 solution
(N x V)Na2S2O3 = (N x V)KIO3
NNa2S2O3 = (N x V)KIO3 / VNa2S2O3
= (mass/Mw) * (1000/100) * val * V / VNa2S2O3
= (0.0906/214) * (1000/100) * 6 * 10 / 9.8
= 0.0259 N

3.2.2. Concentration of dissolved oxygen in sample water

DO (mg/L) = (N * V)Na2S2O3 * 8000 / Vsample water
= 0.0259 * 17.7 * 8000 / 250
= 14.6698 mg/L

3.2.3. Density of sample water

Densitysample = (m3 – m1)/(m2 – m1) * Densityaquadest
= (27.4818–17.4173)/(27.4814–17.4173)*996.026 kg/m3
= 996.065 kg/m3 = 996.065 mg/cm3

3.2.4. Percentage of dissolved oxygen in water

% dissolved oxygen = (ppm * V) / (density * V) * 100%
= (14.6698 * 0.6) / (996.065 * 0.6 * 1000) * 100%
= 0.0015%

3.3.Discussion
3.3.1. Chemical reactions
In the experiment to determine dissolved oxygen in water, there are 3 major
steps to be done: standardization of sodium thiosulphate solution, determination
of water sample density and determination of dissolved oxygen in water.
During the experiment, we use Clear Indiana O2 as the water sample which
has specification of dissolved oxygen (as stated on SNI 6241:2015) approx. 20
mg/L.
A standard solution of sodium thiosulphate is needed to run the titration in
determining the dissolved oxygen amount. To standardize the sodium thiosulphate

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solution, the concept of indirect titration of iodine is used. Iodometry is a
technique to titrate iodine without adding iodine directly. Otherwise, it will use a
redox reaction to form iodine gas in the flask. The addition of potassium iodate
solution as primary standard solution with KI and H2SO4 solution will produce I2
according to this reaction:
5KI + KIO3 + 3H2SO4  3I2 + 3K2SO4 + 3H2O
Then, the iodine will be titrated by sodium thiosulphate according to reaction:
2Na2S2O3 + I2  Na2S4O6 + 2NaI
The indicator used is starch which will produce dark blue-purple color due to the
formation of iodine-starch complex. As the titration reach end point, the color will
turn colorless.

The amount of dissolved oxygen in water can’t be determine directly with

titration of oxygen Therefore, the titration of iodine which has proportional
amount with the oxygen is used. In this process, oxygen is bounded first with
MnSO4 solution to form MnO2 precipitate according to reaction:
MnSO4 + 2OH- + 1/2O2  MnO2 + H2O

figure 3.1. coagulated MnO2 in sample

The MnO2 precipitate is reddish in color and the amount of it roughly indicates
the amount of dissolved oxygen. From our experiment, the amount of precipitate
is big enough, approximately one-fourth of the iodine flask. After dividing the
precipitate with the liquid part of the solution by decantation method, the reaction
to form iodine takes place. The combination of MnO2, H2SO4 and alkali-iodine-
azide solution will form I2 according to reaction:

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 MnO2 + 4H+ + 2I-  I2 + Mn2+ + 2H2O

figure 3.2. clear part of sample after coagulation

The iodine then being titrated with sodium thiosulphate solution. However, there
might be still precipitate left in the liquid part after decantation. This needs to be
titrated as well until all the precipitate has reacted. Therefore, the amount of
oxygen dissolved can be traced back from the amount of iodine titrated.

3.3.2. Sources of error

1. The apparatus was not used in perfect horizontal angle, especially the burette.
2. The water came in contact with air during the experiment.
3. The iodine gas escaped the flask (minimum amount).

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 CHAPTER IV

CONCLUSION

From the experiment we acquired that:

The concentration of dissolved oxygen in the water sample is 14.6698 mg/L.

While the nutrition fact (as stated to be standard on SNI 6241:2015) indicates that:

The concentration of dissolved oxygen in the water sample is 20 mg/L.

Therefore, there is around 5.33 mg/L difference. This difference may be caused by contact
with air and light during or before the experiment. To conclude, the determination of
dissolved oxygen using this method is persistence enough and the difference between
experimental and informed DO is tolerable.

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 REFERENCES

APEC Water. 2017. “How Exactly Does Dissolved Oxygen Affects Water Quality?.”
https://www.freedrinkingwater.com/water_quality/quality1/1-how-dissolved-oxyg
en-affects-water-quality-page2.htm. Accessed on April 27th 2018.

Johnson, R.L, Holman, S, Holmquist, D.D. 1999. Water Quality. Oregon: CBL Vernier
Software.

Oram, Brian, 2014. “Dissolved Oxygen in Water.” https://www.water-research.net/index.ph

p/dissovled-oxygen-in-water. Accesed on April 27th 2018.

Soden, J.M. 2017. “The Winkler Titration Method.” https://sciencing.com/winkler-titration-

method-6076224.html. Accessed on April 27th 2018.

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