CN106783510A - A kind of preparation method of electron spray nozzle needle - Google Patents
A kind of preparation method of electron spray nozzle needle Download PDFInfo
- Publication number
- CN106783510A CN106783510A CN201611246642.5A CN201611246642A CN106783510A CN 106783510 A CN106783510 A CN 106783510A CN 201611246642 A CN201611246642 A CN 201611246642A CN 106783510 A CN106783510 A CN 106783510A
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- CN
- China
- Prior art keywords
- capillary
- nozzle needle
- spray nozzle
- electron spray
- preparation
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0404—Capillaries used for transferring samples or ions
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
- H01J49/165—Electrospray ionisation
- H01J49/167—Capillaries and nozzles specially adapted therefor
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Nozzles (AREA)
Abstract
The invention discloses a kind of electron spray nozzle needle preparation method.The refractory metal silk that external diameter is determined passes through quartz capillary, and nozzle needle is drawn under subsequent high temperature.The present invention is before wire is penetrated first using liquid pump to injecting lubricating fluid in capillary, hot fusing process quartz capillary then removes thermal source to two side stretchings, with capillary cutter by quartz capillary heating part central cutout, extract wire out, obtain determining the electron spray nozzle needle of bore.The inventive method is easy to operate, efficient stable, and prepared nozzle needle bore is controllable, inner wall smooth.
Description
Technical field
Regulation and control electron spray nozzle needle preparation method be can stablize the invention discloses a kind of bore, analytical chemistry and protein belonged to
Group field.
Background technology
The different complex biological sample of, wide dynamic range various for composition species, structural form, high performance liquid chromatography matter
Spectrum GC-MS is the strong means that analysis is separated to it.The wherein object such as polypeptide, polysaccharide, protein carries a large amount of diseases
Sick relevant biomarkers, their qualitative and quantitative analysis play indispensable effect for the diagnosis and treatment of disease.
It is electric spray ion source that current liquid chromatography mass is combined the most widely used ionization technique, uses electron spray
Nozzle needle, is not only the bridge linked between liquid chromatogram and mass spectrum, while being also the key factor for determining ionizing efficiency.Nozzle needle goes out
Intraoral footpath has material impact for the spray discharge pattern of electric spray ion source, voltage, Ionization Efficiency.
Current market commercialization prepares the instrument of electron spray nozzle needle, does not have any control measure for nozzle needle bore, and adopts
The relatively cumbersome complexity of operating process of nozzle needle internal diameter is controlled with chemical etching method, gained nozzle needle outer wall is simultaneously unsmooth, it is also difficult to
Ensure that inwall is not corroded completely.Therefore needs are designed and develop one kind simple and effective can control electron spray needle outlets internal diameter
Method, and use it for the preparation of electron spray nozzle needle.
The content of the invention
The shortcoming of prior art, simple and effective electricity can be controlled it is an object of the invention to provide one kind in view of the above
The method of spraying needle outlets internal diameter, and use it for the preparation of electron spray nozzle needle.
In order to achieve the above object, the present invention is adopted the following technical scheme that：A kind of preparation method of electron spray nozzle needle, the party
Method is comprised the following steps：
1) thermal source and a capillary for being previously implanted lubricating fluid are provided；
2) wire of the fusing point higher than the heat source temperature is provided；
3) wire is penetrated in the capillary；
4) thermal source is positioned over the capillary midsection for melting the capillary；While the wire two ends
Reciprocate vertically；The capillary is then rotated and to two side stretchings along central shaft, then removes thermal source, stops the hair
The rotation of tubule and stretching, the wire continue to reciprocate vertically；
5) capillary midsection using cutter above the thermal source cuts off the capillary；
6) extract wire out to form electron spray nozzle needle from capillary two ends respectively.
In the present invention, the wire external diameter is 1~1000 micron；The wire length is slightly longer than capillary.
In the present invention, the capillary inner diameter is 1~1000 micron, and length is 10~1000 millimeters.
In the present invention, the lubricating fluid is preferably water, ethanol or methyl alcohol.
