CN109827865A - Materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments - Google Patents
Materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments Download PDFInfo
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- 238000004817 gas chromatography Methods 0.000 claims abstract description 18
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000005070 sampling Methods 0.000 claims abstract description 6
- 230000004580 weight loss Effects 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 56
- 239000012495 reaction gas Substances 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- -1 battery electrode Substances 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 claims description 6
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 5
- 229910052734 helium Inorganic materials 0.000 claims description 5
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 238000002411 thermogravimetry Methods 0.000 claims description 5
- 229910000619 316 stainless steel Inorganic materials 0.000 claims description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 4
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 239000003245 coal Substances 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000004451 qualitative analysis Methods 0.000 claims description 3
- 238000004445 quantitative analysis Methods 0.000 claims description 3
- 230000006641 stabilisation Effects 0.000 claims description 3
- 238000011105 stabilization Methods 0.000 claims description 3
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 2
- 241000208125 Nicotiana Species 0.000 claims description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 2
- 239000012620 biological material Substances 0.000 claims description 2
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- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 2
- 238000007405 data analysis Methods 0.000 claims description 2
- 238000004079 fireproofing Methods 0.000 claims description 2
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910052754 neon Inorganic materials 0.000 claims description 2
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- 239000001272 nitrous oxide Substances 0.000 claims description 2
- 239000004033 plastic Substances 0.000 claims description 2
- 229920003023 plastic Polymers 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 239000001294 propane Substances 0.000 claims description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
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- 229910052724 xenon Inorganic materials 0.000 claims description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims 1
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- 238000011065 in-situ storage Methods 0.000 description 2
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- 206010044565 Tremor Diseases 0.000 description 1
- GCNLQHANGFOQKY-UHFFFAOYSA-N [C+4].[O-2].[O-2].[Ti+4] Chemical compound [C+4].[O-2].[O-2].[Ti+4] GCNLQHANGFOQKY-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
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- UKACHOXRXFQJFN-UHFFFAOYSA-N heptafluoropropane Chemical compound FC(F)C(F)(F)C(F)(F)F UKACHOXRXFQJFN-UHFFFAOYSA-N 0.000 description 1
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention discloses materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments, described device includes controllable temperature admission line, mass flow controller, solenoid valve, pressure-control valve, thermogravimetric analyzer, controllable temperature exhaust line, sample introduction clack box, gas chromatography combined with mass spectrometry device, data acquisition unit and computer.Wherein, sampling valve case includes six-way valve, heating unit, quantitative loop, sample introduction adapter.Pass through this device, can qualitative and quantitative reaction and pyrolysis weight loss situation of the research material under different temperatures, pressure and atmosphere, and can in on-line analysis reaction process institute's escaping gas, structure it is reliable, it is easy to operate, equipment support is provided for materials pyrolysis mechanism under research particular surroundings.
Description
Technical field
The present invention relates to the technical fields of materials pyrolysis analytical equipment, and in particular to material under a kind of more atmosphere hyperbaric environments
It is pyrolyzed on-line analysis device.
Background technique
Thermogravimetric analysis by measure material quality under specific temperature program change with time, come research material composition,
A kind of analysis method of phase transition, thermal stability and reaction mechanism is widely used in various inorganic, organic material grind
In studying carefully.In order to further research material composition and Thermal Decomposition Mechanism, thermogravimetric analyzer often with other analytical equipments, such as differential scanning
The combination such as calorimeter, Fourier infrared spectrograph, mass spectrograph, carries out the comprehensive analysis of material property.
Existing Thermogravimetric analysis mostly under normal pressure analyzes the pyrolysis of substance, in addition to protecting gas, general
It is passed through a kind of reaction gas.And produce in practice, such as the energy, chemical industry, metallurgy, aerospace field reaction environment are complicated, very
It is directed to hyperbaric environment more；Special reaction environment and reaction product accurately on-line analysis to material thermal stability and reaction
The further investigation of mechanism is of great significance, and existing analytical equipment is not able to satisfy actual demand.
