CN109425648A - A kind of sample analysis method and device of fast pyrogenation analysis sample introduction - Google Patents
A kind of sample analysis method and device of fast pyrogenation analysis sample introduction Download PDFInfo
- Publication number
- CN109425648A CN109425648A CN201710747029.XA CN201710747029A CN109425648A CN 109425648 A CN109425648 A CN 109425648A CN 201710747029 A CN201710747029 A CN 201710747029A CN 109425648 A CN109425648 A CN 109425648A
- Authority
- CN
- China
- Prior art keywords
- sample
- analysis
- thermal desorption
- desorption chamber
- knob
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- 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
-
- 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
- G01N27/622—Ion mobility spectrometry
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
- G01N35/1009—Characterised by arrangements for controlling the aspiration or dispense of liquids
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N2035/00346—Heating or cooling arrangements
- G01N2035/00425—Heating or cooling means associated with pipettes or the like, e.g. for supplying sample/reagent at given temperature
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N2035/00346—Heating or cooling arrangements
- G01N2035/00445—Other cooling arrangements
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The fast pyrogenation that the present invention discloses a kind of for analyzing sample analyses the sample analysis method and device of sample introduction.Analysis method in the present invention includes simplifying user's operation, while reducing analysis time partially with automatic part manually.Apparatus of the present invention include sample injector, Thermal desorption chamber, sample feeding pipe, sample introduction valve, heating device and cooling device, can be realized the analysis of fast pyrogenation analysis sample.
Description
Technical field
The fast pyrogenation that the present invention relates to a kind of for analyzing sample analyses the sample analysis method and device of sample introduction, is suitable for
The instrument that sample composition can be analyzed, especially suitable for mass spectrum or ion mobility spectrometry.
Background technique
Many sample analysis instruments need to enter sample transfer into analysis cavity, such as spectrum, chromatography, ion mobility spectrometry and matter
The analysis instruments such as spectrum.Compound lower for volatility, the transmission process of sample are to complete the important link of analysis.
In ion mobility spectrometry, it is analyzed the ion and gas collisions of sample, since different plant species collision cross-section is different, is arrived
Time up to detector is also different, to realize the differentiation of analyzed compound.Ion mobility spectrometry need by sample transfer to compared with
In hypobaric analysis cavity, molecular ionization is realized using intracavitary ionization source.
Since mass spectrometer needs very high vacuum at runtime, need to guarantee quality analysis chamber during sample transfer
Interior vacuum degree.Currently, many mass spectrums have used external ionization source, i.e. the ionization source outside that is located at vacuum chamber, such as electron spray
Ion source (ESI), corona discharge ion source (ASAP), atmospheric pressure photoionization source (APPI), atmospheric pressure ionization source (APCI) etc..Electricity
It is intracavitary that ion from after by atmospheric pressure interface is transferred to mass spectrum.Also the mass spectrum having uses internal ionization source, i.e. ionization source is located at
The inside of vacuum chamber, such as electron ionization sources (EI), Single-photon ionization source (SPI) and chemical ionization source (CI).
In the prior art, most atmospheric pressure parsing sampling devices also contain ionization device simultaneously.Such as normal pressure solid point
Corona discharge is utilized by the sample in liquid phase in analysis probe technologies (Atmospheric Solid Analysis Probe, ASAP)
Product parse and ionize (" Analytical Chemistry " magazine, volume 77,7826-7831 pages (2005)).Desorb atmosphere
Press polish ionizes (Desorption Atmospheric Pressure Photoionization, DAPPI) technology using heating
Gas sample molecule is parsed and utilize vacuum-ultraviolet light by ionized sample molecule (" Analytical Chemistry " is miscellaneous
Will, volume 79,7867-7872 pages (2007)).Both technologies are suitable for the nonpolar and weak of the more difficult ionization of ESI and DESI
The analysis of polar micromolecules." Rapid Communication in Mass Spectrometry " magazine, volume 19,
Described in 3701-3704 pages (2005) one kind using ultraviolet laser as desorption tool, using EFI ion beam as ionization tool
Normal pressure direct analysis (EFI assisted laser desorption ionisation ELDI).This method is due to using laser as desorption source, sample table
The desorption area in face has obtained good control, this makes the mass spectrum characterization image under normal pressure become possible.Similar skill therewith
Art such as " Rapid Communication in Mass Spectrometry " magazine, volume 16,681-685 pages (
2002) and Chinese patent (application number 200810033974.4) described in using infrared laser be desorption source, respectively with big
Pressure chemical ionization source is the laser desorption chemi-ionization technology (LDCI) of ion source and using atmospheric pressure photoionization source as ion
The laser desorption photo-ionisation technology (LDPI) in source has with its effective ionization to low polar molecule with above-mentioned ELDI method
Complementary effect.International monopoly (2010121518 A1 of WO) disclose it is a kind of using heating or hot gas purge, by sample
Atmospheric pressure ionization, the thermal analysis apparatus being then introduced into mass spectrum and method after molecule parsing.
