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ABSTRACT

The first objectives for this experiment is 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, get the standardization molarity of the
sodium thiosulphate solution. Firstly, in Part A, the sodium thiosulphate solution was
standardized to get and the molarity after being calculated was 0.1084M. The next objective
was to determined the percentage NaCIO in bleach sample. In this experiment, the bleach
sample being used was Cocorex and Dobi. From the calculation, the percentage of the NaClO
in both bleach were 1%. The percentage of copper in an unknown copper sample was 25.72
%. this percentage shows that the unknown copper (II) is actually copper (II) chloride
pentadehydrate.

OBJECTIVE

1. To standardise the sodium thiosulphate solution


2. To determine percentage of NaCIO 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


(an alternative formula is NaClO). 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:

Cl2(g) + 2 OH- • ClO- + Cl- + H2O

The ability of bleach to serve as an oxidizing agent is reported in terms of “available


chlorine.” Chemically, this is incorrect because the true oxidizing agent in chlorine bleach is
the ClO- anion, not Cl2(aq). Because both Cl2(aq) and ClO- react with a similar stoichiometry,
the term“available chlorine” allows the hypochlorite concentration to be calculated as if
Cl2(aq) wasactually present in the solution.

“Chlorine free” bleaches, typically marketed as safe for use with colors generally
contain other oxidizing agents such as sodium perborate (NaBO3·2 H2O or,
alternatively,NaBO2·H2O2·H2O) which produce hydrogen peroxide, H2O2, when dissolved in
water. These products are commonly referred to as oxygen bleaches. Clorox 2® is an
example of an oxygen bleach. The mechanism of action of both chlorine and oxygen bleaches
is a combination of chlorination and oxidation reactions. Since the active ingredients are
oxidizing agents, they are reduced in the reactions which means they accept electrons from
the compounds undergoing oxidation.

The chromophore or “color center” in most organic dyes or stains involves multiple
bonds such as C=C or N=N groups. These dyes or stains absorb light in a visible region of the
electromagnetic spectrum and reflect other visible colors. A blue dye absorbs red and
thereforeblue is reflected to our eyes. The purpose of using a bleach is to reduce these
chromophores to single bonds through either oxidation or chlorination. If the stain or dye
loses its ability to absorb a particular wavelength, then all wavelengths are reflected which
gives rise to white as the observed color. When this occurs, light will be reflected by the
material rather than absorbed and the material will seem to be both whiter and brighter.

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 :

2 Cu2+ + 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 :

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

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

PROCEDURE

A. Standardisation of the Sodium Thiosulphate Solution

The burette was filled with fresh thiosulphate solution. About 2 g of solid KI was
weighed into a 250ml conical flask. 50.0 ml of 0.010 M KIO3 solution was pipette into the
same flask and then 10 ml of 1.0M H2SO4 was added. the flask was placed in the laboratory
fume hood while adding sulphuric acid to it. The colour was changed to deep brown colour.
The reaction that occurs in the flask is :

IO3 (aq) + 2 I (aq) + H+ (aq) → I2 (or I3-) + H2O(aq) (not balanced)

The solution was immediately titrated in the flask 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 turn blue-black once the starch is added. the titration was
continued after the addition of starch. The titration was stopped until its turn to colorless. The
volume of titrant used was recorded. The reaction that that occurs in the flask between
thiosulphate and triiodide to produce iodide and tetrathionate is :

S2O32- (aq) + I2(aq) (or I3-) → I-(aq) + S2O62- (aq) (not balanced)

The above method was repeated to two more samples.

B. Analysis of Bleach

A clean and dried 100ml volumetric flask was obtained. The weight of empty 100ml
volumetric flask was recorded. 10.0ml of the first bleach sample was pipette into the pre-
weighed 100ml volumetric above. The flask was reweighed and recorded. This will give the
density of the bleach solution. The sample was diluted to the 100ml mark with distilled water.
Then, it was mixed well. The pipette was rinsed with distilled water followed with a little of
the diluted bleach solution and a fresh 10.0ml aliquot was pipette into a 250ml conical flask.
Next, 1.0 g of potassium iodide was added and it was swirled . then, 5.0ml of 6 M HCl was
added to the mixture. The sample was titrated with the standardized sodium thiosulphate
solution until the amber iodine colour begins to fade to light yellow. 2 ml of the starch
solution was added and the titration was continued until the dark colour of the starch-iodine
complex just disappears. The titration was repeated with two more 10.0ml aliquot of the
diluted bleach solution. The analysis with the second branch of bleach sample.

