Estimation of Barium

Experiment No: 1 Date: 8.8.2022

Aim:
Determine the amount of Barium as BaSO 4 from the given solution containing
BaCl2.2H2O and 2N HCl.

Theory:
Barium is precipitated as barium sulphate using hot dilute sulphuric acid. The
reaction is exothermic; hence concentrated sulphuric acid is avoided. A measured
volume of the prepared solution is then treated with dilute sulphuric acid; as a
result barium is precipitated out as barium sulphate.

BaCl2 + H2SO4 → BaSO4 + 2 HCl

The precipitate of BaSO4 is ignited between 900-1000℃ and weighed as

BaSO4.The mass of barium present as a whole in the given solution is calculated
knowing that 233.36g of barium sulphate contains 137.36g.

Requirements:
Chemicals: BaCl2.2H2O, 2N HCl, 4N H2SO4.
Glasswares: whatmann filter paper no. 41, crucible, 100cm 3 standard measuring
flask, 10 cm3 pipette, 250cm3 beaker.

Preparation of Reagents:
1. 4N H2SO4
Molecular Weight = 98.066g,
Molecular weig h t 98.066
Gram equivalent mass = n factor
= 2 = 49.033g,
Density of H2SO4 = 1.84 g/cm3
In laboratory, H2SO4 is present with 98% purity
Density × Purity ×1000 1.84 ×98 × 1000
Normality = Equivalent weig h t × 100 = 49.033 ×100 = 36.77N ≅ 37N
N1V1 = N2V2
37×V 1 = 4×100
 4 ×100
V 1= = 10.8 ml
37
2. 2N HCl
Molecular weight = 36.45g,
Gram equivalent mass = 36.45g,
Density of HCl = 1.18g/cm3
In laboratory, HCl is present with 35% purity
Density × Purity ×1000 1.18× 35 ×1000
Normality = Equivalent weig h t × 100 = 36.45 ×100
= 11.33N ≅ 11N
N1V1 = N2V2
11×V 1 =2× 100
2× 100
V1 = ≅ 18 ml
11

Procedure:
1. The given barium chloride solution is filled up to the mark of 100cm 3 in a
standard measuring flask.
2. Pipette out 20cm3 of this solution in a 250cm3 beaker.
3. Add 5cm3 of 2N HCl, following this add 150cm 3 of distilled water in order
to dilute it.
4. Heat this solution until it starts to boil. Then add a hot solution of 4N H 2SO4
(10-15cm3) drop wise with constant stirring, until a white precipitate of
Barium Sulphate is achieved, which is digested on a water bath for 20
minutes, stirring occasionally.
5. Allow the precipitate to settle down, of then test the supernatant liquid for
complete precipitation with 1-2 drops of dilute sulphuric acid.
6. Filter the fine precipitate using whatmann filter paper No. 42.
7. The precipitate is washed with hot distilled water till free from Chloride and
Sulphate.
8. Dry the precipitate on a cone and transfer it to a previously weighed
crucible.
9. Incinerate the filter paper containing the precipitate of Barium Sulphate.
10.Transfer the crucible to a desiccator and weigh the residue as Barium
Sulphate once it is cool.
Observations and Calculations:
1. Mass of crucible (A) = 17.9336g
2. Mass of crucible + BaSO4 (B) = 17.9680g
3. Mass of BaSO4 (B-A), (C) = 0.0344g = 34.4mg

233.36g of BaSO4 contains 137.36g of Barium

137.36 ×0.0344
Mass of barium in 0.0344g BaSO4 = 233.36
= 0.02025g = 20.25mg

Result:
Mass of Barium in the given solution = 0.02025g.
 DEVARDA’S ALLOY
Experiment No. 4 Date: 3/9/22

Aim:
To analyze the given sample of Devarda’s alloy (Estimation Cu by EDTA
Method).

Theory:
Devarda’s alloy is an alloy of Aluminum (44% - 46%), copper (49% - 51%) and
zinc (4% - 6%). Zinc is found in trace amounts and is not estimated by estimation.
While Aluminum and copper can be estimated by gravimetric and iodometric
estimation respectively. Devarda’s alloy is used as a reducing agent in analytical
chemistry. It is used for determination of nitrate ions that is mixed with aqueous
NaOH. Iodometry is used to determine the concentration of oxidising agents
through an indirect process involving iodine as the intermediary.

