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CN109030679A - A kind of second level pyrolysis analysis system - Google Patents

A kind of second level pyrolysis analysis system Download PDF

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Publication number
CN109030679A
CN109030679A CN201810796118.8A CN201810796118A CN109030679A CN 109030679 A CN109030679 A CN 109030679A CN 201810796118 A CN201810796118 A CN 201810796118A CN 109030679 A CN109030679 A CN 109030679A
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China
Prior art keywords
way valve
interfaces
pipe
hot
desorption
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Pending
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CN201810796118.8A
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Chinese (zh)
Inventor
王平
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Zhejiang Racing Instrument Co Ltd
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Zhejiang Racing Instrument Co Ltd
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Priority to CN201810796118.8A priority Critical patent/CN109030679A/en
Publication of CN109030679A publication Critical patent/CN109030679A/en
Pending legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N30/08Preparation using an enricher
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/06Preparation
    • G01N30/14Preparation by elimination of some components

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

本发明提出了一种二级热解析系统,包括第一六通阀、一级吸附管、第二六通阀、二级吸附管和冷热端切换系统,所述第一六通阀用于对一级吸附管的吸附、脱附进行切换,所述第一六通阀的1、4接口与一级吸附管相连,所述第二六通阀的的1、4接口与二级吸附管相连,所述第一六通阀的5接口与第二六通阀的3接口相连,所述第二六通阀用于对二级吸附管的吸附、脱附进行切换,所述冷热端切换系统用于实现一级吸附管、二级吸附管的低温、高温转换,所述冷热端切换系统采用导轨移动的方式实现吸附管冷端、热端的快速降温、升温切换,采用多级吸附,可以提高气体样品的取样量,通过电动/气动驱动导轨移动的方式,瞬间实现吸附管的升温和降温要求。

The present invention proposes a two-level thermal analysis system, including a first six-way valve, a first-level adsorption tube, a second six-way valve, a second-level adsorption tube, and a hot and cold end switching system. The first six-way valve is used for Switch the adsorption and desorption of the primary adsorption tube, the 1, 4 ports of the first six-way valve are connected with the primary adsorption tube, and the 1, 4 ports of the second six-way valve are connected with the secondary adsorption tube connected, the 5 port of the first six-way valve is connected with the 3 port of the second six-way valve, the second six-way valve is used to switch the adsorption and desorption of the secondary adsorption tube, the hot and cold end The switching system is used to realize the low temperature and high temperature conversion of the primary adsorption tube and the secondary adsorption tube. The cold and hot end switching system adopts the way of moving the guide rail to realize the rapid cooling and heating switching of the cold end and the hot end of the adsorption tube. It adopts multi-stage adsorption , can increase the sampling volume of gas samples, and realize the heating and cooling requirements of the adsorption tube instantly through the electric/pneumatic drive guide rail movement.

