UTAR

FHSC1114 Physical Chemistry

Trimester 1

Topic 2: Precipitation of barium (II) sulphate

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Introduction:
Barium (II) nitrate reacts with sulphuric acid to produce barium (II) sulphate as white
precipitate which is difficult to dissolve in water. If sulphuric acid is in excess compared
to barium (II) nitrate, the entire ion Ba2+ will precipitate as barium (II) sulphate.
Therefore, barium (II) nitrate is a limiting reagent and the quantity of precipitate formed
is determined by this limiting reagent. The excess acid will then be separated using
distilled water.

Apparatus and Equipments:

Pipette (10mL) Hot water bath
Beaker (100mL) Filter funnel
Glass rod Filter paper
Watch glass Electronic balance

Materials:
0.1 M Barium (II) nitrate solution, Ba(NO3)2
0.5 M Sulphuric acid, H2SO4

Procedures:
1. Pipette 10mL of Ba(NO3)2 into a 100mL beaker.
2. Add 10mL of diluted H2SO4 and stir with a glass rod. Allow the precipitate to settle.
3. Weigh a clean and dry watch glass with a filter paper. Then, put the filter paper into
the filter funnel.
4. Carefully filter all the liquid in the beaker.
5. Add 20mL of distilled water into the same beaker, stir for 1 minute, and rinse the
glass rod and the side of the beaker. Wait for a while and filter like the previous step.
6. Decant the filtrate and remove the filter paper with precipitate to the watch glass.
7. Dry the precipitate in the oven until there is no liquid left on the watch glass.
When the precipitate dries, cool and measure the weight. Repeat this step until the
mass is same or less than 0.02g different.

Treatment of Data:
Mass of dry watch glass with filter paper g
Mass of watch glass with filter paper + precipitate g
Mass of BaSO4 precipitate g

Calculation:
1. Calculate the molecular weights of Ba(NO3)2 and BaSO4.
2. Calculate the moles of BaSO4 are produced in this experiment.
3. Calculate the moles of Ba(NO3)2 are required to react with H2SO4.
4. Determine which is limiting reactant in this experiment.
5. Determine the percentage yield of BaSO4.

Lab manual version 4.0

Foundation in Science 7
UTAR
FHSC1114 Physical Chemistry
Trimester 1

Topic 3: Determination of the amount of dissolved oxygen in a water sample by

iodometry – the Winkler’s method
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Introduction:
Myriad forms of life exist in lakes, streams and oceans. These creatures depend on
dissolved oxygen (D.O.) in water for their life support. Occasionally something will
happen which depletes the oxygen content of a natural water system.

The dissolved oxygen content is an important index when considering the suitability of
water for town supply. Good potable water will give a D.O. value close to the theoretical
value for a saturated solution for oxygen in water. When there is pollution from organic
matter and other trade effluents, the D.O. is used up in various biochemical oxidation
processes and it is only slowly replaced through surface adsorption. Such water will give
a low D.O. content until oxidation is completed. Adequate D.O. is necessary for the life
of fish and other aquatic organisms.

Gases which are dissolved in water obey Henry’s law to a first approximation:

Xi = k . Pi

Where Xi is the mole fraction of the gas in solution, k is the Henry’s law constant and P i
is the partial pressure of the gas. For oxygen, at 20 oC, k = 2.5 x 10-5 atm-1 and P (O2) =
0.21 atm for air.

Also, it is approximately true that X (O2) = n (O2) / n (H2O) since n (O2) << n (H2O) and
n (H2O) = 5.5 mol/1. Thus, n (O2) = 2.9 x 10-4 mol/1. The solubility of oxygen is then
S(O2) = 9.3 mg/1 at 20 oC. Experiment indicates that solubility of oxygen is actually 9.2
mg/1 of D.O. in pure water at 20 ºC (Table 1).

The solubility decreases with increasing temperature and increasing electrolyte

concentration.

Table 1: Solubility of oxygen in natural water

T (oC) D.O. in pure water (mg/L)
0 14.6
10 11.3
20 9.2
30 7.6

The method described below for the determination of oxygen in water is based on that
devised by Winkler. Since the D.O. content of a sample is so transitory, the sample must
be ―fixed‖ very soon after collection. The sample is first treated with excess of
manganese (II), potassium iodide and sodium hydroxide. The white manganese (II)
hydroxide that is formed reacts rapidly with oxygen to form brown manganese (III)
hydroxide.

Lab manual version 4.0

Foundation in Science 8
UTAR
FHSC1114 Physical Chemistry
Trimester 1

4Mn(OH)2 (s) + O2 + 2H2O  4Mn(OH)3 (s)

When acidified, the manganese (III) oxidizes iodide which is already present to iodine:

2Mn(OH)3 (s) + 2I- + 6H+  I2 + 6H2O + 2Mn2+

The liberated iodine, which is equivalent to the D.O. content, may then be titrated with
standard sodium thiosulphate:

I2 + 2S2O32-  S4O62- + 2I-

Apparatus:
Volumetric pipette (100 mL) Reagent bottle (1 L)
Conical flask (500 mL) Conical flask stopper
Burette Retort stand
Burette clamp Measuring cylinder (5 mL)
Pasteur pipette

Materials:
Manganese sulfate solution
Alkaline-iodide solution
0.025 M Sodium thiosulphate solution
Concentrated sulphuric acid
Starch solution

Procedures:

1. When sampling water, care must be taken to ensure that a good representative sample
of the water to be analyzed is obtained. For most purposes, this includes attention to
dissolved gases. Therefore, the water sample should be taken in a clean bottle which
must be filled to overflowing and tightly sealed with stopper without introduction of
air. If the water is sampled from a tap, it must be allowed to run for at least 5 minutes
prior to sampling. For this purpose, you may collect the water into a 1 L reagent
bottle fitted with a stopper.
2. Carefully remove the stopper from the conical flask and add 4 mL of the manganese
sulfate solution, discharging the reagent from the tip of a pipette put well below the
water surface. Replace the stopper.
3. Similarly, introduce 4 mL of the alkaline-iodide solution.
4. Place the stopper in the bottle; be sure that no air becomes entrapped. Some overflow
may occur. Thoroughly mix the content by inversion and rotation. Manganese
hydroxide is precipitated and will settle on standing.
5. When the precipitate has settled, introduce 4 mL of concentrated sulfuric acid with
the tip of the pipette well below the surface of the solution.
6. Replace the stopper and mix until the precipitate dissolves completely. The dissolved
oxygen now liberates free iodine from the potassium iodide present.

Lab manual version 4.0

Foundation in Science 9
UTAR
FHSC1114 Physical Chemistry
Trimester 1

7. Pipette 200 mL of the acidified sample into a 500 mL conical flask and titrate with
0.025 M sodium thiosulphate until the solution becomes pale yellow.
8. Add a few drops of starch indicator and continue the titration to the disappearance of
blue color.
(If the blue color doesn’t appear after adding starch, repeat the titration and adding
starch before start of titration)
9. Repeat the titration twice.

Treatment of data:

Titration number 1 2 3
Final reading
Initial reading
Volume used (cm3)

Average volume of titrant required for titration = ____________ cm3

Calculation:
1. Determine the concentration (ppm) of dissolved oxygen (DO) in the water sample.
2. Chemical equation below shows the reaction between iodine and thiosulphate.

I2 + 2S2O3-2  S4O6-2 + 2I-

Calculate the oxidation states for the underlined elements and determine the oxidizing
and reducing agents.

Lab manual version 4.0

Foundation in Science 10