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 1

Index

 Experiment no-1: Determination of the concentration of a solution of NaOH

by titration with a primary standard substance.

 Experiment no-2: Determination of the strength of Na2S2O3 by iodometric

reaction.

 Experiment no-3: Determination of the change of enthalpy of a chemical

reaction by using calorimeter.
 2

Experiment No: 01
Name of the experiment:
Determination of the concentration of a solution of NaOH by titration with a
primary standard matter.
Introduction:
Determination of the concentration of one solution by addition of a stoichiometric
amount of a second solution from burette is a volumetric analysis. By using the
two known volume and one concentration we can determine the another
concentration.
In this filtration, we will use oxalic acid as primary standard and NaOH as
secondary standard. An indictor will be used in this acid-base titration which is a
dye and charges colour over a specific pH range and indicate the ending point.
In this volumetric analysis, firstly we will take an accurate amount of pure
substance and dissolve it in a solvent to produce a solution of accurately known
volume and concentration. In this volumetric analysis we have to calculate the
analysis more precisely and accurately to make it more useful.

Principle:
In this experiment concentration of NaOH solution is determined by a standard
oxalic acid solution.The oxalic acid and NaOH react in a 1:2 ratio.The amount of
NaOH consumed is accurately known.The volume and concentration of NaOH is
also known.By using this information we have to determine the concentration of
NaOH.
 3

Reaction:
COOH (aq) + 2NaOH (aq) COONa (aq) + 2H2O (aq)
COOH COONa

Materials:
 NaOH
 Oxalic acid
 Phenolphthalein
 volumetric flask
 burette
 conical flask
 pipette
 beaker
 measuring cylinder
 spatula
 water
Method:
Preparation of oxalic acid solution:
1. Weigh about 3.2 g of oxalic acid in a conical flask. Record the exact mass of
oxalic acid weighed.
2. Then we have to add about 50 ml of water to make a solution.
3. Without any loss transfer the solution through a funnel into 250 ml volumetric
flask.
4. Add water carefully until the water level is 1 to 2 cm below the graduation mark.
5. Using a dropper, add water drop by drop until the bottom of the meniscus is in
line with the graduation mark on the flask.
6. Calculate the concentration of oxalic acid solution based on the actual mass
weighed out.
 4

Titration of NaOH solution with oxalic acid standard solution:

1. Collect about 100ml NaOH in a clean dry 250 ml beaker/conikal flask.
2. Rinse the burette with 10 ml of water followed by about 10 ml of the NaOH
solution. Then fill the burette with the NaOH solution.
3. Pipette 10 ml of standard oxalic acid solution into a 100 ml conical flask and add
1 or 2 drops of phenolphthalein solution to the flask.
4. Titrate the oxalic acid solution with the NaOH solution.
5. Repeat the titration process until at least three concordant results are obtained.
6. Then we will wash and clean all glassware and apparatus. I have used and return
them to the lab attendant.
7. Calculate the concentration of NaOH solution using the mole ratio of oxalic
acid to NaOH.
Calculation:

COOH (aq) + 2NaOH (aq) COONa (aq) + 2H2O (aq)

COOH COONa

Experiment Volume of Volume of NaOH(ml)

NO. Oxalic acid Initial Ending Net Average
(ml) point Point volume
1 10 0 1.6 1.6
2 10 1.6 3.1 1.5 1.5
3 10 3.9 5.4 1.5

According to the equation-

1 mole H2C2O4≡2 mole NaOH
Mass of oxalic acid= 6.3035×10-3g
 5

6.3035×10−3
Moles of oxalic acid =
126.07

=5×10-5
1000 × 𝑤
∴ Concentration of oxalic acid =
𝑀𝑣
1000×n
=
V

1000×5×10−5
=
10

=5× 10−5

∴ Moles of NaOH = 2 × (5 × 10−5 )