Description

A kind of second level pyrolysis analysis system
[technical field]
The present invention relates to the technical field of Thermal desorption, especially a kind of technical field of second level pyrolysis analysis system.
[background technique]
Thermal desorption technology is a kind of two in one technique: collection sampling with concentrate in one, then by sample from sampling pipe transfer It is detected after being shifted out.Thermal desorption is released organic compound by the way of heating from sampling pipe, rather than is used The method of solvent elution, this makes Thermal desorption technology avoid longer solvent elution time, and the solvent-free peak in chromatogram, Electronic cooling low temperature is unstable in the prior art, and concentration effect is less desirable;Liquid nitrogen refrigerating: temperature is low but troublesome in poeration, A kind of and waste liquid nitrogen, it is proposed that second level pyrolysis analysis system.
[summary of the invention]
The object of the invention is to solve the problems of the prior art, a kind of second level pyrolysis analysis system is proposed, using more Grade absorption, can be improved the sampling amount of gaseous sample, by fast resolving, reduces the widthization of chromatographic peak, driven by electric/pneumatic The mobile mode of dynamic guide rail, moment realize that the heating of adsorption tube and cooling require.
To achieve the above object, the invention proposes a kind of second levels to be pyrolyzed analysis system, including the first six-way valve, primary adsorption Pipe, the second six-way valve, secondary absorption pipe and hot and cold side switching system, first six-way valve is for the suction to primary adsorption pipe Attached, desorption switches over, and 1,4 interfaces of first six-way valve are connected with primary adsorption pipe, and 1, the 4 of second six-way valve Interface is connected with secondary absorption pipe, and 5 interfaces of first six-way valve are connected with 3 interfaces of the second six-way valve, and the described 2nd 6 Port valve for being switched over to the adsorption and desorption of secondary absorption pipe, the hot and cold side switching system for realizing primary adsorption pipe, The low temperature of secondary absorption pipe, high temperature shift, the hot and cold side switching system realized in such a way that guide rail is mobile adsorption tube cold end, The fast cooling in hot end, heating switching, the primary adsorption pipe enter elevated temperature desorption area by hot and cold side switching system and carry out Concentrate desorption, the secondary absorption pipe by hot and cold side switching system enter in refrigeration system carry out low temperature aggregation adsorb or into Enter to elevated temperature desorption area and carries out concentration desorption.
Preferably, 3 interfaces of first six-way valve are connected with pressure maintaining valve and switch valve, the 3 of first six-way valve Interface is purge gass import, and after the switch valve for opening purge gass, foreign gas passes sequentially through the 3 of the first six-way valve, 4 interfaces, so System is blown out by primary adsorption pipe, the 1 of the first six-way valve, 2 interfaces afterwards, 6 interfaces of first six-way valve are connected with pressure stabilizing Valve and flow stabilizing valve, 6 interfaces of first six-way valve are carrier gas injection port, and carrier gas is entered by 6,1 interface of the first six-way valve Then primary adsorption pipe passes sequentially through 4,5 interfaces and enters in the system of the second six-way valve, primary adsorption pipe is de- in high temperature at this time Attached area.
Preferably, 3 interfaces of second six-way valve be carrier gas injection port, 5 interfaces of second six-way valve with point Analyzer device is connected, and the carrier gas that the primary adsorption pipe elevated temperature desorption goes out enters second level suction by 3,4 interfaces of the second six-way valve In attached pipe, low temperature aggregation absorption is carried out, secondary absorption pipe is in refrigeration system at this time, and second six-way valve is in secondary absorption Foreign gas in switching state purge system after pipe completion absorption, then secondary absorption pipe enters elevated temperature desorption by guide rail Area, carrier gas are successively passed through the 4 of the second six-way valve, 5 interfaces and are entered in analysis instrument.
Preferably, being equipped with refrigeration system in the hot and cold side switching system, the refrigeration modes of the refrigeration system are used Low-temperature circulating refrigeration.
Beneficial effects of the present invention: the present invention passes through the first six-way valve, primary adsorption pipe, the second six-way valve, secondary absorption The sampling amount of gaseous sample can be improved using multi-stage absorption in pipe and the cooperation of hot and cold side switching system etc., by quickly solving Analysis, reduces the widthization of chromatographic peak, is driven by electric/pneumatic, and the mobile mode of guide rail, moment realizes the heating and drop of adsorption tube Temperature requires, and ensure that the consistency of sample analysis.
Feature and advantage of the invention will be described in detail by embodiment combination attached drawing.
[Detailed description of the invention]
Fig. 1 is a kind of Technology Roadmap of second level pyrolysis analysis system of the present invention.
