CN105717188B - A kind of device of quick heating fluid sample - Google Patents
A kind of device of quick heating fluid sample Download PDFInfo
- Publication number
- CN105717188B CN105717188B CN201410735743.3A CN201410735743A CN105717188B CN 105717188 B CN105717188 B CN 105717188B CN 201410735743 A CN201410735743 A CN 201410735743A CN 105717188 B CN105717188 B CN 105717188B
- Authority
- CN
- China
- Prior art keywords
- sample
- hole
- sealing plate
- body recess
- capillary
- 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.)
- Active
Links
Abstract
The invention discloses a kind of device of quick heating fluid sample, including capillary seal screw, sealing plate, body recess, sample cell, bottom plate and magnetic valve.Wherein, sample well is provided with sample cell to be used to place fluid sample.The surrounding of body recess is provided with heating rod and is used to heat whole device.The bottom of sample cell is connected with magnetic valve and by the on and off of software control magnetic valve.Heater is set integrally to reach certain temperature the heating rod in body recess by temperature control software, the sample in sample cell is heated to volatilize and be introduced to mass spectrum by capillary and analyzed.Magnetic valve can be opened when changing and analyzing sample sample cell extraction is subjected to replacing sample.
Description
Technical field
Present invention is mainly applied to the gasification sample introduction of difficult volatilised liq sample, is exactly specifically to be waved difficulty using the device
Hair fluid sample continuously enters mass spectrum after being gasified and analyzed.
Background technology
In detection technique, mass spectrum detection with best resolution and qualitative ability because widely being paid close attention to.
Mass spectrum can provide abundant sample molecule structural information by ionizing, separating, detecting ion come authenticating compound sample.
In numerous analyzing detecting methods, Mass Spectrometry detection method is a kind of universal method for being provided simultaneously with high sensitivity and high efficiency, but
Mass spectrum needs to run under vacuum, and this results in the features such as the bulky of mass spectrometer, power consumption are high, expensive.It is right
In the mass spectrum of Liquid sample introduction, because volume can increase by 1000 times or so compared with original after liquid heating and gasifying, this is to mass spectrographic
Vacuum condition requires can be higher, so as to cause the volume of mass spectrum vacuum equipment huger.
More and more urgent to small-sized mass spectrographic demand with the fast development of society, the mass spectrum using VUV lamps as ionization source is
New development was got up in recent years, and it is mainly characterized by that the fragment peak after parent ion is ionized is few, and mass spectrogram is simply easy to identify.
In order to reduce mass spectrographic physical examination, the mass spectrum using VUV lamps as ionization source is mainly to detect sample by capillary direct injected, its
Simple in construction, the detection especially to effumability sample is very suitable.But this sample injection method is to difficult volatile liquid-like
When product are detected it is relatively difficult, it is necessary to hardly possible volatilization fluid sample handled accordingly, while it is also contemplated that instrument in
The vacuum system in portion, it is therefore desirable to find the analysis detection that new method carries out respective sample.
The present invention is that whole device is heated using the heating rod in body recess, makes the fluid sample in sample cell
Gasify after heated, and capillary is entered to enter analysis detection in mass spectrum by the through hole in body recess and sealing plate.This
Device has the characteristics that：
1st, the bottom of device is provided with magnetic valve, and the on and off of magnetic valve is controlled by sequential software, so as to realize control
The analysis time of sample and the replacing of sample.
2nd, the device can realize the analysis of continuous sample introduction, experiment it is reproducible.
