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Thermal mass spectrometry QMS 403/5 Skimmer
Thermal mass spectrometry QMS 403/5 Skimmer
Product details
When conducting thermogravimetric experiments, people often hope to not only obtain data on the mass change of materials with temperature, but also conduct qualitative online analysis of the gas products released during the process. NETZSCH has launched the world leading thermal gravimetric gas mass spectrometry Skimmer combination technology, which has many unique advantages.
The SKIMMER combined system and quadrupole mass spectrometer (QMS) are the most sensitive thermal mass spectrometry systems worldwide. The combined system consists of a synchronous thermal analyzer (STA 409 and STA 429) equipped with a specific furnace body, a quadrupole mass spectrometer for detecting and analyzing product gases, and a two-stage depressurization system.
There is a critical technical issue in the process of gas transfer from thermogravimetric analyzer to gas chromatography-mass spectrometer. Only by transferring truly representative samples of the escaping gas to the QMS of the gas chromatography-mass spectrometer can the accuracy of QMS detection be ensured. Therefore, it is necessary to absolutely avoid gas separation and loss caused by condensation of gas phase components during the transfer process.
The development of Skimmer combined technology has successfully solved this technical problem. The thermal mass connection part has two ventilation holes, one in front and one behind, and maintains the same temperature as the sample. The first vent hole serves as a branching point to form a compressed area, followed by the second vent hole called Skimmer, which continues and forms parallel small particle beams directed towards the ion source of QMS.
Two ventilation holes are directly designed above the sample. Gas particles pass through them over a distance of only a few millimeters, ensuring short lag time and particularly high sensitivity. The condensation of gas components often occurs in capillary combined systems, and is more or less related to the mass number of the component, without correlation, and cannot be corrected. The Skimmer combination system maintains the sample and vent system at the same temperature, effectively reducing the condensation of gas components. Therefore, the experimental results show a significant improvement in sensitivity (depending on the quality, the experimental signal strength can be increased by more than 100 times).
Pulseta can be used®Quantify the mass spectrometry signal. This technique involves injecting a certain amount of required gas into an inert carrier gas stream and observing changes in mass and enthalpy during the reaction process.
For different application scenarios, different Skimmer combination configurations can be selected:
·Aluminum oxide Skimmer system: suitable for oxidizing atmosphere, with a maximum temperature of 1450 ° C.
·Glass carbon Skimmer system: suitable for inert atmosphere, with a maximum temperature of 2000 ° C.
The Skimmer combination system is a very useful tool for material research and process improvement, as well as research in the fields of energy and environment.
QMS 403/5 SKIMMER - Technical specifications
•Temperature range: SiC furnace: RT... 1450 ° C, Skimmer Orifice material is alumina; Graphite furnace: RT... 2000 ° C, Skimmer Orifice material is glassy carbon
•Heating rate: Standard furnace body: 0.001 About 100 K/min
•Scale range: 15000 mg
•Sensor type: DSC, DTA, TG, DSC-cp, Convenient and quick replacement
•Provide glove box extension accessories (optional)
•Provide corrosion-resistant version (optional)
•Provide crucibles of different materials and sizes
•QMS mass to charge ratio range: 1 512 u
•Resolution: 0.5 u
•Measurement mode/scan rate: - Analog scan - Bar chart scan - Multi ion detection (MID)
•Detector: 90 ° SEV, detection limit>10-14 mbar, or>100 ppb
•Skimmer temperature: sample temperature
•Skimmer material: - alumina (1450 ° C) - glassy carbon (2000 ° C)
•Ionization: Electron collision
QMS 403/5 Skimmer software features
The measurement and analysis software for QMS 403/5 Skimmer combined system is based on Microsoft Windows ® Proteus of the system ® Software package, which includes powerful measurement and data analysis functions, has an extremely user-friendly interface, including easy to understand menu operations and automatic operation 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.
