ABSTRACT

The objectives of this experiment are to standardize the sodium thiosulphate solution, to
determine the percentage of NaClO in sample and to determine the percentage of copper in an
unknown copper sample. Firstly, in Part A, the sodium thiosulphate solution was standardized to
get its actual molarity. Then, for analysis of bleach (Part B), 10.0 mL of the bleach sample was
used as sample, and then it was diluted with distilled water into pre-weighed 100 mL volumetric
flask. The volumetric flask was reweighed and the density of the bleach solution was calculated.
The sample was diluted to the 100 mL mark with distilled water. 10.0 mL aliquot of bleach
solution with potassium iodide and hydrochloric acid solution was titrated against the
standardized sodium thiosulphate until the amber iodine color fades to light yellow. Then, add
some starch solution and the titration was continued until the dark color of starch-iodine complex
disappears and turns colorless. The titration procedure from Part B was used in analysis of
copper(II) unknown (Part C) by using copper(II) unknown with potassium iodide and sulphuric
acid solution in a conical flask. The experiment is very important because reactions of oxidation,
reduction, and iodometric were took place together. From the calculation, the percentage of the
NaClO in Cocorex is 1.46 %. The percentage of copper in an unknown copper sample is 20.9 %.
This percentage shows that the unknown copper(II) is actually copper(II) sulphate pentahydrate.

OBJECTIVES

1. To standardise the sodium thiosulphate solution.

2. To determine the percentage of NaClO in bleach sample.
3. To determine the percentage of copper in an unknown copper sample.

INTRODUCTION

Household bleach contains an oxidizing agent known as sodium hypochlorite, NaOCl.

NaOCl is prepared by bubbling chlorine gas into a sodium hydroxide solution. Part of the
chlorine is oxidized to the hypochlorite ion, OCl- , and some is reduced to the chloride ion, Cl - .
The excess hydroxide keeps the resulting solution strongly basic. An equation describing this
process is:
H2O(l) + ClO- + 2I- → I2(aq) + Cl- + 2OH-
I2 + I- → I3-
Thus, we can write the net reaction of hypochlorite with iodide as:
H2O(l) + ClO- + 3I- → I3- + Cl- + 2OH-
The triiodide is then reduced back to iodide by titration with a standardized thiosulphate solution:
I3- + 2S2O32- → 3I- + S4O62-
Therefore, from these equations, it shows that iodide ion does not undergo any net change in the
process but its presence assures that the correct stoichiometry is followed. Its presence is also
provides a visually detectable point. The overall reaction is:

H2O(l) + ClO- + 2S2O32- → S4O62- + Cl- + 2OH-

(Mole ratio of hypochlorite to thiosulphate is 1:2)

One commonly used method for determining oxidizing agents in solution is termed an
“iodometric titration”. Iodide ion is a strong enough a reducing agent that many oxidizing agents
can react completely with the iodide ion resulting in many useful iodometric processes. The
usual procedure involves the addition of an excess of iodide ion to the oxidizing agent analyte
which produces iodine, which can be titrated with standard sodium thiosulfate solution. The
iodine-thiosulfate reaction is quite fast and the equilibrium is far to the product side. In the
hypochlorite titration, the following steps occur.

Copper (II) unknown analysis

The percent by mass of copper in copper (II) unknown can be determined using similar
procedure as for the bleach sample. The copper (II) unknown compound is first dissolved in
dilute acid followed by reacting with excess potassium iodide. This reaction produces triiodide
according to the following equation:
2Cu2+ + 5I- → 2CuI(s) + I3-
The triiodide produced in this reaction is titrated with standardized thiosulphate as in the bleach
titration:
I3- + 2S2O32- → 3I3- + S4O62-
And the overall reaction is:

2Cu2+ + 2I- + 2S2O32 → 2CuI(s) + S4O62-

(Mole ratio of copper (II) to thiosulphate is 1:1)