In the present invention, preferred liquid pump, peristaltic pump or needle tubing are previously implanted lubricating fluid in the capillary.
In the present invention, the thermal source provides 1700 DEG C of temperatures above, preferably Gas spray gun or laser.
In the present invention, the cutter is preferably potsherd, sheet glass or diamond chip cutter.
In the present invention, melting center 30mm scope internal cutting of the cutter above the thermal source.
The present invention has advantages below：
1) once-through operation flow can obtain two internal diameter identical electron spray nozzle needles, be easy to control, can control as needed
Nozzle needle bore processed；
2) operating process is easy, can in a short time prepare the controllable electron spray nozzle needle of a large amount of internal diameters, is easy to screening
Performance is more preferable, internal diameter more suitably nozzle needle；
3) gained nozzle needle inner wall smooth, Ionization Efficiency is higher.
Brief description of the drawings
Fig. 1 is that the present invention prepares operation chart of the controllable with diameter of axle electron spray nozzle needle method；
Fig. 2 is the schematic diagram in heating process of the present invention；
Fig. 3 is the nozzle needle schematic diagram formed after present invention heating terminates；
Component label instructions
Wire 1
Capillary 2
Thermal source 3
Prepare the nozzle needle 4 for completing
Specific embodiment
Embodiments of the present invention are illustrated below by way of specific instantiation, those skilled in the art can be by this specification
Disclosed content understands other advantages of the invention and effect easily.The present invention can also be by specific realities different in addition
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints with application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
As shown in figure 1, for the present invention prepares operation chart of the controllable with diameter of axle electron spray nozzle needle method, it includes gold
Category silk 1, capillary 2 (preferably quartz capillary in the present invention) and thermal source 3.The preparation method of electron spray nozzle needle of the present invention, the party
Method is comprised the following steps：
1) thermal source 3 is provided and one the capillary 2 of lubricating fluid is previously implanted；
2) wire of the fusing point higher than the temperature of the thermal source 3 (maximum temperature) is provided；
3) wire 1 is penetrated in the capillary 2；
4) thermal source 3 is positioned over the capillary midsection for melting the capillary；While the wire two
End reciprocates vertically；The capillary is then rotated and to two side stretchings along central shaft, then removes thermal source, is stopped described
The rotation of capillary and stretching, the wire continue to reciprocate vertically；
5) capillary midsection using cutter above the thermal source cuts off the capillary；
6) extract wire out to form electron spray nozzle needle 4 from the two ends of capillary 2 respectively.
Concrete operation step of the present invention is as follows：1) length range is chosen at 10~1000 millimeters, and inside diameter ranges are 1~1000
The quartz capillary 2 one of micron, water is filled using liquid pump thereto；2) to one length range of insertion in quartz capillary 2
In 1~1000 millimeter, wire 1 of the external diametrical extent at 1~1000 micron；3) capillary, period wire are heated using thermal source 3
1 two ends are constantly axially moveable, and quartz capillary 2 then along central axis and along central axial two side stretching, then removes heat
Source 3；4) rotation and stretching of quartz capillary 2 are stopped, wire 1 is pulled on；5) with capillary cutter by quartzy capillary
The heating part central cutout of pipe 2, extracts wire 1 out, you can obtain the controllable electron spray nozzle needle 4 of bore.
Specifically, in the present embodiment, first providing following material and instrument：Internal diameter is 75 microns of quartz capillary 2 one,
It is long 20 centimetres；Internal diameter is 20 microns of 1 one, tungsten filament, long 25 centimetres；Gas burner 3 one；One, water pump；Capillary cutter
One.
