CN105738542B - A kind of nozzle assembly for miniature flame ionization ditector - Google Patents
A kind of nozzle assembly for miniature flame ionization ditector Download PDFInfo
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- CN105738542B CN105738542B CN201410772021.5A CN201410772021A CN105738542B CN 105738542 B CN105738542 B CN 105738542B CN 201410772021 A CN201410772021 A CN 201410772021A CN 105738542 B CN105738542 B CN 105738542B
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- cutting ferrule
- skirt
- nozzle
- nozzle assembly
- detector body
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Abstract
The present invention provides a kind of nozzle assembly for miniature flame ionization ditector (μ FID), is made up of nozzle, skirt, upper cutting ferrule, sleeve pipe, lower cutting ferrule, detector body and stubborn cap.When stubborn cap is tightened upwards, the top conical bench-type sealing surface of two cutting ferrules is extruded above and below the cone type sealing surface of second groove of detector body endoporus and the rounding taper type sealing surface of stubborn cap, the metal sleeve in the middle of two cutting ferrules extrudes the base plane of two cutting ferrules simultaneously so that the cone type sealing surface of upper cutting ferrule can seal the cone type sealing surface sealing lower channel (being connected with hydrogen) of upper channel, lower cutting ferrule.The nozzle assembly of the present invention has advantages below：Sealed mechanical structure is simple, compact, reliable；Length component is short, reduces μ FID volume；Reduce the dead volume of combustion chamber, air stream is more stable so that μ FID noises are smaller；And nozzle assembly is readily replaceable.
Description
Technical field
The present invention relates to flame ionization ditector technical field, more specifically to a kind of miniature hydrogen flame from
The nozzle assembly of sonization detector.
Background technology
Flame ionization ditector (FID) is most widely used detector on gas chromatograph, and such detector makes
Make ionization source with hydrogen flame, ionize measured matter, the micro-current of generation is detected after being exaggerated.FID outstanding advantages are to several
All organic matters have response, particularly high (ppb grades) to hydrocarbon compound sensitivity, and response is with carbon number into just
Than；It is insensitive to inorganic matter；The change of the operating conditions such as gas flow rate, pressure and temperature responses to which that influence is also little；FID line
Property scope up to 6-7 order of magnitude, the time constant of detector in itself is between 2-5ms, and dead volume is almost nil, it is simple in construction,
It is easy to operate.Portable minisize gas chromatograph is because of its live real-time analytical capability by most attention.Tradition
FID because volume is big, high energy consumption and work gas consumption are high, be not appropriate for portable minisize gas chromatograph.Developed country
Miniature flame ionization ditector (μ-FID) all is being studied, the miniaturization of flame ionization ditector has important grind
Study carefully meaning and practical value.We by further investigate routine FID structure and principle, it was found that combustion air influence base flow make an uproar
The reason for sound, the incorporation way and detector structure of combustion air are redesigned, air has been introduced from the top of detector, it is empty
Gas by upper spiral and under, stable flow field is formed in flame periphery, then turns round supreme, is flowed out by collector centre bore again, had
Inhibit to effect the noise level of detector；Employ high field intensity (800V polarizing voltages) and improve spout particle emission density and first
Speed, while suppressing to produce secondary electron, hence it is evident that improve ionizing efficiency, realizing μ-FID has higher letter than commercialization FID
Make an uproar ratio, and 70% or so (Jianwei Wang, Hua Wang, Chunfeng Duan, Yafeng of gas consumption reduction
Guan*,Micro-flame ionization detector with a novel structure for portable gas
chromatograph,Talanta,82,1022-1026,2010；Guan Yafeng, Wang Jianwei, the primary track universe, Ni Lijuan, Xiong Yan are a kind of
Small-size hydrogen flame ionization detector, Chinese invention patent, the patent No.：ZL200810229985.X).
