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Differential Scanning Calorimeter DSC 204 F1 Phoenix
Differential Scanning Calorimeter DSC 204 F1 Phoenix
Product details
Differential Scanning Calorimetry (DSC), as a classic thermal analysis method for studying the thermal effects of materials at controlled program temperatures, has been widely used in various fields of materials and chemistry, including research and development, process optimization, quality control, and failure analysis.
By using DSC method, we can study the phase transition of inorganic materials, the melting and crystallization process of polymer materials, the polymorphic phenomenon of drugs, the solid/liquid phase ratio of foods such as oils and fats, and so on.
By using DSC method, we can study the phase transition of inorganic materials, the melting and crystallization process of polymer materials, the polymorphic phenomenon of drugs, the solid/liquid phase ratio of foods such as oils and fats, and so on.
In recent years, the differential scanning calorimeter DSC 204 F1 launched by the German company Naich Instruments has made new breakthroughs in the structural design and flexibility of the instrument. Its measuring unit is a cylindrical 3D heating silver furnace body, embedded with heating wires, and externally connected with cooling equipment. The high thermal conductivity of the silver furnace body ensures temperature uniformity inside the furnace body. The integrated electronic flow control system ensures precise flow control under different blowing and protective atmospheres. The structural design of its airtightness allows the outlet end of the furnace to be connected to infrared or mass spectrometry for component analysis of the product gas.
According to the application field and actual needs, users of DSC 204 F1 can freely choose two different types of sensors. The time constant of the τ - type sensor is only 0.6 seconds, ensuring good separation ability for overlapping thermal effects. The μ - type sensor has a sensitivity that is more than ten times higher than ordinary sensors while ensuring peak separation ability, making it particularly suitable for small sample size research in fields such as pharmaceuticals, food, biomaterials, and liquid crystals.
DSC 204 F1 offers four different cooling methods: liquid nitrogen, mechanical refrigeration, air compression, and cooling cup. The use of a new mechanical cooling system can cover a measurement temperature range from -85 ° C to 600 ° C. Of course, if a liquid nitrogen cooling system (LN2) is chosen, it can provide a wider temperature range for measurement, from -180 ° C to 700 ° C.
Other special features and options include the 64 sample grade automatic sampling system ASC, a new ultraviolet light accessory, intelligent BeFlat correction function, advanced DSC correction, temperature modulation DSC (TM-DSC), etc. All of these make the DSC 204 F1 Phoenix®Becoming one of the most flexible and powerful DSC systems on the market today.
DSC 204 F1 Phoenix®-Technical parameters
• Temperature range:- 180 ... 700°C
Heating rate: 0 200K/min
• Cooling rate: 0 200K/min
Equipped with a standard tau type sensor, it has a short time constant and excellent peak separation ability.
Optional ultra high sensitivity μ - type sensor.
BeFlat technology can be used for baseline optimization.
• Airtight design, suitable for use with infrared mass spectrometry.
Two purge gases and one protective gas are used for precise flow setting and control using an integrated mass flow control system and corresponding software functions.
Compressed air cooling: 700 ° C Room temperature.
Mechanical cooling: 600 ° C- 85 ° C.
• Liquid nitrogen cooling: 700- 180 ° C (available in both liquid nitrogen and gaseous nitrogen modes).
ASC automatic sampling system (optional): up to 64 samples/reference positions, can be used in conjunction with the automatic macro analysis function in the analysis software to achieve automatic measurement and analysis.
UV curable accessories (optional)
• Temperature range:- 180 ... 700°C
Heating rate: 0 200K/min
• Cooling rate: 0 200K/min
Equipped with a standard tau type sensor, it has a short time constant and excellent peak separation ability.
Optional ultra high sensitivity μ - type sensor.
BeFlat technology can be used for baseline optimization.
• Airtight design, suitable for use with infrared mass spectrometry.
Two purge gases and one protective gas are used for precise flow setting and control using an integrated mass flow control system and corresponding software functions.
Compressed air cooling: 700 ° C Room temperature.
Mechanical cooling: 600 ° C- 85 ° C.
• Liquid nitrogen cooling: 700- 180 ° C (available in both liquid nitrogen and gaseous nitrogen modes).
ASC automatic sampling system (optional): up to 64 samples/reference positions, can be used in conjunction with the automatic macro analysis function in the analysis software to achieve automatic measurement and analysis.
UV curable accessories (optional)
DSC 204 F1 Phoenix®-Software functions
DSC 204 F1 Phoenix®The analysis and operation software is based on MS®Windows®Proteus of the system®The software package includes all necessary measurement and data analysis functions. This software package has an extremely user-friendly interface, including easy to understand menu operations and automated workflows, and is suitable for various complex analyses. Proteus software can be installed on the control computer of the instrument for online operation, or installed on other computers for offline use.
DSC 204 F1 Phoenix®The analysis and operation software is based on MS®Windows®Proteus of the system®The software package includes all necessary measurement and data analysis functions. This software package has an extremely user-friendly interface, including easy to understand menu operations and automated workflows, and is suitable for various complex analyses. Proteus software can be installed on the control computer of the instrument for online operation, or installed on other computers for offline use.
DSC analysis function:
Peak annotation: It can determine the starting point, peak value, inflection point, and ending point temperature, and can perform automatic peak search.
• Peak area/enthalpy calculation: Multiple types of baselines can be selected for partial area analysis.
Comprehensive analysis of peaks: Various information such as temperature, area, peak height, and peak width can be obtained simultaneously in one annotation.
• Crystallinity calculation.
Comprehensive glass transition analysis.
• Automatic baseline deduction.
• Specific heat testing and analysis.
• BeFlat®Use polynomial fitting to fit and subtract baselines at different heating rates.
Tau-R mode: By incorporating the time constant and thermal resistance factors of the instrument into the calculation and subtracting them, sharper DSC peaks can be obtained.
TM-DSC (temperature modulated DSC, optional): It can separate reversible heat flux (thermodynamic) and irreversible heat flux (kinetic) effects from the total heat flux curve.
There are also special software functions that comply with GLP, GMP, 21CFR and other standards.
DSC 204 F1 Phoenix®-Application examples
The Effect of Cooling Rate on PET Crystallization Behavior
Polyethylene terephthalate (PET) is a semi crystalline thermoplastic polymer with a relatively slow crystallization rate. The different ratios of amorphous (Tg 75 ° C~85 ° C) and crystalline (recrystallized at 146 ° C, melted at 242 ° C) can be measured in DSC. The DSC spectra of melted PET cooled at different cooling rates and then heated again are shown in the figure, indicating the influence of cooling rate on the crystallization behavior of PET. DSC 204 F1 can automatically calculate the crystallinity of the sample. The DSC 204 F1 Phoenix equipped with mechanical refrigeration is used here®.
The Effect of Cooling Rate on PET Crystallization Behavior
Polyethylene terephthalate (PET) is a semi crystalline thermoplastic polymer with a relatively slow crystallization rate. The different ratios of amorphous (Tg 75 ° C~85 ° C) and crystalline (recrystallized at 146 ° C, melted at 242 ° C) can be measured in DSC. The DSC spectra of melted PET cooled at different cooling rates and then heated again are shown in the figure, indicating the influence of cooling rate on the crystallization behavior of PET. DSC 204 F1 can automatically calculate the crystallinity of the sample. The DSC 204 F1 Phoenix equipped with mechanical refrigeration is used here®.
Specific Heat Test of Polystyrene (PS)
Testing the specific heat of various materials is one of the important applications of DSC. The figure shows the specific heat test results of a certain NIST standard substance (NIST SRM 705a, narrow molecular weight distribution polystyrene), with a heating rate of 10K/min. Different analysis methods were used for calculation, and the results showed an average error of<2%.
UV curing of epoxy resin adhesive
This example studies the UV curing of epoxy resin adhesive activated by light, and its mechanism is cationic polymerization reaction. The reaction rate and degree are highly correlated with temperature. Under a constant irradiation time of 60 seconds, a higher reaction temperature (70 ° C, red DSC vs. temperature curve) results in higher reaction activity (faster curing) and higher reaction heat (390 J/g) of the resin system. It is important to be familiar with this characteristic when dealing with dual curing resin systems, whether it is thermosetting or photopolymerization.
Melting of Aluminum Alloy
For modern metal alloy analysis, it is very important to be able to separate the independently composed melting peaks well. The DSC 204 F1 Phoenix equipped with a τ - type sensor®This can be achieved. The legend shows the DSC curve of aluminum alloy, indicating that the melting peaks are clearly separated within the melting range of 510 ° C to 650 ° C.
For modern metal alloy analysis, it is very important to be able to separate the independently composed melting peaks well. The DSC 204 F1 Phoenix equipped with a τ - type sensor®This can be achieved. The legend shows the DSC curve of aluminum alloy, indicating that the melting peaks are clearly separated within the melting range of 510 ° C to 650 ° C.
Glass transition of sorbitol
In a large number of food and drug products, sorbitol is used as a substitute for sugar. After adding 5.5% water to anhydrous sorbitol, the glass transition temperature decreased from -1.7 ° C to -25.6 ° C. After rapid cooling and subsequent heating, the amorphous state was maintained.
In a large number of food and drug products, sorbitol is used as a substitute for sugar. After adding 5.5% water to anhydrous sorbitol, the glass transition temperature decreased from -1.7 ° C to -25.6 ° C. After rapid cooling and subsequent heating, the amorphous state was maintained.
EVA film sample
In this example, DSC 204 F1 Phoenix is used®Test the EVA film sample with a sample mass of about 7 mg and a heating rate of 10 K/min. This test was conducted at the German Federal Association for Materials Research and Testing (BAM).
At one heating (blue curve), the glass transition temperature is -28 ℃ (inflection point), followed by two connected endothermic peaks between 50-100 ℃. This melting phenomenon is related to the layered distribution of sample thickness. The exothermic peak at 158 ℃ is the exothermic crosslinking reaction of the sample. It is worth noting that the reaction enthalpy of the sample (-14.15 J/g) is much lower than that of epoxy resin (usually between -400 J/g and -500 J/g).
During the second heating (red curve), the glass transition temperature is almost the same as the first heating. The double endothermic peak between 40 ℃ and 80 ℃ transforms into a broad shoulder peak, with a peak temperature of 63 ℃. The thicker the crystal layer, the higher the melting temperature. Therefore, the transition from a single endothermic peak to a broad shoulder peak indicates that due to the first heat treatment, the thickness of the sample crystal layer becomes thinner. During the secondary heating process, there was no exothermic reaction peak, indicating that the exothermic crosslinking reaction had been completed during the primary heating.
*Thanks to Dr. W. Stark and Dr. M. Jaunich from the Federal Institute for Materials Research and Testing (BAM) in Berlin for their testing and discussion. The results were published in Polymer Testing 30 (2011) 236-242.
At one heating (blue curve), the glass transition temperature is -28 ℃ (inflection point), followed by two connected endothermic peaks between 50-100 ℃. This melting phenomenon is related to the layered distribution of sample thickness. The exothermic peak at 158 ℃ is the exothermic crosslinking reaction of the sample. It is worth noting that the reaction enthalpy of the sample (-14.15 J/g) is much lower than that of epoxy resin (usually between -400 J/g and -500 J/g).
During the second heating (red curve), the glass transition temperature is almost the same as the first heating. The double endothermic peak between 40 ℃ and 80 ℃ transforms into a broad shoulder peak, with a peak temperature of 63 ℃. The thicker the crystal layer, the higher the melting temperature. Therefore, the transition from a single endothermic peak to a broad shoulder peak indicates that due to the first heat treatment, the thickness of the sample crystal layer becomes thinner. During the secondary heating process, there was no exothermic reaction peak, indicating that the exothermic crosslinking reaction had been completed during the primary heating.
*Thanks to Dr. W. Stark and Dr. M. Jaunich from the Federal Institute for Materials Research and Testing (BAM) in Berlin for their testing and discussion. The results were published in Polymer Testing 30 (2011) 236-242.
The primary and secondary heating process of commercial EVA film
DSC 204 F1 Phoenix®-Related attachments
DSC 204 F1 Phoenix®Multiple cooling devices can be optionally selected. Using CC 200 F1 (switchable between liquid nitrogen LN2 and gas nitrogen GN2 modes), the measurement temperature range can be between -180 ° C and 700 ° C. Alternatively, a closed cycle mechanical refrigeration equipment can be chosen, which is an efficient and economical cooling facility with a temperature measurement range of -85 600 ° C. Air compression cooling can cool to room temperature at the lowest.
Wide range of crucible selection: Nike offers various types of crucibles such as aluminum, silver, gold, copper, platinum, alumina, zirconia, graphite, stainless steel pressure crucibles, etc. to meet almost all possible testing needs.
Equipped with a new replaceable pressure head, the crucible press is compatible with both standard aluminum crucibles and medium pressure stainless steel crucibles.
Wide range of crucible selection: Nike offers various types of crucibles such as aluminum, silver, gold, copper, platinum, alumina, zirconia, graphite, stainless steel pressure crucibles, etc. to meet almost all possible testing needs.
Equipped with a new replaceable pressure head, the crucible press is compatible with both standard aluminum crucibles and medium pressure stainless steel crucibles.
The 3-in-1 sample box designed specifically for the new Concavus crucible provides comprehensive protection for the transportation and storage of crucibles, and prevents adhesion between crucibles caused by static electricity. Each box is equipped with a sample label card for easy archiving of samples and measurement results, which is particularly suitable for applications that require long-term preservation of samples and regular retesting.
DSC 204 F1 Phoenix®Equipped with a newly designed automatic sampling system (ASC), it can be used for batch routine testing. The instrument can work day and night, not only making full use of the instrument but also saving a lot of time (such as conducting calibration tests in an unmanned state on weekends).
This ASC can handle 192 crucibles evenly distributed on two replaceable sample boxes. Multiple types of crucibles can be used, with a maximum diameter of 8mm and a maximum height of 8mm. ASC's four needle gripper can handle different crucibles. For the purpose of calibration and correction testing, ASC provided an additional 12 crucible position fixed injection strips. The crucible in motion can be identified. All crucible and crucible cover information on ASC are stored in the database. There is an automatically controlled transparent box cover above the sample box. After closing the lid, the space above the sample box is purged by the branched gas integrated in the lid. The blowing air is a specialized branch for ASC, designed for opening and closing lids, and its flow rate has been optimized through regulation. The built-in 'remove crucible cover' function can be executed while the sample is waiting to be inserted into the DSC unit. An optional piercing device can also be equipped to pierce the crucible cover before measurement. The DSC system has a recycling bin for discarding crucible covers and non reusable crucibles. Sample boxes can also be used for sample archiving. In order to better identify different samples, each sample box has a unique serial number, and each sample grade on it has a two-dimensional number (such as A5, B2...). The crucible/crucible cover database has tray recognition function. This ASC system can also be used for the new TG 209 F1 Libra®Thermogravimetric analyzer.
Each sample on the injector can be individually set with different experimental conditions and analytical labeling methods, NETZSCH Proteus®The software's easy to understand setup wizard will guide operators to easily complete a series of measurement programs. Moreover, tests that have not been scheduled in advance can also be inserted into pre-set programs, which is very flexible.
For unstable or volatile samples, ASC also provides an automatic perforation device that can be set to puncture the sealed crucible before the measurement begins.
This ASC can handle 192 crucibles evenly distributed on two replaceable sample boxes. Multiple types of crucibles can be used, with a maximum diameter of 8mm and a maximum height of 8mm. ASC's four needle gripper can handle different crucibles. For the purpose of calibration and correction testing, ASC provided an additional 12 crucible position fixed injection strips. The crucible in motion can be identified. All crucible and crucible cover information on ASC are stored in the database. There is an automatically controlled transparent box cover above the sample box. After closing the lid, the space above the sample box is purged by the branched gas integrated in the lid. The blowing air is a specialized branch for ASC, designed for opening and closing lids, and its flow rate has been optimized through regulation. The built-in 'remove crucible cover' function can be executed while the sample is waiting to be inserted into the DSC unit. An optional piercing device can also be equipped to pierce the crucible cover before measurement. The DSC system has a recycling bin for discarding crucible covers and non reusable crucibles. Sample boxes can also be used for sample archiving. In order to better identify different samples, each sample box has a unique serial number, and each sample grade on it has a two-dimensional number (such as A5, B2...). The crucible/crucible cover database has tray recognition function. This ASC system can also be used for the new TG 209 F1 Libra®Thermogravimetric analyzer.
Each sample on the injector can be individually set with different experimental conditions and analytical labeling methods, NETZSCH Proteus®The software's easy to understand setup wizard will guide operators to easily complete a series of measurement programs. Moreover, tests that have not been scheduled in advance can also be inserted into pre-set programs, which is very flexible.
For unstable or volatile samples, ASC also provides an automatic perforation device that can be set to puncture the sealed crucible before the measurement begins.
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