CN114544267A - Volatile gas generation detection system - Google Patents
Volatile gas generation detection system Download PDFInfo
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- CN114544267A CN114544267A CN202210139311.0A CN202210139311A CN114544267A CN 114544267 A CN114544267 A CN 114544267A CN 202210139311 A CN202210139311 A CN 202210139311A CN 114544267 A CN114544267 A CN 114544267A
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- 238000001514 detection method Methods 0.000 title claims abstract description 52
- 239000007789 gas Substances 0.000 claims abstract description 137
- 230000007246 mechanism Effects 0.000 claims abstract description 48
- 238000010438 heat treatment Methods 0.000 claims abstract description 38
- 239000011261 inert gas Substances 0.000 claims abstract description 19
- 239000000523 sample Substances 0.000 claims description 94
- 238000007789 sealing Methods 0.000 claims description 57
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 2
- 239000003546 flue gas Substances 0.000 claims description 2
- 230000007423 decrease Effects 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 230000002349 favourable effect Effects 0.000 abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 235000013399 edible fruits Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000000338 in vitro Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- -1 absolutes Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 238000012863 analytical testing Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002161 passivation Methods 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0011—Sample conditioning
- G01N33/0021—Sample conditioning involving the use of a carrier gas for transport to the sensor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N2001/2244—Exhaled gas, e.g. alcohol detecting
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Engineering & Computer Science (AREA)
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- General Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
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- Food Science & Technology (AREA)
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Abstract
The invention relates to the technical field of gas sample collection, in particular to a volatile gas generation and detection system. The generation detection system includes: the system comprises a gas source, a gas inlet pipeline, a sample bottle, a gas exhaust pipeline, a flowmeter and a gas analyzer; wherein, the sample bottle comprises a bottle body and a base which are detachably connected; the top of the bottle body is provided with an air inlet and an air outlet; the upper surface of the base is provided with a sample table, and the base also comprises a heating mechanism for heating the sample table; the gas source is used for providing high-pressure inert gas as a volatile gas conveying carrier; the air inlet pipeline is arranged between the air source and the air inlet; the flowmeter is arranged on the gas inlet pipeline and used for adjusting the gas flow rate; the exhaust pipeline is connected with the exhaust port; the gas analyzer is connected with the exhaust pipeline and is used for detecting the components of the gas in the exhaust pipeline. The volatile gas generation detection system is favorable for realizing the production and collection of all-component volatile gas of a sample, and has high detection precision and high detection speed.
Description
Technical Field
The invention relates to the technical field of gas sample collection, in particular to a volatile gas generation and detection system.
Background
Fragrances such as essential oils, absolutes, extracts, etc. contain a variety of volatile components such as: ethanol, alkane, aromatic gas, etc., which are often related to the type, origin and extraction of the perfume. The generation and collection of these volatile gases is a prerequisite for their analytical testing and is therefore of great importance for the collection and detection of the volatile gases released by the fragrance.
In the related art, chinese patent CN208984419U discloses a volatile gas collecting device for in vitro tissue of fruit plants, which can be used for collecting volatile gas of in vitro tissue of fruit plants. However, in the volatile sample collection process, some low-volatility gases cannot volatilize from the fruits, and the collected samples cannot completely reflect the components of the samples to be detected. How to improve the detection precision of the volatile gas becomes a technical problem to be solved.
Disclosure of Invention
In order to improve the detection precision of the volatile gas, the invention provides a generation detection system of the volatile gas,
the generation detection system provided by the invention comprises: the system comprises a gas source, a gas inlet pipeline, a sample bottle, a gas exhaust pipeline, a flowmeter and a gas analyzer; wherein,
the sample bottle comprises a bottle body and a base which are detachably connected; the top of the bottle body is provided with an air inlet and an air outlet; the upper surface of the base is provided with a sample table, and the base further comprises a heating mechanism for heating the sample table;
the gas source is used for providing high-pressure inert gas as a delivery carrier of volatile gas;
the air inlet pipeline is arranged between the air source and the air inlet; the flowmeter is arranged on the gas inlet pipeline and used for adjusting the gas flow rate;
the exhaust pipeline is connected with the exhaust port;
the gas analyzer is connected with the exhaust pipeline and used for detecting components of gas in the exhaust pipeline.