One layer of resistant to elevated temperatures insulating sleeve of the skirt overcoat of the μ-FID, to ensure the insulated electro between nozzle and shell
Resistance >=109Ohm.The sealing means of skirt are first with cutting ferrule by high-temp.-resisting insulation sleeve crush seal, if the high temperature resistant 1. used
Insulating sleeve elasticity is preferable, such as polytetrafluoroethylene (PTFE), then by itself and skirt crush seal together；If the high-temperature insulation set 2. used
Elastic bad, such as ceramics of pipe, then be specifically shown in two implementations of the patent with refractory inorganic adhesive by itself and skirt adhering and sealing
Example.Upper air chamber and lower hydrogen chamber all use this sealing means.But this sealing means increase complexity increases body simultaneously
Product：1. two-way is provided between air chamber seal cutting ferrule and combustion chamber, is increased simultaneously which increase complicated in mechanical structure degree
Nozzle assembly, add detector volume；2. it must be provided with above hydrogen chamber hermetic collar and tighten stubborn cap, which increases
Complicated in mechanical structure degree increases nozzle assembly, adds detector volume simultaneously；3. two it is connected with certain length, and air chamber
The seal point of hermetic collar is below two-way, which increase the dead volume of combustion chamber and air stream micro-disturbance, and it is unreliable to add
Factor.
The content of the invention
In order to improve the deficiencies in the prior art, the present invention, which is provided, a kind of new is used for miniature flame ionization ditector
Nozzle assembly, the problem of existing μ-FID sealing machines are complicated, nozzle assembly is long is efficiently solved, while also carrying
The high reliability of detector mentioned nozzle area.
The technical scheme is that：
A kind of nozzle assembly for miniature flame ionization ditector include nozzle, skirt, upper cutting ferrule, sleeve pipe, under
Cutting ferrule, detector body and stubborn cap；Nozzle and skirt are respectively the straight pipe of two end openings；Upper cutting ferrule and lower cutting ferrule are along axis
The cylinder of through hole is offered, the top of cylinder is provided with the sealing surface of truncated cone；
The lower surface of detector body offers tapped circular groove, and it is recessed to offer second in the bottom of circular groove
Groove, the bottom of the second groove is the cone type coordinated with the top conical bench-type sealing surface of upper cutting ferrule, in the upper of cone type
Bottom surface offers manhole, the radial section of manhole and the upper bottom surface area equation of cone type, circular groove, second
The cone type bottom of groove and manhole are coaxially disposed, and form a hollow detector body；The lower end insertion skirt of nozzle
Upper open end, nozzle and skirt be placed in inside detector body, and nozzle and skirt and the manhole of detector body are coaxially disposed；
Be coated with upper cutting ferrule, sleeve pipe, lower cutting ferrule successively under by upper in skirt outside wall surface inside detector body, and upper cutting ferrule and
The sealing surface of the truncated cone of lower cutting ferrule is in one end away from sleeve pipe, and the other end of upper cutting ferrule and lower cutting ferrule connects with sleeve pipe
Touch；
Be screwed with the tapped circular groove of detector body with externally threaded stubborn cap, twist cap upper surface be provided with
The rounding frustum connected in star that the top conical bench-type sealing surface of lower cutting ferrule coordinates, is offered in the bottom surface of rounding frustum connected in star
Manhole, the radial section of manhole and the bottom surface area equation of rounding frustum type, rounding frustum connected in star and circle
The cone type bottom and manhole of through hole and the second groove of detector body are coaxially disposed；The medial side wall of detector body
Provided with a through hole, contact pilotage connects through through hole with sleeve pipe.
The material of nozzle, skirt and sleeve pipe is metal, preferably stainless steel；The material of upper cutting ferrule and lower cutting ferrule is that polyamides is sub-
Amine or Vespel or other high temperature resistant and insulaion resistance are more than 1010The high polymer material of ohm.
The internal diameter of the nozzle is 0.05-0.3mm, and external diameter is 0.15-0.7mm；Nozzle stretches into the length with stretching out skirt
It is 3-5mm.The internal diameter 0.5-1.2mm of the skirt, external diameter 0.8-2.0mm, long 15-35mm；Pass through mechanical compaction or welding
Mode will be sealed at the two contact gap.
By the base plane that upper cutting ferrule and lower two cutting ferrules of cutting ferrule are extruded above and below sleeve pipe；And size design ensures extruding
Afterwards, sleeve pipe is contacted well with skirt, and polarizing voltage is added on nozzle by contact pilotage, sleeve pipe and skirt.