Summary of the invention
The fast pyrogenation that the present invention discloses a kind of for analyzing sample analyses the sample analysis method and device of sample introduction.This hair
Analysis method in bright includes simplifying user's operation, while reducing analysis time partially with automatic part manually.The present invention
Device includes sample injector, Thermal desorption chamber, sample feeding pipe, sample introduction valve, heating device and cooling device, can be realized fast pyrogenation analysis
The analysis of sample.The sample analysis method of the fast pyrogenation analysis sample introduction, it is characterised in that: be inserted into the sample injector containing sample
Thermal desorption is intracavitary and sealed pyrolysis analysis chamber (1), opening sample introduction valve (2) heat Thermal desorption chamber (3), according to the gas in analysis cavity
Pressure opens related device power supply (4), is analyzed (5) sample, closes analysis intracavitary unit power supply (6), begins to cool pyrolysis
It analyses chamber (7), closes sample introduction valve (8), take out sample and replace (9).
The sample analysis method, it is characterised in that: the step (2), (3), (4), (5), (6), (7), (8) are by counting
Calculation machine automatically controls.
The sample analysis method, it is characterised in that: in the step (2), sample introduction valve can control sample rate.
The sample analysis method, it is characterised in that: in the step (3), heating means include resistance heating, infrared
Heating, hot gas is thermally conductive, the means such as laser heating.
The sample analysis method, it is characterised in that: in the step (7), cooling means includes that air is cooling, water cooling
But cooling with oil.
The sample analysis method, it is characterised in that: the step (4) and (6) can be according to different barometric informations
It omits.
The sample analysis method, it is characterised in that: the step (6), the sequence of (7) and (8) can be interchanged, can also
It carries out simultaneously.
The device of the fast pyrogenation analysis sample introduction, including sample injector, Thermal desorption chamber, sample feeding pipe, sample introduction valve, heating dress
It sets, cooling device and analysis cavity.
The sample injector, the device including fixed sample, sealing element and knob.
The knob makes for controlling the connection of Thermal desorption chamber and atmosphere, while can also apply pressure to sample injector
It is sealed with Thermal desorption chamber.
The Thermal desorption chamber is equipped with knob, for controlling the connection of Thermal desorption chamber and atmosphere, while can also be to sample introduction
Device, which applies pressure, seals it with Thermal desorption chamber.
The knob, it is characterised in that: knob is one or more.
The sample injector, it is characterised in that: sample injector contains heat-barrier material, for completely cutting off the intracavitary high temperature of Thermal desorption.
The sample feeding pipe, it is characterised in that: prevent sample cold for heating sample feeding pipe comprising heater strip in sample feeding pipe
It is solidifying.
The sample feeding pipe, it is characterised in that: sample feeding pipe is made of insulating materials.
The Thermal desorption chamber, it is characterised in that: Thermal desorption chamber is equipped with intake valve or air inlet pipe, with more anticyclonic gas
Source is connected, it is therefore intended that introduces gas for Thermal desorption sample and is carried along into analysis cavity.
The sample injector further includes detachable sample brush, and You Duogen high temperature resistant bristle composition is contacted with tested article,
Test compound is adsorbed.