The content of the invention
The present invention enters mass spectral analysis after carrying out heating and gasifying for the fluid sample of difficult volatilization, and the technical scheme of use is such as
Under：
A kind of device of quick heating fluid sample, including be arranged in order from top to bottom capillary seal screw, sealing
Plate, body recess, sample cell, bottom plate and magnetic valve.The middle part of capillary seal screw, which carries, to be used to wear the logical of capillary
Hole, capillary stretch into the platy structure that the sealing plate is upper surface center band cylindrical boss through capillary seal screw.In
Tapped manhole is provided with boss upper center, capillary seal screw is screwed together in manhole.In boss
Through hole is provided with the outside of upper rounded through hole.The body recess is cube structure, in cube bottom set through cube
The rectangular recess of wall at left and right sides of body, be provided with the bottom centre position of rectangular recess with cube upper surface
What is be connected at the heart is used for the through hole of gaseous sample transmission.The sample cell is rectangular parallelepiped structure, in sample cell upper surface
Heart opening position is provided with the blind hole for placing sample to be heated.Sample cell is placed through in rectangular recess, rectangular recess
The height and width of left and right sides end face are consistent with the height and width dimensions of end face at left and right sides of sample cell；The bottom plate is
Plate-like structure, bottom plate are placed in below sample cell and are fixedly connected with body recess, and the center position of plate upper surface is set
Fluted, bottom portion of groove is provided with through hole.The magnetic valve is placed in the groove of bottom plate, and the lower end of magnetic valve is from bottom plate groove
Through hole is stretched out, and upper surface and the sample cell lower surface of magnetic valve abut against.Set in being corresponded to respectively on sealing plate and body recess
The tapped mounting hole of more than 2 is equipped with, wherein screw rod is screwed with, it is by screw rod that sealing plate and body recess is affixed.
In the tapped mounting hole for being correspondingly arranged on more than 2 on bottom plate and body recess respectively, wherein being screwed with screw rod, pass through
Screw rod is affixed by bottom plate and body recess.It is used for the logical of gaseous sample transmission on manhole, body recess on sealing plate
The blind hole for being used to place sample to be heated on hole, sample cell is coaxial.It is provided with the outside of sealing plate boss upper rounded through hole logical
Hole, through hole are discharged for excessive gas, heat the gas volatilized and enter except a small amount of sample is introduced to analytical instrument by capillary
Row analysis is outer, and most gas can be discharged by the through hole of setting, prevent that the air pressure inside whole heater is too high.Sealing
Plate lower surface is provided with O-shaped seal groove, and O-ring seal is placed with O-shaped seal groove, makes sealing plate and master by O-ring seal
Body groove seals.Manhole and through hole on sealing plate are located at O-shaped seal groove.In being provided for putting in the side wall of body recess
The accommodating hole of heating rod and temperature sensor is put, the temperature of sample cell is adjusted by heating rod and temperature sensor, by sample cell
Interior sample heating volatilization.Sealed between capillary and capillary seal screw using cutting ferrule, and internal thread is carried with sealing plate
Manhole carry out fitted seal.Magnetic valve is using sequential software control on and off；When magnetic valve is opened, from body recess
Middle extraction sample cell carries out sample replacing；When closed electromagnetic valve, sample heating is carried out, the gaseous sample volatilized passes through capillary
Pipe is analyzed into mass spectrum.
Brief description of the drawings
Fig. 1 is a kind of schematic device of quick heating fluid sample；1-capillary seal screw, 2-sealing plate, 3-
Body recess, 4-sample cell, 5-bottom plate, 6-magnetic valve.
Embodiment
The present apparatus include be arranged in order from top to bottom capillary seal screw, sealing plate, body recess, sample cell, bottom
Plate and magnetic valve.Through hole at the through hole of through hole, body recess upper surface in device at sealing plate center, sample cell center with
And the through hole at bottom plate center is coaxial configuration.Capillary seal screw is arranged on the surface of sealing plate, capillary and sealing
Sealed between screw using cutting ferrule, prevent gas leakage.Fluid sample to be heated is positioned over the porose sample of center band during experiment
In pond, and heated using heating rod, the temperature of heating is by temperature control software design patterns, and temperature sensor is by the temperature of device
Fed back and shown in software, when the temperature of heating reaches the value of setting, mass spectrum carries out sample analysis again.Sealing
Platy structure with cylinder boss centered on plate, threaded through hole is provided with boss center and is entered with capillary seal screw
Row coordinate, outside the boss be provided with manhole be used for deflate use, heat the gas volatilized except a small amount of sample passes through capillary
Pipe is introduced in mass spectrum analyzed outside, most gas can be discharged by the through hole of setting, be prevented in whole heater
The air pressure in portion is too high, and sealing plate surrounding is provided with through hole and carries out compression sealing using O-ring and body recess.Bottom plate is center
Place is provided with the platy structure of through hole.Body recess is cube structure, bottom set it is fluted, the length and width of groove with
Sample pool size is consistent, and through hole is provided with the center of upper surface and is transmitted for gaseous sample, screwed hole is provided with the outside of through hole
Coaxial cooperation is carried out with the through hole of sealing plate surrounding, through hole is provided with the outside of groove, for placing heating rod and TEMP
Device.Bottom plate surrounding is provided with through hole and fixed for body recess with bottom plate.Magnetic valve is placed at bottom hole, and bottom plate leads at center
The size in hole is identical with magnetic valve size, and magnetic valve is using sequential software control on and off, when magnetic valve is opened, by sample cell
Extraction change it is next want testing sample, when closed electromagnetic valve, the sample that enters to serve a round of liquor to the guests heating, the gas sample volatilized after heating
Product enter capillary by through hole and then analyzed into mass spectrum.