=1× 10−4

𝑛
∴ Concentration of NaOH =
𝑣

1×10−4
=
1.5×10−3

= 0.067𝑀

Result:
The concentration of NaOH is 0.067M
 6

Experiment No: 02
Name of the Experiment:
Determination of the strength of Na2S2O3 by “Iodometric reaction”.
Principal:
Iodometric reaction is an oxidation and reduction reaction. In this reaction we will
use standard K2Cr2O7 solution to determine strength of Na2S2O2. Titration
involving with iodine or iodead are respectively known as iodimetric and
iodimetric titration because I2 is got from KI. The reaction of this experiment is
6KI+ K2Cr2O7 +14HCl=2CrCl3+8KCl+3I2+7H2O
(6I − +14H+ + CrO72- + 6e- =2Cr3++3I2 +7H2O)
2 Na2S2O3+ I2 = Na2S4O6+2NaI
(S2O32- + e- = S2O62- + I-)
In the second step of the reaction a specific indicator is used that is ‘starch’ which
has a significant effect on iodine.
Starch + I2 =Starch – Iodine (blue colour)
Starch- iodine +6 S2O32- =Starch + 6I- + 3S4O62-
If to a solution containing a little iodine ,some starch solution is added and
Na2S2O3 is run in from the burette ,the blue colour of the starch iodine complex
will disappear from the solution as soon all the iodine has been reduced to iodide
ion.
Materials:
 Conical flask
 Burette
 Pipette
 Volumetric flask
 Stand
 Funnel
 K2Cr2O7
 Na2S2O3
 KI
 7

 NaHCO3
 HCl (concentrated)
 Starch (indicator)

Procedure:
1. Firstly we have to take a dry, clean 250 ml conical flask and to which add 25 ml
of water followed by add 0.5g of NaHCO3 and shake the solution to dissolve it.
2. Then we have to add 0.5g and continue to shake.
3. At this point add 5 ml of 1M HCl followed by 10ml of 0.1N K 2Cr2O7 to the
conical flask. Then keep the conical flask in dark inside the locker.
4. Add another 50ml of water to the conical flask. Then add few drops of Na2S2O3
to the conical flask.
5. When most of the I2 liberated the solution turns into a yellowish green colour.
Then add few drops of starch into the flask and the colour will change to deep blue
colour.
6. Addition of Na2S2O3 solution continued drop wise until one drop change the
colour from blue to light green. The end point is sharp and observed in a good light
against a white back ground
Now we have to calculate the strength of Na2S2O3 using V1S1=V2S2
Calculation:
6KI+K2Cr2O7+14HCl=2Cr Cl3+8KCL+3I2+7H2O
2 Na2S2O3+I2=Na2S4O6+2NaI
According to the equation-
14 mole HCl ≡ 3 mole I2 ≡ 6 mole Na2S2O3
14 mole HCl ≡ 6 mole Na2S2O3
Or, 7 mole HCl ≡ 3 mole Na2S2O3

∴ 3 × V(HCl) × S(HCl) =7×V (Na2S2O3) ×S(Na2S2O3)

 8

Experiment Volume of Volume of NaOH(ml)

NO. Oxalic acid Initial Ending Net Average
(ml) point Point volume
1 5 22.3 23.6 1.3
2 5 23.6 25.1 1.5 1.4
3 5 25.1 26.5 1.4

∴ 3 × 5 × 1 = 7 × 1.4 × 𝑆(Na2S2O3)
∴ 𝑆(Na2S2O3) = 1.53 M
Result:
The strength of Na2S2O3 is 1.53 M.
 9

