CN106769621A - A kind of microwave Thermgravimetric Analysis Apparatus and combined system - Google Patents
A kind of microwave Thermgravimetric Analysis Apparatus and combined system Download PDFInfo
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- CN106769621A CN106769621A CN201611047356.6A CN201611047356A CN106769621A CN 106769621 A CN106769621 A CN 106769621A CN 201611047356 A CN201611047356 A CN 201611047356A CN 106769621 A CN106769621 A CN 106769621A
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Abstract
The present invention provides a kind of microwave Thermgravimetric Analysis Apparatus and combined system, including microwave heating system, temperature control system, Quality Monitoring Control System and external combined system.Microwave generator is arranged on device back, by waveguide by microwave transmission to stainless steel microwave resonance inner chamber.Using the temperature of infrared radiation thermometer real-time monitoring sample, microwave output power is adjusted, to meet design temperature needs.Stainless steel intracavity bottom opens up through hole, is connected with bottom electronic balance through hollow cylinder quartz ampoule, and quartz ampoule cantilever tip stretches into stainless steel inner chamber.Quartz reaction bottle is placed on quartz holder, its outlet carries out on line real time through stainless steel inner chamber, the sample introduction pipeline by accessing combination analysis system after valve shunting.Simple structure of the present invention, it is easy to operate, the microwave thermogravimetric analysis under different condition can be obtained, while effectively prevent hot-weighty gas sample loss, it is obtained in that complete sample composition information.
Description
Technical field
The present invention relates to a kind of Thermgravimetric Analysis Apparatus, more particularly to a kind of microwave Thermgravimetric Analysis Apparatus and combined system.
Background technology
Thermogravimetric analysis refers to one kind heat of quality with temperature change relation that testing sample is measured under programed temperature
Analytical technology, is the important method for studying material characteristic and reaction rule for the heat endurance and component of research material.Tradition
Thermogravimetric generally uses electrical heating, belongs to external heat, and environment has certain thermograde with material center, with ambiance temperature
There is certain error in degree, for the heat analysis of the bigger material of size, its test result deviation is bigger instead of temperature of charge.
Heating using microwave has the advantages such as instantaneity, globality and high efficiency, and the chemical reaction carried out in microwave field has
Speed is fast, temperature is low, reactant rate of rotation high and the advantages of good product selectivity, and its heating mechanism causes the heat transfer inside material
The rule different from mass transport process presentation, additionally, for large-size material, the heating of microwave monoblock type can be in certain journey
Ensure the equilibrium of material inside and outside temperature on degree.Therefore, thermogravimetric analysis research of the material under microwave condition is necessary.
Thermogravimetric analysis is often used in conjunction in actual material analysis with other analysis methods, carries out Thermal Synthetic Analysis, comprehensively
Accurate analysis of material.Thermogravimetric can detect directly with infrared GC-MS to escaping gas during thermogravimetric analysis, can
The infrared spectrum information of multiple gases product is obtained simultaneously, and the determination of functional group is carried out according to vibrational spectra.Thermogravimetric joins with mass spectrum
With while material weightlessness information is obtained composition analysis and test can be carried out to emergent gas, for complicated heat chemistry
Reaction can also provide more abundant information, be conducive to preferably studying the heat analysis process and material characteristic of material.
In current practical application, in the presence of some microwave Thermgravimetric Analysis Apparatus, that have been reported is all free-standing behaviour
Make, it is even more to rarely have and is related to the combination of correlation analysis equipment.
The content of the invention
The shortcoming of prior art in view of the above, it is an object of the invention to provide a kind of microwave Thermgravimetric Analysis Apparatus with
Combined system, the shortcoming for being difficult to cooperate with test sample information for solving prior art presence.
In order to achieve the above objects and other related objects, the present invention provides a kind of microwave Thermgravimetric Analysis Apparatus with combination system
System, including：Microwave resonance inner chamber, microwave generator, infrared radiation thermometer, electronic balance, support, reactor, combination analysis system；
The microwave generator is arranged at microwave resonance inner chamber back, by waveguide by microwave transmission to microwave resonance inner chamber；It is described red
Outer temperature measurer is arranged in microwave resonance inner chamber, the temperature of real-time monitoring sample, adjusts microwave generator power output；It is described micro-
Wave resonance intracavity bottom opens up through hole, and the support is connected through the through hole with bottom electronic balance, and frame upper stretches into micro-
In wave resonance inner chamber, and reactor is provided with, the outlet of the reactor is followed by through microwave resonance inner chamber by valve shunting
Enter the sample introduction pipeline of combination analysis system, carry out on line real time.