Claims (8)
- A kind of 1. device of quick heating fluid sample, it is characterised in that：Including be arranged in order from top to bottom capillary seal screw (1), sealing plate (2), body recess (3), sample cell (4), Bottom plate (5) and magnetic valve (6)；The middle part of capillary seal screw (1) carries the through hole for being used for wearing capillary, capillary warp Capillary seal screw (1) is stretched into sealing plate (2)；The sealing plate (2) is the tabular of upper surface center band cylindrical boss Structure；Tapped manhole is provided with boss upper center, capillary seal screw (1) is screwed together in manhole It is interior；Sealing plate (2) lower surface is provided with O-shaped seal groove, compresses and seals for sealing plate (2) and body recess (3)；In convex Position between the outside of the screwed manhole in platform center and O-shaped seal groove is provided with through hole；The body recess (3) For cube structure, the rectangular recess through wall at left and right sides of cube is set in cube bottom, in rectangular recess Bottom centre position at be provided be connected with the center of cube upper surface be used for gaseous sample transmission through hole；It is described Sample cell (4) is rectangular parallelepiped structure, and the center position in sample cell (4) upper surface is provided with for placing sample to be heated Blind hole；Sample cell (4) is placed through in rectangular recess, the height and width and sample cell of the left and right sides end face of rectangular recess (4) height of left and right sides end face and width dimensions are consistent；The bottom plate (5) is plate-like structure, and bottom plate (5) is placed in sample It is fixedly connected below pond (4) and with body recess (3), the center position of bottom plate (5) upper surface sets fluted, groove-bottom Portion is provided with through hole；The magnetic valve (6) is placed in the groove of bottom plate (5), and the lower end of magnetic valve (6) is from bottom plate (5) groove Through hole is stretched out, and upper surface and sample cell (4) lower surface of magnetic valve (6) abut against.
- 2. device according to claim 1, it is characterised in that：In the tapped mounting hole for being correspondingly arranged on more than 2 on sealing plate (2) and body recess (3) respectively, wherein spiral shell Conjunction has screw rod, by screw rod that sealing plate (2) and body recess (3) is affixed；In the tapped mounting hole for being correspondingly arranged on more than 2 on bottom plate (5) and body recess (3) respectively, wherein screwing togather There is screw rod, it is by screw rod that bottom plate (5) and body recess (3) is affixed.
- 3. device according to claim 1, it is characterised in that：The through hole for being used for gaseous sample transmission, sample cell on manhole, body recess (3) on sealing plate (2) are used on (4) It is coaxial in the blind hole for placing sample to be heated.
- 4. device according to claim 1, it is characterised in that：Through hole is provided with the outside of tapped manhole at sealing plate (2) boss center, through hole is arranged for excessive gas Go out, heat the gas that volatilizes in addition to a small amount of sample by capillary is introduced to analytical instrument and analyzed, most gas It can be discharged by the through hole of setting, prevent that the air pressure inside whole heater is too high.
- 5. device according to claim 1, it is characterised in that：Sealing plate (2) lower surface is provided with O-shaped seal groove, is placed with O-ring seal in O-shaped seal groove, is made by O-ring seal Sealing plate (2) seals with body recess (3)；Tapped manhole and the through hole at sealing plate (2) convex platform center The through hole set between O-shaped seal groove is respectively positioned on the inside of O-shaped seal groove.
- 6. device according to claim 1, it is characterised in that：In the accommodating hole for being provided for placing heating rod and temperature sensor in the side wall of body recess (3), by heating rod and The temperature of temperature sensor regulation sample cell (4), the sample in sample cell (4) is heated into volatilization.
- 7. device according to claim 1, it is characterised in that：Sealed between capillary and capillary seal screw (1) using cutting ferrule, and with sealing plate (2) with female circular logical Hole carries out fitted seal.
