LAB #10: DISSOLVED OXYGEN LEVELS IN NATURAL WATERS

DATE:
NAME:
STUDENT ID:
CO-WORKER :

27 November, 2014
Nguyen Van Vu Cuong
20140912
Jiho Lee

INTRODUCTION:
This experiment was designed to develop a proper technique for obtaining a
natural water sample, to determine the dissolved oxygen concentration a natural
water sample, and to learn the chemical reactions involved in fixing and analyzing a
water sample for dissolved oxygen using the Winkler method. In nature, the
concentration of dissolved oxygen in a water sample is an important indicator of
water quality. Water with high oxygen concentrations indicate aerobic conditions:
clean, clear an unpolluted. Low oxygen concentrations indicate aerobic conditions:
high turbidity, foul odors, extensive plant growth on the surface. To determine
dissolved oxygen, in this experiment, we used Winkler Method of Analysis. To do
that, we need fixation of oxygen, oxidation of the iodide ion in water sample and
titration of sample with standardized sodium thiosulfate solution in the presence of
a starch indicator.

MATERIALS AND PROCEDURE:

1. Materials:
- To perform well this experiment, we need the following apparatuses:
o Pipet
o 100 mL flask
o Three 250 mL Erlenmeyer flasks
o Rubber stop
o Stand
o Thermometer
o Buret
o Funnel
-

Chemicals we used:
o 0.1 M Na2S2O3 solution
o Water
o 2.1 M MnSO4 solution
o Basic KI-NaN3 solution
o Conc H2SO4

2. Procedure:

- Part A: A Standard 0.025 M Na2S2O3 Solution

We produced 100 mL 0.025 M Na2S2O3 solution from 25 mL 0.1M
Na2S2O3 solution by adding 75 ml distilled water to 25 mL 0.025 M Na 2S2O3
solution.
- Part B: Collection of Water Sample:
+ We collect water by a clean and dry 250 mL Erlenmeyer flask and
ensure that no bubble form in the flask
+ We then pipet ~ mL of the basic 2.1 M MnSO 4 solution in to the
sample. Do the same with ~ 1 mL of the basic KI-NaN 3 solution.
+ After that, we carefully stoppered the sample and determined the
temperature and the sample
- Part C: Sample Analysis:
+ We add 4 mL of the standard Na2s2O3 solution to the buret, toll the
solution to wet the wall of the buret, and dispense through the buret tip. Fill
the buret with Na2s2O3 and record that initial volume of the solution.
+ Remove the stopper and add ~ 1mL conc H2SO4, stirred to dissolve
precipitate. Then, we transferred ~ 200 mL of the sample to a flask for
titrimetric analysis.
+ We then titrated water sample by slowly dispensing the Na 2S2O3
titrant into the water sample and swirling the flask as titrant is added. Then
the color of the analyte fades to a light yellow-brown, add ~1 mL of the
starch solution. Continue until it turns out to colorless. At that time, we
recorded the volume of remaining Na2S2O3 titrant.

RESULTS
Data:
B. Collection of Water Sample:
Sampling site: Temperature: 18.3 C.
C. Sample Analysis

1. Sample volume (mL)

2. Buret reading, initial (mL)
3. Buret reading, final (mL)
4. Volume Na2S2O3 dispensed (mL)
5. Molar concentration of Na2S2O3
(mol/L), Part A
6. Moles of Na2S2O3 dispensed (mol)
7. Moles of I3- reduced by S2O32- (mol)
8. Moles of O2 (mol)
9. Mass of O2 (mg)
10. Dissolved oxygen, ppm O2 (mg/L,
ppm)
Table 1

200
5.30
14.85
9.55
0.025
2.3875 x 10-4
1.19375 x 10-4
5.96875 x 10-5
1.910
9.55

Calculation:
Part A: A standard 0.025 M Na2S2O3 solution:
We use 25 mL 0.1 M Na2S2O3 solution to produce 0.025 M Na2S2O3
solution. So we should determine how much water we need to add. Let
it be x:
(0.1 x 25 x 10-3) / (25 x 10-3 + x) = 0.025 -> x = 0.075 (L) = 75 (mL)
Part C: Sample Analysis:
Note: In this calculation section, (n) is value in the n-th row in the
table 1 (above) (n = 110).
4. Volume Na2S2O3 dispensed (mL) = (3) (2) = 14.84 5.30 = 9.55
(mL)
6. Moles of Na2S2O3 dispensed (mol) = (4) x (5) = 9.55 x 10 -3 x 0.025 =
2.3875 x 10-4 (mol)
7. Moles of of I3- reduced by S2O32- (mol) = (6) / 2 = = 2.3875 x 10-4 / 2
= 1.19375 x 10-4 (mol) due to the reaction:
I3- (aq) + 2S2O32- (aq) -> 3I- (aq) + S4O62- (aq)
8. Moles of O2 = ( volume (L) S2O32- x mol S2O32- / L S2O32- )
x (1 mol I3- / 2 mol S2O32- )
x (2 mol Mn(OH)2/ 1 mol I3-)
x 1 mol O2/4 mol Mn(OH)3
= 2.3875 x 10-4 / 2 x 2 / 4
= 5.96875 x 10-5 (mol)
9. Mass of O2 (mg) = (8) x 32 = 5.96875 x 10-5 x 32 = 1.910 (g)
10. Dissolved oxygen, ppm O2 (mg/L, ppm) = (9) / (1) =1.910 x 1000 /
(200 x 10-3) = 9.55 (mg/L)
LABORATORY QUESTIONS

1. It would be too low because when temperature increases, the solubility of

oxygen will also decreases. Temperatures change easily makes a big change in the
solubility of the oxygen for this small isolated amount of water rather than we the
sample that is still a part of the body of the water.
2. The dissolved oxygen concentration will be lower than expected because no
precipitate -> iodide ion is hardly oxidized by Mn(OH) 3(solid) -> the volume (or
moles) of Na2S2O3 is very low -> the calculated dissolved oxygen concentration will
be lower.
3. It will be higher than it should be because the calculated value (in case there is
no error) would be 9.0 (corresponding to 21C), which is higher than what the water
chemist expects (8.1 at 27C). Also, in calculation, this incorrect temperature value
(27C) does not affect the final calculated result because we do not need to use
temperature in calculation.

DISCUSSION:
The experiment was related to one method to determine dissolved oxygen
concentration of a natural water sample. Our result is 9.55 (mg/L) at 18.3C which
is very close to the data in table 13.1 (page 344, textbook): 9.5 (mg/L) at 18C.
Firstly, we should be careful to avoid accidental addition of oxygen to the
sample. Water should not be simply poured into a bottle because this will aerate, or
add oxygen to, the sample, which gives a false determination of the dissolved
oxygen in the water. Instead, a flask should be filled slowly with water, shift from
horizontally to upward. There should be no air bubbles present, because air bubbles,
too, add oxygen to the water. The stopper of the collection bottle also needs to be
carefully placed so that the bottle is completely full of water with no pocket of air or
bubbles at the top.
Secondly, ideally, we should dispense titrant slowly (within one-half drop)
near endpoint because the correct point to stop dispensing is only endpoint, if we
surpass it, the amount of Na2S2O3 used would be higher than expected -> the
calculated dissolved oxide concentration is higher than expected.
Winkler titration is the most inexpensive method to determine the amount of
dissolved oxygen in water, but it is also the least accurate and most labor intensive.
Oxygen electrodes and oxygen optodes (different types of oxygen meters) are fast
and accurate, but they can be expensive.

REFERENCES:
http://yeahchemistry.com/
Principles of Modern Chemistry 7th edition Oxtoby Gillis Campion