Chinese patent CN101692076A discloses a kind of based on the suction on-line analysis of the simulated combustion of cigarettes of infra-red furnace and GC-MS
Method and device carries out on-line analysis to materials pyrolysis product using the environment of two-way atmosphere normal pressure, cannot provide material and exist
The variation of weight in pyrolytic process, can not further investigate reaction mechanism.Chinese patent CN101692031A discloses utilization
Thermogravimetric analyzer and GC/MS realize simulated combustion of cigarettes on-line analysis and its device, and thermogravimetric analyzer and GC/MS are joined
With, it solving cracking instrument analysis and uses sample size small, cracking atmosphere can only be indifferent gas, the problem of quantitative inaccuracy, but its
It is only to introduce oxygen all the way more, and reaction pressure not can control, and pyrolysis product heats desorption sample introduction by condensing trapping, is condensing
In heating process, unpredictalbe variation may occur for the physicochemical properties of gas, cannot reach on-line analysis in situ
Purpose.Chinese patent CN102109446A discloses the method and pressurized TGA of control thermobalance analyzer reaction gas channelling
Analyzer, this analyzer can control the pressure of reaction gas to reach 50atm, can be used for the special atmospheres such as vapor, and prevent anti-
It answers has channeling to enter balance and causes the shakiness of balance, but can not achieve multiple atmosphere while being passed through the high pressure pyrolytic reaction of condition, gas
Body is passed through flow and not can control, and pyrolysis evolution gas cannot be analyzed in real time, cumbersome.Chinese patent CN104614272B is public
The high-temperature pressurizing thermobalance and application method opened, this device are passed through inert gas using protection gas and pressurising mouth to meet experiment pressure
Power controls pressure by pressure regulator valve, and pressure control range is narrow, and only from normal pressure to 4Mpa, reaction atmosphere is not able to satisfy more
Road gas is passed through simultaneously, is passed through gas flow and is unable to control, the product of thermal decomposition also can not on-line analysis, experimentation is complicated.
Chinese patent CN105136601A discloses a kind of high-temperature field and the static coupling device analog material of complicated atmosphere exists
High-temperature behavior under controllable a variety of oxidations and aggressive atmosphere environment, this device provide only a high mild oxidation or corrosion
Atmospheric condition research material high-temperature oxidation resistant, resistance to corrosion, balance design and have protection gas thermogravimetric analysis balance phase
It is poorer than stability, it is unable to the pyrolysis problem of analysis of material, evolution gas etc. can not be also further analyzed.Document (Wang Yonggang,
Force, which is practiced, increases the Shanxi high temperature and pressure thermogravimetric device [J] the chemical industry that is used for coal gasification dynamics research, 1989 (2): 25-26；Xu Yue
Year high pressure TGA instrument [J] instrument and meter and research and application, 1995 (1): 36-37) high pressure Thermgravimetric Analysis Apparatus is reported, these
The problems such as device there is adjustable pressure limit is narrow, the reaction atmosphere of experiment is few, cannot be to thermal decomposition product on-line analysis.
Limitation present in existing equipment can not meet simultaneously in more atmosphere, special reaction atmosphere (such as easy liquefied gas)
Accurate in-situ study, integration of equipments are carried out to materials pyrolysis response characteristic and evolution gas physicochemical property under the conditions of reaction under high pressure
Change degree is low, complicated for operation.
Summary of the invention
The purpose of the invention is to meet the pyrolytic reaction mechanism practical study demand to material, analog material is in reality
Pyrolytic process under the more atmosphere reaction environments of border high pressure, and product can be analyzed in real time and a kind of more atmosphere high pressures for proposing
Materials pyrolysis on-line analysis device under environment.
To achieve the goals above, the technical solution adopted in the present invention is as follows:
Materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments, described device include controllable temperature admission line,
Mass flow controller, solenoid valve, pressure-control valve, thermogravimetric analyzer, controllable temperature exhaust line, sample introduction clack box, gas-chromatography
Mass spectrometry device, data acquisition unit and computer；
The controllable temperature admission line, the air supply pipe all the way including reaction gas three road gas supply lines and protective gas
Line；Reaction gas weighs in thermogravimetric analysis instrument for providing the multiple atmosphere environment of materials pyrolysis, protective gas for protecting
The stabilization of balance；
The mass flow controller is installed on thermogravimetric analyzer controllable temperature admission line, by control solenoid valve come
The flow of gas in control piper；
Pressure-control valve is housed on controllable temperature exhaust line, reaction pressure can be monitored, form the height of reaction environment
Press strip part；
The thermogravimetric analyzer is used to provide the weighing of pyrolysis generating device and material weight loss, and pyrolysis furnace body can be born
10Mpa high pressure；
The controllable temperature exhaust line escapes the pipe that gas enters gas chromatography combined with mass spectrometry device after providing materials pyrolysis
Road；
The sampling valve case includes six-way valve, heating unit, quantitative loop, sample introduction adapter, and six-way valve is controllable with quantitative loop
System enters the sample injection time and sample volume of gas chromatography combined with mass spectrometry device emergent gas, by adapter by pipeline and gas phase color
Compose shunting/Splitless injecting samples mouth matching of mass spectrometry device；
The gas chromatography combined with mass spectrometry device is used for qualitative and quantitative analysis emergent gas physicochemical properties；
The data acquisition unit, for line pressure, flow, temperature value and equipment operation feelings in acquisition and recording device
Condition, computer is by controlling parameter compared with setting value；
The computer is for providing device software operation control platform and data analysis function.