[specific embodiment]
Refering to fig. 1, a kind of second level of the present invention is pyrolyzed analysis system, including the first six-way valve, primary adsorption pipe, the two or six logical Valve, secondary absorption pipe and hot and cold side switching system, first six-way valve is for cutting the adsorption and desorption of primary adsorption pipe It changes, 1,4 interfaces of first six-way valve are connected with primary adsorption pipe, and 1,4 interfaces and second level of second six-way valve are inhaled Attached pipe is connected, and 5 interfaces of first six-way valve are connected with 3 interfaces of the second six-way valve, and second six-way valve is used for two The adsorption and desorption of grade adsorption tube switches over, and the hot and cold side switching system is for realizing primary adsorption pipe, secondary absorption pipe Low temperature, high temperature shift, the hot and cold side switching system realize the fast prompt drop of adsorption tube cold end, hot end in such a way that guide rail is mobile Temperature, heating switching, the primary adsorption pipe enters elevated temperature desorption area by hot and cold side switching system and carries out concentration desorption, described Secondary absorption pipe is entered in refrigeration system by hot and cold side switching system to carry out low temperature aggregation absorption or enters elevated temperature desorption Area carries out concentration desorption.3 interfaces of first six-way valve are connected with pressure maintaining valve and switch valve, and the 3 of first six-way valve connect It mouthful is purge gass import, after the switch valve for opening purge gass, foreign gas passes sequentially through the 3 of the first six-way valve, 4 interfaces, then System is blown out by primary adsorption pipe, the 1 of the first six-way valve, 2 interfaces, 6 interfaces of first six-way valve are connected with pressure maintaining valve And flow stabilizing valve, 6 interfaces of first six-way valve are carrier gas injection port, carrier gas enters one by 6,1 interface of the first six-way valve Then grade adsorption tube passes sequentially through 4,5 interfaces and enters in the system of the second six-way valve, primary adsorption pipe is in elevated temperature desorption at this time Area.3 interfaces of second six-way valve are carrier gas injection port, and 5 interfaces of second six-way valve are connected with analysis instrument, described The carrier gas that primary adsorption pipe elevated temperature desorption goes out enters in secondary absorption pipe by 3,4 interfaces of the second six-way valve, carries out low temperature Aggregation absorption, secondary absorption pipe is in refrigeration system at this time, and second six-way valve is cut after secondary absorption pipe completes absorption Foreign gas in state purge system is changed, then secondary absorption pipe enters elevated temperature desorption area by guide rail, and carrier gas is successively passed through 4,5 interfaces of the second six-way valve enter in analysis instrument.Refrigeration system, the refrigeration are equipped in the hot and cold side switching system The refrigeration modes of system are freezed using low-temperature circulating.
The course of work of the present invention:
A kind of working principle of second level pyrolysis analysis system of the present invention are as follows: sample is adsorbed on level-one Thermal desorption by sampling instrument In primary adsorption pipe, sample is in member of the standing committee's state at this time, opens purging exhaust switch valve, the foreign gas in system is purged out is Then system blows out system to 1,2 interfaces by 3,4 interfaces, setting the first six-way valve at this time is the position that solid line leads to;Purging is clean Afterwards, the position that the first six-way valve of switching leads to dotted line, then gas enters primary adsorption pipe by 6,1 interface, then connects by 4,5 Mouth enters in the system of the second six-way valve;The second six-way valve is in the logical position of solid line at this time, will by guide rail (electric/pneumatic) Secondary absorption pipe be pushed into refrigeration system in, for temperature since pipe is small, thermal capacitance is small, thus secondary absorption pipe instantaneous temperature reduction to set Then the elevated temperature desorption area set is desorbed by guide rail (electric/pneumatic), due to the heat of adsorption tube in primary adsorption pipe by low temperature Hold small, sample instants are heated to desorption temperature, and concentration is desorbed out, enter the two of low temperature by the second six-way valve 3,4 interfaces In grade adsorption tube, carries out low temperature and focus absorption;After the completion of absorption, the position led to by the second six-way valve of switching to dotted line, purging Secondary absorption pipe is pushed into the elevated temperature desorption area set by guide rail (electric/pneumatic), due to inhaling by the foreign gas in system The thermal capacitance of attached pipe is small, and sample instants are heated to desorption temperature, enters GC or other analysis instrument systems by 4,5 interfaces.
Above-described embodiment is the description of the invention, is not limitation of the invention, after any pair of simple transformation of the present invention Scheme all belong to the scope of protection of the present invention.