Detailed description of the invention
For objects, features and advantages of the present invention can be clearer and more comprehensible, below in conjunction with attached drawing to specific reality of the invention
The mode of applying elaborates.
Fig. 1 is flow diagram of the present invention.
Fig. 2 is the device of the invention schematic diagram.
Fig. 3 is a preferable implementing device figure of sample injector in the present invention.
Fig. 4 is the sectional drawing of sample injector in the present invention.
Fig. 5 is a preferable implementing device figure of sample injector and Thermal desorption chamber in the present invention.
Specific embodiment
Parsing and ionization technique are by the ion after ionization to the quality analysis being in vacuum cavity under existing atmospheric pressure
Device transmission.In this course, most of ion all with lost in the metal bump in sample feeding pipe.Simultaneously as into
Sample mouth is atmospheric pressure, needs complicated difference air pressure vacuum system, increases the volume and cost of equipment, it is difficult to realize analysis system
Micromation.
For mass spectral analysis chamber, air pressure can not be higher than certain air pressure, otherwise can damage molecular pump.In the analysis process,
Air pressure needs to stablize under lower air pressure, otherwise can Failure analysis equipment.If controlling sample introduction with switch valve, air pressure will cause
It is unable to control, damages molecular pump or mass spectrum intraluminal analysis equipment.In the design of some Thermal desorptions, such as patent CN 103091387
A connects Thermal desorption chamber, mechanical pump and analysis cavity using triple valve to guarantee the intracavitary air pressure of mass spectrum, causes most of testedization
It closes object to be pumped away, the compound parsed, impact analysis sensitivity can not be efficiently used.
During Thermal desorption sample introduction, the problem of condensation there is also sample.Sample is condensed on instrument tube wall can not only drop
Low detection sensitivity, also will cause memory effect.Common method is with heating tube or heating tape heating sample feeding pipe.But into
At sample pipe and vacuum interface, above method can not be heated effectively, will form condensation site, and sample is caused to condense.
When the intracavitary air pressure of Thermal desorption is consistent or close with air pressure in analysis cavity, the compound for being pyrolyzed precipitation is needed by dividing
Sub- expanding enters analysis cavity, this process, which necessarily will cause part of compounds, can not eventually enter into analysis cavity, thus impact analysis
Sensitivity.
The analysis time of single sample, occasion especially bigger in some sample throughputs are particularly important.In common side
In method, to avoid operator from scalding while avoiding the too early Thermal desorption of sample being inserted into, need before taking out sample by Thermal desorption chamber
It is cooling, cause analysis time very long.In addition, needing sealed pyrolysis to analyse chamber after being inserted into sample.Conventional method is using multiple spiral shells
Silk applies pressure to sealing element, encloses seal cavity using O.When opening seal chamber, it is also necessary to steam leak-off valve is opened, so that sealing
Cavity and atmosphere, to take out sample.Above procedure is time-consuming and laborious for operator, cause Thermal desorption sample introduction process without
Method realizes quickly analysis.
In airport security, the application such as illicit drugs inspection, the prior art is wiped, is taken with article to be measured using band-like paper slip
Band test compound.By ours the study found that often there is higher test compound content in the gap of article to be measured.Band
Official form for filing a lawsuit item is difficult to extract to the compound in these gaps.
In the present invention, by a series of innovative designs, problem above is solved.
To solve the problems, such as ion transport losses, ionization source is placed in analysis cavity in the design.Ion is transmitted in lower gas
Pressure has better efficiency of transmission.Thermal desorption chamber is only used for test compound Thermal desorption.
To solve the intracavitary air pressure problem of mass spectral analysis, the present invention utilizes controllable sampling valve, guarantees one side mass spectrum point
Intracavitary air pressure is analysed compared with running under hyperbar, quickly to separate sample molecule with background gas, on the other hand, in mass spectrum chamber
When normal assay, air pressure is kept in the normal range.For instrument in protection analysis cavity, pass through pressure control in measurement analysis cavity
The power supply for analyzing endoluminal, so that interior arrangement be protected not to be damaged.To sum up, the sample introduction that benefit is computerizedd control in the design
Valve is realized to pressure control in analysis cavity, can maximally utilize Thermal desorption compound, while can also protect analytical equipment.
