Experiment 1

Objective:

To calibrate the peristaltic feed pumps

Apparatus:

Measuring cylinder stopwatch Chemical reactor service units

Reagents:

Distilled water

Precautions:

1. Personnel safety:
Check the proper working of residual current circuit breaker (RCCB) at the rear of the Chemical
Reactor service unit
2. Equipment safety:
a) Check the proper working of miniature circuit breakers (MCB) at the rear of chemical
reactor service unit
b) Do not turn on heater of the hot water circulator and agitator motor
3. Chemical safety:
a) Drain any residual water present in the apparatus
b) Distilled water free from any contamination is safe. Consult MSDS for further details.

Procedure:

1. Turn on power supply to the chemical reactor service unit and perform safety checks
2. Drain any residual water or chemicals and rinse apparatus with distilled water
3. Close drain valves and fill each feed vessel with 5 liters of distilled water
4. Alter the pump potentiometer position from 0 to 9 and measure flowrate with measuring cylinder
and stopwatch against each position
5. Take backward readings from 9 to 0
6. Rinse apparatus properly and drain any residual water
7. Turn off electrical connections
Data analysis:

1. Plot the potentiometer position (X) and flowrate (Y) on a graph paper
2. Draw a linear line which best fits through the data points
3. Find slope (B1) and intercept (A1) of this line
4. Write the model in the following form
Y1= A1 + B1 X
5. Select linear regression model on calculator and find out slope (A2) and intercept (B2) of the linear
equation
6. Develop model e.g.
Y2 = A2 + B2 X
7. Check the regression coefficient (r) to verify the fitting of linear model on experimental data
8. Plot the potentiometer position (X) and flowrate (Y) on scatter chart in EXCEL and add linear trend
line
9. Find equation of this model and regression coefficient e.g.
Y3 = A3 + B3 X

Potentiometer True Flowrate Predicted Predicted Predicted Error Error Error

position from flowrate flowrate flowrate (Y1-Y)2 (Y2-Y)2 (Y3-Y)2
(X) experiment from from from
(Y) graphical calculator Excel’s
model model model
(Y1) (Y2) (Y3)

10. Select the best model (with least squares of error)

 Experiment 2

Objective:

Standardization of NaOH using standard HCl solution via back titration

Apparatus:

Glass wares (beakers, conical flasks, burettes, pipettes)

Reagents:

Distilled water Standard HCl Solution Standard Na2CO3 solution

NaOH solutions of unknown concentrations Methyl orange indicator

Precautions:

1. Personnel safety:
Wear lab coat and latex gloves
2. Equipment safety:
Fragile glass wares should be dealt with care
3. Chemical safety:
Acid and alkali solutions are corrosive and toxic. Consult MSDS for further details.

Procedure:

1. Prepare standard solutions of HCl (0.01-0.09 M) and Na2CO3 (0.01-0.05 M)

2. Prepare NaOH solution of unknown concentration
3. Take 10 mL of NaOH solution in conical flask. Add excess but known amount of Standard HCl
solution in it. Add a pinch of methyl orange
4. Titrate it against standard Na 2CO3 solution till indicator changes its color.
5. Calculate amount of free acid left after neutralization with NaOH solution
6. Calculate amount of acid neutralized by NaOH (subtract amount of left acid from total acid added)
7. Calculate concentration of NaOH solution
Calculation:

Na2CO3 : HCl

2M1V1 = M2V2

2𝑀1 𝑉1
V2 (𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑓𝑟𝑒𝑒 𝑎𝑐𝑖𝑑 𝑙𝑒𝑓𝑡 𝑎𝑓𝑡𝑒𝑟 𝑛𝑢𝑒𝑡𝑟𝑎𝑙𝑖𝑧𝑎𝑡𝑖𝑜𝑛 𝑤𝑖𝑡ℎ 𝑁𝑎𝑂𝐻) = 𝑀2

𝑣 (𝑎𝑚𝑜𝑢𝑛𝑡 𝑜𝑓 𝑎𝑐𝑖𝑑 𝑢𝑠𝑒𝑑 𝑏𝑦 𝑁𝑎𝑂𝐻) = 𝑡𝑜𝑡𝑎𝑙 𝑎𝑐𝑖𝑑 𝑎𝑑𝑑𝑒𝑑 −V2

NaOH : HCl

M1V1 = M2v

𝑀2 𝑣
𝑀1 (𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑁𝑎𝑂𝐻 𝑖𝑛 𝑢𝑛𝑘𝑛𝑜𝑤𝑛 𝑠𝑎𝑚𝑝𝑙𝑒) =
𝑉1

Preparation of Primary solution of HCl:

37 % fuming HCl is available in lab. The molarity (normality) of 37 % HCl can be calculated as
following.

370 ml pure HCl 1.19 x 1000 g pure HCl 1 gmole pure HCl

1000 mL of primary HCl

1000 mL pure HCl 36.45 g pure HCl
solution

Molarity of 37 % solution = 12.06 M

Preparation of 250 mL (0.02 M) HCl from stock solution:

HCl Standard (Stock) solution : Primary (Required) HCl solution

M1V1 = M2V2

V1 = (0.02) (250) / 12.07

Dissolve V1 (mL) in distilled water to make 250 mL of solution

 Experiment 3

Objective:

Development of Empirical Model for correlating electrical conductivity with temperature and concentration

Apparatus:

Glass wares (beakers, measuring flasks) Digital weight balance

Glass Thermometer Conductivity Meter

Reagents:

Distilled water

NaOH

Precautions:

1. Personnel safety:
Wear lab coat and latex gloves
2. Equipment safety:
Fragile glass wares should be dealt with care
Check the calibration of the conductivity meters prior to its use in experiment
3. Chemical safety:
Alkali solutions are Strongly corrosive. Consult MSDS for further details.

Procedure:

1. Prepare 250mL NaOH solution of known concentration (0.02, 0.04, 0.06, 0.08 M)
2. Note down the temperature of the solutions (it should be maintained between 20-40 °C)
3. Note down the conductivity of the solutions
4. Put the solutions in water bath and maintain temperature 3 degrees higher than previous (but the
temperature should be in the range of 20-40 °C)
5. Note conductivities at high temperature
6. Repeat steps 4-5 with different temperatures
For NaOH, following linear model is used in the molarity range (0.01-0.1 M) and the temperature range
(293-313 K);

𝜆𝐴 = 𝑘𝑜 [1 + 𝛼 (𝑇 − 𝑇𝑂 )]𝐶𝐴

𝜆𝐴 = 𝑘𝑜 𝐶𝐴 + 𝑘𝑜 𝐶𝐴 𝛼 (𝑇 − 𝑇𝑜 )

𝑇𝑜 = 294 𝐾

Calculation:

For 0.02 M NaOH solution

S.
Temperature (K) T-To (K) 𝜆𝐴 (𝑚𝑆) 𝜆𝐴 (𝑆𝑖𝑒𝑚𝑒𝑛𝑠)
No.

 Plot 𝜆𝐴 (Siemens) vs. (T-To) and find the slope and intercept
 Use regression analysis to find slope and intercept and hence the value of ko and α
 Compare the values of α and ko for different molarities (0.04, 0.06, 0.08 M) by repeating the
procedure and comment
𝛼 = ___________________________
𝑘𝑜 = __________________________
 Experiment 4

Objective:

Determination of Rate Constant for saponification of Ethyl acetate with NaOH via titrimetry followed by
integral analysis using stoichiometric proportions

Apparatus:

Glass wares (beakers, conical flasks, burettes, pipettes)

Magnetic Stirrer

Reagents:

Distilled water Standard HCl Solution Standard Na2CO3 solution

Standard NaOH solution Methyl orange indicator Standard Ethyl acetate solution

Precautions:

1. Personnel safety:
a) Wear lab coat and latex gloves
b) Ensure proper working of Residual current circuit breaker (RCCB)
2. Equipment safety:
a) Fragile glass wares should be dealt with care
b) Ensure proper working of miniature circuit breakers (MCB)
c) Ensure heater of hot water circulator is off
3. Chemical safety:
Acid and alkali solutions are corrosive and toxic. Ethyl acetate is Flammable, Toxic and Irritant.
Consult MSDS for further details.

