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In fields such as polymers, pharmaceuticals, and chemical industries, it is often necessary to know what gaseous products are produced during the curing crosslinking reaction, decomposition, or other reaction processes.
For vacuum sealed thermogravimetric analyzers TG 209 F1, synchronous thermogravimetric analyzers STA 449 F5/F3/F1, STA2500, DIL402 Expedias Select/Supreme, TMA402F1/F3, and even differential scanning calorimetry DSC 404 F1/F3 and DSC 204 F1, Nike provides you with an effective combination system connected to Fourier transform infrared spectroscopy (FTIR). The transmission line and connection adapter to the furnace body can be heated to 230 ° C to prevent condensation of decomposition products as much as possible. There is an expanded gas-phase database that facilitates the analysis of spectra.
The hot red combination technology provides a powerful analytical tool that combines the quantitative analysis ability of TG with the qualitative analysis ability of FT-IR, and has a wide range of applications:
① Decomposition ② dehydration ③ residual solvent content ④ thermal cracking ⑤ gas-solid reaction ⑥ combustion ⑦ oxidation ⑧ corrosion ⑨ desorption ⑩ catalytic reaction ⑪ component analysis ⑫ adhesive burning ⑬ coal analysis ⑭ polymer components ⑮ ash content ⑯ volatilization, gas release
For vacuum sealed thermogravimetric analyzers TG 209 F1, synchronous thermogravimetric analyzers STA 449 F5/F3/F1, STA2500, DIL402 Expedias Select/Supreme, TMA402F1/F3, and even differential scanning calorimetry DSC 404 F1/F3 and DSC 204 F1, Nike provides you with an effective combination system connected to Fourier transform infrared spectroscopy (FTIR). The transmission line and connection adapter to the furnace body can be heated to 230 ° C to prevent condensation of decomposition products as much as possible. There is an expanded gas-phase database that facilitates the analysis of spectra.
The hot red combination technology provides a powerful analytical tool that combines the quantitative analysis ability of TG with the qualitative analysis ability of FT-IR, and has a wide range of applications:
① Decomposition ② dehydration ③ residual solvent content ④ thermal cracking ⑤ gas-solid reaction ⑥ combustion ⑦ oxidation ⑧ corrosion ⑨ desorption ⑩ catalytic reaction ⑪ component analysis ⑫ adhesive burning ⑬ coal analysis ⑭ polymer components ⑮ ash content ⑯ volatilization, gas release
Due to the unique interface design between instruments, excellent working performance is ensured
① The blowing airflow has a small flow rate and a small dilution effect.
② Easy to clean.
③ Standard MCT detector.
④ TG/STA interface with vacuum sealed structure.
⑤ Flexible selection of internal/external combination parts.
⑥ Minimize the mixing and decomposition of escaping gases as much as possible.
⑦ Avoid condensation.
⑧ Short response time.
⑨ Non volatile compounds can be analyzed under reduced pressure conditions.
⑩ High detection sensitivity.
⑪ Can distinguish decomposition steps that are close to overlapping excellently.
① The blowing airflow has a small flow rate and a small dilution effect.
② Easy to clean.
③ Standard MCT detector.
④ TG/STA interface with vacuum sealed structure.
⑤ Flexible selection of internal/external combination parts.
⑥ Minimize the mixing and decomposition of escaping gases as much as possible.
⑦ Avoid condensation.
⑧ Short response time.
⑨ Non volatile compounds can be analyzed under reduced pressure conditions.
⑩ High detection sensitivity.
⑪ Can distinguish decomposition steps that are close to overlapping excellently.
FTIR Transmission Pipeline Combination - Technical Parameters
• Wave number range: FTIR: - 8000cm-1... 340cm-1Combined use: 4400cm-1... 600cm-1(Dual window technology KBr+ZnSe)
•Resolution: better than 0.4cm-1
•Transmission pipeline: up to 230 ° C
•Furnace body adapter: up to 300 ° C
•Transmission pipeline material: PTFE (replaceable)
•Gas chamber window panel material: ZnSe + KBr
•Gas chamber volume/length: 8.7 ml/110 mm
•Detector: DLaTGS, Or MCT
• Wave number range: FTIR: - 8000cm-1... 340cm-1Combined use: 4400cm-1... 600cm-1(Dual window technology KBr+ZnSe)
•Resolution: better than 0.4cm-1
•Transmission pipeline: up to 230 ° C
•Furnace body adapter: up to 300 ° C
•Transmission pipeline material: PTFE (replaceable)
•Gas chamber window panel material: ZnSe + KBr
•Gas chamber volume/length: 8.7 ml/110 mm
•Detector: DLaTGS, Or MCT
The measurement and analysis software of FTIR combined system is based on Microsoft Windows ® OPUS and Proteus of the system ® Software package. Proteus ® The software contains powerful measurement and data analysis functions, with an extremely user-friendly interface that includes easy to understand menu operations and automated processes, 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.
Partial features:
① Using Proteus ® Collect, store, and analyze thermal analysis data using NETZSCH, and collect, store, and analyze infrared spectroscopy data using OPUS (Bruker Optik). Real time synchronization can be achieved between the two.
② OPUS/CHOM software can draw two-dimensional or three-dimensional graphs of FTIR test results, Proteus ® The software can provide a graph of the relationship between TG/DSC measurement curves and time and temperature.
③ OPUS/SEARCH can search spectral databases.
④ Integrated window traces can analyze characteristic temperature and peak area, and can be analyzed together with thermal analysis curves.
⑤ Gram Schmidt plot can be used for temperature and peak area calculations, and can be analyzed together with thermal analysis curves.
① Using Proteus ® Collect, store, and analyze thermal analysis data using NETZSCH, and collect, store, and analyze infrared spectroscopy data using OPUS (Bruker Optik). Real time synchronization can be achieved between the two.
② OPUS/CHOM software can draw two-dimensional or three-dimensional graphs of FTIR test results, Proteus ® The software can provide a graph of the relationship between TG/DSC measurement curves and time and temperature.
③ OPUS/SEARCH can search spectral databases.
④ Integrated window traces can analyze characteristic temperature and peak area, and can be analyzed together with thermal analysis curves.
⑤ Gram Schmidt plot can be used for temperature and peak area calculations, and can be analyzed together with thermal analysis curves.
TGA-FT-IR Polymer Database
The TGA-FT-IR polymer database contains over 129 gas phase spectra from 88 polymers measured by TGA-FT-IR combined technology. From these FT-IR spectra, the composition information of the emitted gases at the decomposition maximum rate point (DTG peak temperature) of these polymers can be obtained. This database is suitable for NETZSCH Burker thermal red combination instrument and can be integrated into OPUS spectral retrieval software.
To access this database, please contact the relevant sales and technical service engineers at Nike.
The TGA-FT-IR polymer database contains over 129 gas phase spectra from 88 polymers measured by TGA-FT-IR combined technology. From these FT-IR spectra, the composition information of the emitted gases at the decomposition maximum rate point (DTG peak temperature) of these polymers can be obtained. This database is suitable for NETZSCH Burker thermal red combination instrument and can be integrated into OPUS spectral retrieval software.
To access this database, please contact the relevant sales and technical service engineers at Nike.
FTIR Combination - Application Examples
The curing process of water-based varnish
The curing process of water-based varnish
The volatile components in coatings may contaminate the environment, and water-based or powder coatings can greatly alleviate this problem.
Weigh 31.9mg of two-component water-based varnish sample and analyze it using TG209F1 Libra FT-IR combined system. The sample was heated to 300 ℃ at a rate of 5K/min in a nitrogen atmosphere, with a nitrogen flow rate of 45ml/min. The main weight loss of the sample at 100 ℃ is due to the evaporation of water, but there is also a portion from hydrocarbon substances such as alkyl acetate and fatty alcohols. The two peaks on the trajectory chart indicate that the maximum volatilization rate of these components is at 154 ℃. Therefore, there is no indication of toxic gas production during the drying process of this water-based varnish.
Weigh 31.9mg of two-component water-based varnish sample and analyze it using TG209F1 Libra FT-IR combined system. The sample was heated to 300 ℃ at a rate of 5K/min in a nitrogen atmosphere, with a nitrogen flow rate of 45ml/min. The main weight loss of the sample at 100 ℃ is due to the evaporation of water, but there is also a portion from hydrocarbon substances such as alkyl acetate and fatty alcohols. The two peaks on the trajectory chart indicate that the maximum volatilization rate of these components is at 154 ℃. Therefore, there is no indication of toxic gas production during the drying process of this water-based varnish.