To solve condensation problem, in the present invention, heater strip is passed through into sample feeding pipe, heat sample feeding pipe from inside, protect
Sample feeding pipe whole process has been demonstrate,proved without cooling position.Heater strip both ends are separately connected power supply, be in entire analytic process compared with
High temperature condition.To prevent short circuit, sample feeding pipe uses insulating materials.
To solve the problems, such as remaining test compound, in the apparatus of the present, be arranged on Thermal desorption chamber intake valve or
Sample feeding pipe makes a small amount of gas enter Thermal desorption chamber by control intake valve or the suitable gas conduction of setting, by remaining testedization
It closes object and is carried along into analysis cavity.
To reduce analysis time, in the apparatus of the present, gas leakage threshold switch and sealing are realized using a knob.Work as rotation
When button is closed, steam leak-off valve is closed, while applying pressure to sample injector seals it with Thermal desorption chamber.When knob is opened, open
Steam leak-off valve, while cancelling the pressure applied to sample injector, to take out sample injector.This design simplifies operation.In the present invention
Method in, due on knob be equipped with heat-barrier material, can be by sample introduction when cavity is begun to cool and is in higher temperature
Device takes out, and realizes that sample injector replacement sample carries out simultaneously with the cooling of Thermal desorption chamber, reduces analysis time.
To solve the problems, such as in gap that sample adsorbs, in the device of the invention, detachable sample brush is equipped on sample injector,
It can quickly be dismantled with sample injector.The bristle that sample paints can go deep into article gap, to improve the detection energy to article
Power and adsorption capacity to untested compound.
A specific embodiment of the invention is as follows:
Fig. 1 illustrates the flow chart of the method for the present invention, a kind of sample analysis method of fast pyrogenation analysis sample introduction, it is characterised in that:
By the sample injector insertion containing sample, Thermal desorption is intracavitary and sealed pyrolysis analysis chamber (1), opens sample introduction valve (2), heats Thermal desorption
Chamber (3) is opened related device power supply (4) according to the air pressure in analysis cavity, is analyzed (5) sample, it is built-in to close analysis cavity
Power supply (6) are set, are begun to cool Thermal desorption chamber (7), are closed sample introduction valve (8), sample is taken out and replace (9).
The step (2), (3), (4), (5), (6), (7), (8) are automatically controlled by a computer.Automatic control simplifies behaviour
The operation for making personnel accelerates analysis speed.
In the step (2), sample introduction valve can control sample rate.Sampling valve is controlled by computer, can be according to analysis
Intracavitary air pressure adjustment air inflow, thus in fact by pressure control in analysis cavity in suitable range.
In the step (3), heating means include resistance heating, and infrared heating, hot gas is thermally conductive, the hands such as laser heating
Section.To control heating speed, Thermal desorption chamber is equipped with temperature detection device, and it is intracavitary can to adjust Thermal desorption according to temperature Real-time Feedback
Temperature.
In the step (7), cooling means includes that air is cooling, and water is cooling and oil is cooling.Air cooling is a kind of simple
The convenient type of cooling, water cooling are more efficient.
The step (4) and (6) can be omitted according to different barometric informations.When in analysis cavity be Ion transfer time spectrum,
Endoluminal is not high to vacuum requirement, can work always, therefore can be omitted step (4) and (6).When in analysis cavity be mass spectrum
When, it can be maintained in OK range by the conductance of control sample feeding pipe, the air pressure for keeping mass spectrum intracavitary, the intracavitary detection of mass spectrum is set
It is standby to work always.Under these conditions, step (4) and (6) can be omitted.
The step (6), the sequence of (7) and (8) can be interchanged, and can also carry out simultaneously.Step (6), between (7) and (8)
The sequencing not determined can also be controlled by computer while be carried out to reduce analysis time.
Fig. 2 illustrates the device of the invention figure, a kind of device of fast pyrogenation analysis sample introduction, including sample injector (22), pyrolysis
It analyses chamber (23), sample feeding pipe (24), sample introduction valve (28), heating device (25), cooling device (26) and analysis cavity (30).
