CN103545166B - Portable electrospray ion source device and mass spectrometer - Google Patents
Portable electrospray ion source device and mass spectrometer Download PDFInfo
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- CN103545166B CN103545166B CN201310539461.1A CN201310539461A CN103545166B CN 103545166 B CN103545166 B CN 103545166B CN 201310539461 A CN201310539461 A CN 201310539461A CN 103545166 B CN103545166 B CN 103545166B
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Abstract
The invention discloses a kind of Portable electrospray ion source device, comprise electron spray module, DC power supply and sheath gas supply module, described electron spray module comprises liquid storage block, capillary hollow and cavity, as sample feeding end bottom the liquid storage tank that one end of described capillary hollow is connected to described liquid storage block, the other end of described capillary hollow stretches into described cavity as spraying end, described sheath gas supply module is communicated to described cavity, the sheath gas of input assisted atomization acts on the spraying end of described capillary hollow, described DC power supply is applied on the sample solution in described capillary hollow, high pressure needed for electron spray is provided.A kind of mass spectrometer, comprises described Portable electrospray ion source device.Volume of the present invention is little, is easy to carry, and spraying is stable, and Ionization Efficiency is high.
Description
Technical field
The present invention relates to field of analytic instrument, particularly relate to a kind of Portable electrospray ion source device and there is the mass spectrometer of this device.
Background technology
Ion source is a part indispensable in mass spectrometer, and its Main Function is by sample ionization, analyzes to import in mass spectrometer.Ionogenic ionization performance determines mass spectrometric analytical performance and application to a certain extent.Electron spray ionisation (ElectrosprayIonization, ESI) be one of ioning method the most frequently used in mass spectrum, it is a kind of Soft ionization techniques, may be used for ionizing most of polar compound, also easily forms multiple-charged ion for macromolecular compound.
The process of electron spray can simply be described as: the fluid sample flowing through capillary end polarizes under the effect of high voltage electric field, the forward position that electric charge in solution constantly can be gathered in liquid forms prominent body, when charge accumulated to a certain extent, when electrostatic repulsion between electric charge has exceeded the surface tension of solution, prominent body will depart from drop surface and form charged drop.Along with the volatilization of solvent in these charged drops, charged drop diameter constantly reduces, and surface charge density constantly increases, COULOMB EXPLOSION will be there is when repulsion exceedes Surface Tension of Liquid Drops when between electric charge, form less drop, constantly repeat this process and finally will generate sample ions for mass spectral analysis.There are two kinds of theoretical explanation ESI ionization mechanisms at present, i.e. " charged residue mechanism (CRM) " and " ion evaporation theory (IEM) ", in addition, there is Ionization Efficiency and the stability that ESI ionization process then can improve ESI again after solution being become fine mist by the mode of carrier gas assisted atomization.
The ionogenic basic structure of ESI utilizes sampling device exactly, sample solution is imported the capillary of hollow, and applies high voltage on the capillary or on solution, form electron spray, under atmospheric pressure produce ion, then import mass spectrometer through vacuum interface, carry out quality analysis.
At present, the sampling device of electric spray ion source generally all adopts syringe, miniflow syringe pump to drive solution to flow in pipeline and realizes sample introduction, add that supporting gas circuit carries out assist gas atomization with nitrogen cylinder, and its high-pressure modular, power module are comparatively large, cause whole device volume large, be not easy to mobile, be unfavorable for carrying, this device is only applicable to laboratory operation, is not suitable for scene and detects analysis in real time, significantly limit its application in miniature instrument especially portable mass spectrometer.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of Portable electrospray ion source device, its volume is little, is easy to carry, and spraying is stable, and Ionization Efficiency is high.
Another object is to provide the mass spectrometer with this Portable electrospray ion source device.
For achieving the above object, the present invention is by the following technical solutions:
A kind of Portable electrospray ion source device, comprise electron spray module, DC power supply and sheath gas supply module, described electron spray module comprises liquid storage block, capillary hollow and cavity, as sample feeding end bottom the liquid storage tank that one end of described capillary hollow is connected to described liquid storage block, the other end of described capillary hollow stretches into described cavity as spraying end, described sheath gas supply module is communicated to described cavity, the sheath gas of input assisted atomization acts on the spraying end of described capillary hollow, described DC power supply is applied on the sample solution in described capillary hollow, high pressure needed for electron spray is provided.