Drying and curing of water-based varnish
medicine
In the research of drugs, excipients, and derivative products, drug stability, shelf life, and solvent residue are very important characterizations. A piece of aspirin is heated at a heating rate of 10K/min in a nitrogen atmosphere until complete decomposition occurs, with a nitrogen flow rate of 45ml/min. Two weight loss steps can be observed on the TG curve, and the volatile gas mixture is mainly composed of acetic acid, salicylic acid, phenol, and CO2. Due to the heating and temperature control of the pipeline, even high boiling point components can smoothly reach the FT-IR gas chamber through the gas transmission pipeline and obtain relevant infrared spectra.
In the research of drugs, excipients, and derivative products, drug stability, shelf life, and solvent residue are very important characterizations. A piece of aspirin is heated at a heating rate of 10K/min in a nitrogen atmosphere until complete decomposition occurs, with a nitrogen flow rate of 45ml/min. Two weight loss steps can be observed on the TG curve, and the volatile gas mixture is mainly composed of acetic acid, salicylic acid, phenol, and CO2. Due to the heating and temperature control of the pipeline, even high boiling point components can smoothly reach the FT-IR gas chamber through the gas transmission pipeline and obtain relevant infrared spectra.
Thermal decomposition of acetylsalicylic acid
From this, the thermal decomposition process of the sample can be obtained, as shown in the following structural formula:
Measurement of high boiling point products under low pressure
When the boiling point temperature of volatiles is much higher than the heating temperature of the transmission pipeline, special conditions are required for the detection of these volatiles. Naichi's hot red combination system is designed for vacuum sealing and can be tested under low pressure. In this way, the boiling point temperature of the volatile sample will be lowered, allowing it to pass through the transmission pipeline without any loss, and can be used to detect high boiling plasticizers in polymers and rubber, such as the Fomblin in the perfluorinated O-ring below ® The testing. Thermogravimetric analysis and pressure control of the entire gas system are maintained at 100 mbar, and the plasticizer Fomblin evaporates at 370 ℃, which can be confirmed by comparing its infrared spectrum with that of its pure substance. At higher temperatures (460 ℃), decomposition products of polymers such as HF and other products can also be detected. The absorption peak indicated by the arrow in the figure is a typical absorption of HF.
Detection of gas emissions during the heating process of perfluororubber under low pressure
When the boiling point temperature of volatiles is much higher than the heating temperature of the transmission pipeline, special conditions are required for the detection of these volatiles. Naichi's hot red combination system is designed for vacuum sealing and can be tested under low pressure. In this way, the boiling point temperature of the volatile sample will be lowered, allowing it to pass through the transmission pipeline without any loss, and can be used to detect high boiling plasticizers in polymers and rubber, such as the Fomblin in the perfluorinated O-ring below ® The testing. Thermogravimetric analysis and pressure control of the entire gas system are maintained at 100 mbar, and the plasticizer Fomblin evaporates at 370 ℃, which can be confirmed by comparing its infrared spectrum with that of its pure substance. At higher temperatures (460 ℃), decomposition products of polymers such as HF and other products can also be detected. The absorption peak indicated by the arrow in the figure is a typical absorption of HF.
Detection of gas emissions during the heating process of perfluororubber under low pressure
building material
The construction industry generally needs to consider energy-saving factors, which requires low thermal conductivity of the wall structure. Therefore, high porosity building bricks are usually used. Adding various organic products to clay can form cavities during the sintering process, thereby increasing the porosity.
As shown in the figure below, the burning loss of organic matter in traditional clay bricks is accompanied by a large amount of heat release (775J/g). During the burning process of adhesive, water and CO2 are the main products, but the hot red combined system can clearly detect the volatilization of HF and SO2 in clay. The detection of volatile products helps optimize the sintering process from the perspectives of economy and ecological environment.
As shown in the figure below, the burning loss of organic matter in traditional clay bricks is accompanied by a large amount of heat release (775J/g). During the burning process of adhesive, water and CO2 are the main products, but the hot red combined system can clearly detect the volatilization of HF and SO2 in clay. The detection of volatile products helps optimize the sintering process from the perspectives of economy and ecological environment.
TG and DSC curves of porous brick clay
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