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Differential Scanning Calorimeter DSC 214 Polyma
Differential Scanning Calorimeter DSC 214 Polyma
Product details
A New Integrated Solution for DSC Measurement
Simple operation, powerful functionality, precise measurement, and convenient daily use - these are the excellent features of the innovative DSC 214 Polyma. This instrument is uniquely designed to meet the needs of both beginners and experienced professionals. Especially with the development of two new software: automatic analysis and curve recognition, which set new standards for DSC, these will trigger a revolution in DSC analysis.
•A novel holistic solution for polymer characterization
•Unprecedented simplicity in sample preparation
•Automated measurement and analysis
Simple operation, powerful functionality, precise measurement, and convenient daily use - these are the excellent features of the innovative DSC 214 Polyma. This instrument is uniquely designed to meet the needs of both beginners and experienced professionals. Especially with the development of two new software: automatic analysis and curve recognition, which set new standards for DSC, these will trigger a revolution in DSC analysis.
•A novel holistic solution for polymer characterization
•Unprecedented simplicity in sample preparation
•Automated measurement and analysis
The first thermal flow DSC with rapid cooling capability
DSC 214 Polyma is equipped with an elliptical furnace body with very low thermal mass (Arena)®The maximum heating/cooling rate of the furnace body can reach 500K/min, which is unprecedented for thermal flow DSC. Compared to the commonly used cooling rates of 10K or 20K/min, a temperature program that is closer to actual processing can be achieved.
DSC 214 Polyma is equipped with an elliptical furnace body with very low thermal mass (Arena)®The maximum heating/cooling rate of the furnace body can reach 500K/min, which is unprecedented for thermal flow DSC. Compared to the commonly used cooling rates of 10K or 20K/min, a temperature program that is closer to actual processing can be achieved.
Pioneering sensor technology
Corona with new patented technology®The middle of the sensor is made of chromium nickel alloy, and the outer ring is made of constantan alloy. Two materials are connected by diffusion welding. Corona®The sensor has extremely high sensitivity and repeatability, coupled with the Concavus patented technology®The crucible achieves perfect reproducibility of the instrument.
Corona with new patented technology®The middle of the sensor is made of chromium nickel alloy, and the outer ring is made of constantan alloy. Two materials are connected by diffusion welding. Corona®The sensor has extremely high sensitivity and repeatability, coupled with the Concavus patented technology®The crucible achieves perfect reproducibility of the instrument.
New aluminum crucible and unique packaging box
Convavus®The crucible is a newly designed aluminum crucible launched together with the DSC 214. A special reinforcement ring has been added to the bottom of the crucible to ensure stable and good thermal contact between the bottom of the crucible and the bottom of the DSC sensor, significantly improving the repeatability of the measurement results. Concavus®The patented technology design of the crucible can improve the repeatability of all DSC measurements, making it suitable for both NETZSCH and all hot flow DSC on the market.
The 3-in1 Box packaging box designed specifically for Concavus crucibles 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.
Convavus®The crucible is a newly designed aluminum crucible launched together with the DSC 214. A special reinforcement ring has been added to the bottom of the crucible to ensure stable and good thermal contact between the bottom of the crucible and the bottom of the DSC sensor, significantly improving the repeatability of the measurement results. Concavus®The patented technology design of the crucible can improve the repeatability of all DSC measurements, making it suitable for both NETZSCH and all hot flow DSC on the market.
The 3-in1 Box packaging box designed specifically for Concavus crucibles 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.
three-in-one
Through Arena with very low thermal quality®Furnace body, sturdy and highly sensitive Corona®Sensors and uniquely designed Concavus®The combination of the crucible and the DSC 214 Polyma results in excellent performance.
Dynamics analysis of epoxy adhesive
Through Arena with very low thermal quality®Furnace body, sturdy and highly sensitive Corona®Sensors and uniquely designed Concavus®The combination of the crucible and the DSC 214 Polyma results in excellent performance.
DSC 214 Polyma - Technical Parameters
• Temperature range:- 170°C ... six hundred
Temperature repeatability: ± 0.01 ° C (standard metal)
• Maximum heating rate: 500 K/min
• Maximum cooling rate: 500 K/min
In response ratio:> 100 mW/K
DSC range: ± 750 mW
• Thermal enthalpy sensitivity: 0.1 μ W
• Enthalpy accuracy: ± 0.05% (standard metal)
Temperature/enthalpy correction: multi-point standard sample, non-linear correction technology
Baseline drift: 10 μ W (-50... 300 ° C)
• Specific heat measurement: optional
• Optional cooling equipment: compressed air, mechanical, liquid nitrogen (can be connected to multiple cooling devices separately or simultaneously, switched through software)
Atmosphere: static and dynamic, inert, oxidizing, reducing
Gas control: 3 independent airflow control devices, software automatically switches 3 independent mass flow control meters, software automatically switches (optional)
Automatic sampler: optional, can accommodate 20 positions, sample and reference positions can be specified arbitrarily
• Temperature modulated DSC: optional, equipped with patented FRC calibration technology
• Software: Proteus®Standard configuration:- Smart Mode- Expert Mode- AutoCalibration- AutoEvaluation- Identify (automatic retrieval)- Tau-R (Advanced DSC Calibration)- Oxidation induction period (O.I.T.)- Autoooling (automatic cooling)- Predefined methods;
• Operating System: The software can run on Windows 7, Windows 8.1, and Windows 10 operating systems, supporting mobile devices such as PCs and tablets
Advanced software: options including thermodynamics, peak separation, purity, thermal simulation, etc
• Temperature range:- 170°C ... six hundred
Temperature repeatability: ± 0.01 ° C (standard metal)
• Maximum heating rate: 500 K/min
• Maximum cooling rate: 500 K/min
In response ratio:> 100 mW/K
DSC range: ± 750 mW
• Thermal enthalpy sensitivity: 0.1 μ W
• Enthalpy accuracy: ± 0.05% (standard metal)
Temperature/enthalpy correction: multi-point standard sample, non-linear correction technology
Baseline drift: 10 μ W (-50... 300 ° C)
• Specific heat measurement: optional
• Optional cooling equipment: compressed air, mechanical, liquid nitrogen (can be connected to multiple cooling devices separately or simultaneously, switched through software)
Atmosphere: static and dynamic, inert, oxidizing, reducing
Gas control: 3 independent airflow control devices, software automatically switches 3 independent mass flow control meters, software automatically switches (optional)
Automatic sampler: optional, can accommodate 20 positions, sample and reference positions can be specified arbitrarily
• Temperature modulated DSC: optional, equipped with patented FRC calibration technology
• Software: Proteus®Standard configuration:- Smart Mode- Expert Mode- AutoCalibration- AutoEvaluation- Identify (automatic retrieval)- Tau-R (Advanced DSC Calibration)- Oxidation induction period (O.I.T.)- Autoooling (automatic cooling)- Predefined methods;
• Operating System: The software can run on Windows 7, Windows 8.1, and Windows 10 operating systems, supporting mobile devices such as PCs and tablets
Advanced software: options including thermodynamics, peak separation, purity, thermal simulation, etc
DSC 214- Software Features
Proteus®7.0: Time saving and labor-saving software
The simplified program settings user interface (SmartMode), one click automatic curve analysis (AutoEvaluation), and identification of unknown curves (Identify) are key features of the software that can greatly save time for other tasks. Even inexperienced users can quickly and safely obtain meaningful results.
After users have mastered DSC operation skills well, they can use Proteus in expert mode®All functions of the software. The results obtained using AutoEvaluation can also be manually processed and recalculated, allowing experienced users to fully grasp the analysis process.
Proteus®The 7.0 version of the software is specifically designed for DSC 214 Polyma and can work with Windows XP, Compatible with Windows 7 or Windows 8.1. The software is compatible with the instrument and can be installed and used on another computer.
The simplified program settings user interface (SmartMode), one click automatic curve analysis (AutoEvaluation), and identification of unknown curves (Identify) are key features of the software that can greatly save time for other tasks. Even inexperienced users can quickly and safely obtain meaningful results.
After users have mastered DSC operation skills well, they can use Proteus in expert mode®All functions of the software. The results obtained using AutoEvaluation can also be manually processed and recalculated, allowing experienced users to fully grasp the analysis process.
Proteus®The 7.0 version of the software is specifically designed for DSC 214 Polyma and can work with Windows XP, Compatible with Windows 7 or Windows 8.1. The software is compatible with the instrument and can be installed and used on another computer.
SmartMode - a shortcut to efficiency
With the launch of DSC 214 Polyma, a new intelligent mode software interface has also been born.
Due to its intuitive interface with clear structure, consistent navigation, and user friendliness, even inexperienced users can quickly find ways to use it.
In the menu directory of Wizards, there are a series of conventional predefined testing methods. These methods require very little input to achieve one click testing. These methods can also be combined with each other. The predefined methods include the testing methods corresponding to all materials in the NETZSCH polymer property poster, which can start testing immediately. The customer setting method allows users to save their previous testing methods for use in the next test.
With the launch of DSC 214 Polyma, a new intelligent mode software interface has also been born.
Due to its intuitive interface with clear structure, consistent navigation, and user friendliness, even inexperienced users can quickly find ways to use it.
In the menu directory of Wizards, there are a series of conventional predefined testing methods. These methods require very little input to achieve one click testing. These methods can also be combined with each other. The predefined methods include the testing methods corresponding to all materials in the NETZSCH polymer property poster, which can start testing immediately. The customer setting method allows users to save their previous testing methods for use in the next test.
AutoEvaluation - a fully automated analysis method
AutoEvaluation is a newly developed software feature that can automatically analyze the curves of unknown materials such as thermoplastic polymers, rubber, and resins with just one click. The automatic analysis function first analyzes key effects such as glass transition and melting peaks on the DSC curve, and then analyzes other thermal effects such as recrystallization. Through the intelligent calculation of software, users can obtain information that originally required professional knowledge, which is a pioneering development in the history of thermal analysis.
AutoEvaluation is a newly developed software feature that can automatically analyze the curves of unknown materials such as thermoplastic polymers, rubber, and resins with just one click. The automatic analysis function first analyzes key effects such as glass transition and melting peaks on the DSC curve, and then analyzes other thermal effects such as recrystallization. Through the intelligent calculation of software, users can obtain information that originally required professional knowledge, which is a pioneering development in the history of thermal analysis.
Identify curves - making every user an expert
Identify is a very special tool that can automatically identify and analyze curves with just a light tap. This part of the software is designed for material identification and quality control. Compared with the software integrated database, the curve characteristics of the given material can automatically identify the type of material. In the field of DSC technology, database comparison is unique. The database with recognition function not only includes the typical polymer curve spectrum library of NETZSCH, but also can be expanded by adding users' own polymer or composite curves. User defined quality standards can be used to set product categories. It is a first in the field of quality control and failure analysis to objectively compare certain batches of samples with others.
Identify is a very special tool that can automatically identify and analyze curves with just a light tap. This part of the software is designed for material identification and quality control. Compared with the software integrated database, the curve characteristics of the given material can automatically identify the type of material. In the field of DSC technology, database comparison is unique. The database with recognition function not only includes the typical polymer curve spectrum library of NETZSCH, but also can be expanded by adding users' own polymer or composite curves. User defined quality standards can be used to set product categories. It is a first in the field of quality control and failure analysis to objectively compare certain batches of samples with others.
AutoCalibration - Simplification of Necessary Steps
Calibration of DSC instruments is a prerequisite for accurate DSC testing. This ensures that the instrument is tested within the preset parameters. But the calibration program itself should be simple and fast, ideally able to be completed in one go. The solution is automatic calibration. This special software feature provides pre-defined calibration methods for standard testing and fully automated analysis of calibration tests, such as analyzing melting peaks, calculating calibration curves, and checking their effectiveness. Therefore, automatic calibration simplifies time-consuming routine tasks.