Further, the device also comprises a first sealing mechanism and/or a second sealing mechanism;
the first sealing mechanism includes: the first sealing cover is in threaded connection with the air inlet; the first sealing cover is provided with a first through hole, and one end of the air inlet pipeline is communicated with the air inlet through the first through hole; the first sealing gasket is arranged between the first sealing cover and the air inlet pipeline;
the second sealing mechanism includes: the second sealing cover is in threaded connection with the exhaust port; the second sealing cover is provided with a second through hole, and one end of the exhaust pipeline is communicated with the exhaust port through the second through hole; the second sealing gasket is arranged between the second sealing cover and the exhaust pipeline.
Further, the upper surface of base is provided with puts the thing recess, it forms to put the thing recess the sample platform, heating mechanism sets up in the below of putting the thing recess.
Further, the device also comprises a temperature control device; the temperature control device includes: temperature acquisition unit and the control unit, the temperature acquisition unit is used for gathering the temperature of putting in the thing recess, the control unit links to each other with temperature acquisition unit and heating mechanism for according to the temperature that the temperature acquisition unit gathered and predetermine the operating condition of temperature control heating mechanism.
Furthermore, the circumferential surface of the base is a frosted conical surface with the size of the section reduced from the bottom end to the top end,
the bottom surface of the bottle body is a frosted circular ring surface; the frosted ring surface of the bottle body is propped against and contacted with the frosted conical surface of the base.
Further, still include: the counterweight mechanism is arranged on the surface of the bottle body; the counterweight mechanism is as follows: a counterweight ring and/or a counterweight; the outer surface of bottle is located along circumference cover to the counter weight circle, the counter weight sets up in the top or circumference of bottle.
Further, still include: connecting the pipeline and the valve component; wherein,
one end of the connecting pipeline is communicated with the air inlet pipeline, and the other end of the connecting pipeline is communicated with the exhaust pipeline;
the valve assembly includes: a first valve, a second valve, and a third valve;
the first valve is arranged on the connecting pipeline;
the second valve is arranged between the air inlet and the connecting pipeline;
the third valve is arranged between the exhaust port and the connecting pipeline.
Further, the gas analyzer is a mass spectrometer, a probe of the mass spectrometer is provided with a capillary tube, one end of the capillary tube extends into the flue gas pipeline, and the other end of the capillary tube is inserted into the probe.
Further, the capillary has an inner diameter of 530 μm, a total length of 30.0cm, and a length of 22.6cm extending into the probe head.
Further, the inner wall of the sample bottle is subjected to passivation treatment or is provided with a quartz liner tube.
From the above, the system for generating and detecting volatile gas provided by the invention has the following advantages:
1. the system is provided with the gas source as a volatile gas conveying carrier, and gas with a relatively small volatilization amount can be discharged from the sample bottle to be detected under the current-carrying effect of the high-pressure inert gas, so that the accuracy of a detection result is improved.
2. The base of the sample bottle can be detached and is provided with a sample table and a heating mechanism. On one hand, the heating mechanism can accelerate the volatilization rate of volatile components in the sample and improve the detection efficiency; on the other hand, for the components with low volatility, the components can be fully volatilized to form volatile gas which is carried to the exhaust pipeline by the high-pressure inert gas to be detected in a heating mode, so that the production and collection of the volatile gas of all the components of the sample are facilitated, and the detection precision of the system is improved. Finally, heating mechanism still is favorable to forming the hot air in the bottom of sample bottle, drives volatile gas and rises together, then is taken away rapidly by the high-pressure inert gas who flows through and enters into exhaust pipe in, and the effectual volatile gas of avoiding remains in the sample bottle bottom, makes from this that the bottle of sample bottle also can not cause the influence to the detection precision with the base is incomplete sealed, guarantees the detection precision when realizing making things convenient for the application of sample promptly.