Skirt is higher by cutting ferrule 0.5-2.5mm, it is low go out lower cutting ferrule 0.5-2.5mm, can with upper cutting ferrule and lower cutting ferrule before extruding
Coordinate for gap or tight fit.
The external diameter of the top conical bench-type sealing surface of the upper cutting ferrule and lower cutting ferrule is outside 3.5-7mm, bottom cylinder
Footpath is 5-10mm, high 4-8mm, 30-90 ° of cone angle.
The external diameter of described sleeve pipe is 4-8mm, high 4-8mm, can be coordinated before extruding with skirt for gap or tight fit, after extruding
Contacted well with skirt.
The material of the detector body, stubborn cap and contact pilotage is metal, preferably stainless steel.
During installation, the top conical bench-type sealing surface of the upward lower cutting ferrule of cap is twisted, the base plane of lower cutting ferrule is squeezed upwards
Gland pipe, the base plane of the upward upper cutting ferrule of sleeve pipe, detector body is pressed down against the top conical bench-type sealing of cutting ferrule
Face；Sleeve pipe and stubborn cap two cutting ferrules of extruding above and below to the top conical bench-type sealing surface and sleeve pipe of two cutting ferrules of extruding up and down
Base plane is used cooperatively, air chamber, lower hydrogen chamber and two cutting ferrules contact with skirt outer radius gap in sealing, it is ensured that spray
Nozzle assembly is air tight；Single piece is formed after nozzle assembly crush seal.
The present invention actually will according to machinery and material principles, the innovative mechanical structure for devising nozzle assembly
The polyimides that the cutting ferrule and high-temp.-resisting insulation sleeve integrator, i.e., a pair of prior art (ZL200810229985.X) are new is bored
Shape cutting ferrule, up and down with the use of crush seal；Further according to machinery and material principles, it is equipped with the middle of two cutting ferrules above and below hard metal pipe
Support, realizes simple seal；Metal tube may be incorporated into polarizing voltage to nozzle in addition to supporting role；Parts are equal
It is one multi-functional.This is it is avoided that use two-way in the prior art between air chamber seal cutting ferrule and combustion chamber, and hydrogen
Stubborn cap is tightened above chamber hermetic collar, air chamber and lower hydrogen chamber is sealed simple, compact, reliable.Nozzle assembly is extruded
Single piece, convenient dismounting, cleaning are formed after sealing.
On the other hand, the flexible deformation of polyimides, can be used for crush seal.Volume of the polyimides at 300 DEG C
Resistance is 1011-1012Ω/cm, it is ensured that still have good electrical insulation capability under μ-FID high temperature；Fire resistant polyimide is long-term
Temperature in use is more than 300 DEG C, and glass transition temperature is more than 320 DEG C, all aromatic polyimides of du pont company's production
(Vespel) it is even more no glass transition temperature, the resistance to pressure of long term high temperature will not soften.Using polyimide material also ensure that μ-
FID has insulation and the pressure-resistant seal performance of stabilization at high temperature.After technical scheme, the μ-FID of prior art
Nozzle assembly length halve, skirt shortens 17mm by 35mm, and performance is more preferably.
During using such scheme, it is used to insulate and seal using polyimide material, adds cooperation crush seal mode, make
New μ-FID can be in steady in a long-term, reliably working at 300-350 DEG C, and μ-FID further advantage, such as air consumption reduce 70%
Deng not changing.
Compared with prior art, nozzle assembly of the invention has the following advantages that：
1st, it is innovative devise above and below taper cutting ferrule and the hard metal pipe of centre coordinate extruding with detector body and stubborn cap
Sealing means, without additional two-way and stubborn cap, make sealing machine structure simpler.
2nd, new Seal Design is without additional two-way and stubborn cap, makes that nozzle assembly is more compact, length halves, reduce μ-
FID volume.
3rd, according to machinery and material principles design, compared to μ-FID before, up and down taper cutting ferrule and centre hard metal
Pipe is all one multi-functional.
4th, new nozzle assembly structure make combustion chamber dead volume and air stream micro-disturbance it is smaller, be conducive to improving μ-FID
Stability.
5th, single piece, convenient dismounting, cleaning are formed after new nozzle assembly crush seal.