Experiment No: 03
Name of the experiment:
Determination of the change of enthalpy of a chemical reaction by using
calorimeter.
Introduction:
There are mainly two kinds of chemical reactions in thermochemistry. These are
exothermic and endothermic reaction. In exothermic reaction, the energy or heat
increases so that the temperatures increase and in endothermic reaction, the energy
or heat is absorbed so that the temperatures decrease.
Generally, we use calorimetric process to determine the change of enthalpy which
is defined by ∆𝐻 which is positive for endothermic reaction and negative for
exothermic reaction and measured in Kilo Joule (KJ) unit.
In calorimetric process, a calorimeter is used to measure the change of enthalpy. A
calorimeter is any well insulated apparatus that can hold the reactants and products,
so the amount of heat, that is absorbed or released by a reaction, can be measured.
The heat is necessary to raise the temperature of the calorimeter and its content can
be calculated from the following equation:
Q= m× Csol × ∆T + Ccal × ∆T
Here, Csol= heat capacity of the solution
m= mass of solution
Ccal= calorimeter heat capacity
∆𝑇= change of temperature
Since the reaction is carried out at constant pressure (because the calorimeter is
open to air), by definition the heat associated with the reaction is equal to the ∆𝐻.
Thus-
∆𝑯 = −(𝒎 × 𝑪𝒔𝒐𝒍 × ∆𝑻 + 𝑪𝒄𝒂𝒍 × ∆𝑻)

One problem in calorimetric is the determination of the temperature change. This

problem can be overcome by measuring the temperature of reactants and products
periodically and extrapolating the temperature graphically to the time of mixing.
 10

Hess’ law states that enthalpy change for chemical reactions equals the sum of the
enthalpy changes for any series of reactions which can be combined to give the
reaction of interest.
NaOH(aq) + HCl(aq) = NaCl(aq) + H2O(aq) (A)
NaOH(s) + HCl(aq) = NaCl(aq) + H2O(l) (B)
NaOH(s) NaOH(aq) (C)

Methods:

Part-A: ∆𝑯 for HCl reacting with NaOH(aq):

NaOH(aq) + HCl(aq) = NaCl(aq) + H2O(aq)

Or, OH- + H+ H2O (l)

1. We have to clean and dry the calorimeter.

2. Then we dispense 60 ml of the standardized NaOH solution directly into the dry
clean calorimeter and record the exact concentration of the base.
3. Dispense 50 ml of the standardized HCl directly into a clean, dry beaker. Record
the exact concentration of HCl.
4. Now we measure the temperature of the NaOH at 0.5 min intervals.
5. At time = 6 mins add the HCl solution to the NaOH solution and stir the solution
for 15 secs. Then measure the temperature by thermometer with 0.5 mins intervals.
6. after 11 mins, we have to give litmus paper to the solution and record the result.

7. Now we have to graph the result on the graph paper and extrapolate the line to
the time of mixing 6 min and determine the change in temperature as shown on the
graph.
 11

8. Calculate the enthalpy change for the reaction by completing out the
calculations.

Concentration of HCl(aq) = 1M

Concentration of NaOH(aq) = 1M

Elapsed time 0 0.5 1 1.5 2 2.5

/min
Temp of NaOH 32 32 32 32 32 32
/℃

Elapsed time /min 3 3.5 4 4.5 5 5.5

Temp of HCl /℃ 32 32 32 32 32 32

Elapsed time 6.5 7 7.5 8 8.5 9 9.5 10 10. 11

/min 5
Temp of mixture 37 37 37 37 37 37 37 37 37 37
/℃

Color of litmus with final solution = Blue.

Final solution is basic.

Temperature of solution obtained from the graph, extrapolated to time of mixing :

NaOH(aq) = 32ºC

HCl(aq) = 32ºC

Mixture = 37ºC

Calculation of ΔT from the temperatures extrapolated to the time of mixing:

ΔT = temperature of mixture – average of temperatures of NaOH(aq) and HCl(aq)

solution

=5
 12

Calculation of the number of moles of H+ neutralized:

[HCl]/molL-1 =1M

Volume of HCl solution/mL = 50 mL

Number of mole of HCl = 0.05 mole

[NaOH]/molL-1 =1M

Volume of NaOH solution/mL = 60 mL

Number of mole of NaOH = 0.06 mole

Limiting reagent is = HCl

Amount of H+ reacted/mole = 0.05 mole

From the calculation, it has found that final solution is basic as excess solution is
NaOH(aq).