The controllable temperature admission line is high pressure resistant and corrosion 1/8 inch of 316 stainless steel tube, controllable temperature exhaust line
For high pressure resistant and corrosion 1/16 inch of 316 stainless steel tube, the sample introduction adapter is that 1/16 inch pipe turns shunt/not to be diverted into
The sample introduction needle adapter of sample mouth.
The controllable temperature inlet and outlet pipeline is wrapped with heating tape, and highest is controllable to be heated to 300 DEG C.Air inlet pipeline
The purpose of controllable temperature is, if the reaction gas boiling point being passed through is higher, into unheated pipeline after can liquefy；Exhaust line
The purpose of controllable temperature is that pipeline of the evolution gas through being subcooled for preventing pyrolysis from generating is agglomerated on tube wall, causes subsequent analysis result
Inaccuracy.
Six-way valve and pipeline package heating tape in the sample introduction clack box, 300 DEG C of temperature controllable highest.Control temperature
Purpose is that the evolution gas for preventing pyrolysis from generating is enriched on tube wall.
The maximum temperature that the thermogravimetric analyzer can be provided pyrolytic reaction is 1100 DEG C.
The pressure limit that the device can control is normal pressure -8Mpa.
The protective gas is one of nitrogen, helium or argon gas.
The protection gas and reaction gas charge flow rate control range is 0-200mL/min.
Heretofore described reaction gas includes but is not limited to air, argon gas, carbon monoxide, carbon dioxide, ethane, second
Alkene, helium, hydrogen sulfide, methane, neon, nitrogen, nitrous oxide, oxygen, propane, propylene, sulfur dioxide, xenon, extinction using gas
Imperial (1211,1301 etc.) extinguishing chemical etc. is breathed out in agent, such as heptafluoro-propane.
The material of heretofore described pyrolysis analysis include but is not limited to timber, tobacco, coal, rock, biological material,
Plastics, battery electrode, metal product, heat preservation and fire proofing, dry powder fire extinguishing agent etc..
Thermogravimetric analyzer can provide heating rate range in the present invention: 0.1-250 DEG C/min, weighing the biggest quality is
500mg, the balance of thermogravimetric analyzer are magnetic suspension balance.Gas chromatography combined with mass spectrometry device is single level four bars gaschromatographic mass spectrometry
Combined instrument.
Compared with prior art, the present invention its advantage is as follows:
1, controllable temperature, control flow three road supply air lines be able to achieve pyrolysis of the material under multiple atmosphere.
2, be able to achieve normal pressure to 8MPa pressure limit accurate heat analysis.
3, thermal decomposition product can be accurately controlled to the sample injection time and sample volume of gaschromatographic mass spectrometry, gas-chromatography can be to this
Thermal decomposition product efficiently separates under part, and mass spectrograph can precisely analyze its physicochemical properties.
4, integration degree is high for device, easy to operate.
Detailed description of the invention
Fig. 1 is materials pyrolysis on-line analysis apparatus structure schematic diagram under a kind of more atmosphere hyperbaric environments of the invention.
Fig. 2 is flow chart of the invention.
Fig. 3 is six-way valve sample states schematic diagram in sample introduction clack box.
Fig. 4 is six-way valve sample introduction state principle figure in sample introduction clack box.
In figure, 1 is controllable temperature admission line；2 be mass flow controller；3 be solenoid valve；4 be thermogravimetric analyzer；5 are
Controllable temperature exhaust line；6 be pressure-control valve；7 be sample introduction clack box；8 be six-way valve；9 be sample introduction adapter；10 be gas-chromatography
Shunting/Splitless injecting samples mouth；11 be gas chromatography combined with mass spectrometry device；12 be gas discharge pipe line；13 be carrier gas line；14 are
Data acquisition unit；15 be computer；16 be quantitative loop.
Specific embodiment
Referring to the drawings and specific embodiment invention is further explained.
As shown in Figure 1, materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments of the invention, including controllable temperature
Admission line 1, mass flow controller 2, solenoid valve 3, thermogravimetric analyzer 4, controllable temperature exhaust line 5, pressure-control valve 6, into
Sample clack box 7, gas chromatography combined with mass spectrometry device 11, data acquisition unit 14 and computer 15.Above-mentioned various pieces pass through electricity
Gas cable and gas piping connect into a set of analytical equipment.