C. Analysis of copper (II) unknown

About 0.3 g of copper (II) unknown was weighed into a 250ml conical flask. The
solid was dissolved with 35ml of 0.05 M sulphuric acid. 1.0 g of potassium iodide was added
and it was swirled. Then, the mixture was titrated with the standardized sodium thiosulphate
solution until the amber color of the triiodide begins to fade. At this point 2 ml of starch
solution was added. the titration was continued until the grey starch-iodine color disappears
to produce a milky white-pinkish color that marks the end point. The titration was repeated
with the two more samples. The percentage by mass of copper was calculated.
CALCULATION

A) Standardisation of the Sodium Thiosulphate Solution


6 H+ + 8 I-- + IO3- → 3 I3- + 3 H2O
M KIO3 = 0.010 M
V KIO3 = 0.05L
0.010 𝑚𝑜𝑙
Mol IO3- = 𝑥 0.05𝐿 = 5x10-4 mol
𝑙

From the equation above,


1 mol IO3- = 3 mol I3-
5 x10-4 mol IO3- = 1.5 X 10-3 mol I3-

During titration,
1 mol I3- = 2 mol S2O3-
0.0015 mol = X mol S2O32-
X = 3 x 10-3 mol S2O32-

Molarity S2O32-
0.003 𝑚𝑜𝑙
Rough = = 0.1075 𝑀
0.0279 𝐿
0.003 𝑚𝑜𝑙
1st titration = = 0.1087 𝑀
0.0276𝐿
0.003 𝑚𝑜𝑙
2nd titration = = 0.1091 𝑀
0.0275 𝐿

Average molarity S2O32-,


0.1075𝑀+0.1087𝑀+0.1091𝑀
= 0.1084 M
3

Molarity of Na2S2O3, = 0.1084M


B) Analysis of bleach
H2O + CIO - + 2S2O32-  2S4O62- + CI - + 2OH –
(mole ratio of hypochlorite to thiosulphate is 1:2)
Brand: Cocorex
Moles Na2S2O3,
𝑚𝑜𝑙
Sample 1= 0.1084 x 3.92 x10 -3 L = 4.2 x 10-4 mol
𝐿
𝑚𝑜𝑙
Sample 2= 0.1084 x 3.4 x10 -3 L = 3.68 x 10-4 mol
𝐿
𝑚𝑜𝑙
Sample 3= 0.1084 x 3.3 x10 -3 L =3.57 x 10-4mol
𝐿

Moles of NaCIO in 10 mL aliquot


Sample 1
1 mol NaCIO
= 4.2 × 10−4 mol Na2S2O3 × 2 mol Na2S2O3

= 2.1 X10-4 mol

Sample 2
1 mol NaCIO
= 3.68 × 10−4 mol Na2S2O3 × 2 mol Na2S2O3

=1.84 × 10−4 moL


Sample 3
1 mol NaCIO
= 3.57 × 10−4 molNa2S2O3 × 2 mol Na2S2O3

= 1.785 x10-4 mol

Moles of NaCIO in 100 mL aliquot

Sample 1

= 2.1 × 10−4mol x 10 dilution factor

= 2.1 × 10−3mol
Sample 2

=1.84 × 10−4mol x 10 dilution factor

= 1.84 × 10−3mol
Sample 3
= 1.78 × 10−4mol x 10 dilution factor

= 1.78 × 10−3mol

Average moles of NaCIO in 10 mL


2.1 ×10−4 + 1.84 ×10−4 +1.78×10−4
= 2
3

= 1.91 x 10 -4 mol

(Gram/ Liter) of NaCIO in bleach

74.4g NaClO 1 1000 ml


= 1.91 × 10−4 mol NaCIO × 1 mol NaClO × 10ml × 1L

= 1.42 g/ L

Mass percent of NaCIO in bleach

Mass of NaCIO titration


= 1.91 x 10 -4 mol x 74.4 g/mol

= 0.0142 g
Mass of bleach titration
= 1.42 g/mL x (10 mL x 10/ 100)
= 1.42 g
Percentage of NaCIO bleach
= (0.0142 g / 1.42 g) x 100 %
= 1.00 %

