ANALYTICAL CHEMISTRY (CHM421)

EXPERIMENT 6
ANALYSIS OF BLEACH AND COPPER(II) UNKNOWN

STUDENTS’ NAME:
NURUL SYAFIQAH BINTI MOHD AINI [2012697062]

NOOR SHUHADA BINTI MUSTAPA [2012411706]

GROUP:

ASB2AC

LECTURER’S NAME:
MADAM SALAMIAH BINTI ZAKARIA

DATE OF EXPERIMENT/DATE OF SUBMISSION:

18 APRIL 2013 / 2 MAY 2013
TITLE:

 Analysis of bleach and copper(II) unknown

OBJECTIVES:

 To standardise the Sodium Thiosulphate Solution

 To determine the percentage of NaClO in bleach sample
 To determine the percentage of Copper in an unknown copper sample

RESULTS:

A. Standardisation of the Sodium Thiosulphate Solution

1 2 3
Final volume of thiosulphate solution (mL) 15.6 31.6 47.0
Initial volume of thiosulphate solution (mL) 0.0 15.6 31.6
Volume of thiosulphate solution (mL) 15.6 16.0 15.4

B. Determination of neutralization capacity of an antacid tablet

Brand of bleach 1 = Kao Bleach, Sodium Hypochlorite 5%

1. Molarity of Na2S2O3 solution = 0.1915 M

2. Mass of volumetric flask + 10 mL bleach = 73.3501g
3. Mass of volumetric flask = 62.9862g
4. Mass of 10 mL bleach = 10.3638g
5. Density of bleach = 1.0364g/mL
 Sample 1 Sample 2 Sample 3
Final volume of thiosulphate solution (mL) 2.00 4.30 46.80
Initial volume of thiosulphate solution (mL) 0.00 2.00 5.00
Volume of thiosulphate solution (mL) 2.00 2.30 1.80
Moles of Na2S2O3 0.000383 0.000440 0.000345
Moles of NaClO in 10mL aliquot1 0.000575 0.000660 0.00051
Moles of NaClO in 100mL aliquot2 0.000288 0.000330 0.000259
Moles of NaClO in 10mL bleach sample 0.0000288 0.0000330 0.0000259
Average moles of NaClO in 10mL bleach 0.0000292
sample
g/L of NaClO in bleach 0.0217
Mass percent of NaClO in bleach 0.00217
Mass percent of NaClO in from 5.0000
manufacturer’s label
Percent deviation between experimental and 99.57
label values

Brand of bleach 2 = Clorox, Sodium Hypochlorite 5.25%

1. Molarity of Na2S2O3 solution = 0.1915 M

2. Mass of volumetric flask + 10 mL bleach= 75.340g
3. Mass of volumetric flask= 64.674g
4. Mass of 10 mL bleach= 10.666g
5. Density of bleach= 1.0666g/mL

Sample 1 Sample 2 Sample 3

Final volume of thiosulphate solution (mL) 4.70 9.40 14.10
Initial volume of thiosulphate solution (mL) 0.00 4.70 9.40
Volume of thiosulphate solution (mL) 4.70 4.70 4.70
Moles of Na2S2O3 0.00090 0.00090 0.047
Moles of NaClO in 10mL aliquot1 0.00135 0.00135 0.00135
Moles of NaClO in 100mL aliquot2 0.000675 0.000675 0.000675
Moles of NaClO in 10mL bleach sample 0.0000675 0.0000675 0.0000675
Average moles of NaClO in 10mL bleach 0.0000675
sample
g/L of NaClO in bleach 0.0502
Mass percent of NaClO in bleach 0.00502
Mass percent of NaClO in from 5.25
manufacturer’s label
Percent deviation between experimental and 99.90
label values
C. Analysis of copper(II) unknown

Molarity of Na2S2O3 solution = 0.1915 M

Sample 1 Sample 2 Sample 3

Mass of copper(II) compound taken (g) 0.304 0.308 0.309
Final volume of Na2S2O3 solution (mL) 7.1 14.1 21.5
Initial volume of Na2S2O3 solution (mL) 0.0 7.1 14.1
Volume of Na2S2O3 solution (mL) 7.1 7.0 7.4
Moles of Na2S2O3 0.00136 0.00134 0.00142
Moles of Cu2+ 0.00136 0.00134 0.00142
Gram of Cu2+ 0.0864 0.0852 0.0902
Weight percent of copper in sample 0.247 0.243 0.258
Average weight percent of copper in 0.249
sample
Theoretical mass percent of copper in 0.877
sample
Percent error 71.61
Name of unknown copper(II) unknown copper (II) sulphate pentahydrate
Chemical formula of unknown copper(II) CuSO4.5H2O
unkmown
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) Acidified iodide ion is added to hypochlorite ion solution, and the iodide is oxidized to
iodine.

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

(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 average molarity of thiosulphate
which is 5.667 M. from this equation :

H2O + ClO- + 2S2O32- S2O62- + 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). The percentage get is 25.45 % copper salts. To know
the unknown copper (II), we compare with the percentage of copper (II) given. From this
calculation, the nearest percentage in this experiment is suit with copper (II) sulphate
pentahydrate.

The difference in the percentage obtained is due to the errors that occur while
conducting the experiment. The first error is while we pipette the bleach to 10mL, we not get
the accurate volume needed because of incorrect reading of the meniscus level for pipette.
Beside, for the repeated sample, it is possible that we forget to add starch to determine the
end point instead we just let the colour of iodine changes to colourless. The volumetric flask
is not cleaned thoroughly thus causing some impurities inside the flask. This will also affect
the mass of sample weight. The 3 replicate sample of copper (II) unknown is not precise with
each other because it left in the weighing boat.

Other error is while determining the end point of the titration. The titration process
should be stopped immediately once the end point is reached. End point is when the colour of
the analytes solution changes to the required colour. Any extra drop of the titrant will affect
the calculation of the molarity of the iodide present in the solution.

There are also error that occurs due to the improperly calibrated burettes and conical
flasks causing them to have volumes slightly different from those indicated by their
graduations. These apparatus should be frequently calibrated in order to obtain more accurate
reading of measurement.

CONCLUSION:

The experiment is very important because it gives the idea of oxidation and reduction at
the same time it views a clear about iodometric reaction. From the calculation, the percentage
by mass of the NaClO in Kao is 0.00217% while in Clorox is 0.00502 %. The percentage of
copper in an unknown copper sample is 25.45%. This percentage shows that the unknown
copper (II) is actually copper (II) sulphate pentahydrate.

REFERENCES:

1. http://www.jesuitnola.org/upload/clark/aplabs.html#Analysis_of_a_Commercial_Bleach
_
2. http://kinardf.people.cofc.edu/153L_HONS_HonorsChemistryLaboratory/Exp4_Chlorin
eBleachTitration.pdf
3. http://chem.lapeer.org/Chem2Docs/APChem2Manual.html#bleach