Requirements:
Chemicals: conc. HCl, conc. HNO3, H2S gas, Fast Sulphone Black Indicator,
0.02N EDTA solution, 2M ammonium acetate, liq. NH3.

Glassware’s and Miscellaneous: Crucible, distilled water, beaker, volumetric

flask, watch glass, etc.

Procedure:
Opening of Alloy:
1. Weigh 0.5g of the supplied sample i.e., Devarda’s alloy in a 250 cm3 beaker.
2. To the weighed sample, add about 5-7 cm3 of aqua regia and mix it properly.
3. Heat the beaker till all the sample particles dissolve completely.
4. Evaporate the solution nearly to dryness and let it cool.
5. Once the beaker is cooled, add 5 cm 3 of dil. HCl slowly. Boil this mixture for a
few minutes and allow it to cool.
6. Once the mixture is cooled transfer it into a 250 cm 3 volumetric flask. Give
washing to the beaker with distilled water for any residue which is left and
transfer it into the volumetric flask.
7. Dilute it to 250 cm3 with distilled water and shake well.
8. This is the stock solution to be used for further estimation.
9. Dissolve accurately 0.5g of an alloy in 5 - 7 cm 3 of aqua regia HCl:HNO3 (1:3)
in 250 ml beakers and heat till all particles of alloy dissolves. Add again 5 cm 3
of aqua regia.
10. Cover with watch glass.
11. Evaporate solution nearly to dryness. Cool and add 5 ml of conc. HCl and boil
for few minutes. Extract the residue with 25 – 30 ml of distilled water and boil
for few minutes.
12. Cool the solution and transfer it to 250 ml standard measuring flask. Wash the
beaker and collect washings in the same standard measuring flask.
13. Dilute it to 250 ml with water and shake well.
Estimation of Cu by EDTA:

1. Prepare 250 ml of 0.02M EDTA solution (1.86g).

2. Pipette out 25 ml in conical flask and add 5 ml of triethyl amine+1 test tube of
distilled water + 4-5 drops 0.5% FSB.
3. Titrate it against 0.02M EDTA till color change blue to dark green is observed.

Reactions:
1. CuC l2+ H 2 S →CuS ↓ 2 HCl
2. Cu ¿
3. 2 AlC l3+ 6 C9 H 7 ON → 2 Al ¿

Preparation of Reagents:
1. For 0.02M EDTA in 250 cm3:
Molecular weight: 373.24 g
 Mass 1000
0.02 = 373.24 × 250

0.02× 373.24 ×250

Mass = 1000
= 1.86g

Observations:
Weight of alloy = 0.5g

Observation Table:
Estimation of Cu by EDTA:

1. Solution of burette: 0.02M EDTA

2. Solution in a conical flask: 25 cm3 stock solution + 5cm3 of liq. NH3 + 5cm3
triethyl amine + FSB
3. End Point: Blue to Dark Green.
Burette
I (cm3) II (cm3) III (cm3) CBR
Readings
Initial 0.0 0.0 0.0
Final 19.8 19.8 19.8
19.8 cm3
Difference 19.8 19.8 19.8
Calculations: -
Estimation of Copper:

25 cm3 of dilute solution requires 19.8 cm3 0f 0.02M EDTA solution.

Therefore, 250 cm3 of dilute solution requires 198 cm3 of EDTA solution.

1000 cm3 of 1M EDTA gives 63.54g of Cu.

63.54 ×0.02 ×198
Therefore, 198 cm3 of 0.02M EDTA solution = 1000

= 0.251g of Cu

0.5g of alloy contains 0.251g of Cu.

 0.251× 100
Therefore, 100g of alloy contains = 0.5

= 50.2g of Cu

= 50.2 % of Cu.

Result:
1. Amount of Copper = 0.251g
2. Percentage of Cu obtained = 50.2%
Inorganic Preparation: Preparation of Tetraamine copper
(II) sulphate monohydrate complex [Cu(NH 3)4(H2O)]SO4

Experiment No. 5 Date:

10.9.2022

Aim: To prepare tetraamine copper sulphate monohydrate complex

[Cu(NH3)4(H2O)]SO4

Theory: When ammonia is added to a solution of copper sulphate, a pale blue

basic salt is precipitated whose composition varies according to the temperature
and concentration of the solution.
CuSO4 + 2NH4OH → Cu(OH)2 + (NH4)2 SO4
4NH3 +CuSO4.5H2O → [Cu(NH3)4] SO4.H20 + 4H2O

This basic salt dissolves in excess of ammonia to form a dark purple blue solution
containing complex ion Cu(NH4)2+ from which it can be crystallized. This is an
example of an octahedral Cu(II) complex in an aqueous medium, where only four
H2O molecules of hex-aquo ions Cu (H2O)6 are replaced by ligands.
The complex is soluble in water but insoluble in alcohol. Therefore, the complex is
isolated by adding alcohol to the aqueous solution.