METHOD

A. Standardisation of the Sodium Thiosulphate Solution

A burette was washed thoroughly with detergent followed by tap water. The burette was
rinsed with distilled water and finally with sodium thiosulphate solution provided. Next, the
cleaned burette was filled with fresh thiosulphate solution. About 2 g of solid KI was
weighed into a conical flask. 50.0 mL of 0.010 M KIO 3 solution was pipetted into the same
flask and then, 10 mL of 1.0 M H2SO4 was added. Immediately the solution was titrated with
the thiosulphate solution until the colour of the solution is light yellow. At this point, 2 mL
of starch indicator was added using a cylinder. The solution was turned into blue-black
solution after starch is added. The titration was continued after the addition of starch. The
titrant was added drop wisely until the solution in the conical flask is clear and colourless.
The whole process was repeated two more times.

B. Analysis of Bleach

A clean and dry 100 mL volumetric flask was obtained and weighed to the nearest 0.001
g. The weight of the empty 100 mL volumetric flask was recorded. a 10.0 mL pipetted was
cleaned and rinsed thoroughly with the first bleach solution. Accurately, 10.0 mL of the
sample was pipetted into the pre-weighed 100 mL volumetric flask above. The flask was
reweighed and its weight was recorded. The sample was diluted to the 100 mL mark with
distilled water. The pipette was rinsed out with distilled water followed with a little of the
 diluted bleach solution, and then a fresh 10.0 mL aliquot of it was pipetted into a 250 mL
conical flask. Next, 1.0 g of potassium iodide was added and the resulting mixture was
swirled. Then, 5.0 mL of 6 M HCl was added to the mixture. The sample was titrated with
the standardised sodium thiosulphate solution until the amber iodine colour begins to fade to
light yellow. 2 mL of starch solution was added and the titration process was continued until
the dark colour of the starch-iodine complex just disappears. An abrupt colour changes from
dark blue to colourless marks the endpoint. The titration was repeated with two more 10.0
mL aliquot of the diluted bleach solution.

C. Analysis of Copper(II) Unknown

Accurately about 0.3 g of the copper(II) unknown was weighed out into a 250 mL conical
flask. The solid was dissolved with 35 mL 0.05 M sulphuric acid. 1.0 g of potassium iodide
was added and the mixture was swirled. Carefully, the mixture was titrated with the
standardised sodium thiosulphate solution until the amber colour of the triiodide begins to
fade. At this point, 2 mL of starch solution was added. The titration process was continued
until the grey starch-iodine colour turns milky white-pinkish colour that marks the endpoint.
The process was repeated for two more samples.

CALCULATION / ANALYSIS

A. Standardisation of the Sodium Thiosulphate Solution

IO3- + I- + 6H+ → I2 + 3H2O

2S2O32- + I2 → 2I- + S4O62-

0.010 mol IO3-

No. of moles of IO3-
= × 0.05 L solution = 0.0005 mol IO3-
1 L solution
 1 mole IO3- : 1 mole I2
∴ 0.0005 mol IO3- : 0.0005 mol I2

2 mol S2 O32-
No. of moles of S2O32- = 0.0005 mol I2 ×
1 mol I2

= 0.001 mol S2O32-

∴ Molarity S2O32- = No. of moles S2O32- ÷ Volume (in litres)

0.001 mol S2 O 32- 1000 mL
= ×
14.5 mL solution 1L
= 0.0690 M sodium thiosulphate (Na2S2O3) solution

B. Analysis of Bleach

H2O(l) + ClO- + 2S2O32- → S4O62- + Cl- + 2OH-

0.0 690 mol S2 O 32- 1 L 1 mol ClO-

No. of moles CIO- = × 5.9 mL solution × ×
1 L solution 1000 m L 2 mol S2 O 32-

= 2.0355×10-4 mol CIO- (in 10 mL aliquot)

No. of moles CIO- in original sample:

2.0355× 10-4 mol ClO-
= × 100 mL
10 mL
= 2.0355×10-3 mol CIO- (in 10 mL bleach sample)

Mass of CIO- = 2.0355×10-3 mol × 77.44 g/mol

= 0.1576 g CIO-

0.1576 g ClO -
Mass percent of CIO- = × 100%
10.8021 g
= 1.46 % of CIO-
 Mass percentage CIO- from the bottle = 5.7 %