6th, taper cutting ferrule is using flexible, high-temperature insulation and seals all preferably polyimide materials, it is ensured that μ-FID
There are stable insulation and pressure-resistant seal performance at 300-350 DEG C of high temperature.
Brief description of the drawings
Fig. 1 is the diagrammatic cross-section of nozzle assembly.In figure：Block under 1- nozzles, 2- skirts, the upper cutting ferrules of 3-, 4- sleeve pipes, 5-
Set, 6- detector bodies, 7- twists hydrogen chamber under cap, 8- contact pilotages, the upper air chambers of 9-, 10-.
Fig. 2 is the μ-FID developed using the new nozzle assembly of the design experiment spectrogram.
Fig. 3 is the experiment spectrogram for the μ-FID that existing patent ZL200810229985.X is developed.
Embodiment
Two taper polyimides cutting ferrules pole that will polarize is insulated with ground up and down, μ-FID is had at 300-350 DEG C excellent exhausted
Edge performance；The air from top to bottom supreme region for flowing through cutting ferrule 3, skirt 2 and nozzle 1 again, detector body is pressed down against card
The top conical surface of set 3 and the base plane of the upward upper cutting ferrule 3 of sleeve pipe 4, make the contact with skirt 2 of cutting ferrule 3 and upper cutting ferrule 3
Sealed at gap air tight；Hydrogen flows through the region of skirt 2 and lower cutting ferrule 5 from the bottom to top, twists the top of the upward lower cutting ferrule 5 of cap
Portion's conical surface and sleeve pipe 4 are pressed down against the base plane of lower cutting ferrule 5, make at lower cutting ferrule 5 and lower cutting ferrule 5 contact with skirt 2 gap
Sealing is air tight；Said process ensure that μ-FID have excellent sealing property at 300-350 DEG C.
Embodiment 1
Using new nozzle assembly develop μ-FID, its diagrammatic cross-section as shown in figure 1, by nozzle 1, skirt 2, upper cutting ferrule 3,
Sleeve pipe 4, lower cutting ferrule 5 and detector body 6 are constituted.The material of nozzle 1, skirt 2 and sleeve pipe 4 is stainless steel, upper cutting ferrule 3 and lower cutting ferrule
5 material is high temperature resistant all aromatic polyimides.The internal diameter of nozzle 1 is 0.18mm, and external diameter is 0.38mm, nozzle 1 stretch into
The length for stretching out skirt 2 is 3mm, covers last layer external diameter 0.6mm between nozzle 1 and skirt 2 again, internal diameter 0.4mm stainless steel tube,
First three stainless steel tubes of mechanical compaction make it coaxially fix, and gas leakage is prevented then at seam crossing silver soldering.The internal diameter 0.8mm of skirt 2, outside
Footpath 1.6mm, long 17mm；Skirt 2 is higher by 1-2mm than upper cutting ferrule 3, it is lower than lower cutting ferrule 5 go out 1-2mm, extruding before with upper cutting ferrule 3 and under
The gap of cutting ferrule 5 coordinates.The top diameter 4mm of upper cutting ferrule 3 and lower cutting ferrule 5, base diameter 6mm, high 5mm, 35 ° of cone angle；Detector
The cone of the cone angle of the cone type sealing surface of the groove of inside second of body 6 and the inner upper rounding taper type sealing surface of stubborn cap 7
Angle is 40 °.External diameter 5mm, the high 5mm of sleeve pipe 4, coordinate with the gap of skirt 2 before extruding, are contacted well with skirt 2 after extruding, pole
Change voltage to be added on nozzle 1 by contact pilotage 8, sleeve pipe 4 and skirt 2.Detector body 6 and stubborn cap 7 two cutting ferrules of extruding above and below
Top conical bench-type sealing surface and sleeve pipe 4 are used cooperatively to the base plane for extruding two cutting ferrules up and down, air chamber in sealing, under
Hydrogen chamber and two cutting ferrules and the contact gap of the outer radius of skirt 2 are air tight.
