We make a heat stability test and thermophysical property measurement by using various analysis methods.
Test Items / Testing / Substances
| temperature | atmosphere | pressure | term | sample vessel | |
|---|---|---|---|---|---|
| Thermogravimeter/Differential thermal analysis (TG-DTA) | room temperature to 1400°C | air, nitrogen gas, etc. | - | - | - |
| Differential scanning calorimetry (DSC) | -100 to 600°C | - | - | - | - |
| High pressure differential scanning calorimetry (HP-DSC) | room temperature to 500°C | non-corrosive inactive, reduced, or oxidized atmosphere | pressure reduction -3.5MPa (G) | - | - |
| Spontaneous ignition test (SIT) | room temperature +10°C to 250°C (constant initial temperature) | air, oxygen concentration control gas | - | Max. one week | - |
| Accelerating rate calorimetry (ARC) | about -20 to 350°C | - | 0 to 174×105Pa (abs) | - | titanium, Hastelloy C, glass, SUS304 |
| Pressure vessel test | - | - | - | - | - |
| BAM heat accumulation storage test | room temperature +10°C to 200°C (constant temperature) | air | - | Max. one week | - |
| Reaction heat (reaction calorimeter) | -10 to 200°C | - | 10kPa to 1MPa (abs) | - | - |
| Reaction heat (C-80) | about 5 degC to 300 degC | - | atmospheric pressure | - | - |
| Specific heat (C-80) | room temperature to 200 degC | - | - | - | - |
| Heat of evaporation C-80 method (liquid) | room temperature to 200°C (constant temperature) | - | - | - | - |
Thermal decompisition and thermal stability
- Thermogravimetry/Differential thermal analysis (TG-DTA)
- Differential scanning calorimetry (DSC)
- High pressure differential scanning calorimetry (HP-DSC)
- Spontaneous ignition tester (SIT)
- Accelerating rate calorimetry (ARC)
- Pressure vessel test with pressure measurement
- BAM heat accumulation storage test
Principle / Commentary / Registration Application
- 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 degC/min in general), and thermopravimeter (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. - 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. - Pressure vessel test with pressure measurement
This test complies with Pressure Vessel Test of the Jpanese Fire Service Act Category V (self-reactive substance). This apparatus equips with a pressure sensor and thermocouple instead of a rupture disk. The maximum pressure, maximum pressure rise of a chemical substance heated in an electric furnace as done in the Japanese Fire Service Act Category V test can be measured for quantitative evaluation for the sensitivity of heat decomposition of the substance. The measurement can be performed with an orifice or the vessel being closed. - 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 degC 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 vaporizaation of solid or liquid, one of the thermal properties, can be measured with DSC or C-80 optional systtem. 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.
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