The sample injector (20), the device (21) including fixed sample, sealing element (31) and knob (22).
The knob (22), for controlling the connection of Thermal desorption chamber (23) and atmosphere, while can also be to sample injector
(20) applying pressure seals it with Thermal desorption chamber (23).
The Thermal desorption chamber (23) is equipped with knob (33), for controlling the connection of Thermal desorption chamber (23) and atmosphere, simultaneously
Pressure can also be applied to sample injector (20) seals it with Thermal desorption chamber (23).
The knob, it is characterised in that: knob (22) or (33) are one or more.When knob is one, knob
Position is equipped with pressure arm preferably on sample injector on Thermal desorption chamber, seals knob by sample injector and Thermal desorption chamber.
The sample injector, it is characterised in that: sample injector (22) contains heat-barrier material, for completely cutting off the intracavitary height of Thermal desorption
Temperature.
The sample feeding pipe, it is characterised in that: include heater strip (29) in sample feeding pipe (27), for heating sample feeding pipe
(27), prevent sample from condensing.
The sample feeding pipe, it is characterised in that: sample feeding pipe (27) is made of insulating materials.
The Thermal desorption chamber, it is characterised in that: Thermal desorption chamber is equipped with intake valve or air inlet pipe (24), and compared with hyperbar
Gas source be connected, it is therefore intended that introduce gas and Thermal desorption sample be carried along into analysis cavity.
The sample injector further includes detachable sample brush (53), and You Duogen high temperature resistant bristle pack (55) is at measured object
Product contact, test compound is adsorbed.
Example one is embodied
Fig. 3, Fig. 4 and Fig. 5 respectively show a kind of sample injector and Thermal desorption chamber specifically designed.
Sample injector in Fig. 3 includes knob (50), thermal insulation layer (51), baffle (52), sample brush (53), fixing groove
(54), bristle (55), groove (56).Fig. 4 is sample injector sectional drawing, is illustrated fixing screws (60), sealed groove (61), gas leakage
Groove (62), Thermal desorption chamber (63).Fig. 5 illustrates the state after the sealing of sample injector (51) and Thermal desorption chamber (63), illustrates
Thermal desorption chamber (63), sample injector (51), knob (50), compression arm (66).
In this example, when knob (50) rotates clockwise 90 to 120 °, by the control of the screw thread on baffle (52), to heat
It is mobile to parse chamber (63) direction, is blocked leakage hole using the sealing ring in gas leakage groove (62), realizes the mesh for closing leakage hole
's.Meanwhile knob (50) also will receive the effect of compression arm (66), squeeze sample injector and Thermal desorption chamber (63) mutually, thus
Realize the sealing of Thermal desorption chamber (63).When knob (50) rotates clockwise 90 to 120 °, by the screw thread on baffle (52)
Control, it is mobile to the direction opposite with Thermal desorption chamber (63), open leakage hole.Meanwhile knob (50) is detached from compression arm (66)
Effect, separate sample injector with Thermal desorption chamber (63).Using the design, Thermal desorption chamber (63) only can be realized by knob
Gas leakage and fixed operation, simplify operating process.
In this example, adsorbent equipment of the sample brush (53) as untested compound is also used.Sample brush by with fixation
Groove (56) cooperation on slot (54), is dismantled in which can be convenient on fixed groove.Bristle (55) on sample brush (53) can be with
The measured object in article gap to be measured is easily extracted, the convenience used and detection success rate are improved.
In this example, heating device is made of the resistance heating wire around Thermal desorption chamber.
In this example, cooling device is made of cooling fan.Cooling fan purges cooling gas to Thermal desorption chamber, will be pyrolyzed
Analysis chamber cools down rapidly.
In this example, bristle (55) is made of glass fibre.
In this example, Thermal desorption chamber is equipped with intake valve, is connected with atmosphere.Intake valve is controlled by computer, can basis
Air pressure adjustment air inflow.
In this example, sample brush (53) can be replaced by stripe shape adsorbent material.