In conclusion, the volatile gas generation and detection system provided by the invention is beneficial to realizing the production and collection of all-component volatile gas of a sample, and has high detection precision and high detection speed.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent by describing in more detail exemplary embodiments thereof with reference to the attached drawings, in which like reference numerals generally represent like parts throughout.
FIG. 1 is a schematic diagram of a volatile gas generation and detection system according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of another embodiment of the present invention showing the structure of a volatile gas generation and detection system;
fig. 3 is a schematic diagram of the connection between the mass spectrometer and the exhaust pipeline and the internal structure of the detection head of the mass spectrometer in another embodiment of the invention.
Description of the reference numerals
1-gas source
2-air inlet pipeline
3-sample bottle
31-bottle body
311-air intake
312-exhaust port
32-base
321-sample stage
322-heating mechanism
4-exhaust line
5-flow meter
6-gas analyzer
71-first sealing cover
72-second sealing cover
81-first sealing gasket
82-second sealing gasket
91-capillary tube
92-probe head
93-ion source
10-connecting line
S1-first valve
S2-second valve
S3-third valve
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in this specification and the appended claims, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It should also be understood that the term "and/or" as used herein refers to and encompasses any and all possible combinations of one or more of the associated listed items.
It should be understood that although the terms "first", "second", "third", etc. may be used herein to describe various information, these information should not be limited to these terms. These terms are only used to distinguish one type of information from another. For example, first information may also be referred to as second information, and similarly, second information may also be referred to as first information, without departing from the scope of the present invention. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
In order to improve the detection accuracy of the volatile gas of the sample, an embodiment of the present invention provides a system for generating and detecting a volatile gas, please refer to fig. 1, the system includes: the device comprises a gas source 1, a gas inlet pipeline 2, a sample bottle 3, a gas exhaust pipeline 4, a flowmeter 5 and a gas analyzer 6; wherein,
the sample bottle 3 comprises a bottle body 31 and a base 32 which are detachably connected; the top of the bottle body 31 is provided with an air inlet 311 and an air outlet 312; a sample stage 321 is arranged on the upper surface of the base 32, and the base 32 further comprises a heating mechanism 322 for heating the sample stage 321;
the gas source 1 is used for providing high-pressure inert gas as a delivery carrier of volatile gas;
the air inlet pipeline 2 is arranged between the air source 1 and the air inlet 311; the flow meter 5 is arranged on the air inlet pipeline 2 and is used for adjusting the flow rate of the gas;
the exhaust pipeline 4 is connected with an exhaust port 312;
the gas analyzer 6 is connected to the exhaust line 4 for detecting the composition of the gas in the exhaust line 4.
The working process of the volatile gas generation detection system provided by the embodiment is as follows:
placing the sample on the sample stage 321 of the base 32 of the sample bottle 3, and installing the base 32 at the bottom of the bottle body 31; turning on the heating mechanism 322; after the volatile gas of the sample is diffused and balanced, opening the gas source 1 and the flowmeter 5; inert gas discharged by a gas source 1 enters a sample bottle 3 through a gas inlet pipeline 2, and volatile gas generated by a sample is loaded into a gas exhaust pipeline 4 through high-pressure inert gas; the gas analyzer 6 analyzes the gas components in the exhaust pipeline 4, and further realizes the detection of the whole-component volatile gas of the sample.
In the volatile gas generation detection system:
the gas source 1 is used for providing high-pressure inert gas, the inert gas continuously enters the sample bottle 3 through the gas inlet pipeline 2, carries volatile gas generated by a sample in the process of flowing through the sample bottle 3, and then is discharged from the gas discharge pipeline 4, so that the volatile gas is conveyed. Therefore, even a volatile gas having a relatively small amount of volatilization can be discharged from the sample bottle 3 and detected by the current-carrying action of the high-pressure inert gas, thereby improving the accuracy of the detection result. In addition, when the detection is finished, the residual sample in the system can be cleaned by starting the gas source 1. The high pressure inert gas provided by gas source 1 is preferably high pressure nitrogen.