- 8. device according to claim 1, it is characterised in that：Magnetic valve (6) is using sequential software control on and off；When magnetic valve (6) is opened, sample is extracted out from body recess (3) Pond (4) carries out sample replacing；When magnetic valve (6) is closed, sample heating is carried out, the gaseous sample volatilized enters by capillary Enter mass spectrum to be analyzed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410735743.3A CN105717188B (en) | 2014-12-05 | 2014-12-05 | A kind of device of quick heating fluid sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410735743.3A CN105717188B (en) | 2014-12-05 | 2014-12-05 | A kind of device of quick heating fluid sample |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105717188A CN105717188A (en) | 2016-06-29 |
| CN105717188B true CN105717188B (en) | 2018-03-20 |
Family
ID=56143764
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410735743.3A Active CN105717188B (en) | 2014-12-05 | 2014-12-05 | A kind of device of quick heating fluid sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105717188B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111781297B (en) * | 2019-04-04 | 2022-09-16 | 中国石油化工股份有限公司 | Simple liquid flammability tester based on high-temperature silicon carbide rod and application thereof |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3077827B2 (en) * | 1991-09-17 | 2000-08-21 | 株式会社日立製作所 | Mass spectrometer |
| JPH05251038A (en) * | 1992-03-04 | 1993-09-28 | Hitachi Ltd | Plasma ion mass spectrometry device |
| CN101294933B (en) * | 2007-04-24 | 2012-01-25 | 中国科学院大连化学物理研究所 | Surface gas flow purging thermal desorption sampling device |
| 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 |
| CN103163013B (en) * | 2011-12-15 | 2015-04-08 | 中国科学院大连化学物理研究所 | Thermal analysis and permeable membrane compound device for solid and liquid sample injection |
| CN203606200U (en) * | 2013-12-05 | 2014-05-21 | 中国科学院大连化学物理研究所 | Rapid thermal desorption sampling device |
-
2014
- 2014-12-05 CN CN201410735743.3A patent/CN105717188B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105717188A (en) | 2016-06-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105181419B (en) | The online and offline detection means and detection method of volatile organic matter in a kind of ultrasonic atomizatio extraction water body | |
| CN203606200U (en) | Rapid thermal desorption sampling device | |
| CN103165388A (en) | Device for mass flow air enrichment analysis mass spectrum sampling in confined space | |
| CN105223122B (en) | A kind of bolt-type core holding unit | |
| TW200739051A (en) | Method and apparatus for spectroscopic analysis | |
| CN205355001U (en) | High atmospheric pressure mass spectrum buffering air inlet unit | |
| CN105717188B (en) | A kind of device of quick heating fluid sample | |
| CN103439150B (en) | A kind of footwear VOC volatilization sampling apparatus and method | |
| CN103094050B (en) | A kind of sensitive glow discharge direct ionization method and device thereof | |
| CN104716001B (en) | A kind of liquid continuous sample introduction device of heating and gasifying | |
| CN209264371U (en) | Volatile organic matter enriching apparatus based on semiconductor chilling plate | |
| CN107290363A (en) | High pressure low temperature in-situ neutron scattering device | |
| CN103439400A (en) | Integrated device used for analyzing trace atmosphere contained in micro volume component | |
| CN203367224U (en) | Normal pressure direct ionization mass spectrum device of concealed ion source | |
| CN204188340U (en) | Product waterproof detection device | |
| CN207472839U (en) | A kind of Thermal desorption module of double cold-traps | |
| CN203519375U (en) | Airflow type combustible liquid sample extraction device | |
| CN203479578U (en) | Footwear VOC (volatile organic compound) volatilization sampling equipment | |
| CN205157490U (en) | But spiral tubulose membrane enrichment device of water -cooling cooling | |
| CN203432939U (en) | Integrated device for analyzing trace atmosphere contained in micro-volume element | |
| CN108181138B (en) | Gas taking device of hydrocarbon source rock hydrocarbon generation thermal simulation reaction kettle | |
| CN111220681B (en) | Thermal desorption sample injection ionization integrated ion generating device under atmospheric pressure | |
| CN104133026B (en) | The oil product pre-treatment degas method of transformer insulated oil gas chromatographic | |
| CN203216933U (en) | Multifunctional continuous sampler for analytical instrument | |
| CN215066398U (en) | Device for analyzing aroma components |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |