Heat stability test

Various types of Thermal decomposition and thermal stability Test performed as

below.

1. Thermogravimetry/Differential thermal analysis (TG-DTA)

2. Differential scanning calorimetry (DSC)

3. High pressure differential scanning calorimetry (HP-DSC)

4. Spontaneous ignition tester (SIT)

5. Accelerating rate calorimetry (ARC)

6. Pressure vessel test with pressure measurement

7. BAM heat accumulation storage test

Thermogravimetry/Differential thermal analysis (TG-DTA)

This analysis simultaneously performs differential thermal analysis (DTA), which

measures the difference of thermal effects between a sample and reference
substance (a-alumina in general) as a function of temperature (time) with the
constant temperature ramp (10 deg C/min in general), and thermogravimeter
(TG), which measures a change of the sample weight as a function of the
temperature (time). Phase transition, melting, solid phase reaction, dehydration,
decomposition, evaporation, and other reactions can be measured with high
sensitivity and the weight change can be measured simultaneously.

Measure change in Weight in relation to change in temperature. Used for

Corrosion Study purpose.

Differential scanning calorimetry (DSC)

When a sample and a reference substance which is as thermally stable as the
sample are heated with the constant temperature ramp (10 degC/min in general),
heat is generated to or absorbed from the circumstance. DSC measures the heat
flow as quantity of heat per unit time. It can quantitatively measure the
generated or absorbed heat involved in transition, melting, or crystallization of
polymers or low-molecular organic substances. In this measurement, a sealed
stainless-steel cell is used to measure the onset temperature at which the heat
generation starts and the amount of absorbed heat, and screening of chemical
products and reaction intermediate products in terms of thermal hazard is
conducted (Sealed Cell-DSC). For a sample (such as halogen) that could react with
stainless steel, a gold plated cell is used.

High pressure differential scanning calorimetry (HP-DSC)

This DSC allows a change of the kind and pressure of the atmosphere gas. It can
be used to measure the thrmal decomposition of a sample having high vapor
pressure, which is difficult to be measured with ordinary DSC, and to make
screening in terms of reactivity with oxygen and thermal hazard of chemical
substances.

Spontaneous ignition test (SIT)

Spontaneous ignition is a phenomenon that a substance spontaneously generates

heat of oxidation in the air at a significantly lower temperature than the
autoignition temperature and the heat accumulates for a long period results in
increasing the temperature to the ignition temperature and then causing ignition.
SCAS can measure the induction time that a sample takes to ignite in an adiabatic
condition and use the result to find a condition for safe handling of chemical
products or substances used in production processes and to analyze spontaneous
ignition characteristics. In addition, SCAS introduced apparatus that allows
measurements at up to 300 degC to use for spontaneous ignition test of carbon
materials and others. The measurement usually continues for up to one week at
a constant temperature.
Accelerating rate calorimetry (ARC)

Currently, ARC is known as the most reliable test method to evaluate thermal
stability of reactive chemical substances. It is the abbreviation of Accelerating
Rate Calorimeter. ARC is an accurate adiabatic calorimeter controlled by a
computer and is used to quantitatively measure the thermal behavior and
generated pressure of reactive chemical substances in the self-accellerating
decomposition under the adiabatic condition. Primary data obtained in the
measurement are analyzed with Sumitomo Chemical’s original method
developed through the long-term experience to find safe temperature and time
to handle the substances. So the measurement data are quite useful for hazard
assessments of production process, transportation, and storage of the reactive
chemicals. In particular, our measurement method can be used below room
temperature, which are unstable at around the room temperature.

BAM heat accumulation storage test

Self-reactive substances gradually react if kept in a high-temperature

circumstance for a long period of time and the reaction heat accumulates inside
the substances, which could cause thermal explosion. The minimum temperature
at which the self-accelerating decomposition occurs (temperature rise more than
6 deg C within seven days) is called SADT (Self-Accelerating Decomposition
Temperature). There are several kinds of SADT tests and BAM heat accumulation
storage test is one of them. In BAM (Federal Institute for Materials Research and
Testing) heat accumulation storage test, 400 ml of sample is put in a 500 ml
Dewar flask, which is then closed with a thermally-insulated lid. The flask is put in
an air circulated condition kept at a constant temperature. Then the induction
time from when the sample temperature reaches the atmosphere temperature
to when the self-accelerating decomposition occurs is measured.

Heat of reaction and specific heat

It is important to have basic thermal data in chemical reactions for process
development and safety. Reaction calorimeter is a calorimeter to accurately
measure in a bench scale the amount of heat involved in a chemical reaction or
phase transition under a bench scale (sample size 500 g).. It can be used to obtain
thermal data for actual equipment, and to optimize the reaction condition.
Temperature at which a reaction starts, heat generation/absorption rate, heat of
reaction, heat of mixing, heat of fusion, heat of crystallization, specific heat, and
overall heat transfer coefficient can be measured. In addition, mixing-reaction
calorimeter (C-80) can be used to measure heat of reaction and heat of mixing of
a liquid-liquid system or solid-liquid system using only a small amount of sample
(1 to 5g).

Heat of vaporization and heat of sublimation

Heat of vaporization of solid or liquid, one of the thermal properties, can be

measured with DSC or C-80 optional system. DSC method measures the heat of
vaporization of a solid sample by constant temperature ramp under at a constant
pressure. C-80 optional system is used to measure the heat of vaporization of
liquid at a constant temperature. SCAS uses both apparatus for the
measurement.