Requirements:
Chemicals: CuSO4. 5H2O, Liquor NH3, Ethyl alcohol, 0.2N HCl, 1% methyl
orange indicator, 2% Ba(NO3)2 Sol, 0.01N Na2S2O3, 2N CH3COOH, 10% KI,
Distilled water.

Glassware: Watch glass, Burette, Pipettes, 250 cm3 Beaker, Water bath.
Miscellaneous: Sand bath, Whatman filter paper, Crucible, Desiccator.

Preparation of Reagents:

1) 0.2N HCl in 100 cm3 of D/W

Density × purity ×1000
Normality ¿ equivalent weight ×100
1.18× 36 ×1000
N= 36.5 ×100
= 11.638N
N1 V1 = N2 V2
0.2× 100
V1 ¿ 11.63 = 1.719 cm3

2) 2N CH3COOH in 100 cm3 of D/W

Number of gram equivalent weight
Normality=
volume
 x
2N = 60
0.1

X = 2 x 0.1 x 60

X = 12g

Mass
Density = Volume

12
1.05 = Volume

Volume = 11.7 cm3

3) 0.01N Na2S2O3 in 250 cm3 of D/W

Number of gram equivalent weight

Normality=
volume
x
0.01N= 158
0.25

X = 0.395g
So, 0.395g to be dissolved in 100 cm3 solution

4) 10% KI solution 10cm3 D/W:

Dissolve 1g of KI and add 10cm3 D/W

5) 2% Ba(NO3)2 solution 10cm3 D/W

Dissolve 0.2g Ba(NO3)2 and add 10cm3 D/W

Procedure:
(I)Preparation of Complex:

1. Dissolve 4g of CuSO4.5H2O in a mixture of 7cm3 of liquor ammonia and 4cm3

of distilled water.
2. Now add 7cm3 of ethyl alcohol to it and allow it to stand for an hour (cool it
thoroughly in an ice bath and do not disturb it).
3. Filter the bluish violet precipitate through a suction pump with a Whatman
filter paper no. 41 with the help of a Buchner funnel.
4. Wash the precipitate first with a mixture of equal volumes of ethyl alcohol and
liquor ammonia and then with ethyl alcohol. Finally wash it with a small volume of
ether to remove the traces of ethyl alcohol.
5. Dry it in a suction pump for 15-20 minutes and then air dry it.
6. Weigh the product (complex) to find out the yield.

(II)Analysis of Tetraamine Copper Sulphate monohydrate

for the percentage of ammonia:

1.Weigh accurately 0.150g of the complex on a watch glass and transfer

quantitatively in a conical flask. Add 25cm3 of distilled water to it and shake well.

2. After the complex dissolves and a bluish turbid solution is obtained, add 1-2
drop of methyl orange indicator till a dirty brown solution form.

3.Titrate it against 0.2N HCl solution from the burette with constant stirring. The
color changes from yellowish brown to greenish yellow to pinkish orange and
finally to bright orange. At the end point turbidity will disappear and the solution
becomes clear.
4. Repeat the above procedure for two times to get a constant burette reading (6.5
cm3).

(III) Analysis of Tetraamine Copper sulphate monohydrate

for the percentage of Sulphate ions:

1. Weigh accurately 0.20g of the complex on a watch glass and transfer

quantitatively in a 250cm3 beaker.

2. Add 2-3cm3of conc. HCl and heat it on the water bath to decompose the
complex and evaporate it to dryness (Repeat it if necessary).

3. Extract the residue with 25-30cm3 of distilled water and boil it.

4. Transfer the beaker on an asbestos sheet and to the hot solution, add hot 2%
Ba(NO3)2 solution drop wise with constant stirring till precipitation gets
completed.