Following technical schemes can be adopted further:
Described sheath gas supply module comprises minipump, described DC power supply comprises chargeable storage and adjustable high-pressure mini module, the sheath gas of the assisted atomization that described minipump produces inputs described cavity, the output voltage of chargeable storage is converted on the sample solution that high voltage is applied in described capillary hollow by adjustable high-pressure mini module, and described electron spray module, described minipump, described chargeable storage and described adjustable high-pressure mini module installation are in a shell.
Also comprise capillary connector and capillary sleeve pipe, described capillary connector is provided with cavity logical in, described capillary sleeve pipe is placed on described capillary hollow, put in cavity logical in described capillary connector, the two ends of described capillary connector are respectively together with described liquid storage block and described cavity compact siro spinning technology.
Capillary connector comprises middle hand and twists by the gradually little pyramidal structure of annulus and two ends, and described pyramidal structure is provided with external screw thread and coordinates to screw with the hickey of described liquid storage block and described cavity.
Described capillary sleeve pipe and described capillary connector are deformable material, described capillary sleeve pipe and described capillary hollow are compressed to be formed to seal with described liquid storage block and the close-connected described capillary connector of described cavity; Described capillary sleeve pipe is elastomeric material, and described capillary connector is PEEK or polytetrafluoroethylmaterial material, and described capillary hollow is capillary glass tube or metal capillary.
There is in described cavity the through hole of three-port structure, the mid portion of described through hole is connected with described sheath gas supply module, one end of described through hole coordinates with described capillary connector, the other end of described through hole is the gradually little sheath gas port of export in aperture, the spraying end of described capillary hollow is in the sheath gas port of export of described cavity, and described spraying end stretches out described cavity 0 ~ 3mm.
Be provided with a lid above described liquid storage tank, press capillary hollow described in solution impregnation that described lid can promote in described liquid storage tank.
Described DC power supply is applied directly on the described capillary hollow of electric conducting material formation, or on the metal sleeve being applied to outside described capillary hollow, or be applied on the described liquid storage block of electric conducting material formation, or on the sample solution being applied in described liquid storage block, be applied on the sample solution in described capillary hollow by this, described electric conducting material is metal.
The sheath gas of described assisted atomization is the mixing of several gas in nitrogen, air, oxygen, argon gas, helium, hydrogen or above-mentioned gas, and the sheath gas velocity of described assisted atomization is 1L/min ~ 10L/min.
A kind of mass spectrometer, comprise mass spectrometer body and described Portable electrospray ion source device, the spraying end of described Portable electrospray ion source device is connected to described mass spectrometer body.
Advantageous Effects of the present invention:
The negative pressure that the present invention utilizes the gravity of sample solution and high speed sheath gas to produce at capillary hollow spraying end completes sample introduction to drive the flowing of liquid, and produce stable ionspray, avoid the use of syringe and miniflow syringe pump, electrospray ion source device is simplified greatly, make the volume-diminished of whole device simultaneously, be easy to carry, versatility is good, be applicable to the ion source of portable mass spectrometer, in addition, device, applying high-tension while, also utilizes auxiliary sheath gas to strengthen atomizing effect, what improve electron spray goes molten effect, enhances ionising effect.This device can be arranged on mass spectrometer front end, also can hand-heldly use.This device can work under atmospheric conditions, highly versatile, is especially suitable as the ion source of portable mass spectrometer, can realize real-time live and detect analysis, comply with the trend of mass spectrometer microminiaturization.The device of sample introduction, assisted atomization and spraying integrates by the present invention, is arranged in a shell, makes the volume-diminished of whole device further.
Accompanying drawing explanation
Fig. 1 is the configuration and principle schematic diagram of embodiment of the present invention Portable electrospray ion source device;
Fig. 2 is the structural representation of a preferred embodiment of Portable electrospray ion source device;
Fig. 3 is the cutaway view of a preferred embodiment of electron spray module in Fig. 2;
Fig. 4 is the cutaway view of another preferred embodiment of electron spray module in Fig. 2;
Fig. 5 is the structural representation of the preferred embodiment that portable electric spraying ion source is connected with mass spectrometer body.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the invention are elaborated.It is emphasized that following explanation is only exemplary, instead of in order to limit the scope of the invention and apply.