Procedure:

1. Prepare 1000 mL (0.06 M) standard solutions of HCl, NaOH and ethyl acetate
2. Prepare 1000 mL standard solution of Na 2CO3 (0.03 M)
3. Dump 500 mL of ethyl acetate and NaOH in batch reactor and start stirring
4. Withdraw 10 mL sample after every 5 minutes and determine the concentration of NaOH in sample
via back titration
 5. Take minimum 9 readings.

Saponification of ethyl acetate is a 2nd order elementary reaction. Hence, the rate law becomes

𝑑𝐶𝐴
−𝑟𝐴 = − = 𝑘𝐶𝐴 𝐶𝐵
𝑑𝑡

For stoichiometric proportions

𝐶𝐴 = 𝐶𝐵

Hence, integrated rate law becomes

1 1
= + 𝑘𝑡
𝐶𝐴 𝐶𝐴𝑜

Calculations:
0.06
Initial concentration of NaOH in reactor (CAo) = 2
= 0.03 𝑀

1 𝑑𝑚 3 Time (t)
S. No. CA (mol/dm3) ( )
𝐶𝐴 𝑚𝑜𝑙 (min)
1
2
3
4
5

1 1
 Plot 𝐶 𝑣𝑠 𝑡 𝑎𝑛𝑑 𝑓𝑖𝑛𝑑 𝑜𝑢𝑡 𝑡ℎ𝑒 𝑠𝑙𝑜𝑝𝑒 (𝑘) 𝑎𝑛𝑑 𝑖𝑛𝑡𝑒𝑟𝑐𝑒𝑝𝑡 (𝐶 )
𝐴 𝐴𝑜

 Compare the calculated value of CAo with experimentally known value and comment on results
 Experiment 5

Objective:

Determination of Rate Constant for saponification of Ethyl acetate with NaOH via titrimetry followed by
integral analysis using Comparable proportions

Apparatus:

Glass wares (beakers, conical flasks, burettes & pipettes etc.)

Magnetic Stirrer

Reagents:

Distilled water Standard HCl Solution Standard Na2CO3 solution

Standard NaOH solution Methyl orange indicator Standard Ethyl acetate solution

Precautions:

1. Personnel safety:
a) Wear lab coat and latex gloves
b) Ensure proper working of Residual current circuit breaker (RCCB)
2. Equipment safety:
a) Fragile glass wares should be dealt with care
b) Ensure proper working of miniature circuit breakers (MCB)
c) Ensure heater of hot water circulator is in off
3. Chemical safety:
Acid and alkali solutions are corrosive and toxic. Ethyl acetate is Flammable, Toxic & Irritant.
Consult MSDS for further details.

Procedure:

1. Prepare 1000 mL (0.06 M) standard solutions of HCl, NaOH and ethyl acetate
2. Prepare 1000 mL standard solution of Na 2CO3 (0.03 M)
3. Dump 600 mL of ethyl acetate and 400 mL NaOH in batch reactor. Start stirring the contents
4. Withdraw 10 mL sample after every 5 minutes and determine the concentration of NaOH in sample
via back titration
 5. Take readings until (pseudo) steady state is reached (nearly 45 minutes)

Saponification of ethyl acetate is a 2nd order elementary reaction. Hence, the rate law becomes

𝑑𝐶𝐴
−𝑟𝐴 = − = 𝑘𝐶𝐴 𝐶𝐵
𝑑𝑡

For comparable proportions, integrated rate law becomes

𝐶𝐵 𝐶𝐵𝑜 𝐶𝐵𝑜
ln( ) = ln( ) + 𝑘𝐶𝐴𝑜 ( − 1)𝑡
𝐶𝐴 𝐶𝐴𝑜 𝐶𝐴𝑜

Calculations:
0.06
Initial concentration of NaOH in reactor (CAo) = 2
= 0.03 𝑀

𝐶𝐵 = 𝐶𝐵𝑜 − 𝐶𝐴𝑜 + 𝐶𝐴 𝐶𝐵
S. CA Time (t) ln( )
𝑚𝑜𝑙 𝐶𝐴
No. (mol/dm3) ( 3) (min)
𝑑𝑚
1
2
3
4
5

𝐶 𝐶𝐵𝑜 𝐶𝐵𝑜
 Plot ln ( 𝐵 ) 𝑣𝑠 𝑡 𝑎𝑛𝑑 𝑓𝑖𝑛𝑑 𝑜𝑢𝑡 𝑡ℎ𝑒 𝑠𝑙𝑜𝑝𝑒 (𝑘𝐶𝐴𝑜 ( − 1)) 𝑎𝑛𝑑 𝑖𝑛𝑡𝑒𝑟𝑐𝑒𝑝𝑡 ln( )
𝐶𝐴 𝐶𝐴𝑜 𝐶𝐴𝑜

 Compare the calculated value of CAo & CBo with experimentally known value and comment on
results
 Experiment 6

Objective:

Determination of Rate Constant for saponification of Ethyl acetate with NaOH via conductometry in a batch
reactor followed by integral analysis using Comparable proportions

Apparatus:

Glass wares (beakers)

Batch reactor (CEB-MKII) mounted on chemical reactor service unit (CEX-MKII)

Conductivity meter

Reagents:

Distilled water

1 liter standard NaOH solution (0.06 M)

1-liter standard Ethyl acetate solution (0.06 M)

Precautions:

1. Personnel safety:
a) Wear lab coat and latex gloves
b) Ensure proper working of Residual current circuit breaker (RCCB)
2. Equipment safety:
a) Fragile glass wares should be dealt with care
b) Ensure proper working of miniature circuit breakers (MCB)
c) Ensure heater of hot water circulator is off
d) Conductivity meter should be in 19.99 mS mode.
3. Chemical safety:
Alkali solutions is corrosive and toxic. Ethyl Acetate is Flammable, Toxic & Irritant. Consult
MSDS for further details.
Calibration check:

1. Record the ambient temperature

2. Rinse the conductivity meter probe with calibration solution and cross check the meter reading with
standard conductivity.
3. Rinse Conductivity meter probe properly with distilled water before using in experiment

Procedure:

1. Prepare 1000 mL (0.06 M) standard solutions each of NaOH and ethyl acetate
2. Dump 600 mL of ethyl acetate 400 mL NaOH in batch reactor and start stirring the contents of the
reactor
3. Note down the conductivity of the NaOH solution from feed vessel at zero time
4. Keep monitoring the temperature (T) and conductivity (𝜆) of the reaction mixture after every 2
minutes
5. Take readings until (pseudo) steady state is achieved i.e. nearly 45 minutes
6. Rinse conductivity meter
7. Drain and wash chemical reactor service unit and batch reactor with distilled water properly
8. Turn off electrical connections

Saponification of ethyl acetate is a 2nd order elementary reaction. Hence, the rate law becomes

𝑑𝐶𝐴
−𝑟𝐴 = − = 𝑘𝐶𝐴 𝐶𝐵
𝑑𝑡

For comparable proportions, integrated rate law becomes

𝐶𝐵 𝐶𝐵𝑜 𝐶𝐵𝑜
ln( ) = ln( ) + 𝑘𝐶𝐴𝑜 ( − 1)𝑡
𝐶𝐴 𝐶𝐴𝑜 𝐶𝐴𝑜

In integrated rate expression A is by default taken as a limiting reactant (L.R).

