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The Differential scanning calorimetry (DSC) technique has been widely used. The differential scanning calorimeter is both a routine quality test tool and a research tool. Measmeasures the temperature, heat flow associated with the thermal transition inside the material. Our instrument is a heat flow type differential scanning calorimeter, with good repetition and high accuracy, which is especially suitable for accurate measurement of specific heat. The equipment is easy to calibrate, uses a low melting point, is fast and reliable, and has a very wide range of applications, especially in material research and development, performance testing and quality control. The properties of materials, such as glass transition temperature, cold crystallization, phase transition, melting, crystallization, product stability, curing / crosslinking, oxidation induction period, etc., are the research fields of differential scanning calorimetry, and different models are selected according to the experimental parameters and experimental requirements.
The application scope of differential scanning calorimeter is: curing reaction temperature and thermal effect of polymer materials, material phase transition temperature and thermal effect measurement, crystallization of polymer materials, melting temperature and thermal effect measurement, glass transition temperature of polymer materials, etc.
The sample and parameters were placed into the crucible separately and placed in the furnace for programmed heating to change the temperature of the sample and parameters. If the heat capacity of the reference and the sample are the same, and the sample has no heat effect, the temperature difference is almost "zero", and a smooth curve is obtained. As the temperature increases, the sample has a thermal effect, and the parameter does not produce a thermal effect, the temperature difference between the two, in the DSC curve, the larger the temperature difference, the greater the temperature difference changes, the more the number of peaks. Peak up are called exothermic and peaks down are called heat absorption.
The following figure is a typical DSC curve showing four types of transitions:
For a secondary transition, it is a change in the horizontal baseline
For the heat absorption peak, it is caused by the melting or melting transition of the test sample
For the heat absorption peak, it is caused by the decomposition or cleavage reaction of the test sample
is the exothermal peak, which is the result of the sample crystalline phase transition
Material is often accompanied by thermal effects during physical and chemical changes, and heat release and heat absorption reflect the thermal enthalpy of matter. A differential heat analyzer is a function of measuring the temperature or time between the test sample and the reference under the same thermal condition.
Differential scanning calorimetry is a technique to measure the power difference between the output material and the parameter under a program-controlled temperature. The instrument of our company is the heat flow type differential scanning calorimeter, with the thermal flow difference between the sample and the parameter in mw. The abscissa is time (t) or temperature (T), increasing from left to right (not meeting this requirement shall be noted).
After the sample and the reference are put into the crucible, they heat up at a certain rate. If the thermal capacity of the reference and the sample is roughly the same, the ideal scanning calorimetric analysis map can be obtained.
The figure T is the temperature curve reflected by the thermocouple interpolated in the reference. Temperature difference curve between the AH-line reaction sample and the reference. If the sample had no thermal effect, then the △T=0 between the sample and the reference showed a baseline as smooth as the AB, DE, GH on the curve. When the temperature of the sample occurs below the temperature of the sample of the parameter. Conversely, peak-up EFG exothermic peaks appear.
The number of peaks, location, peak area, direction, height, width, symmetry in the figure reflects the physical and chemical changes of the sample in the measured temperature range, the temperature range of the transition, thermal effect magnitude and positive and negative. The height, width, and symmetry of the peaks, in addition to the test conditions, the dynamics in the sample change, and the measured results are much more complex than the ideal curve.
DSC300c Liquid Nitrogen Refrigeration Differential Scanning Calorimeter
3.Instrument characteristics
DSC | DSC-300C Differential scanning calorimeter |
DSC range | 0~±600mW |
Temperature range | -45~ 600ºC |
Heat-up rate | 0.1~100ºC/min |
Temperature resolution | 0.001ºC |
Temperature fluctuations | ±0.001ºC |
Temperature reproducibility | ±0.1ºC |
DSC accuracy | 0.001mW |
DSC sensitivity | 0.01uW |
Temperature control method | Heating up and constant temperature (automatic control of the whole program) |
Curve scan | Heating up the scan |
Air control | The instrument switches automatically |
Display mode | The 24bit color 7-inch LCD touchscreen display is shown |
Data interface | Standard USB interface |
Instrument standards | Equipped with standard substances (Sn), the user can correct the temperature and thermal enthalpy |
Note | All technical indicators can be adjusted according to the user needs |
4.1 Instrument Interface
4.1.1 The Initial Status key is used to view the ambient temperature, sample temperature, etc.
4.1.2 The Parameter Settings key is used to set the experimental parameters, generally on the software.
4.1.3 The Device Information key displays the device information. The administrator channel is used for the internal personnel calibration temperature.
4.1.4 The Start Run key to display the current data information after the operation on the computer software.
4.2 Connecting of instruments
4.2.1. thermostatic water bath circulation system, water bath set more than 4ºC, add water, less than 4ºC, add antifreeze, add liquid quantity see the water bath instructions.
4.2.2. When the constant temperature water bath device is set to 0ºC. When the temperature drops to 0ºC or lower, open the differential scanning calorimeter host and set the experimental parameters.The minimum temperature set by the differential host can be 15ºC lower than that of the constant temperature water bath.
4.2.3. The constant temperature water bath device has two hoses connected to the inlet / outlet behind the instrument in no order.
The connection schematic diagram is as follows:
Note: The differential host must wait for the constant temperature water bath to reach the set temperature before running.