Calibration of DSC instruments is a prerequisite for accurate DSC testing. This ensures that the instrument is tested within the preset parameters. But the calibration program itself should be simple and fast, ideally able to be completed in one go. The solution is automatic calibration. This special software feature provides pre-defined calibration methods for standard testing and fully automated analysis of calibration tests, such as analyzing melting peaks, calculating calibration curves, and checking their effectiveness. Therefore, automatic calibration simplifies time-consuming routine tasks.
DSC 214- Application Examples
Using DSC for polymer quality control - incoming inspection
The figure shows the DSC curves of two seemingly identical particles, sample PA66, delivered at different times (cooled at a rate of 20K/min and then heated again). The blue curve (old sample) shows a glass transition at 63 ° C and a melting peak at 263 ° C, both of which are typical manifestations of PA66. On the new material (red curve), double peaks appeared with peak temperatures of 206 ° C and 244 ° C. This indicates that there may be a second polymer blended with PA66 in the new material.
Using DSC for polymer quality control - incoming inspection
The figure shows the DSC curves of two seemingly identical particles, sample PA66, delivered at different times (cooled at a rate of 20K/min and then heated again). The blue curve (old sample) shows a glass transition at 63 ° C and a melting peak at 263 ° C, both of which are typical manifestations of PA66. On the new material (red curve), double peaks appeared with peak temperatures of 206 ° C and 244 ° C. This indicates that there may be a second polymer blended with PA66 in the new material.
Sample quality: 11.96 mg (blue) and 11.85 mg (red); Cool down at 20K/min in a dynamic N2 atmosphere and then raise the temperature to 330 ° C at 20K/min.
Using DSC for polymer quality control - oxidation stability
OIT test (oxidation induction time) is a commonly used testing method for evaluating the oxidation resistance of polymers, especially polyolefins. In this example, two PP samples were heated to 200 ° C under a dynamic nitrogen atmosphere. The endothermic peak detected during the heating process corresponds to the melting of polypropylene. Switch the gas to air at a constant temperature of 200 ° C for 3 minutes. The subsequent exothermic effect is the oxidative decomposition of the polymer. In this example, sample A (OIT 6.6 minutes) underwent oxidation reaction earlier than sample B (OIT 11.6 minutes).
Sample quality: 9.48mg (sample A) and 9.55mg (sample B); Heat to 200 ° C at 20K/min in N2 atmosphere (50 ml/min) and maintain constant temperature for 3 minutes under N2; Maintain a constant temperature of 50ml/min in air until decomposition occurs.
Low temperature performance testing of rubber - secondary heating of SBR rubber
The figure on the right shows the two heating curves of SBR rubber samples between -100 ℃ and 220 ℃. During both heating processes, a glass transition of -47 ℃ (midpoint) was measured, and there was a broad endothermic peak between 0 ℃ and 70 ℃, which is speculated to be the melting of the additive. Only a peak heat release peak of 169 ℃ was detected during one heating process, indicating the post curing process of the elastomer.
The figure on the right shows the two heating curves of SBR rubber samples between -100 ℃ and 220 ℃. During both heating processes, a glass transition of -47 ℃ (midpoint) was measured, and there was a broad endothermic peak between 0 ℃ and 70 ℃, which is speculated to be the melting of the additive. Only a peak heat release peak of 169 ℃ was detected during one heating process, indicating the post curing process of the elastomer.
Thermal performance testing of thermoplastic polyurethane
The following figure shows the test results of thermoplastic polyurethane (TPU) samples. During a heating process, the glass transition occurs at -42 ° C, which is the softening process of the chain segments in the sample. During one heating process, there are two endothermic peaks between 100 ° C and 210 ° C. During the second heating process, only one reversible transformation caused by melting (thermoplastic component) was detected (7.40J/g). The irreversible transformation peak (207 ° C) is the volatilization of volatile components or additives, which leads to an increase in glass transition temperature. The glass transition temperature detected during the second heating process is -28 ° C.
Sample mass: 10.47mg, N2 atmosphere, heated from -100 ° C to 250 ° C at a rate of 10K/min twice
Isothermal crystallization of semi crystalline thermoplastic materials
DSC 214 Polyma combined with IC70 mechanical refrigeration was used to test the isothermal crystallization process of PA66 GF30 (30% wt glass fiber). The lower thermal mass of the furnace body allows for a cooling of 60 ℃ inside the furnace chamber within a few seconds. Under this premise, it is possible to separate the crystallization process of PA66 (crystallization peak around 17 minutes) from the curve fluctuations caused by temperature adjustment (curve fluctuations between 15.4 minutes and 16 minutes). At the same time, it can be seen from the temperature curve that the temperature overshoot is extremely small during rapid cooling, indicating that DSC214 Polyma has outstanding cooling performance.
The Impact of Recycled Materials - Failure Analysis
In this example, two types of recycled polypropylene materials used for injection molding were studied. Material A had fully crystallized at the end of the injection molding process, while material B was still in a molten state. Through DSC testing, the reasons for the differences in crystallization behavior between the two materials can be analyzed.
The exothermic peak during the cooling process is the crystallization process of the polymer. The crystallization starting temperature of recycled material A (blue curve, crystallization starting point 126 ℃) is higher than that of recycled material B (red curve, crystallization starting point 122 ℃).
In addition to the main peaks at 121 ℃ (blue curve) and 118 ℃ (red curve), there is also a peak at 97 ℃ (blue curve) and a shoulder peak at 107 ℃ (red curve). The small endothermic peak indicates the presence of another component in the material, which led to an earlier nucleation process in material A.
The exothermic peak during the cooling process is the crystallization process of the polymer. The crystallization starting temperature of recycled material A (blue curve, crystallization starting point 126 ℃) is higher than that of recycled material B (red curve, crystallization starting point 122 ℃).
In addition to the main peaks at 121 ℃ (blue curve) and 118 ℃ (red curve), there is also a peak at 97 ℃ (blue curve) and a shoulder peak at 107 ℃ (red curve). The small endothermic peak indicates the presence of another component in the material, which led to an earlier nucleation process in material A.
Different crystallization behaviors of PP recycled materials
Sample mass: about 13mg, N2 atmosphere, heated to 200 ℃ and cooled at a rate of 10K/min
Further verification can be obtained through the secondary heating curve. In addition to the endothermic peaks at 165 ℃ and 163 ℃ (typical melting peaks of PP materials), the blue curve also has two endothermic peaks at 110 ℃ and 124 ℃, indicating that material A contains additional components such as LDPE, LLDPE, or HDPE (melting temperature increases with density). On the contrary, material B only has a small endothermic peak at 126 ℃.
Sample mass: about 13mg, N2 atmosphere, heated to 200 ℃ and cooled at a rate of 10K/min
Further verification can be obtained through the secondary heating curve. In addition to the endothermic peaks at 165 ℃ and 163 ℃ (typical melting peaks of PP materials), the blue curve also has two endothermic peaks at 110 ℃ and 124 ℃, indicating that material A contains additional components such as LDPE, LLDPE, or HDPE (melting temperature increases with density). On the contrary, material B only has a small endothermic peak at 126 ℃.
Melting of PP recycled materials mixed with different PE impurities
Sample mass: about 13mg, N2 atmosphere, cooled at a rate of 10K/min and then heated to 200 ℃ at a rate of 10K/min
Sample mass: about 13mg, N2 atmosphere, cooled at a rate of 10K/min and then heated to 200 ℃ at a rate of 10K/min
Optimization of Process Parameters for Injection Molding
The crystallization behavior of semi crystalline polymers (such as PBT) varies with different cooling histories, which is crucial for estimating the temperature of mold opening and removal of finished components in actual production processes.
This example shows the temperature rise curve of PBT material containing 30% wt glass fiber after cooling at various cooling rates (20K/min to 200K/min).