Used as microwave Thermgravimetric Analysis Apparatus of the invention and a kind of preferred scheme of combined system, the outlet of the waveguide is omited
Higher than the center of reactor, and it is attached with stainless steel microwave resonance inner chamber using quartz glass or polyfluortetraethylene plate
Sealing.
As microwave Thermgravimetric Analysis Apparatus of the invention and a kind of preferred scheme of combined system, the infrared radiation thermometer peace
Mounted in the rear side of microwave resonance inner chamber, highly it is consistent with reactor center, and using programmable logic controller (PLC) PLC controls
The power output of microwave generator, realizes that temperature programming regulates and controls.
As microwave Thermgravimetric Analysis Apparatus of the invention and a kind of preferred scheme of combined system, the microwave resonance inner chamber
Shell from being stainless steel casing, its internal each the week side of boss is provided with high-temperature-resistant thermal-insulation material, high-temperature-resistant thermal-insulation material it is hollow in
The size in portion is more than the reactor.
Further, the high-temperature-resistant thermal-insulation material includes one kind of ceramic fibre and high-purity quartz cotton.
As a kind of preferred scheme of microwave Thermgravimetric Analysis Apparatus of the invention and combined system, the electronic balance and electricity
Brain record system is connected, and recording frequency is 50~100ms/ times, and precision is 0.0001g.
As microwave Thermgravimetric Analysis Apparatus of the invention and a kind of preferred scheme of combined system, the microwave resonance inner chamber
Top sets protective gas passage, and protective gas can avoid electronic balance weighing system from being subjected to external air flow to be influenceed, the guarantor
Shield gas includes one or more mixed gas in air, nitrogen, argon gas and carbon dioxide.
Used as microwave Thermgravimetric Analysis Apparatus of the invention and a kind of preferred scheme of combined system, the reactor is quartz
Reaction bulb, the quartz reaction bottle is sealing system, is connected with reacting gas pipeline and outlet conduit by negative and positive ground respectively,
Insulating tube is provided with outside the outlet conduit, the temperature range of insulating tube is 250~300 DEG C.
As microwave Thermgravimetric Analysis Apparatus of the invention and a kind of preferred scheme of combined system, the import of the reactor
It is connected with gas mass flow gauge, heat analysis atmosphere is included in air, oxygen, nitrogen, carbon monoxide, carbon dioxide and methane
One kind, throughput is 30~200ml/min.
As microwave Thermgravimetric Analysis Apparatus of the invention and a kind of preferred scheme of combined system, the reactor outlet
After gas is through threeway valve regulating flow, into combination analysis system, the combination analysis system includes infrared spectrum analyser and mass spectrum
One or two in analyzer, its data is connected with computer analysis system.
As described above, microwave Thermgravimetric Analysis Apparatus of the invention and combined system, have the advantages that：
1) material filling is in sealing quartz reaction bottle, it is to avoid emergent gas is condensed in microwave cavity, pollutes waveguide
Outlet and infrared measurement of temperature instrument probe, the life-span of extension device.
2) microwave resonance inner chamber is interconnected by aperture with space where electronic balance, is passed through protective gas, it is to avoid electricity
Sub- balance weighs system and is subjected to external air flow influence, improves the accuracy of measurement.
3) microwave thermogravimetric is combined with analysis system, while material weightlessness information is obtained, emergent gas is constituted
Analysis and test, there is provided more abundant material composition information.
4) reasonable in design of the present invention, easy to operate, high degree of automation.
Brief description of the drawings
Fig. 1 is shown as the structural representation of microwave Thermgravimetric Analysis Apparatus of the invention and combined system.
Fig. 2 be shown as microwave Thermgravimetric Analysis Apparatus of the invention and combined system bowing using microwave Thermgravimetric Analysis Apparatus
Depending on structural representation.