Figure 1 shows that the configuration and principle schematic diagram of the embodiment of the present invention, electrospray ion source device comprises liquid storage block 1, sample solution 2, capillary hollow 3, DC power supply 4 and cavity 5, as sample feeding end bottom the liquid storage tank that one end of capillary hollow 3 is connected to liquid storage block 1, the other end stretches into cavity 5 as spraying end, cavity 5 passes into the sheath gas X of assisted atomization, act on the spraying end of capillary hollow 3, DC power supply 4 is applied on the sample solution in capillary hollow 3, provides the high pressure needed for electron spray.
As shown in Figure 2, in a preferred embodiment of the invention, this Portable electrospray ion source device comprises electron spray module 16, minipump 12, chargeable storage 13, adjustable high-pressure mini module 14 and shell 15.The sheath gas that minipump 12 produces assisted atomization acts in electron spray module 16, and the high voltage that adjustable high-pressure mini module 14 produces also is applied in electron spray module 16.
As shown in Figure 3, a preferred embodiment of electron spray module 16 comprises liquid storage block 1, capillary hollow 3, capillary sleeve pipe 6, capillary connector 7, cavity 5, assisted gas joint 9 and O-ring seals 8.
In specific embodiment, the external diameter of capillary hollow 3 can be 200 ~ 2000 μm, and internal diameter can be 1 ~ 1000 μm.One end of capillary hollow 3 is connected to bottom liquid storage block 1 as sample end, the other end forms spraying end through cavity, and spraying end can stretch out or not stretch out cavity, is-3 ~ 3mm with the distance of the cavity sheath gas port of export, preferably, spraying end stretches out cavity 0 ~ 3mm.Capillary hollow 3 can for the capillary glass tube drawn, and preferably, its external diameter is at about 1mm, and the internal diameter of nanospray tip is within the scope of 50 ~ 100 μm.Tightly can overlap outside capillary glass tube and have a capillary sleeve pipe 6, be put into after packaging in capillary connector 7.Capillary hollow 3 can move forward and backward in capillary tube connector 7, so that adjusting position when installing.Capillary sleeve pipe 6 preferably adopts elastomeric material, can be out of shape, and both can ensure that capillary glass tube is not pressed down or crushes, can play good sealing function again.
As shown in Figure 3, preferably, capillary connector 7 is a symmetrical structure, middle twists annulus for hand, and annulus can be provided with reticulate pattern or straight burr, conveniently tighten, its two ends are pyramidal structure, and is provided with screw thread and coordinates to screw with the hickey of liquid storage block 1 and cavity 5.Preferably, capillary connector 7 has certain plastic deformation ability, but distortion is also unsuitable excessive, be easy to machining and chemical stability is good, preferably, can use the material such as PEEK or polytetrafluoroethylene.When screwing, capillary connector 7 produces certain deformation effect on capillary sleeve pipe 6, thus compresses capillary 3, and can ensure that sealing is reliable.
Deposit the sample solution 2 of certain volume in the liquid storage tank of liquid storage block 1, bottom liquid storage tank, be provided with through hole, can be connected with capillary connector 7 by screw thread and bellmouth.Preferably, above liquid storage tank, be provided with the lid (not shown) of an insulation, the solution impregnation capillary hollow 3 in liquid storage tank can be made by this lid of pressing, be beneficial to form spraying.The material of liquid storage block 1 can select stainless steel or aluminium alloy.Liquid storage block 1 can be provided with a screwed hole (not shown) to facilitate loading spray voltage.
As shown in Figure 3, preferably, the similar of cavity 5 is in threeway, be the through hole of a hollow in the middle of it, through hole one end is provided with screw thread and bellmouth structure to coordinate with capillary connector 7, and the other end is preferably provided with the gradually little through hole of a diameter, to increase the flow velocity of sheath gas, strengthen atomizing effect.The mid portion of cavity 5 is provided with a screwed hole coordinated with assisted gas joint 9, and the through hole of screwed hole and hollow connects.