Claims (4)

1. a kind of second level is pyrolyzed analysis system, it is characterised in that: including the first six-way valve, primary adsorption pipe, the second six-way valve, second level Adsorption tube and hot and cold side switching system, first six-way valve are described for switching over to the adsorption and desorption of primary adsorption pipe 1,4 interfaces of the first six-way valve are connected with primary adsorption pipe, 1,4 interfaces and the secondary absorption pipe phase of second six-way valve Even, 5 interfaces of first six-way valve are connected with 3 interfaces of the second six-way valve, and second six-way valve is used for secondary absorption The adsorption and desorption of pipe switches over, the hot and cold side switching system for realizing primary adsorption pipe, secondary absorption pipe low temperature, High temperature shift, the hot and cold side switching system realize adsorption tube cold end, the fast cooling in hot end, liter in such a way that guide rail is mobile Temperature switching, the primary adsorption pipe enter elevated temperature desorption area by hot and cold side switching system and carry out concentration desorption, the second level Adsorption tube by hot and cold side switching system enter in refrigeration system carry out low temperature aggregation absorption or enter elevated temperature desorption area into Row concentrates desorption.
2. a kind of second level as described in claim 1 is pyrolyzed analysis system, it is characterised in that: 3 interfaces of first six-way valve connect It is connected to pressure maintaining valve and switch valve, 3 interfaces of first six-way valve are purge gass import, miscellaneous after the switch valve for opening purge gass Matter gas passes sequentially through the 3 of the first six-way valve, 4 interfaces, then by primary adsorption pipe, the 1 of the first six-way valve, the blowout of 2 interfaces System, 6 interfaces of first six-way valve are connected with pressure maintaining valve and flow stabilizing valve, 6 interfaces of first six-way valve be carrier gas into Sample mouth, carrier gas enter primary adsorption pipe by 6,1 interface of the first six-way valve, then pass sequentially through 4,5 interfaces into the two or six In the system of port valve, primary adsorption pipe is in elevated temperature desorption area at this time.
3. a kind of second level as described in claim 1 is pyrolyzed analysis system, it is characterised in that: 3 interfaces of second six-way valve are 5 interfaces of carrier gas injection port, second six-way valve are connected with analysis instrument, the carrier gas that the primary adsorption pipe elevated temperature desorption goes out It is entered in secondary absorption pipe by the 3 of the second six-way valve, 4 interfaces, carries out low temperature aggregation absorption, secondary absorption pipe is at this time In refrigeration system, second six-way valve foreign gas in switching state purge system after secondary absorption pipe completes absorption, so Secondary absorption pipe enters elevated temperature desorption area by guide rail afterwards, and carrier gas is successively passed through the 4 of the second six-way valve, 5 interfaces and entered point In analyzer device.
4. a kind of second level as described in claim 1 is pyrolyzed analysis system, it is characterised in that: be equipped in the hot and cold side switching system The refrigeration modes of refrigeration system, the refrigeration system are freezed using low-temperature circulating.
CN201810796118.8A 2018-07-19 2018-07-19 A kind of second level pyrolysis analysis system Pending CN109030679A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109406692A (en) * 2018-12-28 2019-03-01 苏州天蓝分析仪器有限公司 Continuous quadratic enrichment resolver that is a kind of multistage and running in turn
CN111044649A (en) * 2020-03-18 2020-04-21 山东海慧环境科技有限公司 Gas analysis device
CN111830176A (en) * 2019-04-16 2020-10-27 上海思达分析仪器有限责任公司 A thermal desorption instrument with low temperature adsorption function
CN118688339A (en) * 2024-06-20 2024-09-24 武汉天虹环保科技有限责任公司 A continuous online enrichment and analysis device for ODS and fluorinated greenhouse gases
CN119469944A (en) * 2025-01-09 2025-02-18 深圳市索奥检测技术有限公司 A concentrated sampling device for environmental atmosphere detection

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109406692A (en) * 2018-12-28 2019-03-01 苏州天蓝分析仪器有限公司 Continuous quadratic enrichment resolver that is a kind of multistage and running in turn
CN111830176A (en) * 2019-04-16 2020-10-27 上海思达分析仪器有限责任公司 A thermal desorption instrument with low temperature adsorption function
CN111830176B (en) * 2019-04-16 2025-03-14 上海思达分析仪器股份有限公司 A thermal analyzer with low temperature adsorption function
CN111044649A (en) * 2020-03-18 2020-04-21 山东海慧环境科技有限公司 Gas analysis device
CN118688339A (en) * 2024-06-20 2024-09-24 武汉天虹环保科技有限责任公司 A continuous online enrichment and analysis device for ODS and fluorinated greenhouse gases
CN119469944A (en) * 2025-01-09 2025-02-18 深圳市索奥检测技术有限公司 A concentrated sampling device for environmental atmosphere detection

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Application publication date: 20181218