Fig. 2 is the μ-FID of the nozzle assembly using the technical program chromatogram, and chromatographic condition is：OV-1 chromatographic columns, it is interior
Footpath 0.32mm, long 30m, 0.4 μm of thickness；Carrier gas hydrogen flowing quantity 4ml/min, combustion gas hydrogen flowing quantity 8ml/min, helps gas-air
Flow 96ml/min；150 DEG C of injection port, 40 DEG C of post case, 300 DEG C of detector, sample introduction 1000ppm n-hexane/acetones.Can by figure
See, the baseline of detector is very stable at 300 DEG C, and the detection to n-hexane is limited to 0.5pg/s.
Use prior art (Jianwei Wang, Hua Wang, Chunfeng Duan, Yafeng Guan*, Micro-
flame ionization detector with a novel structure for portable gas
chromatograph,Talanta,82,1022-1026,2010；A kind of small-size hydrogen flame ionization detector, Chinese invention is special
Profit, ZL200810229985.X) embodiment 1 disclosed in μ-FID.Because insulating sealing materials use polytetrafluoroethylene (PTFE), highest
Long-term service temperature only has 200-220 DEG C.If 300 DEG C repeatedly heating and cooling use, the baseline of detector will be unstable, occur
Irregular bob, and big burr is accompanied by, as shown in Figure 3.
It can be seen that, after technical scheme, μ-FID nozzle assembly is simple in construction, contraction in length half, and
Performance more preferably, is resistant to higher operating temperature.
The present invention will not be restricted to embodiment illustrated herein, and be to fit to and General Principle disclosed herein and new
The consistent widest range of clever feature.All any changes without creative work made according to design philosophy of the present invention are all at this
Within the protection domain of invention.
Claims (8)
1. a kind of nozzle assembly for miniature flame ionization ditector, it is characterised in that：Including nozzle（1）, skirt
（2）, upper cutting ferrule（3）, sleeve pipe（4）, lower cutting ferrule（5）, detector body（6）With stubborn cap（7）；Nozzle（1）And skirt（2）Respectively two
The straight pipe of end opening；Upper cutting ferrule（3）With lower cutting ferrule（5）To offer the cylinder of through hole, the top of cylinder along axis
Sealing surface provided with truncated cone；
Detector body（6）Lower surface offer tapped circular groove, it is recessed to offer second in the bottom of circular groove
Groove, the bottom of the second groove is and upper cutting ferrule（3）Top conical bench-type sealing surface coordinate cone type, in cone type
Upper bottom surface offers the first manhole, the radial section of the first manhole and the upper bottom surface area equation of cone type, circle
Connected in star, the cone type bottom of the second groove and the first manhole are coaxially disposed, and form a hollow detector body（6）；
Nozzle（1）Lower end insertion skirt（2）Upper open end, nozzle（1）And skirt（2）It is placed in detector body（6）Inside, spray
Mouth（1）And skirt（2）With detector body（6）The first manhole be coaxially disposed；In detector body（6）Internal skirt
（2）In outside wall surface upper cutting ferrule is coated with successively under by upper（3）, sleeve pipe（4）With lower cutting ferrule（5）, and upper cutting ferrule（3）With lower cutting ferrule
（5）The sealing surface of truncated cone be in away from sleeve pipe（4）One end, upper cutting ferrule（3）With lower cutting ferrule（5）The other end and set
Pipe（4）It is in contact；
In detector body（6）It is screwed with tapped circular groove with externally threaded stubborn cap（7）, twist cap（7）Upper surface
Provided with lower cutting ferrule（5）Top conical bench-type sealing surface coordinate rounding frustum connected in star, under rounding frustum connected in star
Bottom surface offers the second manhole, the radial section of the second manhole and the bottom surface area equation of rounding frustum type, falls
Truncated cone groove and the second manhole and detector body（6）The second groove cone type bottom and the first manhole
It is coaxially disposed；Detector body（6）Medial side wall be provided with a through hole, contact pilotage（8）Through through hole and sleeve pipe（4）Connect.
2. according to the nozzle assembly described in claim 1, it is characterised in that：Pass through sleeve pipe（4）Upper cutting ferrule is extruded up and down（3）With under
Cutting ferrule（5）The base plane of two cutting ferrules；And size design ensures after extruding, sleeve pipe（4）With skirt（2）Contact is good, polarization
Voltage passes through contact pilotage（8）, sleeve pipe（4）And skirt（2）It is added to nozzle（1）On.