Consult Fig. 2 and Fig. 3, chargeable storage 13 voltage is 12V.The gas outlet of minipump 12 can be connected by flexible pipe 11 with assisted gas joint 9, for electrospray ion source device provides the sheath gas of assisted atomization.Minipump 12 is driven by the chargeable storage 13 of 12V, and when opening minipump 12, gas, by assisted gas joint 9, enters cavity 5, is improved the flow velocity of gas by gradually little through hole, forms negative pressure at the spraying end of capillary hollow.Sample solution, under the double action of gravity and pressure reduction, by the capillary 3 infiltrated, and forms spraying under the effect of high voltage and sheath gas.Minipump 12 can pass through voltage-regulation flow, also in gas circuit, can control gas flow by application traffic valve.
High-pressure mini module 14 that middle employing embodiment illustrated in fig. 2 is adjustable, it can convert low pressure to High voltage output, and input voltage is such as 12V, is provided by chargeable storage 13, output voltage range can be-5000V ~ 5000V, and output voltage can be regulated by potentiometer.In Fig. 3 embodiment, the positive pole of adjustable high-pressure mini module is connected on the liquid storage block of conductive material, minus earth, also can be connected on mass spectrometric vacuum interface place.
In embodiment illustrated in fig. 2, electron spray module 16, minipump 12, adjustable high-pressure mini module 14, chargeable storage 13 are enclosed in wherein with the rational layout of one by shell 15, are integrated into that volume is little, the Portable electrospray ion source device of highly versatile.Shell 15 should have the charging inlet of chargeable storage 13, liquid storage block adding mouth, cavity front end exit, adjustable high-pressure mini module voltage adjusting knob, the sheath throughput adjusting knob of assisted atomization and user hand etc.
What Fig. 4 showed is another preferred embodiment of electron spray module 16, and be with the difference of Fig. 3, outside capillary hollow 3, add a metal sleeve 10, DC power supply 4 is applied on metal sleeve, realizes electron spray.In addition, hole logical during capillary connector 7 and the link of cavity 5 are provided with, for by metal sleeve fixed clamp in wherein.
The sheath gas of assisted atomization can be the mixing of several gas in nitrogen, air, oxygen, argon gas, helium, hydrogen or above-mentioned gas.The sheath gas velocity of described assisted atomization is preferably at 1 ~ 10L/min.
The schematic diagram that the electrospray ion source device that Fig. 5 illustrates the embodiment of the present invention is connected with mass spectrometer body 30.Be connected preferably by ion guiding device 20 between cavity 5 with mass spectrometer body 30, the front end of cavity 5 by the ion guiding device 20 that is threaded, and is sealed by O shape circle 21.Ion guiding device 20 can ensure that spraying and ion travel forward, and improves efficiency of transmission.In addition, can add a mechanical pump (not shown) and be extracted out by the excessive gas in ion guiding device 20, form low pressure, this is also conducive to the formation of spraying.Ion guiding device 20 is by Flange joint or be welded on mass spectrometer body 30.The sample ions that electron spray produces enters the intrinsic mass analyzer of mass spectrometer by vacuum interface 31 and carries out analyzing and testing.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (9)
1. a Portable electrospray ion source device, it is characterized in that: comprise electron spray module, DC power supply and sheath gas supply module, described electron spray module comprises liquid storage block, capillary hollow and cavity, as sample feeding end bottom the liquid storage tank that one end of described capillary hollow is connected to described liquid storage block, the other end of described capillary hollow stretches into described cavity as spraying end, described sheath gas supply module is communicated to described cavity, the suction function that the sheath gas of input assisted atomization produces at the spraying end of described capillary hollow is in the spraying end of described capillary hollow, the flowing of liquid is driven to realize sample introduction, described DC power supply is applied on the sample solution in described capillary hollow, high pressure needed for electron spray is provided, described sheath gas supply module comprises minipump, described DC power supply comprises chargeable storage and adjustable high-pressure mini module, the sheath gas of the assisted atomization that described minipump produces inputs described cavity, the output voltage of chargeable storage is converted on the sample solution that high voltage is applied in described capillary hollow by adjustable high-pressure mini module, described electron spray module, described minipump, described chargeable storage and described adjustable high-pressure mini module installation are in a shell.
2. Portable electrospray ion source device as claimed in claim 1, it is characterized in that: also comprise capillary connector and capillary sleeve pipe, described capillary connector is provided with cavity logical in, described capillary sleeve pipe is placed on described capillary hollow, put in cavity logical in described capillary connector, the two ends of described capillary connector are respectively together with described liquid storage block and described cavity compact siro spinning technology.