Calculation of enthalpy of neutralization:

1. Using the total volume of solution and its density to calculate the

mass of the final solution:

Density = 1.02 gmL-1 at 20º

Volume of final solution/mL = 110 mL

⸫ Mass of the final solution/g = 112.2 g

2. By using the mass of the final solution, ΔT and the heat capacity of the solution
to calculate the heat absorbed by the solution:

Cp = 4 Jg-1K-1

Mass of the final solution/g = 112.2 g

Heat absorbed by solution = m × Cp × ΔT

= 112.2 × 4 × 5
 13

= 2244 J

3. By using calorimeter constant and ΔT, we will calculate the heat absorbed by the
calorimeter:

Calorimeter constant = 30 JK-1

Heat absorbed by calorimeter = Cp × ΔT = 30× 5 = 150 J

4. Calculate the associated heat with the chemical reaction,

which is equals = -(heat absorbed by the calorimeter + absorbed by the solution)

Heat associated with reaction = - (150 + 2244) = -2394 J

5. Enthalpy change for the reaction in the calorimeter = -2394 J

2394
6. Molar enthalpy change for the reaction = − 𝐾𝐽
0.05×1000

= −47.88 𝐾𝐽

Part-B : ΔH for HCl reacting with NaOH(s) :

NaOH(s) + HCl(aq) NaCl(aq) + H2O(l)

NaOH(s) + H+(aq) Na+(aq) + H2O(l)

1. First we have to take 1.9-2.1 g of solid NaOH pellets into a dry sample tube and
cap immediately and record the masses of NaOH.

2. Then we will dispense 100 mL of standardized HCl solution directly into a

clean, dry calorimeter.

3. Measure and record to 1 decimal place of temperature of HCl solution at 0.5 min
intervals for a total of 6 measurements.

4. At time = 3.5 mins, we will mix the NaOH pellets to the HCl solution in the
calorimeter.

5. At time = 4 mins, measure the temperature of the solution until time = 11

minutes.
 14

6. Now, we will use red & blue litmus to ensure if the solution is acidic or basic.

7. Extrapolate the line to the time of mixing and determine the change in
temperature.

8. Finally, we will calculate the enthalpy change for the reaction by completing out
the calculation.

Concentration of HCl(aq) = 1M

Mass of the NaOH = 2.1g

Elapsed time 0 0.5 1 1.5 2 2.5 3

/min
Temp of HCl 32 32 32 32 32 32 32
/℃

Elapsed time at mixing = 3.5 min

Elapsed 4 4.5 5 5.5 6 6.5 7 7.5 8 8.5 9 9.5 10 10.5 11 11.5 12

time/min
Temp of 38 41 41 42 42 42 42 41 41 41 41 41 40 40 40 40 40
HCl(aq)/℃
12.5 13 13.5 14 14.5 15

40 40 40 39 39 39

Color of litmus with final solution = red

Is final solution acidic or basic = acidic

Temperature /℃ of solution obtained from the graph, extrapolated to time of

mixing
 15

HCl(aq) : 32 mixture:42.5

Calculation of ∆T from the temperatures extrapolated to the time of mixing:

∆T = temperature of mixture –temperature of HCl(aq) solution

=10.5

Calculation of the number of moles of H+ neutralized:

[HCl]/molL-1 = 1M

Volume of HCl solution /ml = 100 ml

n HCl /mol =0.1 mole

Mass of NaOH /g = 2.1 g

n NaOH /mol = 0.05 mole

Limiting reagent is = NaOH

Amount of H+ reacted /mol = 0.05 mole

Knowing which solution is excess, should the final solution be acidic or basic

= acidic

It is consistent with my observation.

