CN103545166A - Portable electrospray ion source device and mass spectrometer - Google Patents
Portable electrospray ion source device and mass spectrometer Download PDFInfo
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- CN103545166A CN103545166A CN201310539461.1A CN201310539461A CN103545166A CN 103545166 A CN103545166 A CN 103545166A CN 201310539461 A CN201310539461 A CN 201310539461A CN 103545166 A CN103545166 A CN 103545166A
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Abstract
The invention discloses a portable electrospray ion source device. The portable electrospray ion source device comprises an electrospray module, a direct-current power source and a sheath gas supply module, wherein the electrospray module comprises a liquid storage block, a hollow capillary and a cavity, one end of the hollow capillary is connected to the bottom of a liquid storage tank of the liquid storage block to serve as a sample introduction end, the other end of the hollow capillary extends into the cavity to serve as a spray end, the sheath gas supply module is communicated with the cavity, sheath gas which is input and plays a role in atomization assistance acts on the spray end of the hollow capillary, and the direct-current power source acts on a sample solution in the hollow capillary to provide a high voltage needed by electrospray. A mass spectrometer comprises the portable electrospray ion source device. The portable electrospray ion source device and the mass spectrometer with the portable electrospray ion source device are small in size, convenient to carry, stable in spray and high in ionization efficiency.
Description
Technical field
The present invention relates to field of analytic instrument, particularly relate to a kind of portable electric spraying 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, to import in mass spectrometer, analyzes.Ionogenic ionization performance has determined mass spectrometric analytical performance and application to a certain extent.Electron spray ionisation (Electrospray Ionization, ESI) is one of ioning method the most frequently used in mass spectrum, and it is a kind of soft ionization technology, can, for ionizing most of polar compound, for macromolecular compound, also easily form multiple-charged ion.
The process of electron spray can simply be described as: the fluid sample of the capillary end of flowing through polarizes under the effect of high voltage electric field, the forward position that electric charge in solution can constantly be gathered in liquid forms prominent body, when charge accumulated to a certain extent, when the electrostatic repulsion between electric charge has surpassed the surface tension of solution, prominent body will depart from drop surface and form charged drop.Volatilization along with solvent in these charged drops, charged drop diameter constantly dwindles, and surface charge density constantly increases, when surpassing Surface Tension of Liquid Drops, repulsion between electric charge will there is COULOMB EXPLOSION, form less drop, constantly repeat this process and finally will generate the sample ions for mass spectral analysis.There are at present two kinds of theoretical explanation ESI ionization mechanisms, i.e. " charged residue mechanism (CRM) " and " ion evaporation theoretical (IEM) ", in addition after, the mode by carrier gas assisted atomization becomes solution into fine mist, there is again Ionization Efficiency and the stability that ESI ionization process can improve ESI.
The ionogenic basic structure of ESI is utilized sampling device exactly, sample solution is imported to the capillary of hollow, and applies high voltage on capillary or on solution, form electron spray, under atmospheric pressure produce ion, then through vacuum interface, import mass spectrometer, 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 and realize sample introduction in pipeline, with nitrogen cylinder, add that supporting gas circuit carries out assist gas atomization, and its high-pressure modular, power module are larger, 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 the on-the-spot analysis that detects in real time, has greatly limited 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, a kind of portable electric spraying ion source device is provided, its volume is little, be easy to carry, and spraying is stable, and Ionization Efficiency is high.
Another object is to provide the mass spectrometer with this portable electric spraying ion source device.
For achieving the above object, the present invention is by the following technical solutions:
A kind of portable electric spraying ion source device, comprise electron spray module, DC power supply and sheath gas supply module, described electron spray module comprises liquid storage piece, capillary hollow and cavity, one end of described capillary hollow is connected to the liquid storage tank bottom of described liquid storage piece as sample feeding end, 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, provide electron spray required high pressure.
Can further adopt following technical schemes:
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 is inputted described cavity, adjustable high-pressure mini module is converted to high voltage by the output voltage of chargeable storage and is applied on the sample solution in described capillary hollow, and described electron spray module, described minipump, described chargeable storage and described adjustable high-pressure mini module are arranged 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 into described capillary connector in logical cavity, the two ends of described capillary connector closely link together with described liquid storage piece and described cavity respectively.
Hand in the middle of capillary connector comprises is twisted by annulus and the gradually little pyramidal structure in two ends, and described pyramidal structure is provided with external screw thread and screws and coordinate with the hickey with described liquid storage piece and described cavity.
Described capillary sleeve pipe and described capillary connector are deformable material, with described liquid storage piece and the close-connected described capillary connector of described cavity, described capillary sleeve pipe and described capillary hollow are compressed to formation sealing; Preferably, 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.
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 sheath gas port of export, aperture is gradually little, the sheath gas port of export of the spraying end of described capillary hollow in described cavity, preferably, described spraying end stretches out described cavity 0～3mm.
Described liquid storage tank top is provided with a lid, presses described lid and can promote capillary hollow described in the solution impregnation in described liquid storage tank.
Described DC power supply is applied directly on the described capillary hollow of electric conducting material, or be applied on the capillary sleeve pipe of the electric conducting material outside described capillary hollow, or be applied on the described liquid storage piece of electric conducting material, or be applied on the sample solution in described liquid storage piece, be applied to by this on the sample solution in described capillary hollow, preferably, described electric conducting material is metal.
The sheath gas of described assisted atomization is the mixing of several gases in nitrogen, air, oxygen, argon gas, helium, hydrogen or above-mentioned gas, and preferably, the sheath gas velocity of described assisted atomization is 1L/min～10L/min.
, comprising mass spectrometer body and described portable electric spraying ion source device, the spraying end of described portable electric spraying ion source device is connected to described mass spectrometer body.
Useful technique effect of the present invention:
The present invention utilizes the gravity of sample solution and high speed sheath gas in the negative pressure of capillary hollow spraying end generation, to drive the mobile sample introduction that completes of liquid, and produce stable ionspray, avoided 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 is applying the high-tension while, also utilizes auxiliary sheath gas to strengthen atomizing effect, the molten effect of going that has improved electron spray, has strengthened ionization effect.This device can be arranged on mass spectrometer front end, also can hand-heldly use.This device can be worked under atmospheric pressure, and highly versatile is especially suitable as the ion source of portable mass spectrometer, can realize real-time Site Detection analysis, has complied with the trend of mass spectrometer microminiaturization.The present invention integrates the device of sample introduction, assisted atomization and spraying, is arranged in a shell, further makes the volume-diminished of whole device.
Accompanying drawing explanation
Fig. 1 is structure and the principle schematic of embodiment of the present invention portable electric spraying ion source device;
Fig. 2 is the structural representation of a preferred embodiment of portable electric spraying 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 a preferred embodiment being connected with mass spectrometer body of portable electric spraying ion source.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the invention are elaborated.Should be emphasized that, following explanation is only exemplary, rather than in order to limit the scope of the invention and to apply.
Figure 1 shows that structure and the principle schematic of the embodiment of the present invention, electrospray ion source device comprises liquid storage piece 1, sample solution 2, capillary hollow 3, DC power supply 4 and cavity 5, one end of capillary hollow 3 is connected to the liquid storage tank bottom of liquid storage piece 1 as sample feeding end, 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 electron spray required high pressure.
As shown in Figure 2, in a preferred embodiment of the present invention, this portable electric spraying 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 is also applied in electron spray module 16.
As shown in Figure 3, electron spray module 16 preferred embodiment comprises liquid storage piece 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 μ m, and internal diameter can be 1～1000 μ m.One end of capillary hollow 3 is connected to liquid storage piece 1 bottom as sample end, the other end is through cavity and form spraying end, and spraying end can stretch out or not stretch out cavity, with the distance of the cavity sheath gas port of export be-3～3mm, preferably, spraying end stretches out cavity 0～3mm.Capillary hollow 3 can be the capillary glass tube drawing, and preferably, its external diameter, in 1mm left and right, is sprayed most advanced and sophisticated internal diameter within the scope of 50～100 μ m.Capillary glass tube outside can tightly be overlapped and have a capillary sleeve pipe 6, is put in capillary connector 7 after packaging.Capillary hollow 3 can move forward and backward in capillary tube connector 7, so that adjusting position while installing.Capillary sleeve pipe 6 preferably adopts elastomeric material, can be out of shape, and both can guarantee that capillary glass tube is not pressed down or crushes, and can play good sealing function again.
As shown in Figure 3, preferably, capillary connector 7 is a symmetrical structure, middle for the stubborn annulus of hand, on annulus, can be provided with reticulate pattern or straight burr, conveniently tightens, and its two ends are pyramidal structure, and is provided with screw thread and screws and coordinate with the hickey with liquid storage piece 1 and cavity 5.Preferably, capillary connector 7 has certain moulding deformability, but distortion is also unsuitable excessive, be easy to machining and chemical stability good, preferably, can use the materials such as PEEK or polytetrafluoroethylene.While screwing, capillary connector 7 produces certain deformation effect on capillary sleeve pipe 6, thereby compresses capillary 3, and can guarantee that sealing is reliable.
In the liquid storage tank of liquid storage piece 1, deposit the sample solution 2 of certain volume, liquid storage tank bottom is provided with through hole, can be connected with capillary connector 7 by screw thread and bellmouth.Preferably, liquid storage tank top is provided with the lid (not shown) of an insulation, can make the solution impregnation capillary hollow 3 in liquid storage tank by pressing this lid, is beneficial to form spraying.The material of liquid storage piece 1 can be selected stainless steel or aluminium alloy.On liquid storage piece 1, can be provided with a screwed hole (not shown) to facilitate loading spray voltage.
As shown in Figure 3, preferably, the structure of cavity 5 is similar to 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 a through hole that diameter is gradually little, to increase the flow velocity of sheath gas, strengthen atomizing effect.The mid portion of cavity 5 is provided with a screwed hole coordinating with assisted gas joint 9, and the through hole of screwed hole and hollow connects.
Consult Fig. 2 and Fig. 3, chargeable storage 13 voltages are 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, improves the flow velocity of gas by gradually little through hole, in the spraying end formation negative pressure of capillary hollow.Sample solution, under the double action of gravity and pressure reduction, by the capillary 3 of infiltration, and forms spraying under the effect of high voltage and sheath gas.Minipump 12 can pass through voltage-regulation flow, also can in gas circuit, 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 for example 12V, by chargeable storage 13, is provided, output voltage range can be-5000V～5000V, and output voltage can regulate by potentiometer.In Fig. 3 embodiment, the positive pole of adjustable high-pressure mini module is connected on the liquid storage piece of conductive material, and minus earth also can be connected on mass spectrometric vacuum interface place.
In embodiment illustrated in fig. 2, shell 15 is enclosed in electron spray module 16, minipump 12, adjustable high-pressure mini module 14, chargeable storage 13 wherein with a kind of rational layout, is integrated into that volume is little, the portable electric of highly versatile spraying ion source device.Shell 15 should have the sheath throughput adjusting knob of charging inlet, liquid storage piece adding mouth, the cavity front end exit of chargeable storage 13, adjustable high-pressure mini module voltage adjusting knob, assisted atomization and user hand etc.
What Fig. 4 showed is another preferred embodiment of electron spray module 16, is with the difference of Fig. 3, and in capillary hollow 3 outsides, add a metal sleeve 10, DC power supply 4 is applied on metal sleeve, realizes electron spray.In addition, logical hole during the link of capillary connector 7 and cavity 5 is provided with, for by metal sleeve fixed clamp in wherein.
The sheath gas of assisted atomization can be the mixing of several gases 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.
Fig. 5 has shown the schematic diagram that the electrospray ion source device of the embodiment of the present invention is connected with mass spectrometer body 30.Between cavity 5 and mass spectrometer body 30, preferably by ion guiding device 20, be connected, the front end of cavity 5 can be threaded connection ion guiding device 20, and by 21 sealings of O shape circle.Ion guiding device 20 can guarantee that spraying and ion travel forward, and improve efficiency of transmission.In addition, can add a mechanical pump (not shown) the unnecessary gas in ion guiding device 20 is extracted out, form low pressure, this is also conducive to the formation of spraying.Ion guiding device 20 can be connected or is welded on mass spectrometer body 30 by flange.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, can also make some simple deduction or replace, all should be considered as belonging to protection scope of the present invention.
Claims (10)
1. portable electric spraying 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 piece, capillary hollow and cavity, one end of described capillary hollow is connected to the liquid storage tank bottom of described liquid storage piece as sample feeding end, 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, provide electron spray required high pressure.
2. portable electric as claimed in claim 1 spraying ion source device, it is characterized in that: 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 is inputted described cavity, adjustable high-pressure mini module is converted to high voltage by the output voltage of chargeable storage and is applied on the sample solution in described capillary hollow, described electron spray module, described minipump, described chargeable storage and described adjustable high-pressure mini module are arranged in a shell.
3. portable electric as claimed in claim 1 spraying ion source device, 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 into described capillary connector in logical cavity, the two ends of described capillary connector closely link together with described liquid storage piece and described cavity respectively.
4. portable electric as claimed in claim 3 spraying ion source device, it is characterized in that: the hand in the middle of capillary connector comprises is twisted by annulus and the gradually little pyramidal structure in two ends, and described pyramidal structure is provided with external screw thread and screws and coordinate with the hickey with described liquid storage piece and described cavity.
5. portable electric as claimed in claim 3 spraying ion source device, it is characterized in that: described capillary sleeve pipe and described capillary connector are deformable material, with described liquid storage piece and the close-connected described capillary connector of described cavity, described capillary sleeve pipe and described capillary hollow are compressed to formation sealing; Preferably, 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.
6. portable electric as claimed in claim 3 spraying ion source device, 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 sheath gas port of export, and aperture is gradually little, the sheath gas port of export of the spraying end of described capillary hollow in described cavity, preferably, described spraying end stretches out described cavity 0～3mm.
7. the portable electric as described in claim 1 to 6 any one spraying ion source device, is characterized in that: described liquid storage tank top is provided with a lid, presses described lid and can promote capillary hollow described in the solution impregnation in described liquid storage tank.
8. the portable electric as described in claim 1 to 6 any one spraying ion source device, it is characterized in that: described DC power supply is applied directly on the described capillary hollow of electric conducting material, or be applied on the capillary sleeve pipe of the electric conducting material outside described capillary hollow, or be applied on the described liquid storage piece of electric conducting material, or be applied on the sample solution in described liquid storage piece, be applied to by this on the sample solution in described capillary hollow, preferably, described electric conducting material is metal.
9. the portable electric as described in claim 1 to 6 any one spraying ion source device, it is characterized in that: the sheath gas of described assisted atomization is the mixing of several gases in nitrogen, air, oxygen, argon gas, helium, hydrogen or above-mentioned gas, preferably, the sheath gas velocity of described assisted atomization is 1L/min～10L/min.
10. a mass spectrometer, comprises mass spectrometer body, it is characterized in that: also comprise the portable electric spraying ion source device as described in claim 1 to 9 any one, the spraying end of described portable electric spraying ion source device is connected to described mass spectrometer body.
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