Calculations:
400
Initial concentration of NaOH in reactor = (CAo) = (400+600) 0.06 = ______________ 𝑀

Concentration of NaOH in reactor after infinite time = 𝐶𝐴∞ = 0 (𝑁𝑎𝑂𝐻 𝑖𝑠 𝐿. 𝑅)

Concentration of Na-acetate in reactor after infinite time = 𝐶𝐶∞ = 𝐶𝐴𝑂 = ____________ 𝑀

Initial conductivity of solution in reactor at zero time = 𝜆𝑂 = 𝜆𝐴𝑂 + 𝜆𝐶𝑂 = 𝜆𝐴𝑂 (𝜆𝐶𝑂 = 0)

𝜆𝐴𝑂 = 0.195[1 + 0.0184(𝑇 − 294)]𝐶𝐴𝑂

𝜆𝑂 = 𝜆𝐴𝑂 = ___________________________________(𝑆𝑖𝑒𝑚𝑒𝑛𝑠)

𝜆∞ = 𝜆𝐴∞ + 𝜆𝐶∞ = 𝜆𝐶∞ (𝜆𝐴∞ = 0)

𝜆𝐶∞ = 0.070[1 + 0.0284(𝑇 − 294)]𝐶𝐶∞

𝜆∞ = 𝜆𝐶∞ = ______________________________(𝑆𝑖𝑒𝑚𝑒𝑛𝑠)

Change in concentration of NaOH is proportional to change in conductivity of solution hence,

𝐶𝐴𝑂 − 𝐶𝐴 𝜆𝑂 − 𝜆
=
𝐶𝐴𝑂 − 𝐶𝐴∞ 𝜆𝑂 − 𝜆∞

𝜆𝑂 − 𝜆
𝐶𝐴 = (𝐶𝐴∞ − 𝐶𝐴𝑂 ) ( ) + 𝐶𝐴𝑂
𝜆𝑂 − 𝜆∞

𝐶𝐵 𝐶𝐵
𝜆𝑂 − 𝜆 ln( )
Time 𝐶𝐴 = (𝐶𝐴∞ − 𝐶𝐴𝑂 ) ( ) + 𝐶𝐴𝑂 = 𝐶𝐵𝑜 − 𝐶𝐴𝑜 𝐶𝐴
𝜆𝑂 − 𝜆∞
(t) 𝜆 (𝑚𝑆) 𝜆 (𝑆) + 𝐶𝐴
𝑚𝑜𝑙
(min) ( 3) 𝑚𝑜𝑙
𝑑𝑚 ( 3)
𝑑𝑚
0 = 𝜆0
2 .
4 .
. .
. .
𝐶 𝐶 𝐶
 Plot ln (𝐶𝐵 ) 𝑣𝑠 𝑡 𝑎𝑛𝑑 𝑓𝑖𝑛𝑑 𝑜𝑢𝑡 𝑡ℎ𝑒 𝑠𝑙𝑜𝑝𝑒 (𝑘𝐶𝐴𝑜 (𝐶𝐵𝑜 − 1)) 𝑎𝑛𝑑 𝑖𝑛𝑡𝑒𝑟𝑐𝑒𝑝𝑡 ln(𝐶𝐵𝑜 )
𝐴 𝐴𝑜 𝐴𝑜
 Compare the calculated value of CAo & CBo with experimentally known value and comment on
results
 Units of Conductivity (mS or S) should be consistent in calculations.
 Experiment 7

Objective:

Determination of Rate Constant for saponification of Ethyl acetate with NaOH via conductometry in a batch
reactor followed by integral analysis

Apparatus:

Glass wares (beakers)

Batch reactor (CEB-MKII) mounted on chemical reactor service unit (CEX-MKII)

Conductivity meter

Reagents:

Distilled water

1 liter standard NaOH solution (0.06 M)

1-liter standard Ethyl acetate solution (0.06 M)

Calibration Solutions of Conductivity meter

Precautions:

1. Personnel safety:
a) Wear lab coat and latex gloves
b) Ensure proper working of Residual current circuit breaker (RCCB)
2. Equipment safety:
a) Fragile glass wares should be dealt with care
b) Ensure proper working of miniature circuit breakers (MCB)
c) Ensure heater of hot water circulator is off
d) Readings of conductivity meter should be in mS
3. Chemical safety:
Alkali solution is corrosive and toxic. Ethyl acetate is Flammable, Toxic & Irritant. Consult MSDS
for further details.
Calibration check:

1. Record the ambient temperature

2. Rinse the conductivity meter probe with calibration solution and cross check the meter reading with
standard conductivity.
3. Rinse conductivity meter probe properly with distilled water before using in experiment

Procedure:

1. Prepare 1000 mL (0.06 M) standard solutions each of NaOH and ethyl acetate
2. Note down the conductivity & Temperature of NaOH solution from feed vessel at zero time
3. Add 500 mL of ethyl acetate and dump 500 mL NaOH solution in batch reactor; start stirring
4. Keep monitoring the temperature (T) and conductivity (𝜆) of the reaction mixture after every 2
minutes
5. Take readings until (pseudo) steady state is achieved i.e. nearly 45 minutes
6. Rinse conductivity meter probe
7. Drain and wash chemical reactor service unit and batch reactor with distilled water properly
8. Turn off electrical connections

Saponification Reaction:

Saponification of ethyl acetate is a 2nd order reaction. Fortunately, the progress of reaction can also be
measured physically through conductivity.

𝑁𝑎𝑂𝐻 + 𝐶𝐻3 𝐶𝑂𝑂𝐶2 𝐻5 → 𝐶𝐻3 𝐶𝑂𝑂𝑁𝑎 + 𝐶2 𝐻5 𝑂𝐻

𝐴 + 𝐵 → 𝐶 + 𝐷

As only NaOH and Na-acetate effect the conductivity of the solution hence, concentration of these species
can be estimated using conductivity of solution.

Rate law is

𝑑𝐶𝐴
−𝑟𝐴 = − = 𝑘𝐶𝐴 𝐶𝐵
𝑑𝑡
For stoichiometric proportions

𝐶𝐴 = 𝐶𝐵

Hence, integrated rate law becomes

1 1
= + 𝑘𝑡
𝐶𝐴 𝐶𝐴𝑜

Calculations:
0.06
Initial concentration of NaOH in reactor = (CAo) = 2
= 0.03 𝑀

Concentration of NaOH in reactor after infinite time = 𝐶𝐴∞ = 𝐶𝐴𝑂 − 𝐶𝐵𝑂 = 0

Concentration of Na-acetate in reactor after infinite time = 𝐶𝐶∞ = 𝐶𝐴𝑂 = 0.03 𝑀

Initial conductivity of solution in reactor at zero time = 𝜆𝑂 = 𝜆𝐴𝑂 + 𝜆𝐶𝑂 = 𝜆𝐴𝑂 (𝜆𝐶𝑂 = 0)

𝜆𝐴𝑂 = 0.195[1 + 0.0184(𝑇 − 294)]𝐶𝐴𝑂

𝜆𝑂 = 𝜆𝐴𝑂 = _____________________________________(𝑆𝑖𝑒𝑚𝑒𝑛𝑠)

𝜆∞ = 𝜆𝐴∞ + 𝜆𝐶∞ = 𝜆𝐶∞ (𝜆𝐴∞ = 0)

𝜆𝐶∞ = 0.070[1 + 0.0284(𝑇 − 294)]𝐶𝐶∞

𝜆∞ = 𝜆𝐶∞ = ______________________________(𝑆𝑖𝑒𝑚𝑒𝑛𝑠)

Change in concentration of NaOH is proportional to change in conductivity of solution hence,

𝐶𝐴𝑂 − 𝐶𝐴 𝜆𝑂 − 𝜆
=
𝐶𝐴𝑂 − 𝐶𝐴∞ 𝜆𝑂 − 𝜆∞

𝜆𝑂 − 𝜆
𝐶𝐴 = (𝐶𝐴∞ − 𝐶𝐴𝑂 ) ( ) + 𝐶𝐴𝑂
𝜆𝑂 − 𝜆∞
 𝜆𝑂 − 𝜆
𝐶𝐴 = (𝐶𝐴∞ − 𝐶𝐴𝑂 ) ( ) + 𝐶𝐴𝑂
Time (t) 𝜆𝑂 − 𝜆∞ 1 𝑑𝑚3
𝜆 (𝑚𝑆) 𝜆 (𝑆) ( )
(min) 𝑚𝑜𝑙 𝐶𝐴 𝑚𝑜𝑙
( 3)
𝑑𝑚
0 = 𝜆0
2 .
4 .
. .
. .

1 1
 Plot 𝐶 𝑣𝑠 𝑡 𝑎𝑛𝑑 𝑓𝑖𝑛𝑑 𝑜𝑢𝑡 𝑡ℎ𝑒 𝑠𝑙𝑜𝑝𝑒 (𝑘)𝑎𝑛𝑑 𝑖𝑛𝑡𝑒𝑟𝑐𝑒𝑝𝑡 (𝐶 )
𝐴 𝐴𝑜

 Comment on results
 Units of Conductivity (mS or S) should be consistent in calculation
 Experiment 8

Objective:

Determination of Rate Constant for saponification of Ethyl acetate with NaOH via conductometry in CSTR
under Pseudo Steady state conditions

Apparatus:

Glass wares (beakers)

Continuous Stirred Tank Reactor (CEM-MKII) mounted on chemical reactor service unit (CEX-
MKII)

Conductivity meter

Reagents:

Distilled water

5 liters Standard NaOH solution (0.06 M)

5 liters Standard Ethyl acetate solution (0.06 M)

Calibration solutions of conductivity meter

Precautions:

1. Personnel safety:
a) Wear lab coat and latex gloves
b) Ensure proper working of Residual current circuit breaker (RCCB)
2. Equipment safety:
a) Fragile glass wares should be dealt with care
b) Ensure proper working of miniature circuit breakers (MCB)
c) Ensure heater of hot water circulator is in off
d) Conductivity meter should be in 19.99 mS mode
3. Chemical safety:
Alkali solution is corrosive and toxic. Ethyl acetate is Flammable, Toxic & Irritant. Consult MSDS
for further details.
Calibration check:

1. Record the ambient temperature

2. Rinse the conductivity meter probe in calibration solution and cross check the meter reading with
standard conductivity.
3. Rinse conductivity meter probe properly with distilled water before using it in experiment

Procedure:

1. Prepare 5 liter (0.06 M) standard solutions of NaOH and ethyl acetate

2. Rinse feed vessels with distilled water
3. Pour NaOH and ethyl acetate solutions in feed vessels
4. Adjust agitator motor control at 8
5. Adjust peristaltic pumps to deliver 50 mL/min flowrate for each reagent
6. Note down the conductivity of the NaOH in feed vessel
7. Keep monitoring the conductivity and temperature of the reaction mixture after every 3 minutes
8. Take readings till (pseudo) steady state is achieved i.e. nearly 45 minutes
9. Rinse conductivity meter probe
10. Drain CSTR into a measuring flask and note down the volume of reaction mixture in CSTR
11. Wash Chemical Reactor service unit and reactor with distilled water and drain any residual water
12. Turn off electrical connections

Saponification Reaction:

Saponification of ethyl acetate is a 2nd order elementary reaction. Fortunately, the progress of reaction can
also be measured physically through conductivity.

𝑁𝑎𝑂𝐻 + 𝐶𝐻3 𝐶𝑂𝑂𝐶2 𝐻5 → 𝐶𝐻3 𝐶𝑂𝑂𝑁𝑎 + 𝐶2 𝐻5 𝑂𝐻

𝐴 + 𝐵 → 𝐶 + 𝐷

As only NaOH and Na-acetate effect the conductivity of the solution hence, concentration of these species
can be estimated using conductivity of solution.
Observations:

S. Instantaneous 𝜆 (𝑆)
Time (min)
No. conductivity (mS)
1 0 .
2 3 .
3 6 .
4 9 .
. . .
. (Pseudo) steady state 𝜆=
Calculations:

Initial concentration of NaOH in feed vessel 𝐶𝐴𝜇 = 0.06 𝑀

𝑣𝐴 50
Initial concentration of NaOH in mixed feed (C Ao) = 𝑣 𝐶𝐴𝜇 = (50+50) 𝐶𝐴𝜇 = ________________
𝐴 +𝑣𝐵

Concentration of NaOH in reactor after infinite time = 𝐶𝐴∞ = 𝐶𝐴𝑂 − 𝐶𝐵𝑂 = 0

Initial concentration of Na-acetate in mixed feed (CCo) = 0

Concentration of Na-acetate in reactor after infinite time = 𝐶𝐶∞ = 𝐶𝐴𝑂 = _________________

Initial conductivity of solution in reactor at zero time = 𝜆𝑂 = 𝜆𝐴𝑂 + 𝜆𝐶𝑂 = 𝜆𝐴𝑂 (𝜆𝐶𝑂 = 0)

𝜆𝐴𝑂 = 0.195[1 + 0.0184(𝑇 − 294)]𝐶𝐴𝑂

𝜆𝑂 = 𝜆𝐴𝑂 = _________________________________(𝑆𝑖𝑒𝑚𝑒𝑛𝑠)

𝜆∞ = 𝜆𝐴∞ + 𝜆𝐶∞ = 𝜆𝐶∞ (𝜆𝐴∞ = 0)

𝜆𝐶∞ = 0.070[1 + 0.0284(𝑇 − 294)]𝐶𝐶∞

𝜆∞ = 𝜆𝐶∞ = ______________________________(𝑆𝑖𝑒𝑚𝑒𝑛𝑠)

(pseudo) steady state conductivity of solution in reactor = 𝜆 =____________________(Siemens)

Volume of reaction mixture = V = _____________ liters

Change in concentration of NaOH is proportional to change in conductivity of solution hence,

𝐶𝐴𝑂 − 𝐶𝐴 𝜆𝑂 − 𝜆
=
𝐶𝐴𝑂 − 𝐶𝐴∞ 𝜆𝑂 − 𝜆∞

𝜆𝑂 − 𝜆
𝐶𝐴 = (𝐶𝐴∞ − 𝐶𝐴𝑂 ) ( ) + 𝐶𝐴𝑂
𝜆𝑂 − 𝜆∞

𝑚𝑜𝑙
𝐶𝐴 = ________________________________( )
𝑙𝑖𝑡𝑒𝑟
Component material balance (NaOH) around reactor:

Input- output + generation – consumption = Accumulation

CSTR is a steady state reactor. Hence, accumulation term will be zero. Also NaOH is consumed in reactor.

𝑣𝐶𝐴𝑜 − 𝑣𝐶𝐴 − (−𝑟𝐴 )𝑉 = 0

𝑣𝐶𝐴𝑜 − 𝑣𝐶𝐴 − (𝑘𝐶𝐴 2 )𝑉 = 0

𝑣 (𝐶𝐴𝑂 −𝐶𝐴 )
Rate constant (𝑘 ) =
𝑉 𝐶𝐴2

(𝑣𝐴 + 𝑣𝐵 ) (𝐶𝐴𝑂 − 𝐶𝐴 )
(𝑘 ) =
𝑉 𝐶𝐴2

𝑚𝑜𝑙
(𝑘 ) = ______________________( )
𝑑𝑚3𝑠𝑒𝑐

Note: units of volumetric flowrates (𝑣𝐴 , 𝑣𝐵 )should be consistent in calculations.

 Experiment 9

Objective:

Determination of Rate Constant for saponification of Ethyl acetate with NaOH via conductometry in
Tubular Reactor under Pseudo Steady state conditions

Apparatus:

Glass wares (beakers)

Tubular Reactor (CET-MKII) mounted on chemical reactor service unit (CEX-MKII)

Conductivity meter

Reagents:

Distilled water

5 liters Standard NaOH solution (0.06 M)

5 liters standard Ethyl acetate solution (0.06 M)

Calibration solutions of conductivity meter

Precautions:

1. Personnel safety:
a) Wear lab coat and latex gloves
b) Ensure proper working of Residual current circuit breaker (RCCB)
2. Equipment safety:
a) Fragile glass wares should be dealt with care
b) Ensure proper working of miniature circuit breakers (MCB)
c) Ensure heater of hot water circulator is off
d) Conductivity meter should be in 19.99 mS mode
3. Chemical safety:
Alkali solution is corrosive and toxic. Consult MSDS for further details.
Calibration check:

1. Record the ambient temperature

2. Rinse the conductivity meter probe in calibration solution and cross check the meter reading with
standard conductivity.
3. Rinse conductivity meter probe properly with distilled water before using it in experiment

Procedure:

1. Prepare 5 liter (0.06 M) standard solutions of NaOH and ethyl acetate

2. Rinse feed vessels with distilled water
3. Pour NaOH and ethyl acetate solutions in feed vessels
4. Adjust peristaltic pumps to deliver 60 mL/min flowrate for each reagent
5. Note down the conductivity of the NaOH in feed vessel
6. Keep monitoring the conductivity and temperature of the reaction mixture at the outlet of tubular
reactor after every 3 minutes
7. Take readings until (pseudo) steady state is achieved i.e. nearly 45 minutes
8. Rinse conductivity meter probe
9. Wash Chemical Reactor service unit and reactor with distilled water and drain any residual water
10. Turn off electrical connections

Saponification Reaction:

Saponification of ethyl acetate is a 2nd order elementary reaction. Fortunately, the progress of reaction can
also be measured physically through conductivity.

𝑁𝑎𝑂𝐻 + 𝐶𝐻3 𝐶𝑂𝑂𝐶2 𝐻5 → 𝐶𝐻3 𝐶𝑂𝑂𝑁𝑎 + 𝐶2 𝐻5 𝑂𝐻

𝐴 + 𝐵 → 𝐶 + 𝐷

As only NaOH and Na-acetate effect the conductivity of the solution hence, concentration of these species
can be estimated using conductivity of solution.
Observations:

S. Instantaneous
Time (min) 𝜆 (𝑆)
No. conductivity (mS)
1 0 .
2 3 .
3 6 .
4 9 .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. (Pseudo) steady state 𝜆=
Calculations:

Initial concentration of NaOH in feed vessel 𝐶𝐴𝜇 = 0.06 𝑀

𝑣𝑎 60
Initial concentration of NaOH in mixed feed (C Ao) = 𝑣 𝐶𝐴𝜇 = (60+60) 𝐶𝐴𝜇 = ________________
𝑎 +𝑣𝑏

Concentration of NaOH at reactor outlet after infinite time = 𝐶𝐴∞ = 𝐶𝐴𝑂 − 𝐶𝐵𝑂 = 0

Initial concentration of Na-acetate in mixed feed (CCo) = 0

Concentration of Na-acetate at reactor outlet after infinite time = 𝐶𝐶∞ = 𝐶𝐴𝑂 = _________________

Initial conductivity of solution in reactor at zero time = 𝜆𝑂 = 𝜆𝐴𝑂 + 𝜆𝐶𝑂 = 𝜆𝐴𝑂 (𝜆𝐶𝑂 = 0)

𝜆𝐴𝑂 = 0.195[1 + 0.0184(𝑇 − 294)]𝐶𝐴𝑂

𝜆𝑂 = 𝜆𝐴𝑂 = ________________________________(𝑆𝑖𝑒𝑚𝑒𝑛𝑠)

𝜆∞ = 𝜆𝐴∞ + 𝜆𝐶∞ = 𝜆𝐶∞ (𝜆𝐴∞ = 0)

𝜆𝐶∞ = 0.070[1 + 0.0284(𝑇 − 294)]𝐶𝐶∞

𝜆∞ = 𝜆𝐶∞ = ______________________________(𝑆𝑖𝑒𝑚𝑒𝑛𝑠)

(pseudo) steady state conductivity of solution in reactor = 𝜆 =_____________________

Volume of reaction mixture in tubular reactor = V = _____________ liters

Change in concentration of NaOH is proportional to change in conductivity of solution hence,

𝐶𝐴𝑂 − 𝐶𝐴 𝜆𝑂 − 𝜆
=
𝐶𝐴𝑂 − 𝐶𝐴∞ 𝜆𝑂 − 𝜆∞

𝜆𝑂 − 𝜆
𝐶𝐴 = (𝐶𝐴∞ − 𝐶𝐴𝑂 ) ( ) + 𝐶𝐴𝑂
𝜆𝑂 − 𝜆∞

𝑚𝑜𝑙
𝐶𝐴 = ________________________________( )
𝑙𝑖𝑡𝑒𝑟
Calculation of Rate constant:

Performance equation of tubular reactor is

𝑋𝐴
𝜏 1
=∫ 𝑑𝑋
𝐶𝐴𝑂 0 −𝑟𝐴 𝐴

Rate equation is

−𝑟𝐴 = 𝑘𝐶𝐴2

For isothermal conditions, stoichiometric proportions, unconverted feed and constant density system the
integrated expression becomes

1 1
= + 𝑘𝜏
𝐶𝐴 𝐶𝐴𝑂

Where 𝜏 is known as the space time. It can be calculated as

𝑉 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑟𝑒𝑎𝑐𝑡𝑜𝑟
𝜏= = = ___________________
𝑣𝑜 𝑣𝑜𝑙𝑢𝑚𝑒𝑡𝑟𝑖𝑐 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 𝑜𝑓 𝑓𝑒𝑒𝑑

Hence,

1 1 1 𝑚𝑜𝑙
𝑘= ( − ) = _____________________( 3 )
𝜏 𝐶𝐴 𝐶𝐴𝑂 𝑑𝑚 𝑠𝑒𝑐

Repeat the experiment with 80 mL/min for both pumps at constant temperature
 Experiment 10

Objective:

Determination of Rate Constant for saponification of Ethyl acetate with NaOH via conductometry in a
cascade of CSTR’s under Pseudo Steady state conditions

Apparatus:

Glass wares (beakers)

Chemical reactor service unit with cascade of CSTR’s (CEP-MKII)

Conductivity meter

Reagents:

Distilled water

5 liters Standard NaOH solution (0.06 M)

5 liters standard Ethyl acetate solution (0.06 M)

Calibration solutions of conductivity meter

Precautions:

1. Personnel safety:
a) Wear lab coat and latex gloves
b) Ensure proper working of Residual current circuit breaker (RCCB)
2. Equipment safety:
a) Fragile glass wares should be dealt with care
b) Ensure proper working of miniature circuit breakers (MCB)
c) Ensure heater of hot water circulator is off
d) Conductivity meter should be in 19.99 mS mode
3. Chemical safety:
Alkali solution is corrosive and toxic. Ethyl acetate is Flammable, Toxic & Irritant. Consult MSDS
for further details.
Calibration check:

1. Record the ambient temperature

2. Rinse the conductivity meter probe in calibration solution and cross check the meter reading with
standard conductivity.
3. Rinse Conductivity meter probe properly with distilled water before using it in experiment

Procedure:

1. Prepare 5 liter (0.06 M) standard solutions of NaOH and ethyl acetate

2. Rinse feed vessels with distilled water
3. Pour NaOH and ethyl acetate solutions in feed vessels
4. Adjust peristaltic pumps to deliver 50 mL/min flowrate for each reagent
5. Adjust agitator motor control at 8
6. Note down the conductivity of the NaOH in feed vessel
7. Keep monitoring the conductivity and temperature of the reaction mixture after every 3 minutes
8. Take readings until (pseudo) steady state is achieved i.e. nearly 45 minutes
9. Rinse conductivity meter
10. Drain CSTR tanks into a measuring flask and note down the volume of reaction mixture in CSTR
11. Wash Chemical Reactor service unit and reactor with distilled water and drain any residual water
12. Turn off electrical connections

Saponification Reaction:

Saponification of ethyl acetate is a 2nd order elementary reaction. Fortunately, the progress of reaction can
also be measured physically through conductivity.

𝑁𝑎𝑂𝐻 + 𝐶𝐻3 𝐶𝑂𝑂𝐶2 𝐻5 → 𝐶𝐻3 𝐶𝑂𝑂𝑁𝑎 + 𝐶2 𝐻5 𝑂𝐻

𝐴 + 𝐵 → 𝐶 + 𝐷

As only NaOH and Na-acetate effect the conductivity of the solution hence, concentration of these species
can be estimated using conductivity of solution.
Observations:

Temperature Instantaneous conductivity (mS)

S. No. Time (min)
(k) 𝜆1 𝜆2 𝜆3
1 0 . . .
2 3 . . .
3 6 . . .
4 9 . . .
. . . . .
. . . . .
. . . . .
. . . . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
. . .
(Pseudo) steady
. 𝜆= 𝜆= 𝜆=
state
Calculations:

Initial concentration of NaOH in feed vessel 𝐶𝐴𝜇 = 0.06 𝑀

𝑣𝑎 50
Initial concentration of NaOH in mixed feed (C Ao) = 𝑣 𝐶𝐴𝜇 = (50+50) 𝐶𝐴𝜇 = ________________
𝑎 +𝑣𝑏

Concentration of NaOH in reactor after infinite time = 𝐶𝐴∞ = 𝐶𝐴𝑂 − 𝐶𝐵𝑂 = 0

CSTR 1 & CSTR 2:

Initial concentration of Na-acetate in mixed feed (CCo) = 0

Concentration of Na-acetate in reactor after infinite time = 𝐶𝐶∞ = 𝐶𝐴𝑂 = _________________

Initial conductivity of solution in reactor at zero time = 𝜆𝑂 = 𝜆𝐴𝑂 + 𝜆𝐶𝑂 = 𝜆𝐴𝑂 (𝜆𝐶𝑂 = 0)

𝜆𝐴𝑂 = 0.195[1 + 0.0184(𝑇 − 294)]𝐶𝐴𝑂

𝜆𝑂 = 𝜆𝐴𝑂 = _________________________________(𝑆𝑖𝑒𝑚𝑒𝑛𝑠)

𝜆∞ = 𝜆𝐴∞ + 𝜆𝐶∞ = 𝜆𝐶∞ (𝜆𝐴∞ = 0)

𝜆𝐶∞ = 0.070[1 + 0.0284(𝑇 − 294)]𝐶𝐶∞

𝜆∞ = 𝜆𝐶∞ = ______________________________(𝑆𝑖𝑒𝑚𝑒𝑛𝑠)

(pseudo) steady state conductivity of solution in reactor = 𝜆 =_____________________

Volume of reaction mixture = V = _____________ liters

Change in concentration of NaOH is proportional to change in conductivity of solution hence,

𝐶𝐴𝑂 − 𝐶𝐴 𝜆𝑂 − 𝜆
=
𝐶𝐴𝑂 − 𝐶𝐴∞ 𝜆𝑂 − 𝜆∞

𝜆𝑂 − 𝜆
𝐶𝐴 = (𝐶𝐴∞ − 𝐶𝐴𝑂 ) ( ) + 𝐶𝐴𝑂
𝜆𝑂 − 𝜆∞

𝑚𝑜𝑙
𝐶𝐴2 = ________________________________( )
𝑙𝑖𝑡𝑒𝑟

CSTR 3:
𝑚𝑜𝑙
Initial concentration of Na-acetate in mixed feed (CCo3) = 𝐶𝐴𝑜 − 𝐶𝐴2 = ________________ (𝑙𝑖𝑡𝑒𝑟 )
Concentration of Na-acetate in reactor after infinite time = 𝐶𝐶∞ = 𝐶𝐴𝑂 = _________________

Initial conductivity of solution in reactor at zero time = 𝜆𝑂 = 𝜆𝐴𝑂 + 𝜆𝐶𝑂

𝑚𝑜𝑙
𝐶𝐴03 = 𝐼𝑛𝑖𝑡𝑖𝑎𝑙 𝑁𝑎𝑂𝐻 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑖𝑛 𝑡𝑎𝑛𝑘 3 = 𝐶𝐴2 = ______________ ( )
𝑙𝑖𝑡𝑒𝑟

𝜆𝐴𝑂 = 0.195[1 + 0.0184(𝑇 − 294)]𝐶𝐴𝑂3

𝜆𝐴𝑂 = __________________________________(𝑆𝑖𝑒𝑚𝑒𝑛𝑠)

𝜆𝐶𝑜 = 0.070[1 + 0.0284(𝑇 − 294)]𝐶𝐶𝑜3

𝜆𝐶𝑜 = _____________________________________(𝑆𝑖𝑒𝑚𝑒𝑛𝑠)

𝜆𝑜 = _____________________________________(𝑆𝑖𝑒𝑚𝑒𝑛𝑠)

𝜆∞ = 𝜆𝐴∞ + 𝜆𝐶∞ = 𝜆𝐶∞ (𝜆𝐴∞ = 0)

𝜆𝐶∞ = 0.070[1 + 0.0284(𝑇 − 294)]𝐶𝐶∞

𝜆∞ = 𝜆𝐶∞ = ______________________________(𝑆𝑖𝑒𝑚𝑒𝑛𝑠)

(pseudo) steady state conductivity of solution in reactor = 𝜆 =_____________________

Volume of reaction mixture in 3rd tank = V3 = _____________ liters

Change in concentration of NaOH is proportional to change in conductivity of solution hence,

𝐶𝐴𝑂3 − 𝐶𝐴 𝜆𝑂 − 𝜆
=
𝐶𝐴𝑂3 − 𝐶𝐴∞ 𝜆𝑂 − 𝜆∞

𝜆𝑂 − 𝜆
𝐶𝐴3 = (𝐶𝐴∞ − 𝐶𝐴𝑂 ) ( ) + 𝐶𝐴𝑂
𝜆𝑂 − 𝜆∞

𝑚𝑜𝑙
𝐶𝐴3 = ________________________________( )
𝑙𝑖𝑡𝑒𝑟
Component material balance (NaOH) around reactor:

Input- output + generation – consumption = Accumulation

CSTR is a steady state reactor. Hence, accumulation term will be zero. Also NaOH is consumed in reactor.

𝑣𝐶𝐴𝑜 − 𝑣𝐶𝐴 − (−𝑟𝐴 )𝑉 = 0

𝑣𝐶𝐴𝑜 − 𝑣𝐶𝐴 − (𝑘𝐶𝐴 2 )𝑉 = 0

𝑣 (𝐶𝐴𝑂 −𝐶𝐴 )
Rate constant (𝑘 ) =
𝑉 𝐶𝐴2

(𝑣𝐴 + 𝑣𝐵 ) (𝐶𝐴𝑂 − 𝐶𝐴 )
(𝑘 ) =
𝑉 𝐶𝐴2

CSTR 1 & CSTR 2:

(𝑣𝑎 + 𝑣𝑏 ) (𝐶𝐴𝑂 − 𝐶𝐴1)

(𝑘1) = 2
𝑉1 𝐶𝐴1

𝑚𝑜𝑙
(𝑘1) = ______________________( )
𝑑𝑚3𝑠𝑒𝑐

(𝑣𝑎 + 𝑣𝑏 ) (𝐶𝐴𝑂 − 𝐶𝐴2)

(𝑘2 ) = 2
𝑉2 𝐶𝐴2

𝑚𝑜𝑙
(𝑘2 ) = ______________________( 3 )
𝑑𝑚 𝑠𝑒𝑐

CSTR 3:

(𝑣𝑎 + 𝑣𝑏 ) (𝐶𝐴𝑂3 − 𝐶𝐴3)

(𝑘3 ) = 2
𝑉3 𝐶𝐴3

𝑚𝑜𝑙
(𝑘3 ) = ______________________( 3 )
𝑑𝑚 𝑠𝑒𝑐

Note: units of volumetric flowrate (𝑣𝑎 , 𝑣𝑏 )should be consistent in calculations.

 Experiment 11

Objective:

Determination of Arrhenius Parameters for saponification Reaction via titrimetry

Apparatus:

Glass wares (beakers, conical flasks, auto piston burettes & pipettes etc.)

Batch reactor (CEB-MKII) mounted on chemical reactor service unit (CEX-MKII)

Reagents:

Distilled water Standard HCl Solution Standard Na2CO3 solution

Standard NaOH solution Methyl orange indicator Standard Ethyl acetate solution

Precautions:

1. Personnel safety:
a) Wear lab coat and latex gloves
b) Ensure proper working of Residual current circuit breaker (RCCB)
2. Equipment safety:
a) Fragile glass wares should be dealt with care
b) Ensure proper working of miniature circuit breakers (MCB)
c) Ensure heater of hot water circulator is off while working at ambient temperature
d) Hot water circulator should be properly primed with distilled water before turning on the
heater
3. Chemical safety:
Acid and alkali solutions are corrosive and toxic. Ethyl acetate is Flammable, Toxic & Irritant.
Consult MSDS for further details.

Procedure:

1. Note down the temperature of reaction mixture (ambient temperature)

2. Perform experiment according to the procedure of Experiment 4.
3. Find rate constant (k1) at this temperature.
4. Turn on hot water circulator and adjust the temperature to a set point of 10 °C above ambient.
 5. Again perform the experiment according to the procedure of experiment 4.
6. Again Find rate constant (k1) at 2nd temperature.

