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Ion mobility spectrometre

Ion mobility spectrometre
IPC classes for russian patent Ion mobility spectrometre (RU 2390069):
H01J49 - Particle spectrometers or separator tubes (for measuring gas pressure H01J0041100000)
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Method and device for sorting out charged particles by specific charge Method and device for sorting out charged particles by specific charge / 2276426
Mass analyzer built around confined ion trap and designed to improve consumer properties as well as to extend service life of mass spectrometers using hyperboloid electrode systems has hyperboloid butt-end electrode and plane-confined annular one, cylindrical shielding and focusing electrodes, as well as semitransparent flat correcting electrode. Charged particles are produced due to electron shock in space between annular and correcting electrodes beyond working space of mass analyzer. Ions are entered in analyzer under action of accelerating voltage across correcting and focusing electrode; period and phase of accelerating voltage are coordinated with those of variable field and with original coordinates and speeds of charged particles. Sorted out ions are brought out through annular electrode hole and through semitransparent correcting electrode under action of positive voltage across butt-end electrode.

FIELD: physics.

SUBSTANCE: ion mobility spectrometre has an ion formation chamber, an ion source, a drift tube with a collector and an aperture element which form an ejection region, an ejection electrode and an ion valve, a drift gas inlet into the drift region. The power system of the ion source has an ioniser housing with an axially symmetric shape. On the walls of the ioniser housing there are radially directed inlet devices and devices for ionising samples of the analysed substance. The point of intersection of the axes of inlet devices lies opposite the top of the aperture element which is made in form of convex wall with an ion inlet opening at its top. The collector is detachable. The aperture element is made in form of a hemisphere or cone.

EFFECT: increased selectivity, increased sensitivity, faster operation, possibility of working on different modes.

5 cl, 7 dwg

 

The invention relates to the field of analytical instrumentation, in particular for the determination of the composition of the liquid and gas samples prior to separation of samples into fractions in mass spectrometry. The ion mobility spectrometers are most widely used for the identification of explosives and drugs, medicines, monitoring of toxic substances of industrial origin.

A device for obtaining and analyzing ions of the analyte containing the target nanostructured surface, means for directing the analyte to the target, the laser, the means for selecting ions of the analyte, the means for directing to the target analyte and a means for selecting ions of the analyte, made in the form of the drift tube, which is connected with the node of the input samples, comprising a housing with connections for collection of samples and output gas stream from the field ionization, in the housing with the possibility of reciprocating movement is set to target nanostructured surface, the site of continuous blowing of the investigated object is located along the axis of the input and output sockets on the opposite inner the end of the drift tube collector is connected to the amplifier, the amplifier output is connected to the computer input. The drift tube is made in the form of ring electrodes separated by dielectr the ical rings. Node input samples provided with the insulator, inside of which is a metal Cup with a grid and heating element. The laser performed pulse-periodic, one of the outputs of the laser through the synchronizer is connected to the computer input. The target is equipped with a host control. The patent of Russian Federation №2346354, IPC: H01J 49/00, 2009, the Device provides a typical ion mobility spectrometers selectivity. For producing ions in the device using the target nanostructured surface and the laser for forming ions of the analyte. For detection of ion bunches using a collector connected to the amplifier.

Known ion mobility spectrometer containing the camera inobtrusive inside of the ion source and the drift chamber, within which there is a reservoir of ions and the aperture grid forming region eject, eject the electrode and the grid shutter, aperture for entry of the analyte in the mixture with the carrier gas in the area inobtrusive, the insertion opening for the drift gas in the drift region and the holes for the output of the drift gas and the mixture of the analyte with the carrier gas from the field to push the Camera inobtrusive with the ion source is outside the scope of the ejection of ions and connected to the adapter with Cana is om. (Patent of Russian Federation №2328791, IPC: H01J 49/40; G01N 27/62, prototype). The prototype provides only typical for ion mobility spectrometers selectivity and operates in the same mode.

This invention eliminates these drawbacks.

The technical result of the invention is to improve the selectivity, increased sensitivity, increased speed, ability to work in different modes (universality).

The technical result is achieved by the fact that in the ion mobility spectrometer containing the camera inobtrusive, the ion source, drift tube with a reservoir and the aperture element forming region eject, eject the electrode and the ion gate, enter the drift gas in the drift region, the power supply system. The ion source includes a housing ionizer axially symmetric forms on the inside of the ionizer is installed radially directed input device and ionization of the sample analyte, the point of intersection of the axes of the input device is positioned opposite the top of the aperture element made in the form of a wall of a convex shape with an opening for entry of ions on its top, and the manifold is made removable. The aperture element is designed as a hemisphere or a cone. Input devices and ionization of the sample analyte installed with the possibility of the independence of the ima alignment and inclusion. Input devices and ionization of the sample analyte contain ionizers in the form of electronicdevices, and/or ionizer by corona discharge, and/or photoinitiator, and/or a laser ionizer, and I spray the liquid sample, and/or gas samples, and/or desorber. The collector is made on the basis of the plate Faraday or mass spectrometer. Input devices and ionization of the sample analyte is installed with the possibility of independent adjustment and inclusion. Input devices and ionization of the sample analyte contain ionizers in the form of electronicdevices, and/or ionizer by corona discharge, and/or photoinitiator, and/or a laser ionizer, and I spray the liquid sample, and/or gas samples, and/or the substrate to enter the solid sample, and/or desorption with elektrorazpredelenie. The collector is made on the basis of the plate Faraday or mass spectrometer.

The invention is illustrated in figure 1-6.

1 schematically shows a device with a collector detector for analyzing gas samples, where 1 - electroepilation (in OFF position), 2 - ionizer based on corona discharge (in ON position), 2.1 - needle ionizer by corona discharge, 2.2 - channel high voltage supply, 3 - photoionization (in ON position), 4 - input device of the gas sample (in ON position), 4.1 - channel gas sample, 4.2 - heater, 5 - spray idca samples (in OFF position), 6 - the body of the ionizer, 7 - camera inobtrusive, 8 - wall convex form, 9 - hole at the top of the convexity of the wall, 10 - region desolvatation, 11 - ion inlet gate or hub, 12 - drift region, 13 - discharge ion gate, 14 - detector based plate Faraday (collector detector), 15 - channel, 16 - heater, 17 - channel pumping the drift gas and the sample 18 to the input channel of the cooled air to operate at a lower temperature or a rapid change in temperature mode, 19 - channel output of the cooled air, 20 - the case of the ion mobility spectrometer, 21 - connector for input supply voltages, 22 - electrometric amplifier, 23 - high-voltage modules, 24 controller 25 controller inlet of the ion gate or drive ions, the 26 - controller heater, 27 controller prom ion shutter 28 is an analyte.

Figure 2 schematically shows the device with the collector detector for analyzing liquid samples, where 1 - electroepilation (in ON position), 1.1 - input channel capillary feed samples, 1.2 - needle electronicdevices, 1.3 - channel gas spray, 1.4 - channel high voltage supply, 2 - ionizer based on corona discharge (in OFF position), 3 - photoionization (in OFF position), 4 - input device of the gas sample (in OFF position), 5 - spray liquid samples (in OFF position), 6 - case is ionizator, 7 - camera inobtrusive, 8 - wall convex form, 9 - hole at the top of the convexity of the wall, 10 - region desolvatation, 11 - ion inlet gate or hub, 12 - region drift, 13 - discharge ion gate, 14 - detector based plate Faraday (collector detector), 15 - channel, 16 - heater, 17 - channel pumping the drift gas and the sample 18 to the input channel of the cooled air to operate at a lower temperature or a rapid change in temperature mode, 19 - channel output of the cooled air, 20 - case spectrometer ion mobility, 21 - connector for input supply voltages, 22 - electrometric amplifier, 23 - high-voltage modules, 24 controller 25 controller inlet of the ion gate or drive ions, the 26 - controller heater, 27 controller prom ion shutter 28 is an analyte.

Figure 3 schematically shows the device with quadrupole-flight mass spectrometer, where 1 - electroepilation, 2 - ionizer based on corona discharge, 2.1 - needle ionizer by corona discharge, 4 - input device of the gas sample (in ON position), 5 - spray liquid samples (in ON position), 6 - ionizer housing, 7 - camera inobtrusive, 8 - wall convex form, 9 - hole at the top of the convexity of the wall, 10 - region desolvatation, 11 - ion inlet gate or hub, 12 - region is of Rafe, 13 - discharge ion shutter 16 to the heater 28 is an analyte, 29 - gas curtain of the mass spectrometer used as the drift gas, 30 - the first step interface differential pumping of the mass spectrometer, 31 - transport quadrupole in the second stage of the interface of differential pumping of the mass spectrometer, 32 - radio frequency quadrupole lens, 33 - quadrupole filter mass, 34 - collisional quadrupole, 35 - orthogonal accelerator, 36 ion mirror, the 37 - ion detector, 38, 39, 40 - turbomolecular pumps.

Figure 4 schematically shows the device with the collector detector when using desorption of the substrate, which can be used with ionization-stimulated matrix laser desorption (MALDI), laser desorption from porous silica surface (DIOS), stimulated elektrorazpredelenie desorption (DESI shown in the drawing), where 1 - electroepilation (in ON position), 1.1 - input channel capillary feed samples, 1.2 - needle electronicdevices, 1.3 - channel gas spray, 1.4 - channel high voltage supply, 2 - ionizer based on corona discharge (in OFF position), 41 - desorber, 41.1 - desorption substrate, 41.2 - channel high voltage supply, 6 - ionizer housing, 7 - camera inobtrusive, 8 - wall convex form, 9 - hole at the top of the convexity of the wall, 10 - region deal the operation, 11 - ion inlet gate or hub, 12 - region drift, 13 - discharge ion gate, 14 - detector based plate Faraday (collector detector), 15 - channel, 16 - heater, 17 - channel pumping the drift gas and the sample 20 - the case of the ion mobility spectrometer, 21 - connector for input supply voltages, 22 - electrometric amplifier, 23 - high-voltage modules, 24 controller 25 controller inlet of the ion gate or drive ions, the 26 - controller heater, 27 controller prom ion shutter 28 - analyzed substance.

Figure 5 presents the distribution of the above mobility 2-6-datatravelermini (resolution of 100)obtained by the detector on the base plate Faraday during ionization by corona discharge.

Figure 6(a) shows the distribution of the above mobility solution for 2-6-datatravelermini in acetonitrile with 0.1% additive formic acid and 0.1% water (resolution 100) resolution, obtained by ionization elektrorazpredelenie with mass-selective (192 Amu) detection (quadrupole-time-of-flight mass spectrometer).

Figure 6(b) shows the distribution of the above mobility solution for 2-6-datatravelermini in acetonitrile with 0.1% additive formic acid and 0.1% water (resolution 50)obtained by ionization e is chronosystem with mass-selective (192 Amu) detection (quadrupole-time-of-flight mass spectrometer).

The device operates as follows.

When working with ionizer based on corona discharge 2 or photoionization 3 electronicdigital 1 is disabled. (Figure 1).

An analyte 28 in the gas phase is fed through the input gas samples 4 through the channel 4.1, heated by the heater 4.2.

An analyte 28 in the liquid phase is injected through an orthogonal set spray liquid samples 5.

In the camera inobtrusive 7 in the process of corona discharge or photoionization born ions, which through the opening 9 at the top of the convex wall 8 coming into the region desolvatation 10, pass through the ion inlet gate or hub 11 and enter the drift region 12. Through the channel 15 in the drift region 12 is constantly serves the drift gas (high purity nitrogen or dry cleaned the air with a flow rate of 0.5-2 l/min).

The drift tube consists of the area desolvatation 10 and the drift region 12, a divided inlet shutter or hub phase 11.

Region desolvatation 10 drift and 12 in the radial direction is limited by a set of cylindrical electrodes forming an electric field. Driving under the influence of an electric field, under atmospheric pressure and the ions of the analyte 28 collide with molecules of the drift gas. In the field desolvatation 10 happen drainage, declustering the ions. The inlet shutter or hub phase 11 generates localized in space group containing ions of the analyte 28. This group, moving under the influence of an electric field in the drift region in a counter drift gas is divided into a series of groups containing components with different degree of retention of the molecules selected drift gas. Each of these groups reaches the outlet of the ion gate 13 during drift associated with the mobility component forming this group, and enters the collector and the detector 14.

Collector detector 14 is connected with electrometric amplifier 22 (Fig 1), the analog signal which is converted into digital form and transmitted to the controller 24. Ionic groups due to different mobility register at different times.

When working with electroepilation 1 (figure 2) ionizer based on corona discharge 2, photoionization 3, the input device of the gas samples 4 and the spray liquid samples 5 off (switched to the OFF position). An analyte 28 in the liquid phase is fed through a channel 1.1. For spraying, use a carrier gas is supplied through the channel 1.3. The dispersion produced in the electric field generated between the needle 1.2 and a wall 8 having a convex shape. And then born of ions through the opening 9 at the top of the convex wall 8 coming into the region JASS is lutzii 10, pass through the ion inlet gate or hub 11 and enter the drift region 12. Through the channel 15 in the drift region 12 is constantly serves the drift gas (high purity nitrogen or dry cleaned the air with a flow rate of 0.5-2 l/min).

When working with desorber 41 (4) an analyte is applied to the substrate 41.1, and desorption and the ionization is carried out by laser radiation (methods MALDI and DIOS) with a laser installed in place of electronicdevices 1. Or elektrorazpredelenie solvent (method DESI) using electronicdevices 1. The solvent 42 in the liquid phase is fed through a channel 1.1. For spraying, use a carrier gas supplied through the channel 1.3. The dispersion produced in the electric field generated between the needle 1.2, the substrate 41.1 and a wall 8 having a convex shape. Between the substrate and 41.1 wall 8 put-off potential. And then born of ions through the opening 9 at the top of the convex wall 8 coming into the region desolvatation 10, pass through the ion inlet gate or hub 11 and enter the drift region 12. Through the channel 15 in the drift region 12 is constantly serves the drift gas (high purity nitrogen or dry cleaned the air with a flow rate of 0.5-2 l/min).

The resulting signal represents the chromatogram of the peaks of different amplitude.

The chromatogram of transformer the Ute in the distribution of a given mobility by the following formula: K 0=273LP/(760ETt), where K0- the mobility (cm2/Bc), E - tension drift field (V/cm), t is the time drift of ions (C), P is pressure (mm Hg), T - temperature (K).

Components identify the value of a given mobility corresponding to the maximum peak, and the amplitude or peak area to determine their concentration in the original sample analyte 28.

Ionization and separation of ions by mobility occur in the ion mobility spectrometer. For the detection of mass-selective detector 37 spectrometer ion mobility combined with quadrupole-time-of-flight (figure 4) or other mass spectrometer. For each group divided by the mobility of ions recorded mass spectrum. The identification component to produce 3-dimensional information (see mobility, mass, intensity).

Increased sensitivity is achieved for the following reason. Due to the fact that the aperture element has a conical shape, the electric field in the chamber inobtrusive increases in the area of the holes on the top of the convex wall, which provides preferential movement of ions in the direction of the hole in the aperture element. On the other hand, the conical structure of the flow of drift gas creates the effect of the nozzle, which improves the cleaning of the surfaces of the holes in pertorm element from contamination and increases the security of the drift tube from penetrating neutral particles, clusters and droplets of solvent.

The increase of selectivity is achieved through better drainage ions of the sample from the solvent due to the effect of the nozzle on the top of the convex wall, and due to the fact that ions of the sample are introduced into the drift tube in the form of a narrow beam, defined by the insertion of the sample.

The performance increase is achieved by the fact that for a given geometry minimizes the time for switching between different modes of ionization.

One of the criteria of selectivity of the ion mobility spectrometer resolution is determined by one peak, as R=t/δt, where t is the time drift of ions, a δt is the duration of the ion pulse in detector level provisory maximum peak. This equation leads to the form R=K/δk means, where K is the mobility of ions, and δk means the range of mobility corresponding to the duration of the peak of the analytical signal at half-height of its intensity. The resolution reflects the minimal differences in the mobility required for the resolution of peaks in a given range of mobility.

1. The ion mobility spectrometer containing the camera inobtrusive, the ion source, drift tube with a reservoir and the aperture element, ion shutter, enter the drift gas in the drift region, the power supply system, characterized in that the ion source content is t ionizer housing axially symmetric shape, on the inside of the ionizer is installed radially directed input device and ionization of the sample analyte, the point of intersection of the axes of the input device is positioned opposite the top of the aperture element made in the form of a wall of a convex shape with an opening for entry of ions on its top, and the manifold is made removable.

2. The ion mobility spectrometer according to claim 1, wherein the aperture element is designed as a hemisphere or a cone.

3. The ion mobility spectrometer according to claim 1, characterized in that the input device and ionization of the sample analyte is installed with the possibility of independent adjustment and on.

4. The ion mobility spectrometer according to claim 1, characterized in that the input device and ionization of the sample analyte contain ionizers in the form of electronicdevices, and/or ionizer by corona discharge, and/or photoinitiator, and/or a laser ionizer, and/or enter the spray of the liquid sample, and/or the input of gas samples, and/or substrates for desorption from the surface.

5. The ion mobility spectrometer according to claim 1, characterized in that the collector is made on the basis of the plate Faraday or mass spectrometer.

 

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