Intertek India Pvt. Ltd.

Safety Testing Laboratory

nd
F Wing, 2 Floor, Tex Centre,
Chandivali Farm Road, Off saki
vihar road, Andheri (East),
Mumbai 400 072
Tel. +9122 42450203 / 206

Reaction Calorimeter Report

REPORT NO. – RC/2018/015 Date: 20/11/2018
PAGE NO. 1 OF 3

Mr. Kamal Dujodwala

Test Requested by Mangalam Organics Limited.,
812, Tulsiani Chambers,
Nariman Point, Mumbai -400 021,
India
Sample ID STL/18/453
Reaction Isomerization Reaction
Date of Sample Receipt 15/11/2018

1) INTRODUCTION:
The thermal behavior during Isomerization Reaction was studied in a reaction
calorimeter for Mangalam Organics Limited., Mumbai.

2) EXPERIMENTAL:
i) RC1:
Mettler make AP 01 500 ml capacity all glass reactor equipped with a pitch blade
type down flow agitator, jacketed with controlled temperature circulator, addition
funnel, condenser and the probes.

ii) Experiment:
1) 200 gm of freshly distilled Alpha pinene and 1.2 gm of Activated Catalyst charged to
the reactor at RT.
2) Then Reaction Mass was heated at 50°C.
3) Then Reaction Mass was heated at 155°C
4) Then Reaction Mass was maintained for 120 minutes.

Contd….2

These results are valid only for the sample tested. The test results reported are valid under the stated conditions of
measurements. This report may not be reproduced, except in full. Any correction invalidates this report
 Intertek India Pvt. Ltd.
Safety Testing Laboratory
nd
F Wing, 2 Floor, Tex Centre,
Chandivali Farm Road, Off saki
vihar road, Andheri (East),
Mumbai 400 072
Tel. +9122 42450203 / 206

REPORT NO. – RC/2018/015

PAGE NO. 2 OF 3

3) RESULT & DISCUSSION:

The evolution of heat of reaction was calculated using Q flow (exchange from
jacket), Q accumulation (of reaction mass), Q dosing (heat input by dosed reactants)
& Q loss (to surrounding from reactor). Initialization parameters and plots of various
parameters, calibration, specific heat determination and heat of reaction are given in
Annexure-I.

4) HEAT OF REACTION:

a. The overall heat evolved during maintaining for 120 minutes is 37.224 KJ
(exotherm) for 0.201 Kg of reaction mass i.e 185.194 KJ/Kg of
reaction mass.

Contd….3

These results are valid only for the sample tested. The test results reported are valid under the stated conditions of
measurements. This report may not be reproduced, except in full. Any correction invalidates this report
 Intertek India Pvt. Ltd.
Safety Testing Laboratory
nd
F Wing, 2 Floor, Tex Centre,
Chandivali Farm Road, Off saki
vihar road, Andheri (East),
Mumbai 400 072
Tel. +9122 42450203 / 206

REPORT NO. – RC/2018/015

PAGE NO. 3 OF 3

5) CONCLUSION:

i) The overall heat evolved for 0.201 kg of reaction mass is 37.224 KJ

(exotherm) for during maintaining for 120 minutes i.e. 185.194 KJ/Kg of
reaction mass for during maintaining for 120 minutes. This can lead to
adiabatic temperature rise for maintaining for 120 minutes is 121°C.

ii) The Maximum Heat Generation Rate during maintaining for 120 minutes
is 132.94 W/Kg of reaction mass. The Maximum Temperature Synthesis
of Reaction (MTSR) during maintaining for 120 minutes is 276°C.

These results are valid only for the sample tested. The test results reported are valid under the stated conditions of
measurements. This report may not be reproduced, except in full. Any correction invalidates this report
 Intertek India Pvt. Ltd.
Safety Testing Laboratory
nd
F Wing, 2 Floor, Tex Centre,
Chandivali Farm Road, Off saki
vihar road, Andheri (East),
Mumbai 400 072
Tel. +9122 42450203 / 206

7) COMMENTS:

i) The overall heat of reaction during maintaining for 120 minutes is

exothermic; Severity of reaction during maintaining for 120 minutes is
Medium.

Authorized Signatory
Mr. Avinash Kamble
Technical Manager
Safety Testing Laboratory
Prepared & Checked Intertek India

These results are valid only for the sample tested. The test results reported are valid under the stated conditions of
measurements. This report may not be reproduced, except in full. Any correction invalidates this report
 Annexure-I
Experiment: Mangalam- Isomerization Reaction
Started: November 15, 2018 12:06 Author: INTERTEKCP-RC1\admin

1 Chemistry

Mol Stoic. Actual Actual

Chemical Type Conc. Notes
Weight Coeff Moles Amount
Freshly distilled Alpha Limiting 136.23 100
1 1.4681 200 g
pinene Reagent g/mol w/w%
Activated Catalyst 79.86 100
Catalyst - 0.015026 1.2 g
(Tio2) g/mol w/w%

Results of Reactions Value

Actual Yield Reaction 1 n/a
Total Est. Actual Weight 201 g
Total Est. Actual Volume 230 ml

2 Setup
RC1e Description
Device RC1e
Reactor AP01-0.5-3w Glass
Cover Cover PTFE AP01-0.5
Stirrer Pitch blade down
Calibration Heater Cal. heater, 5 W
Tr sensor Tr

RD10 Description
Name : Dist Set
Output : V1
Distillation FCE ID : Reflux divider
Set Temp. Diff. : Temp. Difference sensor on A2
Vapor Temp : Pt100 on A1

Generated: November 20, 2018 12:25 1/2

 Annexure-I
Experiment: Mangalam- Isomerization Reaction
Started: November 15, 2018 12:06 Author: INTERTEKCP-RC1\admin

3 Calorimetric Calculations
Integral Results
Start End
Trend Name Integral Baseline Type ∆Tad
Time Time
qr_hf Maintained for 2hrs. 01:54:29 03:59:28 37.224 kJ Proportional To Conversion 121.13 K

Virtual Volume (Vv)

Time Vv (used) Interpolation
00:00:06 229.77 ml Proportional to Vr
00:07:28 250 ml Proportional to Vr
05:13:18 210 ml Constant offset

Heat Transfer Coefficient (U)

Time U (used) Calculated by Tr Interpolation
00:23:38 161.89 W/K*m^2 Standard method 47.39 °C Proportional to Vv_observed
01:03:38 165.25 W/K*m^2 Standard method 50.40 °C Proportional to Vv_observed
05:30:44 173.45 W/K*m^2 Standard method 53.44 °C Proportional to Vv_observed
06:10:46 171.36 W/K*m^2 Standard method 50.45 °C Hold value

Specific Heat (cpr)

Time cpr (used) Calculated by Tr Interpolation
00:43:44 1.6743 J/g*K Standard method 48.29 °C Proportional to Mr
05:50:48 1.4438 J/g*K Standard method 51.67 °C Hold value

Various Parameters
qr definition qr_hf = qflow_hf - qc + qaccu + qdos
qdos averaged yes
cpi at 200 ml 12.31 J/K
cpi at 500 ml 23.25 J/K
Reactor Time Constant 15 s
∆Tad calculation Use mr and cpr at the end of the integral

Generated: November 20, 2018 12:25 2/2