Component label instructions
101 protective gas steel cylinders
102 gas flowmeters
103 reacting gas steel cylinders
104 gas flowmeters
105 protective gas passages
The shell of 106 microwave resonance inner chambers
107 microwave resonance inner chambers
108 waveguide outlets
109 high-temperature-resistant thermal-insulation materials
110 reactors
111 gas connection pipes
112 insulating tubes
113 supports
114 electronic balances
115 triple valves
116 combination analysis systems
117 computers
118 infrared radiation thermometers
119 microwave generators
Specific embodiment
Embodiments of the present invention are illustrated below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages of the invention and effect easily.The present invention can also be by specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
Refer to Fig. 1~Fig. 2.It should be noted that the diagram provided in the present embodiment only illustrates this in a schematic way
The basic conception of invention, package count when only display is with relevant component in the present invention rather than according to actual implementation in illustrating then
Mesh, shape and size are drawn, and the kenel of each component, quantity and ratio can be a kind of random change during its actual implementation, and its
Assembly layout kenel is likely to increasingly complex.
Embodiment 1
Fig. 1 is shown as the structural representation of microwave Thermgravimetric Analysis Apparatus of the invention and combined system.Fig. 2 is shown as this hair
Bright microwave Thermgravimetric Analysis Apparatus use the top view of microwave Thermgravimetric Analysis Apparatus with combined system.Specifically, 101 is protection
Gas bomb, 102 is gas flowmeter, and 103 is reacting gas steel cylinder, and 104 is gas flowmeter, and 105 is protective gas passage,
106 is the shell of microwave resonance inner chamber, and 107 is microwave resonance inner chamber, and 108 is waveguide outlet, and 109 is high-temperature-resistant thermal-insulation material
109,110 is reactor (quartz reaction bottle), and 111 is reacting gas pipeline, and 112 is outlet insulating tube, and 113 is support (stone
English support), 114 is precision electronic balance, and 115 is triple valve, and 116 is combination analysis system, and 117 is computer, and 118 is infrared survey
Wen Yi, 119 is microwave generator.
The present invention carries out heat analysis using heating using microwave to material, with the real time record material thermal histories of electronic balance 114
In mass change, while carry out on-line analysis to emergent gas in heat analysis, to obtain more materials composition information.
As shown in Fig. 1~Fig. 2, the present embodiment provides a kind of microwave Thermgravimetric Analysis Apparatus and combined system, including：Microwave is humorous
Shake inner chamber 107, microwave generator 119, infrared radiation thermometer 118, electronic balance 114, support 113, reactor 110, combination analysis
System 116；The microwave generator 119 is arranged at the back of microwave resonance inner chamber 107, by waveguide that microwave transmission is humorous to microwave
Shake inner chamber 107；The infrared radiation thermometer 118 is arranged in microwave resonance inner chamber 107, the temperature of real-time monitoring sample, is adjusted micro-
The power output of wave producer 119；The bottom of microwave resonance inner chamber 107 opens up through hole, the support 113 through the through hole with
Bottom electronic balance 114 is connected, and the top of support 113 is stretched into microwave resonance inner chamber 107, and is provided with reactor 110, described anti-
The outlet of device 110 is answered through microwave resonance inner chamber 107, by the sample introduction pipeline of access combination analysis system 116 after valve shunting,
Carry out on line real time.
As an example, the outlet of the waveguide is slightly above the center of reactor 110, and use quartz glass or poly- four
PVF plate is attached sealing with stainless steel microwave resonance inner chamber 107.
As an example, the infrared radiation thermometer 118 is arranged on the rear side of microwave resonance inner chamber 107, with the center of reactor 110
Highly it is consistent, and the power output of microwave generator 119 is controlled using programmable logic controller (PLC) PLC, realizes program liter
Temperature regulation and control.
As an example, it is stainless steel casing 106 that the shell 106 of the microwave resonance inner chamber 107 is selected, its internal each the week side of boss
High-temperature-resistant thermal-insulation material 109 is provided with, the size of the hollow inside of high-temperature-resistant thermal-insulation material 109 is more than the reactor 110.Enter one
Step ground, the high-temperature-resistant thermal-insulation material 109 includes one kind of ceramic fibre and high-purity quartz cotton.
As an example, the electronic balance 114 is connected with the record system of computer 117, recording frequency is 50~100ms/ times,
Precision is 0.0001g.
As an example, the top of the microwave resonance inner chamber 107 sets protective gas passage 105, protective gas can be avoided
The weighing system of electronic balance 114 is subjected to external air flow influence, and the protective gas includes air, nitrogen, argon gas and carbon dioxide
In one or more mixed gas.
As an example, the reactor 110 is quartz reaction bottle, the quartz reaction bottle is sealing system, is passed through respectively
Negative and positive ground is connected with reacting gas pipeline 111 and outlet conduit, and insulating tube 112, insulating tube are provided with outside the outlet conduit
112 temperature range is 250~300 DEG C.
As an example, the import of the reactor 110 is connected with gas mass flow gauge, heat analysis atmosphere include air,
One kind in oxygen, nitrogen, carbon monoxide, carbon dioxide and methane, throughput is 30~200ml/min.
As an example, after the gas of the outlet of the reactor 110 is through the regulation flow of triple valve 115, into combination analysis system
System 116, the combination analysis system 116 includes one or two in infrared spectrum analyser and mass spectrometer, its data and electricity
The analysis system of brain 117 is connected.
Specifically, microwave generator 119 is arranged on device back, by waveguide by microwave transmission to stainless steel microwave resonance
Inner chamber 107, waveguide outlet 108 is slightly above material center position, and micro- with stainless steel using quartz glass or polyfluortetraethylene plate
Wave resonance inner chamber 107 is attached sealing.Microwave input power is 0~5kW, using PLC controls, microwave output power and temperature
Curve links, power output real-time change, to ensure that actual temperature meets scenario earthquake.Infrared radiation thermometer 118 is arranged on
The rear side of stainless steel microwave resonance inner chamber 107, with quartz reaction bottle centre-height be consistent, using PLC control temperature with it is micro-
Ripple power output, realizes that temperature programming regulates and controls.The temperature range of infrared radiation thermometer 118 is 0~1200 DEG C, infrared focal length 20cm,
Spot size is 10~15mm.
High temperature resistant hollow heat insulating brick is provided with inside stainless steel microwave resonance inner chamber 107, its boring size is more anti-than quartz
Answer bottle bigger, material is ceramic fibre or high-purity quartz cotton.The bottom of stainless steel microwave resonance inner chamber 107 opens up aperture, uses
Hollow quartzy pipe holder is connected with electronic balance 114, and cantilever tip places quartz reaction bottle, and quartz holder pipe external diameter is less than stainless
Steel small hole at bottom part internal diameter.The quality test of electronic balance 114 is connected with the record system of computer 117, and recording frequency is 84ms/ times, essence
It is 0.0001g to spend.The top of stainless steel microwave resonance inner chamber 107 sets protective gas passage 105, and bottom is by aperture and electronics day
Flat 114 place spaces are interconnected, and use air as protective gas, and flow is 100ml/min, to avoid electronic balance 114
Weighing system is subjected to external air flow influence.
Weigh a certain amount of material and be placed in quartz reaction bottle, quartz reaction bottle is sealing system, by negative and positive ground and gas
Body pipeline is connected, and insulating tube 112 is provided with outside outlet conduit, and the temperature of insulating tube 112 is 250 DEG C.Quartz reaction bottle import with
Gas mass flow gauge is connected, and heat analysis atmosphere is oxygen, and throughput is 50ml/min.Microwave thermal reppears gas through triple valve
After 115 regulation flows, into infrared spectrum analyser, its data is connected with the analysis system of computer 117, then carries out post processing calculating.
Embodiment 2
The present embodiment provides a kind of microwave Thermgravimetric Analysis Apparatus and combined system, and heat point is carried out to material using heating using microwave
Analysis, with the mass change in the real time record material thermal histories of electronic balance 114, while being carried out to emergent gas in heat analysis
Line analysis, to obtain more material composition information.