5. Digest the precipitate on a boiling water bath for 30-45 minutes.

6. Check for the complete precipitation and filter the precipitate through
Whatman paper no.42

7. Wash the precipitate with hot distilled water till the filtrate is free from Cl -
ions.

8. Dry the precipitate on a sand bath using a drying cone.

9. Transfer the dried precipitate of BaSO 4 on a glazed paper and cover it with a
funnel constant weight.

10.Incinerate the filter paper in a previously weighed crucible and heat it for 30-
40 minutes.

11.Transfer the crucible on an asbestos sheet and cool it.

 12.Cool the crucible in a desiccator and weigh it. Note down the weight of
crucible and residue (x g).

(IV)Analysis of Tetraamine Copper Sulphate monohydrate

for the percentage of Copper:

1. Prepare 250cm3 of 0.01 N Na2S2O3.5H2O solution (Dissolve 0.395g of

Na2S2O3.5H2O in 250cm3 of distilled water)

2. Weight accurately 0.250g of the complex on a watch glass and transfer

quantitatively to a 250cm3beaker.

3. Add 5-7 cm3 of conc. HCl and heat it on a sand bath to decompose the
complex and evaporate it to dryness.

4. Extract the residue with 25-30cm3 of distilled water and heat it to boiling.

5. Cool the solution and transfer it to a 100 cm 3 standard measuring flask, wash
the beaker 2-3 cm3 with little distilled water and transfer the washings in the
same flask.

6. Dilute the solution with distilled water up to the mark and shake well for
uniform mixing.

7. Pipette out 100 cm3 of the distilled solution in a conical flask and add 10 cm 3
of distilled water to it.

8. Add anhydrous solid Na2CO3 pinch wise with constant shaking till a faint
precipitate of Cu(OH)2 forms.

9. Dissolve the precipitate by adding 2N CH3COOH drop wise with constant

shaking until a clear solution is obtained or effervescence of CO2 ceases.

10. Add one and a half test tube of 10% KI solution to it and shake well.
 11. Titrate the liberated I2 against 0.01N Na2S2O3 solution from the burette
using freshly prepared starch indicator. End point will be from blue to
colourless.

Reactions:

1. CuSO4 + 4NH3 + H2O → [Cu(NH3)4]SO4.H2O

2. [Cu(NH3)4]SO4 + 4H2O →Cu2(OH)2+ (NH4)2SO4 + 2NH4OH

3. Cu(OH)2 + 2NH4OH + 4HCl→2NH4Cl +CuCl2 + 4H2O

4. [Cu(NH3)4]SO4 + 2HCl → CuCl2 +H2SO4 +4NH3

5. H2SO4 + Ba(NO3)2 →BaSO4 + 2HNO3

6. CuCl2 + 4KI → Cu2I2 + 4KCl + I2

7. I2 + Na2S2O3Na2S4O6+ 2NaI

Observations and Calculations:

(I)Yield of the Complex:

(A) Observed yield of the complex =3.6 g

 (B) Theoretical yield of the complex:

249.54g of CuSO4.5H2O = 245.54g of [Cu(NH3)4]SO4.H2O

245.54 x 4
Therefore, 4g of CuSO4.5H2O = 249.54

= 3.935g of the complex

(II)Analysis of the complex of percentage of Ammonia:

(A) Theoretical percentage of Ammonia:

245.54g of [Cu(NH3)4]SO4.H2O contains 68g of NH3

10.2
Therefore, 0.15g will contain 245.54 g of NH3

= 0.0415g of NH3

0.15g of the complex contains 0.0415g of NH3

write the calculation
0.15- 0.0415
So, 100-x
X=
Therefore, 100g of the complex contains 27.67% of NH3.
 (B) Observed percentage of Ammonia:

Burette solution: 0.2N HCl

Solution in conical flask: 0.15g of complex + 25cm3 of distilled water
Indicator: Methyl orange
End point: Turbid to clear solution
Burette I(cm3) II(cm3) III(cm3) CBR(cm3)
readings
Initial 0.0 0.0 0.0
Final 6.4 6.5 6.5 6.5
Difference 6.4 6.5 6.5

0.15g of the complex required = 6.5cm3of 0.2N HCl Solution

1000cm3of 2N HCl =60g of (en)2
6.5 x 0.2 x 60
Therefore, 6.5cm3 of 0.2N HCl = 1000 x 2
g= 0.039g of NH3
0.15g of the complex contains 0.039g of NH3
0.039 x 100
100g of the complex contains 0.15
gof NH3

=0.26g of NH3
= 26% of NH3

(III)Analysis of the complex of percentage of Sulphate ions:

0.2g of the complex [Cu(NH3)4]SO4.H2O gave ‘a’ = 0.15g of BaSO4

(A) Theoretical percentage of Sulphate ions:

245.54g of [Cu(NH3)4]SO4.H2O contains 96g of Sulphate ions.