Using the method for the present invention carry out controllable with diameter of axle electron spray nozzle needle preparation when, concretely comprise the following steps：1) choose
At 20 centimetres, internal diameter fills water to length thereto in 75 microns of quartz capillary 2 one using water pump；2) to quartzy capillary
It is 25 centimetres that a length is inserted in pipe 2, and external diameter is 20 microns of tungsten filament 1, and both sides respectively reserve 2.5 centimetres of tungsten filament 1；3) utilize
The flame envelope of gas burner 3 heating capillary center section.This process continues 5 seconds, schematic diagram such as Fig. 2.Remove blowtorch 3；4) capillary is used
Tubing cutter extracts the heating part central cutout of quartz capillary 2 out tungsten filament 1, that is, obtain the EFI that exit inside diameter is 20 microns
4 two, spray painting pin, schematic diagram such as Fig. 3.
The electron spray nozzle needle controllable present invention aim at bore is prepared；Present invention uses relatively simple easy-operating side
Method, is efficiently prepared for that exit inside diameter is controllable, inner wall smooth electron spray nozzle needle.
According to the embodiment of the present invention, device includes wire 1, quartz capillary 2, thermal source 3, obtained EFI spray painting
Pin bore is identical with the external diameter of wire 1.
Wire 1 is used to control to draw nozzle needle bore, needs first to inject lubricating fluid before being penetrated capillary；Thermal source 3 is used
In vitreous silica capillary (including external skin), cut off using capillary cutter after fusion draw；
According to the embodiment of the present invention, the wire 1 has certain hardness and heat endurance, and its fusing point is than thermal source institute
There is provided temperature high；
According to the embodiment of the present invention, the external diametrical extent of the wire 1 is 1~1000 micron, and the length of wire 1 is slightly longer
In quartz capillary 2, it is ensured that it runs through capillary 2 and is easy to extract out after drawing；
According to the embodiment of the present invention, 1~1000 micron of 2 inside diameter ranges of the quartz capillary, length range 10~
1000 millimeters；
According to the embodiment of the present invention, can be any liquid that can play lubrication, preferably water, ethanol, first
Alcohol；
According to the embodiment of the present invention, can by various means inject capillary in, preferably liquid pump, peristaltic pump,
Needle tubing；
According to the embodiment of the present invention, it is sufficient to which 1700 DEG C of temperatures above, preferably Gas spray gun, laser are provided.
According to the embodiment of the present invention, all kinds can cut off the utensil of capillary, preferably potsherd, glass
Piece, diamond chip.
According to the embodiment of the present invention, the cutter cuts position of capillary 2 is in the range of melting immediate vicinity 30mm；
According to the embodiment of the present invention, drawing the process temperature of quartz capillary 2 should keep it to have certain melting speed
Rate, it is to avoid local temperature is too high；
According to the embodiment of the present invention, extract wire 1 out to be extracted out from capillary afterbody, it is to avoid damage spout；
The present invention has advantages below：
1) once-through operation flow can obtain two internal diameter identical electron spray nozzle needles, be easy to control, can control as needed
Nozzle needle bore processed；
2) operating process is easy, can in a short time prepare the controllable electron spray nozzle needle of a large amount of internal diameters, is easy to screening
Performance is more preferable, internal diameter more suitably nozzle needle；
3) gained nozzle needle inner wall smooth, Ionization Efficiency is higher.
So, the present invention effectively overcomes various shortcoming of the prior art and has high industrial utilization.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
The personage for knowing this technology all can carry out modifications and changes under without prejudice to spirit and scope of the invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
Into all equivalent modifications or change, should be covered by claim of the invention.
Claims (8)
1. a kind of preparation method of electron spray nozzle needle, it is characterised in that：The method is comprised the following steps：
1) thermal source (3) and a capillary (2) for being previously implanted lubricating fluid are provided；
2) wire (1) of the fusing point higher than the heat source temperature is provided；
3) wire (1) is penetrated in the capillary (2)；
4) thermal source is positioned over the capillary midsection for melting the capillary；While wire (1) two ends
Reciprocate vertically；The capillary (2) then rotates and to two side stretchings along central shaft, then removes thermal source (3), stops
The rotation of the capillary (2) and stretching, the wire (1) continue to reciprocate vertically；
5) capillary midsection using cutter above the thermal source cuts off the capillary；
6) extract wire (1) out to form electron spray nozzle needle from capillary two ends respectively.