Specifically, the microwave Thermgravimetric Analysis Apparatus include with combined system：Microwave generator 119 is carried on the back installed in device
Portion, by waveguide by microwave transmission to stainless steel microwave resonance inner chamber 107, waveguide outlet 108 is slightly above material center position, and
Sealing is attached with stainless steel microwave resonance inner chamber 107 using quartz glass or polyfluortetraethylene plate.Microwave input power is 0
~5kW, using PLC controls, microwave output power links with temperature curve, power output real-time change, to ensure actual temperature
Meet scenario earthquake.Infrared radiation thermometer 118 is arranged on the rear side of stainless steel microwave resonance inner chamber 107, with quartz reaction bottle
Centre-height is consistent, and temperature and microwave output power are controlled using PLC, realizes that temperature programming regulates and controls.Infrared radiation thermometer 118
Temperature range be 0~1200 DEG C, infrared focal length 20cm, spot size be 10~15mm.
High temperature resistant hollow heat insulating brick is provided with inside stainless steel microwave resonance inner chamber 107, its boring size is more anti-than quartz
Answer bottle bigger, material is ceramic fibre or high-purity quartz cotton.The bottom of stainless steel microwave resonance inner chamber 107 opens up aperture, uses
Hollow quartzy pipe holder is connected with electronic balance 114, and cantilever tip places quartz reaction bottle, and quartz holder pipe external diameter is less than stainless
Steel small hole at bottom part internal diameter.The quality test of electronic balance 114 is connected with the record system of computer 117, and recording frequency is 84ms/ times, essence
It is 0.0001g to spend.The top of stainless steel microwave resonance inner chamber 107 sets protective gas passage 105, and bottom is by aperture and electronics day
Flat 114 place spaces are interconnected, and it is protective gas to employ nitrogen as, and flow is 100ml/min, to avoid electronic balance 114
Weighing system is subjected to external air flow influence.
Weigh a certain amount of material and be placed in quartz reaction bottle, quartz reaction bottle is sealing system, by negative and positive ground and gas
Body pipeline is connected, and insulating tube 112 is provided with outside outlet conduit, and the temperature range of insulating tube 112 is 300 DEG C.Quartz reaction bottle enters
Mouth is connected with gas mass flow gauge, and heat analysis atmosphere is carbon monoxide, and throughput is 200ml/min.Microwave thermal is reppeared implication
After body is through the regulation flow of triple valve 115, into mass spectrometer, its data is connected with the analysis system of computer 117, then place after carrying out
Reason is calculated.
As described above, microwave Thermgravimetric Analysis Apparatus of the invention and combined system, have the advantages that：
1) material filling is in sealing quartz reaction bottle, it is to avoid emergent gas is condensed in microwave cavity, pollutes waveguide
Outlet 108 is popped one's head in infrared radiation thermometer 118, the life-span of extension device.
2) microwave resonance inner chamber 107 is interconnected by aperture with the place space of electronic balance 114, is passed through protective gas,
Avoiding the weighing system of electronic balance 114 from being subjected to external air flow influences, and improves the accuracy of measurement.
3) microwave thermogravimetric is combined with analysis system, while material weightlessness information is obtained, emergent gas is constituted
Analysis and test, there is provided more abundant material composition information.
4) reasonable in design of the present invention, easy to operate, high degree of automation.
So, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
The personage for knowing this technology all can carry out modifications and changes under without prejudice to spirit and scope of the invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
Into all equivalent modifications or change, should be covered by claim of the invention.
Claims (10)
1. a kind of microwave Thermgravimetric Analysis Apparatus and combined system, it is characterised in that including：Microwave resonance inner chamber, microwave generator,
Infrared radiation thermometer, electronic balance, support, reactor, combination analysis system；The microwave generator is arranged at microwave resonance inner chamber
Back, by waveguide by microwave transmission to microwave resonance inner chamber；The infrared radiation thermometer is arranged in microwave resonance inner chamber, in real time
The temperature of sample is monitored, microwave generator power output is adjusted；The microwave resonance intracavity bottom opens up through hole, and the support is worn
Cross the through hole to be connected with bottom electronic balance, frame upper is stretched into microwave resonance inner chamber, and be provided with reactor, it is described anti-
Answer the outlet of device through microwave resonance inner chamber, the sample introduction pipeline by accessing combination analysis system after valve shunting is carried out online
Analysis in real time.