Percent deviation between experimental and actual

= 1.00 -5.25 × 100 %


5.25
= 80.95%
Brand: Dobi

Moles of Na2S2O3
Sample 1
0.1084 mol
= x 4.1 x 10-3 L
1𝐿

= 4.44 x 10-4 mol

Sample 2
0.1084 mol
= x 3.2 x10-3 L
1𝐿

= 3.47 x 10-4 mol

Sample 3
0.1084 mol
= x 3 x10-3 L
1𝐿

= 3.25 x 10-4 mol

Moles of NaCIO in 10 mL aliquot

Sample 1

1 mol NaCIO
=4.4 x 10-4 mol Na2S2O3 × 2 mol Na2S2O3

=2.22 x 10-4 mol

Sample 2
1 mol NaCIO
=3.47 x 10-4 Na2S2O3 × Na2S2O3
2 mol Na2S2O3

=1.735 x 10-4 mol

Sample 3
1 mol NaCIO
=3.25 x 10-4 mol Na2S2O3 x 2 mol Na2S2O3

=1.625 x 10-4 mol


Moles of NaCIO in 100 mL aliquot

Sample 1
= 2.22 x 10-4 mol x 10 dilution factor
=2.22 x 10 -3 mol
Sample 2
= 1.735 x 10-4 mol x 10 dilution factor
= 1.735 x 10 -3 mol
Sample 3
= 1.625 x 10-4 mol x 10 dilution factor
= 1.625 x 10 -3 mol

Average moles of NaCIO in 10 mL


2.2 ×10−4 + 1.735 ×10−4 + 1.625 ×10−4
= 2
3

= 1.853 x 10 -4 mol

(Gram/ Liter) of NaCIO in bleach

74.4g NaClO 1 1000 ml


= 1.853 x 10−4 mol NaCIO × 1 mol NaClO × 10ml × 1L

= 1.37 g/ L

Mass percent of NaCIO in bleach

Mass of NaCIO titration


= 1.853 x 10 -4 mol x 74.4 g/mol

= 0.0137 g
Mass of bleach titration
= 1.37 g/mL x (10 mL x 10/ 100)
= 1.37 g
Percentage of NaCIO bleach
= 0.0137 g / 1.37 g x 100 %
= 1.00 %
Percent deviation between experimental and actual

= 1.00-5.25 × 100 %
5.25
= 80.95 %

C) Analysis of Copper (ii) Unknown

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

Moles of Na2S2O3,
0.1084 𝑚𝑜𝑙
Sample 1 = x (11.6 x 10-3 L) = 1.25 x 10-3 mol
𝐿

0.1084 𝑚𝑜𝑙
Sample 2 = x (11.1 x 10-3 L) = 1.20 x 10-3 mol
𝐿

0.1084 𝑚𝑜𝑙
Sample 3 = x (11.9 x 10-3 L) = 1.28 x 10-3 mol
𝐿

From the equation above we can conclude that Number of moles Cu 2+ = Moles of Na2S2O3
Gram Cu2+,
63.546 𝑔
Sample 1 = 1.25 x 10-3 mol x = 0.0794 g
𝑚𝑜𝑙

63.546 𝑔
Sample 2 = 1.20 x 10-3 mol x = 0.0762 g
𝑚𝑜𝑙

63.546 𝑔
Sample 3 = 1.28 x 10-3 mol x = 0.0813 g
𝑚𝑜𝑙

Weight percent of Copper in sample,


0.0794 𝑔
Sample 1 = 0.3187 𝑔 x100 = 24.99 %

0.0762 𝑔
Sample 2 = 0.3007 𝑔 x 100 = 25.34 %

0.0813 𝑔
Sample 3 = 0.3030 𝑔 x 100 = 26.83 %

Average weight percent of copper in sample,


24.99 + 25.34 + 26.83
= 25.72 %
3
Theoretical mass percent copper in compound,

Copper (II) acetate monohydrate

63.546 g/mol Cu2+ x 100 = 31.83%

199.65 g/mol Cu( CH3COO)2. H2O

Copper (II) chloride dehydrate

63.546 g/mol Cu2+ x 100 = 37.27%

170.48 g/mol CuCl2.2H2O

Copper (II) sulphate pentahydrate

63.546 g/mol Cu2+ x 100 = 25.45%

199.65 g/mol Cu2SO4.5H2O

𝑬𝒙𝒑𝒆𝒓𝒊𝒎𝒆𝒏𝒕 𝒗𝒂𝒍𝒖𝒆 – 𝒂𝒄𝒄𝒆𝒑𝒕 𝒗𝒂𝒍𝒖𝒆


Percent error = x 100
𝒂𝒄𝒄𝒆𝒑𝒕 𝒗𝒂𝒍𝒖𝒆

25.72−25.45
= 𝑥 100 = 1.06 %
25.45

Name of unknown copper (ii) unknown : Copper (ii) sulphate pentahydrate

Chemical formula of copper 9II) unknown: Cu2SO4.5H2O


DISCUSSION

This experiment was carried out to analyse the bleach and copper (ii) unknown. The
first onjective was to standardise the Sodium Thiosulphate Solution.