2. the preparation method of electron spray nozzle needle according to claim 1, it is characterised in that：Wire (1) external diameter is 1
~1000 microns；Wire (1) length is slightly longer than capillary (2).
3. the preparation method of electron spray nozzle needle according to claim 2, it is characterised in that：Capillary (2) internal diameter is 1
~1000 microns, length is 10~1000 millimeters.
4. the preparation method of electron spray nozzle needle according to claim 1, it is characterised in that：The lubricating fluid be preferably water,
Ethanol or methyl alcohol.
5. the preparation method of electron spray nozzle needle according to claim 1, it is characterised in that：In the capillary (2) preferably
Liquid pump, peristaltic pump or needle tubing are previously implanted lubricating fluid.
6. the preparation method of electron spray nozzle needle according to claim 1, it is characterised in that：The thermal source (3) provides 1700
DEG C temperatures above, preferably Gas spray gun or laser.
7. the preparation method of electron spray nozzle needle according to claim 1, it is characterised in that：The cutter is preferably ceramics
Piece, sheet glass or diamond chip cutter.
8. the preparation method of electron spray nozzle needle according to claim 1, it is characterised in that：The cutter is on the thermal source
The melting center 30mm scope internal cuttings of side.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611246642.5A CN106783510B (en) | 2016-12-29 | 2016-12-29 | A kind of preparation method of electron spray nozzle needle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611246642.5A CN106783510B (en) | 2016-12-29 | 2016-12-29 | A kind of preparation method of electron spray nozzle needle |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106783510A true CN106783510A (en) | 2017-05-31 |
| CN106783510B CN106783510B (en) | 2018-07-06 |
Family
ID=58929039
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611246642.5A Active CN106783510B (en) | 2016-12-29 | 2016-12-29 | A kind of preparation method of electron spray nozzle needle |
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| Country | Link |
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| CN (1) | CN106783510B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650705A (en) * | 2018-12-24 | 2019-04-19 | 东南大学 | A kind of preparation method of glass micropipette |
| CN112863995A (en) * | 2021-01-17 | 2021-05-28 | 复旦大学 | Method for manufacturing nano-spray needle of electrospray ion source |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57133077A (en) * | 1981-02-12 | 1982-08-17 | Ricoh Co Ltd | Manufacture of nozzle for ink jet |
| JPS62151346A (en) * | 1985-12-26 | 1987-07-06 | Canon Inc | Production of ink jet nozzle |
| JP2005190767A (en) * | 2003-12-25 | 2005-07-14 | Tsutomu Masujima | Electrospray ionization nozzle for mass spectrometry |
| WO2006049333A1 (en) * | 2004-11-04 | 2006-05-11 | Gl Sciences Incorporated | Spray needle for esi and process for producing the same |
-
2016
- 2016-12-29 CN CN201611246642.5A patent/CN106783510B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57133077A (en) * | 1981-02-12 | 1982-08-17 | Ricoh Co Ltd | Manufacture of nozzle for ink jet |
| JPS62151346A (en) * | 1985-12-26 | 1987-07-06 | Canon Inc | Production of ink jet nozzle |
| JP2005190767A (en) * | 2003-12-25 | 2005-07-14 | Tsutomu Masujima | Electrospray ionization nozzle for mass spectrometry |
| WO2006049333A1 (en) * | 2004-11-04 | 2006-05-11 | Gl Sciences Incorporated | Spray needle for esi and process for producing the same |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109650705A (en) * | 2018-12-24 | 2019-04-19 | 东南大学 | A kind of preparation method of glass micropipette |
| CN112863995A (en) * | 2021-01-17 | 2021-05-28 | 复旦大学 | Method for manufacturing nano-spray needle of electrospray ion source |
| CN112863995B (en) * | 2021-01-17 | 2022-05-20 | 复旦大学 | Manufacturing method of nano-spray needle of electrospray ion source |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106783510B (en) | 2018-07-06 |
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