The flowmeter 5 is arranged on the air inlet pipeline 2 and used for adjusting the flow rate of gas in the system, and the flow rate of gas in the system can be adjusted by a person skilled in the art according to the characteristics and other factors of the sample and the gas analyzer 6, so that the detection efficiency and sensitivity of volatile gas can be improved.
The sample bottle 3 is a split structure and includes a bottle body 31 and a base 32 which are detachably connected. Wherein:
the top of the bottle body 31 is provided with an air inlet 311 and an air outlet 312, and the high-pressure carrier gas enters the sample bottle 3 from the air inlet 311, flows through the bottle and carries volatile gas to be discharged from the air outlet 312. In order to prevent the sample from remaining in the sample bottle 3, the inner wall of the sample bottle 3 is preferably passivated or a quartz liner is used.
Furthermore, in order to improve the tightness of the gas transmission pipeline in the system, the volatile gas generation and detection system further comprises a first sealing mechanism and/or a second sealing mechanism; referring to fig. 1, the first sealing mechanism includes: a first sealing cover 71 and a first sealing gasket 81, wherein the first sealing cover 71 is in threaded connection with the air inlet 311; the first sealing cover 71 is provided with a first through hole, and one end of the air inlet pipeline 2 is communicated with the air inlet 311 through the first through hole; the first sealing gasket 81 is arranged between the first sealing cover 71 and the air inlet pipeline 2 and is used for sealing a gap between the air inlet pipeline 2 and the first through hole of the first sealing cover 71; similarly, the second sealing mechanism includes: a second seal cap 72 and a second seal gasket 82, the second seal cap 72 being threadably connected to the vent 312; the second sealing cover 72 is provided with a second through hole, and one end of the exhaust pipeline 4 is communicated with the exhaust port 312 through the second through hole; the second sealing gasket 82 is disposed between the second sealing cover 72 and the exhaust pipe 4, and is used for sealing a gap between the exhaust pipe 4 and the second through hole of the second sealing cover 72. In this embodiment, the port portions of the air inlet 311 and the air outlet 312 are provided with external threads, and the first sealing cover 71 and the second sealing cover 72 are provided with internal threads, so that when the air inlet 311 and the air outlet are connected, the first sealing cover 71 is screwed down with the air inlet 311, then one end of the air inlet pipeline 2 passes through the first through hole of the first sealing cover 71, and finally the first sealing gasket 81 is sleeved between the air inlet pipeline 2 and the first sealing cover 71 to seal a gap between the air inlet pipeline 2 and the first sealing cover 71. The second seal cap 72 and second seal gasket 82 are installed as described above. The first sealing gasket 81 and the second sealing gasket 82 may be silica gel gaskets or teflon gaskets.
The base 32 has both sample holding and sample heating functions. Heating mechanism 322 that base 32 set up can realize the heating to sample platform 321, and its effect lies in: on one hand, the volatilization rate of volatile components in the sample is accelerated, and the detection efficiency is improved; on the other hand, for the components with low volatility, the components can be fully volatilized to form volatile gas in a heating mode, and then the volatile gas is carried to the exhaust pipeline 4 by the high-pressure inert gas to be detected, so that the production and collection of the volatile gas with all components of the sample are facilitated, and the detection precision of the system is improved. Finally, heating mechanism 322 still is favorable to forming hot air in the bottom of sample bottle 3, the in-process that the hot air rises can drive volatile gas and rise together, then take away rapidly by the high-pressure inert gas that flows through and enter into exhaust pipe 4 in, effectual volatile gas of avoiding remains in sample bottle 3 bottom, even make even the bottle 31 of sample bottle 3 and base 32 even not totally sealed also can not cause the influence to detecting the precision, guarantee when realizing making things convenient for the application of sample promptly and detect the precision.
