LABORATORY REPORT CHM421

EXPERIMENT 6A : ANALYSIS OF
BLEACH AND COPPER (II) UNKNOWN

NAME : MAWADDAH BINTI AHMAD NABIL

MATRIC NO. : 2017442624

GROUP : AS2532A1

PARTNER’S NAME : MIMI MUSFIERA BT MAHMOOD

LECTURER’S NAME : PN RUHANI BINTI IBRAHIM

DATE OF EXPERIMENT : 18 APRIL 2019

DATE OF SUBMISSION : 25 APRIL 2019

ABSTRACTS
The main objective in this experiment is to determine the percentage of NaClO on
sample and to determine the percentage of copper in an unknown copper sample. The
sodium thiosulphate solution was standardised to get the actual molarity which is M. For
analysis of bleach in part B, 10 mL of the bleach samples which is Cocorex and Deepax brand
were used as samples and it was diluted with distilled water into preweighed 100 mL
volumetric flask. The volumetric flask was reweighed and the density of bleach solution was
calculated. The sample was diluted to the 100 mL mark with distilled water. 10 mL aliquot of
bleach solution, potassium iodide and hydrochloric acid solution was titrated against the
standardized sodium thiosulphate until 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 in 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.

OBJECTIVE
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
Sodium hypochlorite, NaClO is an oxidizing agent that usually used in household
bleach. NaClO is prepared by bubbling chlorine gas into a sodium hydroxide solution. Part
of chlorine is oxidizing to the hypochlorite ion, OCl and some reduced to chloride ion, Cl-.
The excess hydroxide keeps the resulting solution strongly basic. An equation describing this
process is

H2O + ClO-  I2 + 2OH

I2 + I-  I3-

Thus, the net reaction of hypochlorite with iodide is

H2O + ClO- + 3I-  I3- + Cl- + 2OH

PROCEDURE
A. Standardisation of the Sodium Thiosulphate solution.
1. A burette was thoroughly washed with detergent followed by tap water. The
burette was rinsed with distilled water and finally with thiosulphate solution that
was provided. The cleaned burette was filled with fresh thiosulphate solution.
2. 2 g of solid KI was weight and transferred into 250 mL conical flask. 50 mL of
0.010 M of KIO3 solution was pipette into the same flask and 10 mL of 1.0 M of
H2SO4 was added. The flask was placed in fume hood while 1.0 M of H2SO4 was
added into it. The colour of the solution in flask was turned to a deep brown. The
reaction that occurred in the flask is:
IO3- + I- + H+  I2 + H2O
3. The solution was immediately titrated in the flask with thiosulphate solution until
the colour of solution was changed to light yellow.
4. 2 mL of starch indicator was added using cylinder at this point. The solution was
turn to blue-black when the starch was added.
5. The titration was continued after the starch was added. The titrant drop was
added wisely until the solution in the conical flask was clear and colourless. The
volume of the titrant used was recorded. The reaction that occurred in the flask
between thiosulphate and triiodide to produced iodide and tetrathionate is:
S2O32- + I2  I- + S4O62-
6. The whole process was repeated for two times.

B. Analysis of bleach.
1. 100 mL of clean and dry volumetric flask was obtained. The weight of the empty
100 mL volumetric flask was recorded into notes book.
2. 10 mL of pipette was thoroughly cleaned and rinsed with first bleach solution. 10
mL of the sample was pipette into the pre-weighed 100 mL volumetric flask. The
flask was reweight and recorded. This gave the density of the bleach solution.
3. The sample was diluted to the 100 mL mark with distilled water. The dropper
was used towards the end. The flask was stopper and mixed well.
4. The pipette was rinsed out with distilled water followed with a little of the
diluted bleach solution and a 10 mL of fresh aliquot was pipetted into a 250 mL
conical flask. 1 g of potassium iodide was added and swirl the resulting mixture. 5
mL of 6 M HCl was added to the mixture.
5. The sample was titrated with standardised sodium thiosulphate solution above
until the amber iodine colour begins faded to light yellow. 2 mL of starch solution
was added and was continued to titration process until the dark colour of the
starch-iodine complex appeared. ½ drop quantities was used as near to the end-
point by swiftly turning the stopcock 180°. An abrupt colour changed from dark
 blue to colourless marks the endpoint. The titration was repeated with two more
10 mL aliquot of the diluted bleach solution.
6. The analysis was repeated with the second brand of bleach sample.

C. Analysis of Copper (II) Unknown

1. 0.3 g of copper (II) unknown was weight accurately and transfer into 250 mL
conical flask.
2. The solid was dissolved with 35 mL of 0.05 M sulphuric acid. 1 g of potassium
iodide was added and swirled.
3. The mixture was carefully titrated with standardised sodium thiosulphate
solution until the amber colour of the triiodide begins to fade. 2 mL of starch was
added at this point.
4. The titration was continued until grey starch-iodine colour disappeared that
produced milky white-pinkish colour that marks the end point. The process was
repeated for two more samples.
RESULT AND DATA
A. Standardisation of sodium thiosulphate solution
1 2 3
Final reading of 28.3 28.3 28.3
thiosulphate
solution
Initial reading of 0 0 0
thiosulphate
solution
Volume of 28.3 28.3 28.3
thiosulphate
solution

B. Analysis of Bleach
Brand of bleach I = Cocorex bleach
1. Molarity of Na2S2O3 = 0.0353
2. Mass of volumetric flask + 10 mL bleach = 76.8080 g
3. Mass of volumetric flask = 65.6598 g
4. Mass of 10 mL bleach = 11.1482 g
5. Density of bleach = 1.11482 g/mL

Sample 1 Sample 2 Sample 3

Final reading of thiosulphate solution 5.20 8.40 11.60
Initial reading of thiosulphate solution 0 5.20 8.40
Volume of thiosulphate solution (mL) 5.20 3.20 3.20
Moles of Na2S2O3 0.0353 0.0353 0.0353
Moles of NaClO in 10 mL aliquot1
Moles of NaClO in 10 mL aliquot2
Moles of NaClO in 10 mL bleach sample
Average moles of NaClO in 10 mL bleach
sample
Gram/L of NaClO in bleach
Mass percent of NaClO in bleach
Mass percent of NaClO manufacturer’s
label
Percent deviation between experimental
and label values
 C. Analysis of copper (II) Unknown
1. Molarity of Na2S2O3 solution = M
Sample 1 Sample 2 Sample 3
Mass of copper(II) compound taken (g) 0.30 0.30 0.30
Final reading Na2S2O3 solution 11.70 11.70 11.70
Initial reading Na2S2O3 solution 0 0 0
Volume of Na2S2O3 solution (mL) used 11.70 11.70 11.70
Moles of Na2S2O3
Moles of Cu2+
Gram of Cu2+
Weight percent of copper in sample taken
Average weight percent of copper in sample
Theoretical mass percent of copper in
compound
Percent error
Name of unknown copper(II) unknown
Chemical formula of copper(II) unknown

CALCULATION
A. Standardisation of Sodium Thiosulphate Solution.
2S2O32- + I3-  3I- + S4O62-

MaVa = 2MbVb
Ma = 2MbVb/Va

Ma1 = 2(0.01x50.0)/28.3
= 0.0353M
Ma2 = 2(0.01x50.0)/28.3
= 0.0353M
Ma3 = 2(0.01x50.0)/28.3
= 0.0353M
Average Ma = (0.0353+0.0353+0.0353)/3
= 0.0353 M

B. Analysis of Bleach

Cocorex Bleach
ClO- + 2S2O32-  S4O62- + Cl- + 2OH-
MaVa = 2McVc
Mc = MaVa/2Vc
Mc1 = (0.0353x5.20)/2(10)
= 0.0091 M
Mc2 = (0.0353x3.20)/2(10)
= 0.0056 M
Mc3 = (0.0353x3.20)/2(10)
= 0.0056 M
Mc Average = (0.0091+0.0056+0.0056)/3
= 0.0068 M

1) No of moles S2O32- = 0.0353 x 0.0052

= 1.8356x10-4 mol
2) No of moles S2O32- = 0.0353 x 0.0032
= 1.1296x10-4 mol
3) No of moles S2O32- = 0.0353 x 0.0032
= 1.1296x10-4 mol

Average no of moles of S2O32- = ((1.8356x10-4)+(1.1296x10-4)+(1.1296x10-4))/3

= 1.3649x10-4 mol

No of moles ClO- = (1.8356x10-4)/2

= 9.178x10-5
No of moles ClO- = (1.1296x10-4)/2
= 5.648x10-5
No of moles ClO- = (1.1286x10-4)/2
= 5.648x10-5

Average no of moles of ClO- = ((9.178x10-5)+(5.648x10-5)+(5.648x10-5))/3

= 6.8247x10-5 mol

No of moles ClO- in 10 mL original bleach

= (6.8247x10-5 mol) x 10
= 6.8247x10-4 mol

Mass of ClO- mol = no. of moles ClO- x molar mass of ClO-

= 6.8247x10-4 mol x 74.45 g/mol
= 0.0508 g

Density of NaClO (in bleach) g/L

= 6.8247x10-4 mol x (74.45g/1mol) x (1/10mL) x (1000mL/1L)
= 5.0810g/L or 5.0810x10-4 g/mL
 Mass % of NaClO- in bleach
= (5.0810x10-3/1.00197) x 100%
= 0.5071 %

Deepax Bleach
ClO- + 2S2O32-  S4O62- + Cl- + 2OH-
MaVa = 2McVc
Mc = MaVa/2Vc

Mc1 = (0.0353x1.20)/2(10)
= 0.0021 M
Mc2 = (0.0353x1.40)/2(10)
= 0.0025 M
Mc3 = (0.0353x1.30)/2(10)
= 0.0023 M
Mc Average = (0.0021+0.0025+0.0023)/3
= 0.0023 M

1) No of moles S2O32- = 0.0353 x 0.0021

= 7.413x10-5 mol
2) No of moles S2O32- = 0.0353 x 0.0025
= 8.825x10-5 mol
3) No of moles S2O32- = 0.0353 x 0.0023
= 8.119x10-5 mol

Average no of moles of S2O32-- = ((7.413x10-5)+(8.825x10-5)+(8.119x10-5))/3

= 8.119x10-5 mol

No of moles ClO- = (7.413x10-5)/2

= 3.7065x10-5
No of moles ClO- = (8.825x10-5)/2
= 4.412x10-5
No of moles ClO- = (8.119x10-5)/2
= 4.0595x10-5

Average no of moles of ClO- = ((3.7065x10-5)+(4.412x10-5)+(4.0595x10-5))/3

= 4.0593x10-5 mol
 No of moles ClO- in 10 mL original bleach
= (4.0593x10-5 mol) x 10
= 4.0593x10-4 mol

Mass of ClO- mol = no. of moles ClO- x molar mass of ClO-

= 4.0593x10-4mol x 74.45g/mol
= 0.0302 g

Density of NaClO (in bleach) g/L

= 4.0593x10-4 mol x (74.45g/1mol) x (1/10mL) x (1000mL/1L)
= 3.0221g/L or 3.0221x10-4 g/mL

Mass % of NaClO- in bleach

= (3.0221x10-3/1.0022) x 100%
= 0.2995 %

C. Analysis of copper(II) unknown

2Cu2+ + 2I- + 2S2O32-  2CuI + S4O62-

Cu2+ = 63.546g/mol
CuSO4. 5H2O = 63.546 + 96.07 + 90 = 246.616g/mol

1. No of moles Cu2+ = 0.0353M x 0.0117

= 4.1301x10-4

Mass of Cu2+ = (4.1301x10-4) x 63.546g/mol

= 0.0262g

%weight = (0.0262g/0.3000) x 100

= 8.73%

2. No of moles Cu2+ = 0.0353M x 0.0117

= 4.1301x10-4

Mass of Cu2+ = (4.1301x10-4) x 63.546g/mol

= 0.0262g

%weight = (0.0262g/0.3000) x 100

= 8.73%
3. No of moles Cu2+ = 0.0353M x 0.0117
= 4.1301x10-4

Mass of Cu2+ = (4.1301x10-4) x 63.546g/mol

= 0.0262g

%weight = (0.0262g/0.3000) x 100

= 8.73%

Average % weight = (8.73 + 8.73 + 8.73)/3

= 8.73%

Mass of Cu2+/mass of unknown Cu = atomic mass of Cu/molar mass of unknown Cu

Experimental

23.03g/100g = 63.546/ molar mass of unknown Cu

Molar mass of unknown Cu = 192.3887g/mol

Copper (II) acetate monohydrate

(63.546g/mol / 199.482g/mol) x 100 = 31.83%

Copper (II) chloric dihydrate

(63.546g/mol / 170.428g/mol) x 100 = 37.27%

Copper (II) sulphate pentahydrate

(63.546g/mol / 249.64g/mol) x 100 = 25.46%

 DISCUSSION

In this experiment, the amount of hypochlorite ion in a solution of bleach is

determined by an oxidation and reduction titration, the iodine thiosulphate titration
procedure. In acid solution, hypochlorite ion oxidize iodide ions to form iodine,I2.
The iodine that formed is then titrated with a standard solution of sodium
thiosulphate.

The analysis takes place in a series of step;

1) Acidified iodide ion is added to hypochlorite ion solution and the iodide is
oxidised to iodine.

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

2) Iodine is only slightly soluble in water. It dissolves very very well in an aqueous
solution of iodide ion, in which it forms a complex ion called triiodide ion. The
iodide 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 thiosulphate ions, which

reduces the iodine back to iodide ions

In part A, the standardisation of the sodium thiosulphate solution was done and
the average molarity is 0.0353 M. Three samples was done with one rough and the
average was get to determine the accurate titrant needed in order to turn the blueblack
color to colorless.

Figure 1
 In part B, two samples of bleach was got to analyse the percentage of NaClO in
bleach samples. For Cocorex bleach sample, the molarity is 0.0353 M and the density of
bleach is 1.11482g/mL. Percent deviation between experimental and label for Cocorex
sample was 50.710% and for Deepax sample was 40.100%. It shows large amount of NaClO
in bleach sample as it was a good bleach to remove any dirt on clothes. Some error was
occurred during the experiment which is the titrant was added a little more than as it
should, this error was affect the results and the results obtained are not accurate.

In part C, the copper(II) unknown was weighed in three sample which is sample 1, 2
and sample 3 which is 0.3g, 0.3g and 0.3g respectively. The number of moles of Na2S2O3 is
0.0353 and number of moles for Cu2+ is 4.1301x10-4 for all three samples as all three
samples has same weight. The weight percent of copper(II) in sample is 8.73% and the
theoretical mass percent of copper in compound is 31.83%. For copper(II) unknown was
determine by calculating the percent copper in compound, the copper(II) unknown is
copper(II) acetate monohydrate, C4H8CuO5.

Figure 2
CONCLUSION

In this experiment, the sodium thiosulphate solution was successful standardised

and the percentage of NaClO in bleach sample is 0.5071% in Cocorex sample and 0.2995% in
Deepax sample. The percentage of copper in an unknown sample is 8.73%.

REFERENCES

1) Laboratory manual CHM421 Analytical Chemistry

2) www.scienceteacherprogram.org