Arrhenius equation is

𝐸𝐴
𝑘 = 𝑘𝑜 𝑒 −𝑅𝑇

𝐸𝐴
𝑙𝑛𝑘 = 𝑙𝑛𝑘𝑜 + (− ) ln(𝑒)
𝑅𝑇

𝐸𝐴 1
𝑙𝑛𝑘 = 𝑙𝑛𝑘𝑜 + (− )
𝑅 𝑇

Calculations:

At Ambient Temperature (T1):

0.06
Initial concentration of NaOH in reactor (CAo) = 2
= 0.03 𝑀

Time (t) 𝑚𝑜𝑙 1 𝑑𝑚 3

S. No. 𝐶𝐴 ( 3 ) ( )
(min) 𝑑𝑚 𝐶𝐴 𝑚𝑜𝑙
1
2
3
4
5

1 1
 Plot 𝐶 𝑣𝑠 𝑡 𝑎𝑛𝑑 𝑓𝑖𝑛𝑑 𝑜𝑢𝑡 𝑡ℎ𝑒 𝑠𝑙𝑜𝑝𝑒 (𝑘1 ) 𝑎𝑛𝑑 𝑖𝑛𝑡𝑒𝑟𝑐𝑒𝑝𝑡 (𝐶 )
𝐴 𝐴𝑜

 Compare the calculated value of CAo with experimentally known value and comment on results
At high Temperature (T2):
0.06
Initial concentration of NaOH in reactor (CAo) = 2
= 0.03 𝑀

Time (t) 𝑚𝑜𝑙 1 𝑑𝑚 3

S. No. 𝐶𝐴 ( 3 ) ( )
(min) 𝑑𝑚 𝐶𝐴 𝑚𝑜𝑙
1
2
3
4
5

1 1
 Plot 𝐶 𝑣𝑠 𝑡 𝑎𝑛𝑑 𝑓𝑖𝑛𝑑 𝑜𝑢𝑡 𝑡ℎ𝑒 𝑠𝑙𝑜𝑝𝑒 (𝑘2 ) 𝑎𝑛𝑑 𝑖𝑛𝑡𝑒𝑟𝑐𝑒𝑝𝑡 (𝐶 )
𝐴 𝐴𝑜

 Compare the calculated value of CAo with experimentally known value and comment on results

1 Rate constant
S. No. Temperature (K) ln(k)
𝑇 (k)
1
2

𝐸𝐴
 Plot ln (k) vs. 1/T and find the slope (– ) and intercept (𝑙𝑛𝑘𝑜 )
𝑅

 Find EA and ko
 Experiment 12

Objective:

Determination of Arrhenius Parameters for saponification Reaction via Conductometry in batch reactor

Apparatus:

Glass wares (beakers)

Batch reactor (CEB-MKII) mounted on chemical reactor service unit (CEX-MKII)

Conductivity Meter

Reagents:

Distilled water Standard NaOH solution Standard Ethyl acetate solution

Standard Conductivity Calibration solutions

Precautions:

1. Personnel safety:
a) Wear lab coat and latex gloves
b) Ensure proper working of Residual current circuit breaker (RCCB)
2. Equipment safety:
a) Fragile glass wares should be dealt with care
b) Ensure proper working of miniature circuit breakers (MCB)
c) Ensure heater of hot water circulator is off while working at ambient temperature
d) Hot water circulator should be properly primed with distilled water before turning on the
heater
e) Conductivity meter should be in 19.99 mS mode.
3. Chemical safety:
Acid and alkali solutions are corrosive and toxic. Ethyl acetate is Flammable, Toxic & Irritant.
Consult MSDS for further details.

Procedure:

1. Note down the temperature of reaction mixture (ambient temperature)

 2. Perform experiment according to the procedure of Experiment 6.
3. Find rate constant (k1) at this temperature.
4. Turn on hot water circulator and adjust the temperature to a set point of 10 °C above ambient.
5. Again perform the experiment according to the procedure of experiment 6.
6. Again Find rate constant (k2) at 2nd temperature.

Arrhenius equation is

𝐸𝐴
𝑘 = 𝑘𝑜 𝑒 −𝑅𝑇

𝐸𝐴
𝑙𝑛𝑘 = 𝑙𝑛𝑘𝑜 + (− ) ln(𝑒)
𝑅𝑇

𝐸𝐴 1
𝑙𝑛𝑘 = 𝑙𝑛𝑘𝑜 + (− )
𝑅 𝑇

Observations:

At Temperature T1:

S. No. Time (min) 𝜆 (𝑚𝑆) 𝜆 (𝑆)

1 0
2 3
3 6
. .
. .

k1=____________________
At Temperature T2:

S. No. Time (min) 𝜆 (𝑚𝑆) 𝜆 (𝑆)

1 0
2 3
3 6
. .
. .

k2=____________________

Calculations:

1 Rate constant
S. No. Temperature (K) ln(k)
𝑇 (k)
1
2

𝐸𝐴
 Plot ln (k) vs. 1/T and find the slope (– 𝑅
) and intercept (𝑙𝑛𝑘𝑜 )

 Find EA and ko
 Experiment 13

Objective:

Determination of Arrhenius Parameters for saponification Reaction via Conductometry in CSTR

Apparatus:

Glass wares (beakers)

Continuous Stirred Tank Reactor (CEM-MKII) mounted on chemical reactor service unit (CEX-
MKII)

Conductivity meter

Reagents:

Distilled water

5 liters Standard NaOH solution (0.06 M)

5 liters standard Ethyl acetate solution (0.06 M)

Calibration solutions of conductivity meter

Precautions:

1. Personnel safety:
a) Wear lab coat and latex gloves
b) Ensure proper working of Residual current circuit breaker (RCCB)
2. Equipment safety:
a) Fragile glass wares should be dealt with care
b) Ensure proper working of miniature circuit breakers (MCB)
c) Ensure heater of hot water circulator is off while working at ambient temperature
d) Hot water circulator should be properly primed with distilled water before turning on the
heater
e) Conductivity meter should be in 19.99 mS mode
 3. Chemical safety:
Alkali solutions is corrosive and toxic. Ethyl acetate is Flammable, Toxic & Irritant. Consult MSDS
for further details.

Calibration check:

1. Record the ambient temperature

2. Rinse the conductivity meter probe in calibration solution and cross check the meter reading with
standard conductivity.
3. Rinse conductivity meter probe properly with distilled water before using it in experiment

Procedure:

1. Perform experiment according to the procedure of Experiment 7.

2. Find rate constant (k1) at this temperature.
3. Turn on hot water circulator and adjust the temperature to a set point of 10 °C above ambient.
4. Again perform the experiment according to the procedure of experiment 7.
5. Again Find rate constant (k2) at 2nd temperature.

Arrhenius equation is

𝐸𝐴
𝑘 = 𝑘𝑜 𝑒 −𝑅𝑇

𝐸𝐴
𝑙𝑛𝑘 = 𝑙𝑛𝑘𝑜 + (− ) ln(𝑒)
𝑅𝑇

𝐸𝐴 1
𝑙𝑛𝑘 = 𝑙𝑛𝑘𝑜 + (− )
𝑅 𝑇

Observations:

At Temperature T1:

S. No. Time (min) 𝜆 (𝑚𝑆) 𝜆 (𝑆)

1 0
2 3
3 6
 . .
. .
k1=____________________

At Temperature T2:

S. No. Time (min) 𝜆 (𝑚𝑆) 𝜆 (𝑆)

1 0
2 3
3 6
. .
. .

k2=____________________

Calculations:

1 Rate constant
S. No. Temperature (K) ln(k)
𝑇 (k)
1
2

𝐸𝐴
 Plot ln (k) vs. 1/T and find the slope (– 𝑅
) and intercept (𝑙𝑛𝑘𝑜 )

 Find EA and ko
 Experiment 14

Objective:

Determination of Arrhenius Parameters for saponification Reaction via Conductometry in Tubular Reactor

Apparatus:

Glass wares (beakers)

Tubular Reactor (CET-MKII) mounted on chemical reactor service unit (CEX-MKII)

Conductivity meter

Reagents:

Distilled water

3 liters Standard NaOH solution (0.06 M)

3 liters standard Ethyl acetate solution (0.06 M)

Calibration solutions of conductivity meter

Precautions:

1. Personnel safety:
a) Wear lab coat and latex gloves
b) Ensure proper working of Residual current circuit breaker (RCCB)
2. Equipment safety:
a) Fragile glass wares should be dealt with care
b) Ensure proper working of miniature circuit breakers (MCB)
c) Ensure heater of hot water circulator is off while working at ambient temperature
d) Hot water circulator should be properly primed with distilled water before turning on the
heater
e) Conductivity meter should be in 19.99 mS mode
3. Chemical safety:
Alkali solutions is corrosive and toxic. Ethyl Acetate is Flammable, Toxic & Irritant. Consult
MSDS for further details.
Calibration check:

1. Record the ambient temperature

2. Rinse the conductivity meter probe in calibration solution and cross check the meter reading with
standard conductivity.
3. Rinse conductivity meter probe properly with distilled water before using it in experiment

Procedure:

1. Perform experiment according to the procedure of Experiment 8.

2. Find rate constant (k1) at this temperature.
3. Turn on hot water circulator and adjust the temperature to a set point of 10 °C above ambient.
4. Again perform the experiment according to the procedure of experiment 8.
5. Again Find rate constant (k2) at 2nd temperature.

Arrhenius equation is

𝐸𝐴
𝑘 = 𝑘𝑜 𝑒 −𝑅𝑇

𝐸𝐴
𝑙𝑛𝑘 = 𝑙𝑛𝑘𝑜 + (− ) ln(𝑒)
𝑅𝑇

𝐸𝐴 1
𝑙𝑛𝑘 = 𝑙𝑛𝑘𝑜 + (− )
𝑅 𝑇

Observations:

At Temperature T1:

S. No. Time (min) 𝜆 (𝑚𝑆) 𝜆 (𝑆)

1 0
2 3
3 6
. .
. .
k1=____________________
At Temperature T2:

S. No. Time (min) 𝜆 (𝑚𝑆) 𝜆 (𝑆)

1 0
2 3
3 6
. .
. .

k2=____________________

Calculations:

1 Rate constant
S. No. Temperature (K) ln(k)
𝑇 (k)
1
2

𝐸𝐴
 Plot ln (k) vs. 1/T and find the slope (– 𝑅
) and intercept (𝑙𝑛𝑘𝑜 )

 Find EA and ko
 Experiment 15

Objective:

Determination of Arrhenius Parameters for saponification Reaction via Conductometry in CSTR battery

Apparatus:

Glass wares (beakers)

Chemical reactor service unit with cascade of CSTR’s (CEP-MKII)

Conductivity meter

Reagents:

Distilled water

5 liters Standard NaOH solution (0.06 M)

5 liters standard Ethyl acetate solution (0.06 M)

Calibration solutions of conductivity meter

Precautions:

1. Personnel safety:
a) Wear lab coat and latex gloves
b) Ensure proper working of Residual current circuit breaker (RCCB)
2. Equipment safety:
a) Fragile glass wares should be dealt with care
b) Ensure proper working of miniature circuit breakers (MCB)
c) Ensure heater of hot water circulator is off while working at ambient temperature
d) Hot water circulator should be properly primed with distilled water before turning on the
heater
e) Conductivity meter should be in 19.99 mS mode.
3. Chemical safety:
Alkali solution is corrosive and toxic. Ethyl Acetate is Flammable, Toxic & Irritant. Consult MSDS
for further details.
Calibration check:

1. Record the ambient temperature

2. Rinse the conductivity meter probe in calibration solution and cross check the meter reading with
standard conductivity.
3. Rinse conductivity meter probe properly with distilled water before using it in experiment

Procedure:

1. Perform experiment according to the procedure of Experiment 9.

2. Find rate constant (k1, k2, k3) at this temperature.
3. Turn on hot water circulator and adjust the temperature to a set point of 10 °C above ambient.
4. Again perform the experiment according to the procedure of experiment 9.
5. Again Find rate constant (k1, k2, k3) at 2nd temperature.

Arrhenius equation is

𝐸𝐴
𝑘 = 𝑘𝑜 𝑒 −𝑅𝑇

𝐸𝐴
𝑙𝑛𝑘 = 𝑙𝑛𝑘𝑜 + (− ) ln(𝑒)
𝑅𝑇

𝐸𝐴 1
𝑙𝑛𝑘 = 𝑙𝑛𝑘𝑜 + (− )
𝑅 𝑇

Observations:

At Temperature T1:

S. Time
𝜆1 (𝑚𝑆) 𝜆2 (𝑚𝑆) 𝜆3 (𝑚𝑆) 𝜆1 (𝑆) 𝜆2 (𝑆) 𝜆3 (𝑆)
No. (min)
1 0
2 3
3 6
. .
. .
k1=____________ k2=____________ k3=____________
At Temperature T2:

S. Time
𝜆1 (𝑚𝑆) 𝜆2 (𝑚𝑆) 𝜆3 (𝑚𝑆) 𝜆1 (𝑆) 𝜆2 (𝑆) 𝜆3 (𝑆)
No. (min)
1 0
2 3
3 6
. .
. .

k1=____________ k2=____________ k3=____________

Calculations:

1 Rate constant
S. Temperature ln(k)
𝑇 (k)
No. (K)
k1 k2 k3

𝐸𝐴
 Plot ln (k) vs. 1/T and find the slope (– 𝑅
) and intercept (𝑙𝑛𝑘𝑜 )

 Find EA and ko
 Experiment 16

Objective:

To determine rate constant for acid catalyzed hydrolysis of Ethyl Acetate via titrimetry

Apparatus:

Glass wares (beakers, burettes, pipettes, conical flasks)

Reagents:

Distilled water

2 liters Standard NaOH solution (0.1 M)

2 liters Standard HCl solution (0.5 M)

40 mL Standard Ethyl acetate analytical grade solution

Ice cubes/crushed ice

Precautions:

1. Personnel safety:
a) Wear lab coat and latex gloves
2. Equipment safety:
a) Fragile glass wares should be dealt with care
3. Chemical safety:
Acid & Alkali solutions are corrosive and toxic. Ethyl Acetate is Flammable, Toxic & Corrosive.
Consult MSDS for further details.

Procedure:

1. Prepare standard solutions of HCl and NaOH

2. Take crushed ice/ice cubes in atleast 6 conical flasks (ice acts as an inhibitor to stop the hydrolysis
reaction at once)
3. In separate conical flask, put 5mL pure ethyl acetate into 100mL (large excess) HCl solution
 4. Immediately withdraw a 10 mL sample from mixed solution and transfer it into conical flasks with
ice cubes (hydrolysis reaction will stop at once)
5. Titrate it against NaOH with phenolphthalein indicator
6. Find out the concentration of the ethyl acetate in the solution

Hydrolysis of ester is a (pseudo) first order reaction due to the large excess of water present. The
concentration of water doesn’t change appreciably before or after the reaction. Hence,

𝐶𝐻3 𝐶𝑂𝑂𝐶2 𝐻5 + 𝐻2 𝑂 → 𝐶𝐻3 𝐶𝑂𝑂𝐻 + 𝐶2 𝐻5 𝑂𝐻

−(𝑟𝐴 ) = 𝑘𝐶𝐴

Integrated rate law becomes,

𝐶𝐴𝑜
ln ( ) = 𝑘𝑡
𝐶𝐴

𝐼 𝐶𝐴𝑜
𝑘 = ln( )
𝑡 𝐶𝐴

NaOH is used to find out the Concentration of the acetic acid in given sample formed as a result of the
hydrolysis reaction. Stoichometrically, moles formed of acetic acid are equal to moles consumed of ethyl
acetate.
Calculations:

NaOH : CH3COOH

𝑀1 𝑉1 𝑀2𝑉2
=
𝑁1 𝑁2

𝑉2 = 10 𝑚𝐿

𝑀2 = __________________ = 𝐶𝐴

𝑚𝑜𝑙 1 𝐶𝐴𝑜
S. No. Time (min) 𝐶𝐴 ( 3 ) 𝑘 = ln ( ) (𝑚𝑖𝑛−1 )
𝑑𝑚 𝑡 𝐶𝐴