In a preferred embodiment of the present invention, a storage recess is formed in an upper surface of the base 32, the storage recess forms the sample stage 321, and the heating mechanism 322 is disposed below the storage recess. In this embodiment, a circular storage groove is disposed on the upper surface of the base 32 for fixing the position of the sample. The heating mechanism 322 is preferably disposed below the storage recess, and more preferably, referring to fig. 2, the heating mechanism 322 is disposed below and around the storage recess to uniformly heat the space in the storage recess, so that the volatile components of the sample can be more completely volatilized. Further, the system for generating and detecting a volatile gas provided by the embodiment further comprises a temperature control device; this temperature control device includes: the temperature acquisition unit is used for acquiring the temperature in the object placing groove, and the control unit is connected with the temperature acquisition unit and the heating mechanism 322 and is used for controlling the working state of the heating mechanism 322 according to the temperature acquired by the temperature acquisition unit and the preset temperature. The temperature acquisition unit specifically can be temperature sensor, sets up in putting the thing recess, and it is used for gathering in real time puts the temperature in the thing groove to send this temperature for the control unit. The control unit judges according to the temperature sent by the temperature acquisition unit and the preset temperature, and if the temperature sent by the temperature acquisition unit is lower than the preset temperature, the operating power of the heating mechanism 322 is increased until the temperature sent by the temperature acquisition unit is equal to the preset temperature; if the temperature sent by the temperature collection unit is higher than the preset temperature, the operation power of the heating mechanism 322 is reduced or the heating mechanism 322 is controlled to stop working until the temperature sent by the temperature collection unit is equal to the preset temperature. The preset temperature can be adjusted in real time according to factors such as sample characteristics and efficiency requirements, so that the temperature of the sample stage 321 can be continuously adjusted.
The body 31 and the base 32 of the sample bottle 3 are detachable, thereby facilitating the addition and removal of the sample. In order to reduce the difficulty of processing and facilitate the operation, the bottle body 31 and the base 32 are preferably connected as follows: the circumferential surface of the base 32 is a frosted conical surface with the size of the section reduced from the bottom end to the top end; the bottom surface of the bottle body 31 is a frosted circular ring surface; the frosted circular ring surface of the bottle body 31 is in abutting contact with the frosted conical surface of the base 32. In this way, the self-weight of the bottle body 31 is utilized to enable the frosted contact surfaces between the bottom of the bottle body 31 and the circumferential surface of the base 32 to be embedded into each other, and the sealing performance is improved. Because the bottle body 31 and the base 32 are mostly glass structures, the requirements on the processing difficulty and the processing precision of the frosted surface on the surface of the glass are low, and therefore, the production cost and the processing difficulty can be reduced while the connection sealing performance is improved by adopting the mode. In addition, the assembly and disassembly of the two are also more convenient. Further preferably, the volatile gas generation detection system further includes: and a weight mechanism disposed on the surface of the bottle body 31, wherein the weight mechanism is used for increasing the weight of the bottle body 31 to increase the pressure of the contact surface between the bottle body 31 and the base 32, so as to further improve the sealing performance. The counterweight mechanism can be: a counterweight ring and/or a counterweight; the counterweight ring is circumferentially sleeved on the outer surface of the bottle body 31, and the counterweight is arranged at the top or in the circumferential direction of the bottle body 31. Further, in order to arrange the weight ring and/or the weight block conveniently, the surface of the bottle body 31 may be provided with a protrusion structure for placing or fixing the weight ring and/or the weight block.
The gas analyzer 6 is provided in the exhaust line 4, and analyzes and detects a gas component in the exhaust line 4. Gas analyzer 6 includes, but is not limited to: thermal conductivity type gas analyzers, electrochemical gas analyzers, infrared absorption type analyzers, photoelectric colorimetric analyzers, and the like. In order to improve the detection precision and sensitivity, a mass spectrometer is preferably adopted in the embodiment of the invention, and the mass spectrometer has the advantages of high detection speed and high sensitivity.