Calculation of Enthalpy of neutralization:

1. Calculation of the mass of final solution:

Volume of HCl(aq) /ml =100 ml

Density = 1.02 g/L

Mass of HCl(aq) /g = 102g

Mass of NaOH (s) /g = 2.1g

 16

Mass of final solution = mass of HCl + mass of NaOH

=104.1 g

2. Mass of final solution /g =104.1 g

Here Cp = 4 Jg-1K-1

Heat absorbed by solution = m × Cp × ∆T

=4372.2 g

3. Calorimeter constant = 30 J/K

Heat absorbed by calorimeter = Cp × ∆T

=252 J

4. Heat associated with reaction = - 4624.3 J

5. Enthalpy change for the reaction in the calorimeter = - 4624.2 g

6. Molar enthalpy change for the reaction =

Part C- ∆H for dissolution of solid NaOH:

NaOH(s) NaOH(aq)

NaOH(s) Na+ +OH-

1. Firstly we have to weight 1.9-2.1 g of solid NaOH and then dissolve it into 100
ml of water.

2. Now we have to measure and record 1 decimal place of the temperature of the
water at 0.5 intervals for a total of 6 measurements.

3. At time = 3.5 mins, we will add the solid NaOH pellets to the water in the
calorimeter & stir it properly.
 17

4. At time = 4 mins, we will start to measure and record the temperature until time
= 11 mins.

5. Then we will use red & blue litmus to determine if the solution is acidic or basic.

6. Finally we will rinse the temperature probe on the thermometer and dry it.

7. At last, we will determine the enthalpy change of solution by completing the

calculation.

Mass of NaOH added to the calorimeter = 2.1 g

Elapsed time/min 0 0.5 1 1.5 2 2.5 3

Temp. of H2O/ºC 31 31 31 31 31 31 31

Elapsed 4 4.5 5 5.5 6 6.5 7

time/min
Temp. of 34 35 35 36 36 36 36
H2O/ºC
7.5 8 8.5 9 9.5 10
36 36 36 36 36 36

Temperature t℃ of solution from the graph extrapolated to time of mixing-

H2O(l) =

NaOH(aq) = 35.7

Calculation of ∆T from the temperature extrapolated to time of mixing:

∆T = temperature of NaOH(aq) – temperature of H2O(l)

Calculation of the neutralized moles of NaOH:

Mass of NaOH /g =

n NaOH / mol =
 18

Calculation of enthalpy of reaction:

1. Calculation of mass of final solution:

Volume of water /mL =

Density =

Mass of water /g =

Mass of dissolved NaOH =

Mass of final solution = mass of water + mass of NaOH(s)

2. By using the mass of the final solution, ∆𝑇 and the heat capacity of the solution,
we can calculate the heat absorbed by the solution:
Mass of the final solution= 101.8 g
Cp= 3.9 jg-1K-1
Heat absorbed by the solution=m× Cp ×∆T
=101.8 × 3.9 × 4.7
=1865.99 J
3. Calorimeter constant= 3o JK-1
Heat absorbed by calorimeter= Cp × ∆𝑇
=30× 4.7
=141 J
4. Heat associated with reaction= - (heat absorbed by the calorimeter + absorbed
by the solution)
= - (1865.99 + 141) J
= - 2006.94 J
5. The enthalpy change equals to the heat associated with chemical reaction.
 19

Enthalpy change for the reaction in the calorimeter= - 2006.94 J

6. Molar enthalpy change for the dissolution of NaOH(s),

2006.94
∆HC =− KJ
1000×0.05

= - 40.14 KJ
According to Hess’ law:
∆𝐻B = ∆𝐻A + ∆𝐻C
Here, the value of ∆𝐻B = - 92.48KJ
So, the value of (∆𝐻A + ∆𝐻C) = (-47.88) + (-40.14) KJ
= - 88.02 KJ
So, the reaction approximately follows the Hess’ law.