∴ Percent deviation between experimental and label values:

= (5.7 – 1.46) %
= 4.24 %

C. Analysis of Copper(II) Unknown

2Cu2+ + 2I- + 2S2O32 → 2CuI(s) + S4O62-

0.0 690 mol S2 O 32- 1 L 2 mol C u2+

No. of moles Cu 2+
= × 14.3 mL solution × ×
1 L solution 1000 m L 2 mol S2 O 32-

= 9.867×10-4 mol Cu2+

Mass of Cu2+ = 9.867×10-4 mol × 63.54 g/mol = 0.0627 g Cu2+

0. 0627 g C u 2+
2+
Weight percent Cu in sample = × 100% = 20.9 %
0.3 g sample

Theoretical mass of copper in compound:

Copper(II) acetate monohydrate = 31.8 %
Copper(II) chloride dehydrate = 37.28 %
Copper(II) sulphate pentahydrate = 25.45 % ☑

Percent error = (25.29 – 20.9) % = 4.39 %

Name of unknown copper(II) unknown = Copper(II) sulphate pentahydrate
Chemical formula = CuSO4.5H2O

DISCUSSION
 In this experiment the amount of hypochlorite ion present in a solution of bleach is
determined by an oxidation-reduction titration, the iodine-thiosulfate titration procedure. In acid
solution, hypochlorite ions oxidize iodide ions to form iodine, I2. The iodine that forms is then
titrated with a standard solution of sodium thiosulfate.

The analysis takes place in a series of steps:

 (1) Iodide ion is added to hypochlorite ion solution, and the iodide is oxidized to iodine.

H2O(l) + ClO-(aq) + 2I-(aq) → Cl-(aq) + I2(aq) + 2OH-(aq)

(2) Iodine is only slightly soluble in water. It dissolves very well in an aqueous solution of iodide
ion, in which it forms a complex ion called the triiodide ion. The triiodide ion is yellow in dilute
solution, and dark red-brown when concentrated.

I2(aq) + I-(aq) → I3-(aq)

 (3) The triiodide is titrated with a standard solution of thiosulfate ions, which reduces the iodine
back to iodide ions:

I3-(aq) + 2S2O32-(aq) → 3I-(aq) + S4O62-(aq)

During this last reaction the red-brown color of the triiodide ion fades to yellow and then
to the clear color of the iodide ion. It is possible to use the disappearance of the color of the
I3- ion as the method of determining the end point, but this is not a very sensitive procedure.
Addition of starch to a solution that contains iodine or triiodide ion forms a reversible blue
complex. The disappearance of this blue colored complex is a much more sensitive method of
determining the end point. The quantity of thiosulfate used in step (3) is directly related to the
amount of hypochlorite initially present.

To know the copper (II) unknown is, we calculate first the molarity of thiosulphate which is
0.0690 M from this equation:

H2O + ClO- + 2S2O32- → S4O62- + Cl- + 2OH-

 We can get the number of moles of ClO - . After this, we can calculate the mass of
hypochlorite in an unknown copper(II). From the mass we will divide with the mass used for this
experiment and multiply by 100 to get the percentage. The percentage of ClO - from experiment
was 1.46 %, while from the bottle is 5.7 %. So, the percent deviations between these two values
are 4.24 %.

For analysis of copper(II) unknown, the percent of copper(II) in the sample was 20.9 %.
This shown that the unknown copper was actually copper(II) sulphate pentahydrate.

CONCLUSION

The molarity of sodium thiosulphate solution after standardization is 0.0690 M. The percentage
of the NaClO in Cocorex is 1.46 %. The percentage of copper in an unknown copper sample is
20.9 %.

REFERENCES

1. Iodometric Titration. Retrieved November 14, 2016.

http://chemistry.tutorvista.com/analytical-chemistry/iodometric-titration.html
2. Iodometric Titration. Retrieved November 16, 2016. http://www.titrations.info/iodometric-
titration