Further, referring to fig. 3, in order to realize real-time sensitive detection of volatile gas in the exhaust pipe 4, the probe 92 of the mass spectrometer is provided with a capillary 91, one end of the capillary 91 extends into the exhaust pipe 4, and the other end is inserted into the probe 92, and the capillary 91 is used for guiding the gas (hollow round in fig. 3) in the exhaust pipe 4 into an ion source 93 of the mass spectrometer. The capillary 91 is preferably a quartz tube or an inerted metal capillary, and more preferably an inerted metal capillary. On one hand, the metal capillary tube subjected to inert treatment has high strength, is not easy to damage and has long service life, and the sample can be effectively prevented from being remained through inert treatment.
The inventor of the present application has found that the inner diameter and length of the capillary 91 have an influence on the sample volume, and further, in consideration of the connection between the capillary 91 and the exhaust pipe 4 and the maximum diameter of the through hole of the sample injection region, the inner diameter of the capillary 91 is set to 530 μm, the total length of the capillary 91 is set to 30.0cm, and the length of the capillary 91 extending into the probe 92 is set to 22.6 cm. The capillary 91 of this size is not only satisfactory for connection to the exhaust line 4, but also has a large sample volume.
Referring to fig. 2, there is shown another embodiment of the present invention for detecting generation of volatile gas, which is different from the above-mentioned system in that a connecting line 10 and a valve assembly are additionally provided; wherein,
one end of the connecting pipeline 10 is communicated with the air inlet pipeline 2, and the other end is communicated with the exhaust pipeline 4;
the valve assembly includes: a first valve S1, a second valve S2, and a third valve S3; the first valve S1 is disposed in the connecting line 10; the second valve S2 is provided between the intake port 311 and the connecting pipe 10; the third valve S3 is disposed between the exhaust port 312 and the connecting line 10.
The function of adding connecting line 10 and valve component lies in: the operation of being convenient for carry out the edulcoration to system inside before carrying out the sampling specifically operates as follows:
before the sample is added, the first valve S1, the second valve S2, and the third valve S3 are opened, and the gas source is turned on. Filling the system with an inert gas, such as nitrogen;
then, the second valve S2 and the third valve S3 are closed, the base 32 is removed, the sample is added into the sample platform 321 of the base 32, and the base 32 is mounted on the vial 31;
after the volatile gas is diffused and balanced in the bottle 31, the heating mechanism 322 is turned on for a period of time, the second valve S2 and the third valve S3 are opened, and the first valve S1 is closed, so that the volatile sample in the sample is generated and collected.
Through setting up connecting line 10 and first valve S1, realize that air inlet pipeline 2 and exhaust pipe 4 can communicate when removing the edulcoration, mutual isolation when sampling. The second valve S2 and the third valve S3 are arranged, so that the bottle body 31 is communicated with the gas source 1 during impurity removal and sampling, and is isolated from the gas source 1 during the initial generation (non-diffusion equilibrium) of volatility. Therefore, the influence of miscellaneous gas in the system on the detection result can be reduced, and the operation is simple and easy.
As can be seen from the above, the generation and detection system for volatile gas provided by the embodiment of the present invention has the following advantages:
1. the system is provided with the gas source as a volatile gas conveying carrier, and gas with a relatively small volatilization amount can be discharged from the sample bottle to be detected under the current-carrying effect of the high-pressure inert gas, so that the accuracy of a detection result is improved.
2. The base of the sample bottle can be detached and is provided with a sample table and a heating mechanism. On one hand, the heating mechanism can accelerate the volatilization rate of volatile components in the sample and improve the detection efficiency; on the other hand, for the components with low volatility, the components can be fully volatilized to form volatile gas which is carried to the exhaust pipeline by the high-pressure inert gas to be detected in a heating mode, so that the production and collection of the volatile gas of all the components of the sample are facilitated, and the detection precision of the system is improved. Finally, heating mechanism still is favorable to forming the hot air in the bottom of sample bottle, drives volatile gas and rises together, then is taken away rapidly by the high-pressure inert gas who flows through and enters into exhaust pipe in, and the effectual volatile gas of avoiding remains in the sample bottle bottom, makes from this that the bottle of sample bottle also can not cause the influence to the detection precision with the base is incomplete sealed, guarantees the detection precision when realizing making things convenient for the application of sample promptly.