In the design, also uses thermal insulation layer (51) and be connected with baffle (52), for completely cutting off on Thermal desorption chamber (63)
High temperature is realized and takes out sample injector operation under high temperature.
In this example, sample introduction valve is made of high frequency high temperature resistant vacuum solenoid, and is controlled by computer, is located at and is leaned on
Near-thermal parses at chamber position, and the temperature to guarantee sampling valve is consistent with Thermal desorption chamber, and sample is avoided to condense.
In this example, use capillary as sample feeding pipe, heater strip is passed through from capillary tube hub.Heater strip one end and direct current
Power supply connects, and the other end is connected to ground.
Example two is embodied
Embodiment two is similar with embodiment one, unlike:
In this example, Thermal desorption chamber is hollow cylinder, and sample injector is also equally cylinder.Cylindrical sample is used in sample injector
Brush.
In this example, knob is arranged on Thermal desorption chamber.Knob connects globe valve, and Thermal desorption chamber may be implemented by knob
With the connection of atmosphere.Meanwhile it is similar with embodiment one, knob can also apply pressure to sample injector by spiral arm, reach close
Seal the purpose of Thermal desorption chamber.
In this example, knob is two, applies pressure to sample injector respectively.
In this example, Thermal desorption chamber is equipped with air inlet pipe, has higher flow resistance in air inlet pipe, makes air inflow in suitable model
In enclosing.
In this example, bristle is made of high-temperature fibre.
In this example, heating device is made of the intracavitary heating rod of insertion Thermal desorption.
The present invention does not limit to and above embodiment, has this professional experiences personage to design frame of the present invention with can be convenient
Under a variety of implementation configurations.For example, heating method uses common infrared lamp, the forms such as infrared laser or flame heating.It is all similar
Operating method or device in the present invention, are considered as within protection scope of the present invention.
Claims (17)
1. a kind of sample analysis method of fast pyrogenation analysis sample introduction, it is characterised in that: the sample injector containing sample is inserted into pyrolysis
Intracavitary and sealed pyrolysis analysis chamber (1) is analysed, is opened sample introduction valve (2), heats Thermal desorption chamber (3), is beaten according to the air pressure in analysis cavity
Related device power supply (4) are opened, sample is analyzed (5), analysis intracavitary unit power supply (6) is closed, begins to cool Thermal desorption chamber
(7), sample introduction valve (8) are closed, take out sample and replaces (9).
2. sample analysis method according to claim 1, it is characterised in that: the step (2), (3), (4), (5), (6),
(7), (8) are automatically controlled by a computer.
3. sample analysis method according to claim 1, it is characterised in that: in the step (2), sample introduction valve can be controlled
Sample rate processed.
4. sample analysis method according to claim 1, it is characterised in that: in the step (3), heating means include electricity
Resistance heating, infrared heating, hot gas is thermally conductive, the means such as laser heating.
5. sample analysis method according to claim 1, it is characterised in that: in the step (7), cooling means includes sky
Air cooling, water is cooling and oil is cooling.
6. sample analysis method according to claim 1, it is characterised in that: the step (4) and (6) can be according to differences
Barometric information omit.
7. sample analysis method according to claim 1, it is characterised in that: the step (6), the sequence of (7) and (8) can
To exchange, can also carry out simultaneously.
8. a kind of device of fast pyrogenation analysis sample introduction, including sample injector, Thermal desorption chamber, sample feeding pipe, sample introduction valve, heating device,
Cooling device and analysis cavity.
9. sample injector according to claim 8, the device including fixed sample, sealing element and knob.
10. knob according to claim 9, for controlling the connection of Thermal desorption chamber and atmosphere, while can also be to sample introduction
Device, which applies pressure, seals it with Thermal desorption chamber.
11. Thermal desorption chamber according to claim 8 is equipped with knob, for controlling the connection of Thermal desorption chamber and atmosphere, simultaneously
Pressure can also be applied to sample injector seals it with Thermal desorption chamber.
12. knob described in 0 and 11 according to claim 1, it is characterised in that: knob is one or more.
