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Differential Scanning Calorimeter DSC 3500 Sirius
Differential Scanning Calorimeter DSC 3500 Sirius
Product details
The DSC 3500 Sirius combines the latest technology and has high sensitivity. The measurement system is stable, durable, and easy to operate, with a temperature range of -170 ° C to 600 ° C. The most outstanding performance of the DSC 3500 Sirius measurement unit is the long service life of its silver furnace heating unit, and the integrated sensor structure has high stability and excellent resolution.
For large-scale sample testing, we offer an Automatic Sample Injector (ASC) that can accommodate up to 20 samples and references, and can use different types of sample crucibles.
The design of DSC 3500 Sirius can be used not only for routine testing of quality inspection and failure analysis, but also for characterization of textile technology, food production, packaging industry, polymer industry, cosmetics industry, and even organic or inorganic materials.
DSC 3500 Sirius - Technical Parameters
• Temperature range:- 170°C ... 600°C
Heating rate: 0.001 K/min 100 K/min
Cooling rate: 0.001 K/min 100 K/min (depending on temperature range)
• Sensor: heat flow type
• Calorimetry range: ± 650mW
• Temperature accuracy: 0.1K
• Enthalpy accuracy:<1% (standard metal)< 2% (for the vast majority of materials)
Atmosphere: oxidizing, inert (static, dynamic)
Automatic Sample Injector (ASC): capable of loading up to 20 samples or references at once (optional)
DSC testing of three different polymer film packaging bags. Sample quality: 0.692mg (sample A), 1.45mg (sample B), 0.919mg (sample C). Crucible: Al， Cover and puncture.
Before the secondary heating, heat the sample at a rate of 20K/min until it melts and cool it at a rate of 20K/min to eliminate the influence of thermal history.
The figure on the right shows the results of using peak separation software to separate the peaks of sample B between 100 ℃ and 125 ℃. It can be seen that the overlapping peaks were separated into three independent peaks, with peak temperatures of 107 ℃, 117 ℃, and 121 ℃, respectively. The measured curve (dotted line) almost completely overlaps with the total curve (red) fitted by the three calculated curves, indicating a good separation effect. Peak separation helps to accurately calculate the peak value and peak area of a single peak.
Cooling curves for two samples. Sample quality: 6.47mg (lot1), 7.05mg (lot2). Crucible: Al， Cover and puncture.
Temperature program: Heat up, cool down, heat up to 250 ℃, with a heating/cooling rate of 10K/min.
Rapeseed oil DSC test: sample size: 1.19mg; Crucible: Al crucible with open mouth; Temperature program: Heat up to 140 ℃, 160 ℃, 180 ℃ at 10K/min under N2 atmosphere, maintain constant temperature for 5 minutes, and then switch to air;
Constant temperature: 140 ℃ (green curve); 160 ℃ (blue curve); 180 ℃ (red curve).
DSC testing of epoxy resin. Sample quality: 0.47 mg; Crucible: alumina, covered;
Temperature program: 2 heating cycles, both reaching 200 ℃; Heating/cooling rate: 10 K/min.
For large-scale sample testing, we offer an Automatic Sample Injector (ASC) that can accommodate up to 20 samples and references, and can use different types of sample crucibles.
The design of DSC 3500 Sirius can be used not only for routine testing of quality inspection and failure analysis, but also for characterization of textile technology, food production, packaging industry, polymer industry, cosmetics industry, and even organic or inorganic materials.
DSC 3500 Sirius - Technical Parameters
• Temperature range:- 170°C ... 600°C
Heating rate: 0.001 K/min 100 K/min
Cooling rate: 0.001 K/min 100 K/min (depending on temperature range)
• Sensor: heat flow type
• Calorimetry range: ± 650mW
• Temperature accuracy: 0.1K
• Enthalpy accuracy:<1% (standard metal)< 2% (for the vast majority of materials)
Atmosphere: oxidizing, inert (static, dynamic)
Automatic Sample Injector (ASC): capable of loading up to 20 samples or references at once (optional)
DSC 3500 Sirius - Software Features
The analysis and operation software of DSC 3500 Sirius 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®The software can be installed on the control computer of the instrument to work online, or installed on other computers for offline use.
The analysis and operation software of DSC 3500 Sirius 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®The software can be installed on the control computer of the instrument to work online, or installed on other computers for offline use.
DSC related 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 correction (optional): By incorporating the time constant and thermal resistance factors of the instrument into the calculation and correcting them, sharper DSC peaks can be obtained.
TM-DSC (temperature modulated DSC, optional): can separate reversible heat flux (thermodynamic) and irreversible heat flux (kinetic) effects from the total heat flux curve.
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 correction (optional): By incorporating the time constant and thermal resistance factors of the instrument into the calculation and correcting them, sharper DSC peaks can be obtained.
TM-DSC (temperature modulated DSC, optional): can separate reversible heat flux (thermodynamic) and irreversible heat flux (kinetic) effects from the total heat flux curve.
DSC 3500 Sirius - Application Examples
Specific Heat Test of Inorganic Materials - From Low to High Temperature
Sapphire is a commonly used reference sample for specific heat testing, and its specific heat value is known. The DSC 3500 Sirius tested the specific heat of sapphire in the range of -140 ℃ to 500 ℃ and compared it with the theoretical values provided by NIST. The maximum deviation between the measured value and the theoretical value within the tested temperature range is 0.8%.
Sapphire is a commonly used reference sample for specific heat testing, and its specific heat value is known. The DSC 3500 Sirius tested the specific heat of sapphire in the range of -140 ℃ to 500 ℃ and compared it with the theoretical values provided by NIST. The maximum deviation between the measured value and the theoretical value within the tested temperature range is 0.8%.
Image: Sapphire specific heat test, sample mass: 112.25mg, crucible: Pt， Cover up. Heating rate: 10K/min.
Packaging Material - DSC, Professional Identification Tool
DSC is a fast and easy tool for identifying materials. The figure shows the secondary heating curves of three different packaging materials from 30 ℃ to 300 ℃ at a rate of 10K/min. Before the secondary heating, the samples are heated to melt and then cooled at a rate of 20K/min. The first heating curve contains the thermal history information of the polymer, while the second heating curve can reflect the properties of the material itself.
The following figure shows the secondary heating curves of samples A, B, and C. Film A and B have endothermic peaks at 247 ℃ and 253 ℃, respectively, corresponding to the melting process of different types of polyamides. The endothermic peaks at 126 ℃ and 140 ℃ are the melting process of different types of polyethylene. Film C's endothermic peak at 159 ℃ is likely to be the melting process of polypropylene.
The following figure shows the secondary heating curves of samples A, B, and C. Film A and B have endothermic peaks at 247 ℃ and 253 ℃, respectively, corresponding to the melting process of different types of polyamides. The endothermic peaks at 126 ℃ and 140 ℃ are the melting process of different types of polyethylene. Film C's endothermic peak at 159 ℃ is likely to be the melting process of polypropylene.
DSC testing of three different polymer film packaging bags. Sample quality: 0.692mg (sample A), 1.45mg (sample B), 0.919mg (sample C). Crucible: Al， Cover and puncture.
Before the secondary heating, heat the sample at a rate of 20K/min until it melts and cool it at a rate of 20K/min to eliminate the influence of thermal history.
The figure on the right shows the results of using peak separation software to separate the peaks of sample B between 100 ℃ and 125 ℃. It can be seen that the overlapping peaks were separated into three independent peaks, with peak temperatures of 107 ℃, 117 ℃, and 121 ℃, respectively. The measured curve (dotted line) almost completely overlaps with the total curve (red) fitted by the three calculated curves, indicating a good separation effect. Peak separation helps to accurately calculate the peak value and peak area of a single peak.
Using peak separation software to separate three overlapping peaks of sample B
Quality Control of Solder Materials
The DSC 3500 Sirius can be used for quality control of alloy samples. In this example, two types of solder with the same composition but different sampling positions were tested, with a temperature range from 25 ℃ to 250 ℃. Each sample was subjected to two heating tests, and the results of the two heating tests were compared separately. During the two heating processes, both samples exhibited endothermic peaks (starting at 217 ℃), indicating the melting of the alloy. The melting process of samples taken from different positions is very similar, not only with similar curve shapes, but also with similar peak temperatures and areas.
The first and second heating curves of two solder samples. Sample quality: 6.47mg (lot1), 7.05mg (lot2). Crucible: Al， Cover and puncture. Temperature program: Heat up, cool down, heat up to 250 ℃, with a heating/cooling rate of 10K/min.
However, the cooling curves of the two samples (cooling after one heating) are not exactly the same. Lot1 (blue curve) has a crystallization temperature of 189 ℃ (endpoint), while Lot2 (red curve) requires greater undercooling for crystallization. The initial crystallization temperature is lower than Lot1, and the endpoint temperature is 187 ℃. The difference in crystallization temperature is related to the varying impurity content in the sample. This example demonstrates that the DSC 3500 Sirius can perform rapid quality inspection on samples. In addition, it also emphasizes the importance of cooling tests, especially when the temperature rise curves of the samples are similar.
However, the cooling curves of the two samples (cooling after one heating) are not exactly the same. Lot1 (blue curve) has a crystallization temperature of 189 ℃ (endpoint), while Lot2 (red curve) requires greater undercooling for crystallization. The initial crystallization temperature is lower than Lot1, and the endpoint temperature is 187 ℃. The difference in crystallization temperature is related to the varying impurity content in the sample. This example demonstrates that the DSC 3500 Sirius can perform rapid quality inspection on samples. In addition, it also emphasizes the importance of cooling tests, especially when the temperature rise curves of the samples are similar.
Cooling curves for two samples. Sample quality: 6.47mg (lot1), 7.05mg (lot2). Crucible: Al， Cover and puncture.
Temperature program: Heat up, cool down, heat up to 250 ℃, with a heating/cooling rate of 10K/min.
Testing of Melting and Crystallization Behavior of Edible Oil
The DSC 3500 Sirius is also suitable for research in the food industry. Here we present the DSC measurement results of rapeseed oil. The sample is first cooled to -150 ℃ and then heated to 40 ℃. The cooling rate is 10K/min, and due to the crystallization of the oil, an exothermic peak begins to appear at -18 ℃. The curve shows the minimum values at -45 ℃, -64 ℃, and -69 ℃, indicating that the main components of rapeseed oil are various saturated and unsaturated fatty acids such as oleic acid, linoleic acid, and linolenic acid- The exothermic peak at 4 ℃ may be due to the crystallization of additives. During the subsequent heating process, a cold crystallization peak appeared at -53 ℃, followed by melting peaks of various components in rapeseed oil (peak temperatures -27 ℃, -18 ℃, and -12 ℃).
Rapeseed oil DSC test: sample size: 1.19mg; Crucible: Aluminum crucible with lid; Temperature program: Cool down to -150 ℃, then heat up to 40 ℃; Heating and cooling rate: 10K/min.
Oxidation Induction Period Test (O.I.T) of Rapeseed Oil
The oxidation stability of hydrocarbons can be determined based on the duration of the oxidation induction period. These can be easily achieved on the DSC 3500 Sirius. Here are the measurement results of rapeseed oil samples raised three times to different temperatures under an inert atmosphere (N2 atmosphere). After 5 minutes of equilibration time, the atmosphere switches to air. The DSC curve on the right shows the effect of different test temperatures on the oxidation cracking of the sample. The higher the temperature, the earlier the sample oxidation begins: it takes 63 minutes for the sample to start oxidation at 140 ℃, while it only takes 4 minutes at 180 ℃.
Rapeseed oil DSC test: sample size: 1.19mg; Crucible: Al crucible with open mouth; Temperature program: Heat up to 140 ℃, 160 ℃, 180 ℃ at 10K/min under N2 atmosphere, maintain constant temperature for 5 minutes, and then switch to air;
Constant temperature: 140 ℃ (green curve); 160 ℃ (blue curve); 180 ℃ (red curve).
Thermal curing of epoxy resin
Differential Scanning Calorimetry (DSC) can conveniently analyze and optimize thermosetting materials.
The following figure shows the DSC spectrum of epoxy resin, tested using a DSC 3500 Sirius instrument.
When heated once, the sample solidifies, and the peak temperature of the exothermic peak is 135.5 ℃. When heated to 200 ℃, the epoxy resin is completely cured. According to the secondary heating, the glass transition temperature of the cured sample is 115.0 ℃ (midpoint temperature).
The following figure shows the DSC spectrum of epoxy resin, tested using a DSC 3500 Sirius instrument.
When heated once, the sample solidifies, and the peak temperature of the exothermic peak is 135.5 ℃. When heated to 200 ℃, the epoxy resin is completely cured. According to the secondary heating, the glass transition temperature of the cured sample is 115.0 ℃ (midpoint temperature).
DSC testing of epoxy resin. Sample quality: 0.47 mg; Crucible: alumina, covered;
Temperature program: 2 heating cycles, both reaching 200 ℃; Heating/cooling rate: 10 K/min.
DSC 3500 Sirius - Related attachments
The DSC 3500 Sirius can be equipped with various accessories according to demand to further optimize performance. Multiple cooling systems (air compressors or pressurized air) can cool the furnace body to room temperature, and the liquid nitrogen cooling system can cool down to below -170 ° C.
The cost-effective mechanical refrigeration equipment IC40 can cool down to a minimum of -40 ° C and can be used as a substitute for liquid nitrogen systems in a not too low temperature range.
The more powerful mechanical refrigeration equipment IC70 can provide faster cooling rates, with a minimum cooling of -70 ° C.
All cooling options can be obtained by upgrading the DSC 3500 Sirius.
For the study of oxidation stability (such as oxidation induction time testing), the DSC 3500 Sirius can be equipped with a software controlled MFC gas flow control system to accurately control three different purge and protective gases.
The DSC 3500 Sirius can be equipped with various accessories according to demand to further optimize performance. Multiple cooling systems (air compressors or pressurized air) can cool the furnace body to room temperature, and the liquid nitrogen cooling system can cool down to below -170 ° C.
The cost-effective mechanical refrigeration equipment IC40 can cool down to a minimum of -40 ° C and can be used as a substitute for liquid nitrogen systems in a not too low temperature range.
The more powerful mechanical refrigeration equipment IC70 can provide faster cooling rates, with a minimum cooling of -70 ° C.
All cooling options can be obtained by upgrading the DSC 3500 Sirius.
For the study of oxidation stability (such as oxidation induction time testing), the DSC 3500 Sirius can be equipped with a software controlled MFC gas flow control system to accurately control three different purge and protective gases.
We offer various types of crucibles (aluminum, copper, silver, platinum, stainless steel pressure crucibles, etc.) to meet almost all testing needs.
NETZSCH provides the SampleCutter sample preparation tool, which can quickly prepare samples such as glass fiber filled particles or small plastic parts.
The crucible press with replaceable pressure head is compatible with all cold pressed aluminum crucibles, and stainless steel crucibles can be used for a maximum pressure of 20 bar.
For batch routine testing, an automatic sampling system (ASC) with 20 samples/references can also be equipped, and different types of crucibles can be used in one automatic sampling test.
NETZSCH provides the SampleCutter sample preparation tool, which can quickly prepare samples such as glass fiber filled particles or small plastic parts.
The crucible press with replaceable pressure head is compatible with all cold pressed aluminum crucibles, and stainless steel crucibles can be used for a maximum pressure of 20 bar.
For batch routine testing, an automatic sampling system (ASC) with 20 samples/references can also be equipped, and different types of crucibles can be used in one automatic sampling test.
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