The heating process uniformly adopts a heating rate of 50K/min, and the typical β - phase shoulder peak of PBT material can be clearly seen in the heating curve (red) after cooling at a rate of 20K/min; After cooling at a rate of 50K/min, the temperature of the endothermic peak of the β phase on the curve (blue) decreases and separates more from the main peak; On the curves cooled at rates of 100K/min and 200K/min (corresponding to green and black, respectively), only the exothermic cold crystallization process was observed, without the endothermic peak of the β phase.
This example shows the temperature rise curve of PBT material containing 30% wt glass fiber after cooling at various cooling rates (20K/min to 200K/min).
The heating process uniformly adopts a heating rate of 50K/min, and the typical β - phase shoulder peak of PBT material can be clearly seen in the heating curve (red) after cooling at a rate of 20K/min; After cooling at a rate of 50K/min, the temperature of the endothermic peak of the β phase on the curve (blue) decreases and separates more from the main peak; On the curves cooled at rates of 100K/min and 200K/min (corresponding to green and black, respectively), only the exothermic cold crystallization process was observed, without the endothermic peak of the β phase.
Heating curve of PBT GF30 after cooling at different rates
Sample quality: 10.1mg, heating rate: 50K/min
Meanwhile, the following figure illustrates the effect of different cooling rates on the crystallization behavior of PBT. When cooling at a rate of 20K/min (red), PBT crystallization begins at 194 ℃, with a peak crystallization temperature of 188 ℃. When cooling at a rate of 200K/min (black), the crystallization initiation temperature is 171 ℃, the peak temperature is 156 ℃, and the curve shows a bend at 120 ℃, but the crystallization heat release process has not yet been completed.
Sample quality: 10.1mg, heating rate: 50K/min
Meanwhile, the following figure illustrates the effect of different cooling rates on the crystallization behavior of PBT. When cooling at a rate of 20K/min (red), PBT crystallization begins at 194 ℃, with a peak crystallization temperature of 188 ℃. When cooling at a rate of 200K/min (black), the crystallization initiation temperature is 171 ℃, the peak temperature is 156 ℃, and the curve shows a bend at 120 ℃, but the crystallization heat release process has not yet been completed.
Cooling curves of PBT at different cooling rates
Sample quality: 10.1mg, N2 atmosphere, cooling rates of 20K/min, 50K/min, 100K/min, and 200K/min
Sample quality: 10.1mg, N2 atmosphere, cooling rates of 20K/min, 50K/min, 100K/min, and 200K/min
Dynamics analysis of epoxy adhesive
By using the Nike Dynamics software to establish a kinetic model of chemical reaction processes, the behavior of the chemical reaction system can be predicted under user-defined temperature conditions for process optimization.
This study investigates the curing process of a two-component epoxy adhesive. Three samples were heated to 200 ℃ at different rates (2K/min, 5K/min, and 10K/min), and the peak temperature of the curing reaction increased with increasing heating rate. The kinetic model of single step reaction basically coincides with the experimental curve, with a correlation coefficient higher than 0.999. Therefore, this model can be used to predict reactions under isothermal and user-defined temperature programs.
This study investigates the curing process of a two-component epoxy adhesive. Three samples were heated to 200 ℃ at different rates (2K/min, 5K/min, and 10K/min), and the peak temperature of the curing reaction increased with increasing heating rate. The kinetic model of single step reaction basically coincides with the experimental curve, with a correlation coefficient higher than 0.999. Therefore, this model can be used to predict reactions under isothermal and user-defined temperature programs.
Comparison between the measured curve (dashed line) and the theoretical curve (solid line) of a single step reaction
The following figure shows the variation of the curing degree of the sample with time under constant temperature at different temperatures, calculated by software based on a kinetic model. At a constant temperature of 120 ℃ for 3 minutes, the curing degree of the sample reaches 95%, while at 110 ℃, the same curing degree requires a constant temperature of more than 5 minutes.
Prediction of isothermal curing reactions at different temperatures
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