As shown in Fig. 2, being put into thermogravimetric analyzer 4 after sample weighing to be analyzed, setting is reacted in the computer 15
Heat tape temperature, temperature program are wrapped up outside pressure, each pipeline flow of air inlet, each pipeline.Reaction condition reaches the condition of setting
Afterwards, start pyrolytic process, material reduced gravity situations record in real time.Thermal decomposition product can enter six-way valve 8 by gas discharge pipe line 12,
According to the weight-loss curve of material, the different time sections that materials pyrolysis occurs are determined to control 8 sample injection time interval of six-way valve, are divided
Stream/not shunt mode can be selected according to specific pyrolytic material sample introduction gas concentration, thermal decomposition product after gas-chromatography separates,
Qualitative and quantitative analysis is carried out into mass spectrum.
Gas transport pipeline in the present invention, including controllable temperature admission line 1, controllable temperature exhaust line 5, sample introduction clack box 7
In six-way valve 8 outer wall be all enclosed with heat tape, control temperature according to the property of reaction gas and pyrolysis emergent gas, prevent
Only its liquefaction is attached on tube wall, and controllable maximum temperature is 300 DEG C, by data acquisition unit 14 and computer 15 to temperature
Control.The flow of three road reaction gas is set by computer 15, mass flow controller 2 and solenoid valve 3 carry out control piper stream
Amount, to realize the reaction atmosphere environment of different ratio.
Materials pyrolysis reaction under high pressure environment is realized by the pressure-control valve 6 in controllable temperature exhaust line 1 in the present invention.?
In pyrolysis procedure setting, reaction pressure is preset, after being passed through reaction gas in the high voltage bearing pyrolysis chamber of thermogravimetric analyzer 4,
Data acquisition unit 14 can acquire pressure data at pressure-control valve 6 in real time, and computer 15 is by actual pressure and preset pressure
Compare, then (pressure is lower than preset pressure, reduces flow of exhaust amount by control pressure-control valve 6；Pressure is higher than preset value,
Then increase flow of exhaust amount) come maintain setting reaction pressure stabilization.
Six-way valve operating mode is as follows in the present invention:
Fig. 3 indicates that six-way valve goes to sample states: the gas of thermogravimetric analyzer discharge is through controllable temperature exhaust line 5 through quantitative
Ring 16 is discharged by gas discharge pipe line 12；Carrier gas in pipeline 13 through sample introduction adapter 9 and shunting/Splitless injecting samples mouth into
Enter gas chromatography combined with mass spectrometry device.
Fig. 4 indicates that six-way valve goes to sample introduction state: carrier gas brings the pyrolysis evolution gas in quantitative loop 16 into gas-chromatography matter
Spectrum combined apparatus is analyzed, and the gas of thermogravimetric analyzer discharge is discharged through gas discharge pipe line 12.
Embodiment 1
The sample for weighing 5-20mg is placed in thermogravimetric analyzer crucible, according to experiment condition, sets the pressure of pyrolytic reaction
Heat tape temperature (room temperature -300 is wrapped up outside (local air pressure -8MPa), each pipeline flow (0-200mL/min) of air inlet, each pipeline
DEG C), pyrolysis temperature program (0.1-250 DEG C of heating rate/min, 1100 DEG C of maximum temperature), reach setting condition in reaction condition
Afterwards, start pyrolytic process, material reduced gravity situations are recorded in real time by data acquisition module.Pyrolysis emergent gas enters six-way valve,
According to the weight-loss curve of material, the different phase of materials pyrolysis is determined, to set the time interval of six-way valve sampling.Quantitative loop
Volume is determined according to materials pyrolysis product gas amount.Thermal decomposition product carries out qualitative, quantitative after gas-chromatography separates, into mass spectrum
Analysis.The sample introduction mode and gas chromatography combined with mass spectrometry device analysis condition of chromatogram arrangement injection port should be according to specific pyrolysis materials
Material and used instrument are determined.
Embodiment 2
Certain the moulded coal powder for weighing 5mg is placed in thermogravimetric analyzer crucible, sets reaction pressure as 5MPa, set protection gas as
Nitrogen, flow 50mL/min, reaction gas are respectively nitrogen, flow 70mL/min, methane, flow 10mL/min, titanium dioxide
Carbon, flow 50mL/min, admission line do not heat, and exhaust line and six-way valve external heat band set temperature are 200 DEG C, are heating up
1000 DEG C are raised under 20 DEG C/min of rate, balances 5min at 1000 DEG C；Six-way valve sampling time interval is 5min, quantitative ring body
Product is 1mL, is analyzed into gas chromatography combined with mass spectrometry device.