3. the nozzle assembly according to claims 1, it is characterised in that：Described nozzle（1）, skirt（2）And sleeve pipe
（4）Material be metal；Upper cutting ferrule（3）With lower cutting ferrule（5）Material is polyimides or other high temperature resistant and insulaion resistance is big
In 1010The high polymer material of ohm.
4. nozzle assembly according to claim 1, it is characterised in that：The nozzle（1）Internal diameter be 0.05-0.3 mm,
External diameter is 0.15-0.7 mm；Skirt（2）Internal diameter 0.5-1.2 mm, external diameter 0.8-2.0 mm, long 15-35 mm, nozzle（1）Stretch
Enter with stretching out skirt（2）Length be 3-5 mm, will be sealed by mechanical compaction or welding manner at the two contact gap.
5. nozzle assembly according to claim 1, it is characterised in that：Described skirt（2）It is higher by cutting ferrule（3）0.5-
2.5 mm, it is low go out lower cutting ferrule（5）0.5-2.5 mm, with upper cutting ferrule before extruding（3）With lower cutting ferrule（5）Gap coordinates or tight fit.
6. nozzle assembly according to claim 1, it is characterised in that：The upper cutting ferrule（3）With lower cutting ferrule（5）Top circle
The external diameter of frustum type sealing surface is 3.5-7 mm, and the external diameter of bottom cylinder is 5-10 mm, high 4-8 mm, 30-90 ° of cone angle.
7. nozzle assembly according to claim 1, it is characterised in that：Described sleeve pipe（4）External diameter 4-8 mm, high 4-8
Mm, extrudes preceding and skirt（2）Coordinate for gap or tight fit, with skirt after extruding（2）Contact is good.
8. nozzle assembly according to claim 1, it is characterised in that：The detector body（6）, twist cap（7）And contact pilotage（8）
Material be metal.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410772021.5A CN105738542B (en) | 2014-12-11 | 2014-12-11 | A kind of nozzle assembly for miniature flame ionization ditector |
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| CN201410772021.5A CN105738542B (en) | 2014-12-11 | 2014-12-11 | A kind of nozzle assembly for miniature flame ionization ditector |
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| CN105738542A CN105738542A (en) | 2016-07-06 |
| CN105738542B true CN105738542B (en) | 2017-08-25 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107477581B (en) * | 2017-08-21 | 2023-06-27 | 宁波艾克米金属工贸有限公司 | Cutting nozzle structure |
| CN110749686B (en) * | 2018-07-24 | 2021-08-10 | 中国科学院大连化学物理研究所 | Nozzle assembly for miniature hydrogen flame ionization detector |
| EP3911946A4 (en) * | 2019-01-14 | 2022-10-19 | Agilent Technologies, Inc. | Versatile tube-free jet for gc detector |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1335347A (en) * | 1970-01-24 | 1973-10-24 | Becker Delft Nv | Gas chromatography apparatus |
| NL7703583A (en) * | 1977-04-01 | 1978-10-03 | Wti Instr | FLAME IONIZATION DETECTOR. |
| SU762540A1 (en) * | 1977-12-15 | 1986-03-15 | Sp K B I Orch Khim Im N D Zeli | Flame-ionization detector |
| SU1608576A1 (en) * | 1989-01-20 | 1990-11-23 | Всесоюзный научно-исследовательский и конструкторский институт хроматографии | Flame-ionization detector |
| CN2524244Y (en) * | 2002-02-10 | 2002-12-04 | 复旦大学 | Miniature flame ionizing detector |
| CN101750463B (en) * | 2008-12-19 | 2012-07-25 | 中国科学院大连化学物理研究所 | Small-size hydrogen flame ionization detector |
| CN203981645U (en) * | 2014-06-21 | 2014-12-03 | 克拉玛依广陆有限责任公司 | The burner noz(zle) device of gas chromatograph fid detector for well logging |
| CN104181264B (en) * | 2014-08-19 | 2015-12-30 | 北京大学 | A kind of pressure hydrogen flame ionization detector |
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2014
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