0.2g of complex contains 0.0782g of Sulphate ions

 100g will contains 39.1g (39.1% of Sulphate ions).

(B) Observed percentage of Sulphate ions:

0.2g of [Cu(NH3)4]SO4.H2Ogave 0.15g of BaSO4

233.36g 0f BaSO4 = 96g of SO42-ions

96 x 0.18
0.18g of BaSO4 = 233.36 g= 0.0740g of SO42-
0.0740
100g complex contains = x 100%= 37%of sulphate ions.
0.2

(IV)Analysis of the complex of percentage of Copper:

1. Theoretical percentage of Copper:

245.54g of [Cu(NH3)4]SO4.H2O contains 63.54g of Copper

63.54 x 0.25
Therefore, 0.25g of the complex contains = 245.54
g.
= 0.0647g of Copper
100g contains = 0.0647× 4 ×100
=25.88% of Copper.

2. Observed percentage of copper:

 1. Burette solution: 0.01N Na2S2O3 solution
2. Solution in conical flask: 10cm3 of distilled water + 100cm3 of distilled
solution + solid Na2CO3 +2N CH3COOH +10% KI
3. Indicator: Starch Indicator
4. End point: Blue to colourless

Burette I(cm3) II (cm3) III (cm3) CBR (cm3)

readings
Initial 0.0 0.0 0.0
Final 9.4 9.5 9.5 9.5
Difference 9.4 9.5 9.5
1

10cm3 of the distilled solution required 9.5cm3of 0.01N Na2S2O3Solution

100cm3of the distilled solution will require 95cm3of 0.01N Na2S2O3 Solution
63.54 x 0.01 x 95
95cm3of 0.01N Na2S2O3 = 1000

= 0.0603g of copper.

Now, 0.25g of [Cu(NH3)4]SO4.H2O contains 0.0603g of Copper

0.0603 x 100
100g of the complex contains = 0.25
g of Copper

= 24.14g

= 24.14% of Copper

Results:
(1) Yield of the complex (x) = 3.6g

(2) Percentage of NH3 present in the given complex = 26%

(3) Percentage of SO42- ions in the given complex = 37.02%

(4) Percentage of copper present in the given complex = 24.14%
 INORGANIC PREPARATION: Bis (ethylene
diamine) copper sulphate [Cu(C 2H4(NH2)2]SO4
Experiment No. - 06 Date-17.09.2022

Aim –
Preparation of Bis (ethylene diamine) copper sulphate

Theory-
Cu(II) reacts with ethylene diamine, which is ambidentate ligand, to form insoluble
chelate complex. The co-ordination number of copper ion is four as its bonded to
bidentate ligand.

CuSO4 + 2 C2H4(NH2)2 → Cu[C2H4(NH2)2]2SO4

Cu+2 + Na2C10H14O8N2 → Cu[C10H14O4N2]2SO4 + 2Na+

Requirements-
Chemicals: Copper sulphate, Ethylene diamine, ethyl alcohol, 0.05% Fast
Sulphone Black F indicator, 0.01M EDTA solution.
Glassware and miscellaneous: Watch glass, Whatman filter paper No. 42, 250 cm 3
beaker, Distilled water, 100cm3 standard measuring flask, water bath, sand bath,
Buchner funnel.

Preparation of reagents –
1) 0.01 M EDTA Solution in 200 cm3 of Distilled water
1 M 1000 cm3 EDTA = 336.22 g/mol
336.22 X 0.01 X 200
0.01 M 200 cm3 EDTA = 1000
= 0.6724 g of EDTA
2) For 0.05% Fast Sulphone Black indicator
Chemical Formula – C30H20N4O11S3
Molecular Weight – 708.695 g/mol
To make 100 % in 100 cm3 requires = 100 g of compound
100 X 100 X 0.05
 0.05 % in 100 cm3 requires = 100 X 100
= 0.05 g of indicator
Dissolve 50 mg of FAS indicator in 100 cm3 in distilled water
3) For 80% ethylenediamine in of distilled water
Chemical Formula – C2H8N2
Molecular Weight – 60.10 g/mol
To make 100 % in 100 ml requires = 100 ml of ethylene diamine
10 X 80 X 100
 80 % in 10 ml requires = 100 X 100 = 8 ml of ethylene diamine
Take 8ml of ethylenediamine in a 10 ml standard measuring flask and dilute
with distilled water up to mark.
4) For 0.05% Murexide indicator
Chemical Formula – C8H8N6O6
Molecular Weight – 284.188 g/mol
To make 100 % in 100 cm3 requires = 100 g of compound
0.05 X 100 X 100
 0.05 % in 100 cm3 requires = 100 X 100
= 0.05 g of indicator
Dissolve 50 mg of murexide indicator in 10 cm3 of distilled water
 Procedure-
I) Preparation of the Complex:
1.
Dissolve 4g of CuSO4.5H2O in 10 cm3 of distilled water in a 250 cm3 beaker.
2.
Warm it on wire gauze and add dropwise ethylene diamine from the burette
with constant stirring till bright blue color precipitate forms. Add a few more
drops.
3.
Stir the mixture and digest it on a boiling water bath for 30 minutes.
4.
Cool the solution and keep it aside for about 30-45 minutes.
5.
Filter off the bright blue precipitate through Whatman filter paper No. 41
using a Buchner funnel at the suction pump.
6.
Wash the precipitate thirst with distilled water 2-3 times and then with ethyl
alcohol.
7.
Dry it at the suction pump for 15-20 minutes and then in air.
8.
Weigh the product to find out yield (x g).

II) Analysis of Bis (ethylene diamine) copper sulphate for the percentage of
copper

1. Weigh accurately 0.23g of the complex on watch glass and transfer to a 250 cm3
of beaker.
2. Add 5-7 cm3 of conc. HNO3 and heat it in a sand bath, covering the beaker
partially with a watch glass. Heat it nearly to dryness.
3. Extract the residue with 20-25 cm3 of distilled water and boil it for 5 minutes.
4. Cool the solution and transfer it in a100cm3 standard measuring flask.
5. Wash the beaker 2-3 times with 5-7 cm 3 of distilled water each time and
transfer the washings also.
6. Dilute the solution in a standard measuring flask to 100 cm 3 with distilled water
and shake it well.
7. Pipette out 10cm3 of the diluted solution in a conical flask and add one test tube
of distilled water to it.
8. Add 5-7cm3 of liq. NH3 and 4-5 drops of Fast Sulphon Black F indicator to it.
9. Titrate it against 0.01M EDTA solution from the burette till the color changes
from blue to dark green.
10.Repeat the titration to get constant readings (x cm3).
III. Analysis of Bis (ethylene diamine) copper sulphate for the percentage
of Sulphate ions:
1. Weigh accurately 0.2g of the complex on a watch glass and transfer
quantitatively in a 250 cm3 beaker.
2. Add 2-3 cm3 of conc. HCl and heat it on a water bath to decompose the complex
and evaporate it to dryness. (Repeat it if necessary)
3. Extract the residue with 25-30cm3 of distilled water and boil it.
4. Transfer the beaker on an asbestos sheet and to the hot solution, add hot 2% Ba
(NO3) solution dropwise with constant stirring till precipitation gets completed.
5. Digest the precipitate on a boiling water bath for 30-45 minutes.
6. Check for the complete precipitation and filter the precipitate through Whatman
filter paper No 42.
7. Wash the precipitate with hot distilled water till the filtrate is free from Cl - ions.
8. Dry the precipitate on a sand bath using a drying cone.
9. Transfer the dried precipitate of BaSO4, on a glazed paper and cover it with a
funnel.
10.Incinerate the filter paper in a previously weighed silica crucible and heat it till it
becomes white ash.
11.Transfer the crucible on an asbestos sheet and cool it. Transfer the precipitate in
the crucible and heat it for 30-40 minutes.
12.Cool the crucible in a desiccator and weigh it. Note down the weight of crucible
and residue (X g).
13.Heat the crucible again for 15-20 minutes and weigh the crucible after cooling to
get a constant weight.

IV. Analysis of Bis (Ethylene diamine) copper sulphate for the percentage of
Ethylene diamine

1. Weigh accurately 0.15 g of the complex on a watch glass and transfer

quantitatively in a conical flask. Add 25cm 3 of distilled water to it and shake
well.
2. After the complex dissolves and a bluish turbid solution is obtained, add 1-2
drops of methyl orange indicator. Dirty yellowish-brown solution forms.
3. Titrate it against 2 N HCl solution from the burette with constant stirring.
4. The color changes from yellowish brown to greenish yellow to pinkish orange
and finally to bright orange. At the end point turbidity will disappear and
solution becomes clear.
Observation and calculation-
I) Yield of complex

A) Observed yield of the complex (X) = 4.71 g

B) Theoretical Yield of complex:
249.54 g of CuSO4.5H2O = 279.54 g of Cu(en)2SO4
279.54 X 10
10 g of CuSO4.5H2O = 249.54
= 11.20 g of complex

II) Analysis of complex of the percentage of copper:

Burette reading (I) (II) (III) CBR (cm3)

for 0.01 M EDTA
Initial 0.0 0.0 0.0
Final 8.8 8.6 8.8 8.8
Difference 8.8 8.6 8.8

A) Theoretical % of copper:
10 cm3 of the diluted solution required 8.8 cm3 of 0.01M EDTA solution
100 cm3 of the diluted solution required 88 cm3 of 0.01M EDTA solution
1000 cm3 of 1M EDTA = 63.54g of copper cm3 of 0.01M EDTA
63.54 X 88 X 0.01
 88 cm3 of 0.01 M EDTA = 1000
= 0.0559 g of copper

279.54g of Cu(en2)SO4 contains 63.54 gm of Copper

63.54 X 0.25
 0.25 gm of Cu(en2)SO4 contains = 276.54
= 0.0568 g of copper

0.0568 X 100
Now, 100 gm of Cu(en2)SO4 contains = 0.25
= 22.72 % of copper
B) Observed % of copper:
 0.25 gm of salt contain 8.8 cm3 of 0.1 N EDTA solution
1000 cm3 1 N EDTA solution = 63.54 g of Cu
63.54 X 8.8 X 0.1
8.8 cm3 1 N EDTA solution = 1000
=0.0559 g of Cu
0.25 gm of Cu(en2)SO4 contain 0.0559 gm of copper
0.0559 X 100
100 gm of Cu(en2)SO4 contain = 0.25
= 22.36 g of copper
 percentage of copper ions = 22.36 %

III) Analysis of the complex for the percentage of Sulphate ion:

A) Theoretical % of sulphate ion:

279.54 gm of [Cu(en)2)]SO4 contains 96 gm of SO4-2 ion
96 X 0.20
0.20 gm of [Cu(en)2)]SO4 contains = 279.54
= 0.06879 g of SO4-2 ion
0.06879 X 100
 percentage of SO4-2 ions = 0.20
= 34.35 %

B) Observed % of sulphate ion:

0.20 gm of [Cu(en)2)]SO4 contains 0.1624 gm of BaSO4

233.36 gm of BaSO4 = 96 gm of SO4-2 ion

96 X 0.1624
0.1624 gm of BaSO4 = 233.36
= 0.0668 gm of SO4-2 ion

0.2 gm of [Cu(en)2)]SO4 contains 0.0668 gm of SO4-2 ion

0.0668 X 100
100 gm of [Cu(en)2)]SO4 contains = 0.2
= 33.4 gm of SO4-2 ion
 percentage of SO4-2 ions = 33.4 %
IV) Analysis of the complex for the percentage of Ethylene diamine(en):

Burette reading (I) (II) (III) CBR (cm3)

for 0.01 M EDTA
Initial 0.0 0.0 0.0
Final 2.4 2.6 2.6 2.6
Difference 0.0 2.6 2.6
A) Theoretical % of (en) ion:
279.54 g of [Cu(en)2)]SO4 contains = 120.2 g of ethylene diamine ion
0.15 X 120.02
0.15 g of [Cu(en)2)]SO4 contains = 279.54
= 0.0645 g (en) ion
100 X 0.0645
100 g of [Cu(en)2)]SO4 contains = 0.15
= 43 g of (en) ion

 Percentage of ethylene diamine ions = 43%

B) Observed % of (en) ion:
0.15 g requires 2.6 ml 0.2 N HCl solution

1000 ml 1 N HCl solution = 120.2 g of (en) ion

2.6 X 120.2
2.6 ml 1 N HCl solution = 1000
= 0.0625 g of (en) ion

0.0625 X 100
Percentage of ethylene diamine ions = 0.15
= 41.67%

Result-
1. Yield of the complex (X) = 4.71 gm
2. Observed percentage of sulphate ion =33.4 %
3. Observed percentage of copper ion = 22.36 %
4. Observed percentage of ethylene ion = 41.67%
 Determination of Copper (II) ions spectrometrically by
titration with EDTA

Experiment No: 7 Date:

26.9.2022

Aim:
To determine the copper (II) ions spectrometrically by titration with EDTA.

Theory:
The beer Lamberts Law is a linear relationship of absorbance with thickness and
concentration. The mathematical statement of law is A = ƐCL.

Where,

A=Absorbance measured

C=Concentration of the solution

L=Thickness of the light absorbing material

Ɛ=molar extinction coefficient

The amount of copper present can be determined by spectrophotometer. The

titration is carried out at 745 nm at pH 2.4, where the molar extinction coefficient
is highest for copper EDTA complex.

Requirements:
Chemicals: 0.04M CuSO4.5H2O, 1M HCl, Sodium acetate, 0.05M EDTA,
Distilled water

Glassware and miscellaneous: Standard flask 100 cm3, 250 cm3 beaker, pipette
10 cm3, glass rod, pH meter, spectrophotometry, cuvette, tissue
Preparation of Reagents:
1. For 0.04 M CuSO4.5H2O in 250 cm3 distilled water
Molecular weight = 250g
W × 1000
M = MW ×Vol ( ml )
M × MW ×Vol(ml)
W=
1000
0.04 ×249.68 × 250
W= 1000

W = 2.496g

2. For 1M HCl in 250 mL of distilled water

Molecular Weight = 36.5g

N1V1=N2V2
12 ×V 1=1 ×250

250
V 1=
12

V1 =20.83 mL

3. For 1 M of Sodium Acetate in 250mL of Distilled water

Molecular Weight = 82g
M × MW ×Vol(ml)
W=
1000
1× 82.03 ×250
W= 1000
W = 20.50g
4. For 0.05M EDTA in 250mL of Distilled water
Molecular weight = 372.24
M × MW ×Vol(ml)
W=
1000
0.05 ×372.24 × 250
W= 1000
W = 4.653g
Procedure:
1. Pipette out 10ML of 0.04 molar copper (II) ion solution and add it add to
each twelve 100 mL standard measuring flasks.
2. Add 20mL of buffer solution to each flask.
3. Pipette out 0.0, 1.0, 2.0, up to 11.0 mL of 0.05 molar EDTA solution and
transfer to each of the standard measuring flask in increasing order.
4. Diluted solution 200mL. By adding distilled water.
5. Measure absorbance of each solution at 745 nm against reagent blank.
6. Plot the graph of absorbance of. Observance against 0.05 molar EDTA
solution.
7. From the graph, the intersection of two straight lines gives the endpoint, that
is the amount of 0.05 molar EDTA required by 10mL of diluted Cu (II)

Observation:
Filter used: 745 nm

Flask no. Cu (II) Buffer solution 0.05 Final Absorbance

ion (pH=2.4) EDTA volume in
Solution solution cm3
(cm3)
1 10 20 0 100 0.053
2 10 20 1 100 0.072
3 10 20 2 100 0.096
4 10 20 3 100 0.133
5 10 20 4 100 0.179
6 10 20 5 100 0.185
7 10 20 6 100 0.207
8 10 20 7 100 0.232
9 10 20 8 100 0.263
10 10 20 9 100 0.264
11 10 20 10 100 0.262
12 10 20 11 100 0.265
Graph:
Chart Title
0.3
0.263 0.264 0.262 0.265
0.25 0.232
0.207
0.2 0.185
0.164
Absorbance

0.15 0.133
0.096
0.1 0.072
0.053
0.05

0
1 2 3 4 5 6 7 8 9 10 11 12

0.05M of EDTA (mL)

Calculation:
10 cm3 of dilute copper ion solution requires ‘9’cm3 of 0.05 M EDTA
∴250 cm3 of dilute copper ion solution requires 25 × 9

1000 cm3 of 1M EDTA = 63.54 g of copper

∴1 cm3 of 1M EDTA = 63.54 mg of copper

63.54 ×225 × 0.05

∴225 cm3 of 0.05 M EDTA = = 714.825 mg of Cu
1

Result:
1. 10 cm3 of dilute copper ion solution requires 9 cm3 of 0.05M EDTA
solution.
2. Amount of copper present in the given solution is 714.825 mg.