DSC PT 10
DSC PT 10 The differential scanning calorimetry method is widely used to examine and characterize substances, mixtures, and materials. This technique is internationally standardized under DIN 51007, DIN 53765, ISO/DIN L409 and ASTM D3418. The principle of operation is a measurement of the heat flux between the sample and reference. This is done over a well-defined area where the heat is moving. The heat flux is measured while the temperature is changing. The results are very important for many applications and provide valuable infor mation for the characterization of materials. The following applications of DSC measurements are very important: research and development quality control quality assurance process optimizing defect analysis The three main user groups interested in DSC instruments are: plastics and rubber industry pharmaceutical industry food industry The following interesting physical properties of materials can be measured: enthalpy, melting energy specific heat glass point crystalinity reaction enthalpy thermal stability oxidation stability aging purity phase transformation eutectics polymorphs product identification Applications The following application notes show many typical uses for the Linseis DSC. Because of limited space only a few appli cations are shown. For further application notes please contact Linseis directly. thermoplastics duroplastics elastomers PEEK/PEI blends recycling of polymers Phenolic resin NBR rubber blends DSC PT 10 2
Technical Specifications DSC PT 10 Principle Technical Specifications DSC PT 10 Temperature range 150 C up to 700 C Heating/cooling rates Temperature accuracy Time constant 0.1 up to 50 C/min +/-0,2 C (substance calibration) 4...8 s Resolution 0.125 µw RMS Noise 1.5 µw Data acquisition rate Atmospheres Measuring range Calibrations material Calibration 0.1 s up to 3600 s / data point N 2, Argon, O 2 etc., reducing and oxidizing +/- 2,5 up to +/- 250 mw included recommended 6 month interval DSC System (Differential Scanning Calorimeter) complete with software and hardware including standard kits and accessories Data acquisition software to control DSC with full parameter setup Including temperature programming, atmosphere control, timed cycling etc. Principle Gas OUT Cooling OUT Cooling IN Gas IN Cooling system Heating system Sample Sensor Reference Sensor Heatflow path 3
Features Features Sample preparation and crucibles Various crucibles are available to achieve superior measurement results. Open or closed crucibles crucibles can be used in the system. When using closed crucibles it is necessary to use a crucible press (see picture) with special lids. The crucible press uses a special tool set to seal the crucible. Aluminum and platinum crucibles are available. KREG: DSC with controlled cooling Using this option the DSC can be operated using controlled cooling rates. The control gauges are mounted on an existing dewar (normally 50 l). The controller consists of a supply tube into the dewar, a pressure gauge, and an electronic control valve. Through an additional control circuit the LN2 is fed to the DSC measuring cell. It is achieved using the pressure of the evaporating LN2 in the dewar. The Data acquisition card in the computer uses a control loop to determine how much LN2 is required for cooling. DSC Press KREG Software All LINSEIS Thermal Analysis instruments are controlled through sophisticated Windows software. The complete program consists of 3 sections: temperature control, data acquisition and data evaluation. Essential sample information is entered in the data acquisition section. Data acquisition section Essential data for each sample test includes: operator, laboratory, atmosphere, gas flow, material, sample file name, zero file name, commands, sample length, measuring range, max. temperature, duration of run, sampling frequency, heating and cooling -rate, and number of cycles. All menus are easily understood and intuitive. The software is quickly mastered with min. training needed. Evaluation section The evaluation is part of the complete windows software. It features a number of functions enabli ng a full evaluation of all types of data. All evaluation and data collection can be performed simultaneously. Data can be corrected using zero and calibrati on correction. Data evaluation includes: signal corrections and smoothing, derivation, relative mass change, mass calculation, curve arithmetic, data pick evaluation, glass point evaluation, slope cor rection A mean curve with statistical analysis can be performed on multiple curves. Graphical displays can be printed on all windows, compatible printers or plotters. Data can be displayed and printed in a table format. The softwar e also includes an ASCII export feature. 4
Applications Lanthanum-galliumoxid Because of the high sensitivity of the DSC even small caloric effects like the change of the crystal structure of Lanthan-Galiumoxid (LaGaO 3 ) can be made visible. The substance is very interesting especially when fast oxygen/ion conductors are needed, applications do exist with the use of lambda sensors for the catalytic converters. Heat flow [ml/s] 8.0 7.0 6.0 5.0 4.0 3.0 2.0 1.0 heating rate: 10K/min sample weight: 104.8 mg LaGaO 3 point of reaction 152.1 C 154.8 C Enthalpy 1.02 J/g Offset 164.6 C Onset 150.3 C 0.0-1.0-2.0 40 60 80 100 120 140 160 180 200 220 240 Temperature [ C] Heat flow [mw] 16 14 12 10 8 6 4 2 0-2 -4-6 -8 Polyethylen terephthalate (PET) sample weight: 5mg heating rate: 10K/min point of glass transition: 76.9 C Onset: 124.4 C Offset: 144.6 C : 131.0 C point of reaction: 126.5 C Onset: 252.6 C Offset: 273.9 C : 264.6 C point of reaction: 262.6 C exo Polyethylenenterephthalat (PET) Polyethylenenterephthalat (PET) shows at about 77 C a significant endother mal glass point, which is quite special for partly cristalin thermoplasts. The relation between the exothermal cold crysta llization (131 C) and the endothermal melting peak is a measure for the degree of crystallization of the material. In the case of PET the cristalin part is very small which results in good transparency of the material. This is why many drinking bottles are made out of PET. 40 60 80 100 120 140 160 180 200 220 240 260 280 300 320 Temperature [ C] Fruktose und glucose Each of the substances shows characteristic melting points. These melting points can be determined exactly by means of differential scanning calorimetry (DSC). This is why this analyzing method is being used quite frequently in or der to identify unknown substances or mixture of substances. Even mixtures with substances with equal molecular weight (eg fructose and glucose) can thus be identified. Differential Temperature 1600 1500 1400 161.9 C 1300 1200 1100 131.3 C 193.3 C 1000 900 800 700 600 500 400 300 Fructose 200 100 Saccharose 0-100 Glucose Offset Offset Onset Offset 196.5 C -200 166.3 C 115.9 C 137.7 C -300 Onset Onset 156.7 C 189.1 C -400-500 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 Temperature [ C] 5
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