3. Portable electrospray ion source device as claimed in claim 2, it is characterized in that: capillary connector comprises middle hand and twists by the gradually little pyramidal structure of annulus and two ends, and described pyramidal structure is provided with external screw thread and coordinates to screw with the hickey of described liquid storage block and described cavity.
4. Portable electrospray ion source device as claimed in claim 2, it is characterized in that: described capillary sleeve pipe and described capillary connector are deformable material, with described liquid storage block and the close-connected described capillary connector of described cavity described capillary sleeve pipe and described capillary hollow compressed to be formed and seal; Described capillary sleeve pipe is elastomeric material, and described capillary connector is PEEK or polytetrafluoroethylmaterial material, and described capillary hollow is capillary glass tube or metal capillary.
5. Portable electrospray ion source device as claimed in claim 2, it is characterized in that: the through hole in described cavity with three-port structure, the mid portion of described through hole is connected with described sheath gas supply module, one end of described through hole coordinates with described capillary connector, the other end of described through hole is the gradually little sheath gas port of export in aperture, the spraying end of described capillary hollow is in the sheath gas port of export of described cavity, and described spraying end stretches out described cavity 0 ~ 3mm.
6. the Portable electrospray ion source device as described in any one of claim 1 to 5, is characterized in that: be provided with a lid above described liquid storage tank, presses capillary hollow described in solution impregnation that described lid can promote in described liquid storage tank.
7. the Portable electrospray ion source device as described in any one of claim 1 to 5, it is characterized in that: described DC power supply is applied directly on the described capillary hollow of electric conducting material formation, or on the metal sleeve being applied to outside described capillary hollow, or be applied on the described liquid storage block of electric conducting material formation, or on the sample solution being applied in described liquid storage block, be applied on the sample solution in described capillary hollow by this, described electric conducting material is metal.
8. the Portable electrospray ion source device as described in any one of claim 1 to 5, it is characterized in that: the sheath gas of described assisted atomization is the mixing of several gas in nitrogen, air, oxygen, argon gas, helium, hydrogen or above-mentioned gas, the sheath gas velocity of described assisted atomization is 1L/min ~ 10L/min.
9. a mass spectrometer, comprises mass spectrometer body, it is characterized in that: also comprise the Portable electrospray ion source device as described in any one of claim 1 to 8, and the spraying end of described Portable electrospray ion source device is connected to described mass spectrometer body.
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| CN201310539461.1A CN103545166B (en) | 2013-11-04 | 2013-11-04 | Portable electrospray ion source device and mass spectrometer |
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| CN201310539461.1A CN103545166B (en) | 2013-11-04 | 2013-11-04 | Portable electrospray ion source device and mass spectrometer |
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| CN1830056A (en) * | 2003-07-24 | 2006-09-06 | 普渡研究基金会 | Electrosonic spray ionization method and device for the atmospheric ionization of molecules |
| CN101356012A (en) * | 2005-12-07 | 2009-01-28 | 玛丽皇后与西田学院 | An electrospray device and a method of electrospraying |
| CN101809706A (en) * | 2007-06-01 | 2010-08-18 | 珀金埃尔默健康科学股份有限公司 | Atmospheric pressure ion source performance enhancement |
| CN102709147A (en) * | 2012-06-21 | 2012-10-03 | 清华大学深圳研究生院 | Electrospray ion source and mass spectrometer |
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| US8759757B2 (en) * | 2010-10-29 | 2014-06-24 | Thermo Finnigan Llc | Interchangeable ion source for electrospray and atmospheric pressure chemical ionization |
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| CN1830056A (en) * | 2003-07-24 | 2006-09-06 | 普渡研究基金会 | Electrosonic spray ionization method and device for the atmospheric ionization of molecules |
| CN101356012A (en) * | 2005-12-07 | 2009-01-28 | 玛丽皇后与西田学院 | An electrospray device and a method of electrospraying |
| CN101809706A (en) * | 2007-06-01 | 2010-08-18 | 珀金埃尔默健康科学股份有限公司 | Atmospheric pressure ion source performance enhancement |
| CN102709147A (en) * | 2012-06-21 | 2012-10-03 | 清华大学深圳研究生院 | Electrospray ion source and mass spectrometer |
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