13. sample injector according to claim 8, it is characterised in that: sample injector contains heat-barrier material, for completely cutting off Thermal desorption
Intracavitary high temperature.
14. sample feeding pipe according to claim 8, it is characterised in that: include heater strip in sample feeding pipe, for heating sample introduction
Pipe, prevents sample from condensing.
15. sample feeding pipe according to claim 8, it is characterised in that: sample feeding pipe is made of insulating materials.
16. Thermal desorption chamber according to claim 8, it is characterised in that: Thermal desorption chamber is equipped with intake valve or air inlet pipe, with
More anticyclonic gas source is connected, it is therefore intended that introduces gas for Thermal desorption sample and is carried along into analysis cavity.
17. sample injector according to claim 8 further includes detachable sample brush, You Duogen high temperature resistant bristle composition, with quilt
Article contact is surveyed, test compound is adsorbed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710747029.XA CN109425648B (en) | 2017-08-28 | 2017-08-28 | Sample analysis method and device for rapid thermal desorption sample injection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710747029.XA CN109425648B (en) | 2017-08-28 | 2017-08-28 | Sample analysis method and device for rapid thermal desorption sample injection |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109425648A true CN109425648A (en) | 2019-03-05 |
| CN109425648B CN109425648B (en) | 2022-05-24 |
Family
ID=65501800
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710747029.XA Active CN109425648B (en) | 2017-08-28 | 2017-08-28 | Sample analysis method and device for rapid thermal desorption sample injection |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109425648B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110849701A (en) * | 2019-11-04 | 2020-02-28 | 山东见微生物科技有限公司 | Sample processing apparatus |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101294933A (en) * | 2007-04-24 | 2008-10-29 | 中国科学院大连化学物理研究所 | Surface gas flow purging thermal desorption sampling device |
| CN202002838U (en) * | 2010-11-30 | 2011-10-05 | 中国科学院大连化学物理研究所 | Integrated online concentration and desorption device |
| CN102478543A (en) * | 2010-11-30 | 2012-05-30 | 中国科学院大连化学物理研究所 | Sample introduction apparatus for ion mobility spectrometry |
| CN103091387A (en) * | 2011-11-02 | 2013-05-08 | 中国科学院大连化学物理研究所 | Solid sample rapid thermal desorption mass spectrometry sampling device |
| CN103675082A (en) * | 2012-09-13 | 2014-03-26 | 中国科学院大连化学物理研究所 | Sample introduction device for improving detection sensitivity of ion mobility spectrometry (IMS) |
| CN203745242U (en) * | 2014-02-27 | 2014-07-30 | 郑州大学 | Sampler for ferric sulfide grain |
| CN104483423A (en) * | 2014-12-31 | 2015-04-01 | 同方威视技术股份有限公司 | Sample collection and thermal analysis sampling device and method as well as trace detection device |
| CN104569228A (en) * | 2014-12-31 | 2015-04-29 | 同方威视技术股份有限公司 | Sample injection device |
| CN104807899A (en) * | 2015-04-07 | 2015-07-29 | 上海大学 | On-line analysis device for volatile carbonyl compounds |
| CN104819885A (en) * | 2015-05-13 | 2015-08-05 | 河南理工大学 | Thermal analysis device of elemental mercury in gold amalgam adsorption tube |
| CN105300765A (en) * | 2015-10-27 | 2016-02-03 | 中国科学院广州地球化学研究所 | Atmospheric aerosol organic carbon (OC)/element carbon (EC) visualized separation and preparation device |
-
2017
- 2017-08-28 CN CN201710747029.XA patent/CN109425648B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101294933A (en) * | 2007-04-24 | 2008-10-29 | 中国科学院大连化学物理研究所 | Surface gas flow purging thermal desorption sampling device |
| CN202002838U (en) * | 2010-11-30 | 2011-10-05 | 中国科学院大连化学物理研究所 | Integrated online concentration and desorption device |
| CN102478543A (en) * | 2010-11-30 | 2012-05-30 | 中国科学院大连化学物理研究所 | Sample introduction apparatus for ion mobility spectrometry |