QMS analysis function:
Simulated scanning, scanning rate>0.2 s/amu
Scan the bar chart at a scanning rate>200 ms/amu
Multi ion detection (MID) mode, capable of detecting up to 64 selectable mass numbers simultaneously, with a scanning rate>10 ms/amu
• Characteristic temperature (starting point, peak and ending point)
Peak area integration, combined with PulseTA ® Technology for quantitative analysis and calibration
Subtraction of mass spectrometry curves
QMS 403/5 Skimmer Application Example
The SKIMMER combined system and quadrupole mass spectrometer (QMS) are the most sensitive thermal mass spectrometry systems worldwide. The combined system consists of a synchronous thermal analyzer (STA 409 and STA 429) equipped with a specific furnace body, a quadrupole mass spectrometer for detecting and analyzing product gases, and a two-stage depressurization system.
There is a critical technical issue in the process of gas transfer from thermogravimetric analyzer to gas chromatography-mass spectrometer. Only by transferring truly representative samples of the escaping gas to the QMS of the gas chromatography-mass spectrometer can the accuracy of QMS detection be ensured. Therefore, it is necessary to absolutely avoid gas separation and loss caused by condensation of gas phase components during the transfer process.
The development of Skimmer combined technology has successfully solved this technical problem. The thermal mass connection part has two ventilation holes, one in front and one behind, and maintains the same temperature as the sample. The first vent hole serves as a branching point to form a compressed area, followed by the second vent hole called Skimmer, which continues and forms parallel small particle beams directed towards the ion source of QMS.
Two ventilation holes are directly designed above the sample. Gas particles pass through them over a distance of only a few millimeters, ensuring short lag time and particularly high sensitivity. The condensation of gas components often occurs in capillary combined systems, and is more or less related to the mass number of the component, without correlation, and cannot be corrected. The Skimmer combination system maintains the sample and vent system at the same temperature, effectively reducing the condensation of gas components. Therefore, the experimental results show a significant improvement in sensitivity (depending on the quality, the experimental signal strength can be increased by more than 100 times).
Pulseta can be used®Quantify the mass spectrometry signal. This technique involves injecting a certain amount of required gas into an inert carrier gas stream and observing changes in mass and enthalpy during the reaction process.
For different application scenarios, different Skimmer combination configurations can be selected:
·Aluminum oxide Skimmer system: suitable for oxidizing atmosphere, with a maximum temperature of 1450 ° C.
·Glass carbon Skimmer system: suitable for inert atmosphere, with a maximum temperature of 2000 ° C.
The Skimmer combination system is a very useful tool for material research and process improvement, as well as research in the fields of energy and environment.
QMS 403/5 SKIMMER - Technical specifications
•Temperature range: SiC furnace: RT... 1450 ° C, Skimmer Orifice material is alumina; Graphite furnace: RT... 2000 ° C, Skimmer Orifice material is glassy carbon
•Heating rate: Standard furnace body: 0.001 About 100 K/min
•Scale range: 15000 mg
•Sensor type: DSC, DTA, TG, DSC-cp, Convenient and quick replacement
•Provide glove box extension accessories (optional)
•Provide corrosion-resistant version (optional)
•Provide crucibles of different materials and sizes
•QMS mass to charge ratio range: 1 512 u
•Resolution: 0.5 u
•Measurement mode/scan rate: - Analog scan - Bar chart scan - Multi ion detection (MID)
•Detector: 90 ° SEV, detection limit>10-14 mbar, or>100 ppb
•Skimmer temperature: sample temperature
•Skimmer material: - alumina (1450 ° C) - glassy carbon (2000 ° C)
•Ionization: Electron collision
QMS 403/5 Skimmer software features
The measurement and analysis software for QMS 403/5 Skimmer combined system is based on Microsoft Windows ® Proteus of the system ® Software package, which includes powerful measurement and data analysis functions, has an extremely user-friendly interface, including easy to understand menu operations and automatic operation 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.
QMS analysis function:
Simulated scanning, scanning rate>0.2 s/amu
Scan the bar chart at a scanning rate>200 ms/amu
Multi ion detection (MID) mode, capable of detecting up to 64 selectable mass numbers simultaneously, with a scanning rate>10 ms/amu
• Characteristic temperature (starting point, peak and ending point)
Peak area integration, combined with PulseTA ® Technology for quantitative analysis and calibration
Subtraction of mass spectrometry curves
QMS 403/5 Skimmer Application Example
Lead chloride
7.92mg of lead chloride was subjected to a temperature rise test in an argon atmosphere at 150ml/min. The figure shows the volatilization process starting from the melting range (487 ° C). The molecular ions (PbCl2 m/z=278) and fragment ions generated by splitting and ionization (PbCl m/z=243, Pb m/z=208, Cl m/z=37, CL m/z=35) can be clearly detected below the boiling point of the raw material.
7.92mg of lead chloride was subjected to a temperature rise test in an argon atmosphere at 150ml/min. The figure shows the volatilization process starting from the melting range (487 ° C). The molecular ions (PbCl2 m/z=278) and fragment ions generated by splitting and ionization (PbCl m/z=243, Pb m/z=208, Cl m/z=37, CL m/z=35) can be clearly detected below the boiling point of the raw material.
Asphalt carbon powder
Asphalt based carbon powder (55.2mg) mainly decomposes into aromatic compounds with higher molecular weight before 600 ° C under a nitrogen atmosphere (50ml/min). The figure extracts several signals from the MID curve, including pyrene (m/z=202), phenanthrene (m/z=228), benzo (a) pyrene (m/z=252), benzo (ghi) naphthalene (m/z=276), and dibenzopyrene (m/z=302).
Asphalt based carbon powder (55.2mg) mainly decomposes into aromatic compounds with higher molecular weight before 600 ° C under a nitrogen atmosphere (50ml/min). The figure extracts several signals from the MID curve, including pyrene (m/z=202), phenanthrene (m/z=228), benzo (a) pyrene (m/z=252), benzo (ghi) naphthalene (m/z=276), and dibenzopyrene (m/z=302).
Thin film photovoltaics (Skimmer)
The band width of CuGaSe2 is 1.68 eV, making it a promising semiconductor material in the field of thin-film photovoltaics. It can serve as the top layer battery for photovoltaic series connected cell devices, while the bottom layer battery is CuInSe2. CuGaSe2 is synthesized from the elements Cu, Ga, and Se in stoichiometric ratios. At 450 ° C, Se3 evaporation can be detected through the isotopic distribution of mass numbers m/z 230 and m/z 245, indicating that this is a non stoichiometric material.
The appearance of elemental iodine is as a mineralizer in the synthesis process. Elemental selenium Se was detected at temperatures above 900 ° C, due to the decomposition of CuGaSe2. Adjusting the vapor pressure of Se can control the synthesis stoichiometry (tested using QMS 403/5 Skimmer).
The band width of CuGaSe2 is 1.68 eV, making it a promising semiconductor material in the field of thin-film photovoltaics. It can serve as the top layer battery for photovoltaic series connected cell devices, while the bottom layer battery is CuInSe2. CuGaSe2 is synthesized from the elements Cu, Ga, and Se in stoichiometric ratios. At 450 ° C, Se3 evaporation can be detected through the isotopic distribution of mass numbers m/z 230 and m/z 245, indicating that this is a non stoichiometric material.
The appearance of elemental iodine is as a mineralizer in the synthesis process. Elemental selenium Se was detected at temperatures above 900 ° C, due to the decomposition of CuGaSe2. Adjusting the vapor pressure of Se can control the synthesis stoichiometry (tested using QMS 403/5 Skimmer).
STA-MS SKIMMER testing chalcopyrite CuGaSe2
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