Gas chromatography combined with mass spectrometry device imposes a condition:
Chromatographic column: 30m × 0.25mm × 0.25 μm methylsiloxane chromatographic column, 80 DEG C of initial column temperature, with 10 DEG C/min liter
Warm rate keeps 10min to 260 DEG C；280 DEG C of injector temperature, sample introduction mode Splitless injecting samples, sampling volume 1mL；Carrier gas is
Helium, constant current mode, 1mL/min；Ionization mode EI, 275 DEG C of ion source temperature, 280 DEG C of transmission line temperature.
The above is only the preferred embodiment for the present invention, and the scope of the present invention is not limited to the above embodiment, all categories
Technical solution under thinking of the present invention all belongs to the scope of protection of the present invention.
Claims (10)
1. materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments, it is characterised in that: described device includes controllable temperature
Admission line, mass flow controller, solenoid valve, pressure-control valve, thermogravimetric analyzer, controllable temperature exhaust line, sample introduction clack box,
Gas chromatography combined with mass spectrometry device, data acquisition unit and computer；Wherein:
The controllable temperature admission line, the gas supply line all the way of three road gas supply lines and protective gas including reaction gas；
Reaction gas weighs balance for protecting for providing the multiple atmosphere environment of materials pyrolysis, protective gas in thermogravimetric analysis instrument
Stabilization；
The mass flow controller is installed on thermogravimetric analyzer controllable temperature admission line, is controlled by control solenoid valve
The flow of gas in pipeline；
Pressure-control valve is housed on controllable temperature exhaust line, reaction pressure can be monitored, form the high-pressure section of reaction environment
Part；
The thermogravimetric analyzer is used to provide the weighing of pyrolysis generating device and material weight loss, and pyrolysis furnace body can bear height
Pressure；
The controllable temperature exhaust line escapes the pipeline that gas enters combined gas chromatography mass spectrometry device after providing materials pyrolysis；
The sampling valve case includes six-way valve, heating unit, quantitative loop, sample introduction adapter, can control and enters chromatographic mass spectrometry connection
With the sample injection time and sample volume of device emergent gas, and matched with the shunting of combined gas chromatography mass spectrometry device/Splitless injecting samples mouth；
The gas chromatography combined with mass spectrometry device is used for the physicochemical property of qualitative and quantitative analysis emergent gas；
The data acquisition unit, for line pressure, flow, temperature value and equipment operation in acquisition and recording device, meter
Calculation machine is by controlling parameter compared with setting value；
The computer is for providing device software operation control platform and data analysis function.
2. materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments according to claim 1, it is characterised in that:
The controllable temperature admission line is high pressure resistant and corrosion 1/8 inch of 316 stainless steel tube, and controllable temperature exhaust line is high pressure resistant
With 1/16 inch of 316 stainless steel tube of corrosion, the sample introduction adapter be 1/16 inch pipe turn shunting/Splitless injecting samples mouth into
Sample needle adapter.
3. materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments according to claim 1, it is characterised in that:
The controllable temperature inlet and outlet pipeline is wrapped with heating tape, and highest is controllable to be heated to 300 DEG C.
4. materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments according to claim 1, it is characterised in that:
Six-way valve package heating tape in the sample introduction clack box, 300 DEG C of temperature controllable highest.
5. materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments according to claim 1, it is characterised in that:
The maximum temperature that the thermogravimetric analyzer can be provided pyrolytic reaction is 1100 DEG C.
6. materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments according to claim 1, it is characterised in that:
The pressure limit that the device can control is normal pressure -8MPa.
7. materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments according to claim 1, it is characterised in that:
The protective gas is one of nitrogen, helium or argon gas.
8. materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments according to claim 1, it is characterised in that:
The protection gas and reaction gas charge flow rate control range is 0-200mL/min.
9. materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments according to claim 1, it is characterised in that:
The reaction gas can be air, argon gas, carbon monoxide, carbon dioxide, ethane, ethylene, helium, hydrogen sulfide, methane, neon
Gas, nitrogen, nitrous oxide, oxygen, propane, propylene, sulfur dioxide, xenon, gas extinguishing agent.
10. materials pyrolysis on-line analysis device under a kind of more atmosphere hyperbaric environments according to claim 1, feature exist
In: the material for pyrolysis analysis can be timber, tobacco, coal, rock, biological material, plastics, battery electrode,
Metal product, heat preservation and fire proofing, dry powder fire extinguishing agent.
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