In summary, the volatile gas generation detection system provided by the embodiment of the invention is beneficial to realizing production and collection of all-component volatile gas of a sample, and has high detection precision and high detection speed.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen in order to best explain the principles of the embodiments, the practical application, or improvements made to the technology in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Claims (10)
1. A volatile gas generation detection system, comprising: the system comprises a gas source, a gas inlet pipeline, a sample bottle, a gas exhaust pipeline, a flowmeter and a gas analyzer; wherein,
the sample bottle comprises a bottle body and a base which are detachably connected; the top of the bottle body is provided with an air inlet and an air outlet; the upper surface of the base is provided with a sample table, and the base further comprises a heating mechanism for heating the sample table;
the gas source is used for providing high-pressure inert gas as a delivery carrier of volatile gas;
the air inlet pipeline is arranged between the air source and the air inlet; the flowmeter is arranged on the gas inlet pipeline and used for adjusting the gas flow rate;
the exhaust pipeline is connected with the exhaust port;
the gas analyzer is connected with the exhaust pipeline and used for detecting components of gas in the exhaust pipeline.
2. The volatile gas generation detection system of claim 1, further comprising a first sealing mechanism and/or a second sealing mechanism;
the first sealing mechanism includes: the first sealing cover is in threaded connection with the air inlet; the first sealing cover is provided with a first through hole, and one end of the air inlet pipeline is communicated with the air inlet through the first through hole; the first sealing gasket is arranged between the first sealing cover and the air inlet pipeline;
the second sealing mechanism includes: the second sealing cover is in threaded connection with the exhaust port; the second sealing cover is provided with a second through hole, and one end of the exhaust pipeline is communicated with the exhaust port through the second through hole; the second sealing gasket is arranged between the second sealing cover and the exhaust pipeline.
3. The system according to claim 1, wherein a storage groove is formed in an upper surface of the base, the storage groove forms the sample stage, and the heating mechanism is disposed below the storage groove.
4. The volatile gas generation detection system of claim 3, further comprising a temperature control device; the temperature control device includes: temperature acquisition unit and the control unit, the temperature acquisition unit is used for gathering the temperature of putting in the thing recess, the control unit links to each other with temperature acquisition unit and heating mechanism for according to the temperature that the temperature acquisition unit gathered and predetermine the operating condition of temperature control heating mechanism.
5. The system of claim 1, wherein the base has a circumferential surface that is a frosted cone having a cross-sectional dimension that decreases from a bottom end to a top end,
the bottom surface of the bottle body is a frosted circular ring surface; the frosted circular ring surface of the bottle body is in abutting contact with the frosted conical surface of the base.
6. The volatile gas generation detection system of claim 5, further comprising: the counterweight mechanism is arranged on the surface of the bottle body; the counterweight mechanism is as follows: a counterweight ring and/or a counterweight; the outer surface of bottle is located along circumference cover to the counter weight circle, the counter weight sets up in the top or circumference of bottle.
7. The volatile gas generation detection system of claim 1, further comprising: connecting the pipeline and the valve component; wherein,
one end of the connecting pipeline is communicated with the air inlet pipeline, and the other end of the connecting pipeline is communicated with the exhaust pipeline;
the valve assembly includes: a first valve, a second valve, and a third valve;
the first valve is arranged on the connecting pipeline;
the second valve is arranged between the air inlet and the connecting pipeline;
the third valve is arranged between the exhaust port and the connecting pipeline.
8. The system for detecting the generation of a volatile gas according to claim 1, wherein the gas analyzer is a mass spectrometer, a probe of the mass spectrometer is provided with a capillary tube, one end of the capillary tube extends into the flue gas duct, and the other end of the capillary tube is inserted into the probe.
9. The system for detecting the generation of a volatile gas according to claim 8, wherein the capillary has an inner diameter of 530 μm, a total length of 30.0cm, and a length of 22.6cm from which the capillary protrudes into the probe head.
10. The system for detecting the generation of a volatile gas according to claim 1, wherein the inner wall of the sample bottle is passivated or a quartz lining tube is used.
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