FIGURE 1

A)

B)

C)

D)
Figure 1 below shows the color result from first procedure which was the
standardisation of the sodium thiosulphate solution. This procedure involve the balanced
equation: IO3- + 5I- + 6H+  3I2 (or I3-) + 3H2O

By an oxidation-reduction titration In this experiment the amount of sodium


hypochlorite ion present in a solution of bleach was determined. Hypochlorite ions oxidize
iodide ions to form iodine, I2 in acid solution. During the titration process, red-brown color of
the triiodide ion fades to light yellow . At the point where the I3- was consumed by titration,
the titration solution turn from blue-black to colorless (D) of the iodide ion after the starch
was added. Starch indicator being used in this reaction to detect the endpoint of the titration.
In order to determine the copper (II) unknown is, the average molarity of standardization
sodium thiosulphate, NaCIO have been calculated which was 0.1084 M. This average
molarity will also being used in next procedure analysis of bleach.

FIGURE 2 (COCOREX)

A) B)

C) D)
In the next experiment, Dobi and Cocorex were the bleach brand being used to
determine its percentage of NaCIO. The percentage of sodium hypoclorite in both sample
was recorded to be 5.25%. Figure 2 shows the colour appear in solution from the before
titration (A) , after titrate with standardised sodium thiosulphate solution (B) and then when
2mL starch was added the solution turned to dark color (C) and the process continue with
titration until dark color of starch-iodine disappeared (D). In this experiment, the result
obtained for the percentage mass of NaCIO in Cocorex bleach was 1.00% same as Dobi
bleach .From the result, it can be indicates percentage error of Cocorex was the same as in
Dobi bleach which was 80.95% . The presence of error maybe due to several sources of
errors happen while handle this experiment. For example, failure of properly align the
meniscus with volume mark when using pipette in 10mL of the bleach where eyes must be
perpendicular to the reading marked.

FIGURE 3

A) B)

C)

Figure 3 shows the last experiment which was the analysis of copper (II) unknown.
The mixture of 1 g potassium iodide and dissolve solid with 35 ml 0.005M sulphuric acid
titrated produces the amber color (B) of the triiodide which later begins to fade. When 2 mL
starch indicator was added, the titration process was continued until grey starch-iodine color
disappeared and produce milky white pinkish color (C). From this experiment, we can
analyse the name of unknown copper (ii) unknown that we gain from the sample and
compared with theoretical mass percent of copper both 3 copper salts: Copper (II) acetate
monohydrate, copper (II) acetate dehydrate and copper (II) sulphate pentahydrate in
compound and compared with our average weight percent of copper. Based on the result
obtained, the average weight percent of copper in sample is 25.72 % which the value was
nearer to the copper (II) sulphate pentahydrate value. From this, it can be concluded that the
unknown copper (II) sample is copper (II) sulphate pentahydrate with chemical formula
Cu2SO4.5H2O.

There is some precaution should be considered when carried out the experiment
Firstly wearing lab coat is compulsory when enter the laboratory .Both acids and bases can be
corrosive to human tissue. When it concentrated it can break down the human tissue. This
experiment involves some chemicals such as sulphuric acid. When handling sulphuric acid ,it
must not contact directly to our hand, so we use glove when handle the substance.

CONCLUSION

In conclusion, the molarity of sodium thiosulphate solution is 0.1084 M. Next, the


percentage of the NaClO was 1.00% for both Dobi and Cocorex bleach sample. The
percentage of copper in an unknown copper sample was 25.72 %. This percentage shows that
the unknown copper (II) is actually copper (II) sulphate pentahydrate, Cu2SO4.5H2O.

REFERENCES

1) Purdue University. Sources of error in Pipetting. Retrieved from


http://chemed.chem.purdue.edu/genchem/lab/equipment/pipet/error.html
2) Tucker, K. Purpose adding starch to the titration mixture. Retrieved from
https://education.seattlepi.com/purpose-adding-starch-titration-mixture-6791.html

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