2. microwave Thermgravimetric Analysis Apparatus according to claim 1 and combined system, it is characterised in that：The outlet of the waveguide
The slightly above center of reactor, and connected with stainless steel microwave resonance inner chamber using quartz glass or polyfluortetraethylene plate
Connect sealing.
3. microwave Thermgravimetric Analysis Apparatus according to claim 1 and combined system, it is characterised in that：The infrared radiation thermometer
Installed in the rear side of microwave resonance inner chamber, highly it is consistent with reactor center, and using programmable logic controller (PLC) PLC controls
The power output of microwave generator processed, realizes that temperature programming regulates and controls.
4. microwave Thermgravimetric Analysis Apparatus according to claim 1 and combined system, it is characterised in that：In the microwave resonance
From being stainless steel casing, its internal each the week side of boss is provided with high-temperature-resistant thermal-insulation material to the shell in chamber, high-temperature-resistant thermal-insulation material it is hollow
Internal size is more than the reactor.
5. microwave Thermgravimetric Analysis Apparatus according to claim 4 and combined system, it is characterised in that：The high-temperature-resistant thermal-insulation
Material includes one kind of ceramic fibre and high-purity quartz cotton.
6. microwave Thermgravimetric Analysis Apparatus according to claim 1 and combined system, it is characterised in that：The electronic balance with
Computer record system is connected, and recording frequency is 50~100ms/ times, and precision is 0.0001g.
7. microwave Thermgravimetric Analysis Apparatus according to claim 1 and combined system, it is characterised in that：In the microwave resonance
Top of chamber sets protective gas passage, and protective gas can avoid electronic balance weighing system from being subjected to external air flow to be influenceed, described
Protective gas includes one or more mixed gas in air, nitrogen, argon gas and carbon dioxide.
8. microwave Thermgravimetric Analysis Apparatus according to claim 1 and combined system, it is characterised in that：The reactor is stone
English reaction bulb, the quartz reaction bottle is sealing system, is connected by negative and positive ground and reacting gas pipeline and outlet conduit respectively
Connect, insulating tube is provided with outside the outlet conduit, the temperature range of insulating tube is 250~300 DEG C.
9. microwave Thermgravimetric Analysis Apparatus according to claim 1 and combined system, it is characterised in that：The reactor enters
Mouth is connected with gas mass flow gauge, and heat analysis atmosphere is included in air, oxygen, nitrogen, carbon monoxide, carbon dioxide and methane
One kind, throughput be 30~200ml/min.
10. microwave Thermgravimetric Analysis Apparatus according to claim 1 and combined system, it is characterised in that：The reactor goes out
Mouthful gas through threeway valve regulating flow after, into combination analysis system, the combination analysis system include infrared spectrum analyser and
One or two in mass spectrometer, its data is connected with computer analysis system.
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| CN108380155A (en) * | 2018-05-03 | 2018-08-10 | 山东大学 | Study microwave and the interactive experimental system of medium and application under multiple physical field |
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| CN108680458A (en) * | 2018-08-14 | 2018-10-19 | 青岛迈可威微波创新科技有限公司 | Microwave Thermgravimetric Analysis Apparatus |
| CN108680458B (en) * | 2018-08-14 | 2024-02-27 | 青岛迈可威微波创新科技有限公司 | Microwave thermogravimetric analysis device |
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| CN110514282A (en) * | 2019-09-23 | 2019-11-29 | 华北电力大学（保定） | A kind of movement state response sample quality interval on-line measurement device |
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| CN111929193A (en) * | 2020-09-02 | 2020-11-13 | 辽宁科技大学 | Dielectric barrier discharge low-temperature plasma thermal balance and working method thereof |
| CN112432876A (en) * | 2020-11-17 | 2021-03-02 | 中广核工程有限公司 | Thermal degradation experimental system and thermal degradation testing method for radioactive waste |
| CN115452882A (en) * | 2022-08-10 | 2022-12-09 | 山东大学 | Device and method for measuring bulk temperature of sample in microwave field |
| CN115452543A (en) * | 2022-09-21 | 2022-12-09 | 中国原子能科学研究院 | Rapid preprocessing device and method for total alpha and beta measurement |
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