| CN103091387A (en) * | 2011-11-02 | 2013-05-08 | 中国科学院大连化学物理研究所 | Solid sample rapid thermal desorption mass spectrometry sampling device |
| CN103675082A (en) * | 2012-09-13 | 2014-03-26 | 中国科学院大连化学物理研究所 | Sample introduction device for improving detection sensitivity of ion mobility spectrometry (IMS) |
| CN203745242U (en) * | 2014-02-27 | 2014-07-30 | 郑州大学 | Sampler for ferric sulfide grain |
| CN104483423A (en) * | 2014-12-31 | 2015-04-01 | 同方威视技术股份有限公司 | Sample collection and thermal analysis sampling device and method as well as trace detection device |
| CN104569228A (en) * | 2014-12-31 | 2015-04-29 | 同方威视技术股份有限公司 | Sample injection device |
| CN104807899A (en) * | 2015-04-07 | 2015-07-29 | 上海大学 | On-line analysis device for volatile carbonyl compounds |
| CN104819885A (en) * | 2015-05-13 | 2015-08-05 | 河南理工大学 | Thermal analysis device of elemental mercury in gold amalgam adsorption tube |
| CN105300765A (en) * | 2015-10-27 | 2016-02-03 | 中国科学院广州地球化学研究所 | Atmospheric aerosol organic carbon (OC)/element carbon (EC) visualized separation and preparation device |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110849701A (en) * | 2019-11-04 | 2020-02-28 | 山东见微生物科技有限公司 | Sample processing apparatus |
| CN110849701B (en) * | 2019-11-04 | 2023-02-28 | 山东见微生物科技有限公司 | Sample processing apparatus |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109425648B (en) | 2022-05-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP6042965B2 (en) | Sample introduction device | |
| JP6182705B2 (en) | Ion source for direct sample analysis | |
| CN105588872B (en) | A kind of quick online atmospheric pressure photoionization mass spectrometric apparatus for active ingredient in complex matrices | |
| CN103415908B (en) | Evacuate sample room | |
| WO2010075769A1 (en) | Device for desorption ionization | |
| CN101871914A (en) | Method and device thereof for desorption ionization | |
| US11187629B2 (en) | Sample probe inlet flow system | |
| CN109870341A (en) | Volatile organic matter original position cold-trap enrichment-Thermal desorption sample pretreatment device | |
| CN105021718B (en) | A kind of liquid chromatogram and open type ionization massspectrum on-line coupling interface and detection method | |
| CN106841367A (en) | A kind of Ion transfer spectrum detection method of time resolution Dynamic Thermal parsing | |
| CN104950065B (en) | A kind of whole smoke trapping and on-line analysis apparatus and method | |
| US6144029A (en) | Method for trace detection by solvent-assisted introduction of substances into an ion mobility spectrometer | |
| CN110391129A (en) | Ionization apparatus, mass spectrograph, ionic migration spectrometer and ioning method | |
| CN206225322U (en) | ESI ion source devices, mass spectrograph and liquid chromatography mass combined instrument | |
| CN108802161A (en) | A kind of method and apparatus of mass spectrum Thermal desorption sample introduction | |
| CN109425648A (en) | A kind of sample analysis method and device of fast pyrogenation analysis sample introduction | |
| CN209264371U (en) | Volatile organic matter enriching apparatus based on semiconductor chilling plate | |
| CN209591975U (en) | One kind being used for mass spectrometric ion source device | |
| US7270020B2 (en) | Instrument assemblies and analysis methods | |
| CN109979797A (en) | One kind being used for mass spectrometric ion source device and its application method | |
| CN205404478U (en) | A quick online atmospheric pressure photo ionization mass spectrum device for active ingredient among complicated matrix | |
| JP3808482B2 (en) | Ion source, mass spectrometry method and mass spectrometer | |
| CN114975069A (en) | Detection device and detection method for difficult-to-volatilize organic matters by laser desorption sample injection proton transfer reaction mass spectrum | |
| US8835838B2 (en) | Method and apparatus for analysis and ion source | |
| CN111220681B (en) | Thermal desorption sample injection ionization integrated ion generating device under atmospheric pressure |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |