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Device for production and analysis of analyte ions

Device for production and analysis of analyte ions
IPC classes for russian patent Device for production and analysis of analyte ions (RU 2346354):

H01J49 - Particle spectrometers or separator tubes (for measuring gas pressure H01J0041100000)
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FIELD: physics; measurement.

SUBSTANCE: invention relates to analytical instrumentation, in particular, to detection of ultratraces of hazardous substances - explosives, drugs, toxic substances. Technical effect is achieved as follows: device comprises a drift tube connected to the sample introduction device, which comprises a casing with nozzles for sample input and for gas bleeding from ionisation zone. The casing comprises a reciprocable target with nanostructured surface; continuously operating blower is positioned along the inlet and outlet nozzles axis; at the opposite inner end of the drift tube there is a collector connected to an amplifier; the amplifier output is connected to computer input. The target is provided with temperature controlling assembly.

EFFECT: enhanced sensitivity to traces of hazardous substances, express analysis possibility, reduced device dimensions.

5 cl, 7 dwg

 

The invention relates to the field of analytical instrumentation, in particular to the definition of microshadow hazardous substances: explosives, drugs, toxic substances, etc. when going through checkpoints at airports, railway stations, exhibitions, searching for hidden tabs explosives and drugs at customs checkpoints, airports, railway stations, industrial and residential premises.

Known system for remote selection of air samples from the surface and from the unpackaged object containing the blow-off device object with compressed air, comprising a booster injection of air flow, a suction device received from the object of the air flow, equipped with a booster intake air flow and the device selection transported from the object sample.

The blow-off device provided with a swirl air flow and a channel for transporting the pressurized air flow from the pump to swirl. The patent of Russian Federation №2279051, IPC: G01N 1/22, 2006 total system for remote selection of air samples cumbersome and inefficient.

A device detecting traces of hazardous substances on the surfaces of objects under inspection, containing an input device of the inspected object, booster air flow, cooling the surface is to be object, the heater and the detector connected to the output of the input device of the inspected object. As the examined object is used, the surface requirements of the control of the document.

The device is further provided with an air cleaning filter, and the detector uses a spectrometer ion mobility increment (SPIP). Output SPIP is connected via the pump flow to the input of the filter. Input input devices of the inspected object and the input SPIP connected to the output of the filter, in addition, the heater is located directly above the surface of the document, and the input device of the inspected object is performed in a sealed chamber that protects the target surface of the document from the external atmosphere. The patent of Russian Federation №2288459, IPC: G01N 13/00, 2006

The device is designed for small target objects.

Known apparatus for forming and analyzing ions of the analyte containing the target nanostructured surface, means for directing the analyte to the target, the laser energy source to heat the nanostructured surface of the target, means for determining a component of the analyte. U.S. patent No. 6825477, IPC: H01J 49/00, 2004, the prototype (analyte (word analysis) in modern terminology - the object of study, mainly gotoblas the th state).

Essentially, the prototype provides a list of nodes and devices, which could give the opportunity to the formation and analysis of analyte ions.

The technical result of the invention of the model is to increase the sensitivity of detection of traces of hazardous substances, the opportunity for rapid analysis, the compactness of the device.

The technical result is achieved in that 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 are 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 the lugs on the opposite inner 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 dielectric rings. Uz the l input samples provided with the insulator, inside of which is a metal Cup with a grid and heating element. The laser performed pulse-periodic, and one of the outputs of the laser through the synchronizer is connected to the computer input. The target is equipped with a host of control.

The invention is illustrated in figure 1-7.

1 schematically shows a longitudinal section of a variant of the node of the input samples, where 1 - body, 2 - Teflon insulator, 3 - metal glass, 4 - mesh, 5 - solid target, 6, 7 - liners, 8 - quartz window, 9 - Teflon rod 10 to the heating element.

Figure 2 presents the basic projection of another version of node input samples, where the 5 target 6 insert 7 insert 11 - tube for collection of samples, 12 - tube for the output gas stream from the field ionization, 8 - quartz window, 9 - Teflon rod.

Figure 3 schematically shows a diagram of the joining node input samples 13 to the drift tube 14.

Figure 4 schematically shows a variant of the drift tube 14 connected to a node of the input samples 13, 15 where the collector 16 of the ring electrode 17 - dielectric ring, 18 - amp 19 - the direction of buffer flow, 20 - rounds with molecular sieves, 21 - direction drift of ions, 22 - sampling the thread 23 of the laser beam perpendicular to the figure. The drift tube 14 is a system of alternating metal Kohl is of evich electrodes 16, separated by dielectric rings 17.

Figure 5 presents the spectra of positive ions hexagona (RDX), and plastid based on it (A31) using laser radiation with λ=266 nm.

Figure 6 presents a range of ion mobility of negative ions TNT (the laser radiation parameters: λ=266 nm, q=8·105W/cm2that ν=GC).

Figure 7 presents a range of ion mobility signal background ionization and ionization signal TNT vapors from the target of NPK (negative ions; λ=532 nm, q=2·107W/cm2; the mode of destruction of the target).

Apparatus for forming and analyzing ions of the analyte works as follows.

Sampling stream 22 is formed by a pump (not shown). Sampling stream 22 allows a continuous fence vapors of the compounds under investigation.

From the sampling stream 22 molecules are sorbed analyte nanoporous surface of the target 5. Laser radiation for ionization process or desorption of molecules introduced through the quartz window 8, transparent to UV laser radiation (λ1=354 nm, λ2=266 nm).

Case 1 inlet node of the 13 samples (figure 1, figure 3) vacuumable join with field enter the drift tube 14. In case 1 inlet node samples 13 is made of two coaxial holes for mounting the Teflon rod 9 target 5 inserts 6, 7 or protected area for the ical (quartz) Windows 8 for input UV laser radiation.

Metal glass 3 is separated from the housing Teflon insulator 2. At its end, near to the intake hole, fixed metal mesh 4 mesh size of 1-2 mm For input generated negative ions in the field enter the spectrometer on the metal Cup 3 grid 4 support the potential of -50 to -200 In relation to the earth.

Target 5 nanostructured surface for laser desorption or ionization fixed on the end of the Teflon rod 9, which can be screwed into the insert 7, changing the location of the target 5. The target 5 is equipped with a control element (not shown). In analysing the changes of temperature of the nanostructured surface of the target 5, changing its properties, sorption, initiating or slowing down the process of ionization.

Node input samples 13 includes a heating element 10, made in the form of a spiral. The heating element 10 provides heating of the housing 1 to a temperature of 70-100°that reduces the sorption of the analyte with the test substance on the inner walls of the inlet node of samples 13 and subsequent distortion of the recorded signals.

The mode of operation of the laser pulse-periodic, with a pulse frequency of at least 20 Hz; wavelength 532-265 nm; energy laser pulses 100-1000 µj/pulse; the duration of the laser pulses of 10-6-10-9with; the power density radiated by the I on the surface of the target 10 5-107W/cm2.

As a result of such exposure laser radiation is heated nanostructured surface of a solid target 5 and the subsequent ionization and desorption of previously captured molecules of the analyte.

Figure 4 drift tube 14 is shown with attached input node of the sample 13.

Aperture for withdrawal and the formation of a flow of ions into the drift tube 14 is a two first electrode drift tube. These electrodes are structurally designed in the form of shaped apertures, separated by a thin dielectric layer. The irradiated target 5, which is part of the input device, the sample is on the other side of the diaphragm with respect to the drift tube 14.

To provide the necessary movement of ions along the drift tube 14 toward the collector 15, near the axis of the drift tube with annular electrodes 16 produce a uniform electric field with a strength of 100 to 300 V/cm For this on an adjacent ring electrodes 16 serves the potential difference 100-300, and the total voltage drop across the drift tube 14 is 1200-3500 C. the polarity of the voltage in the process of change analysis, which gives the opportunity to explore the spectra of both positive and negative ions.

In order to improve the homogeneity of the field in the end of the drift tube 14, the latter to Lavoy the electrode is made with a parabolic surface (figure 4 left).

Driving under the influence of an electric field to the manifold 15, the ionized molecules acquire average speed

ν=μ·E,

where μ - the mobility of the ion in the gas, E is the electric field.

The mobility of the ions depends on their mass m, charge q, the cross section of collision with the molecules of the buffer gas tube σ, buffer gas density n, mass of its molecules M and temperature T, and is defined as follows:

Due to the difference in the value of mobility as drift of ions is their spatial separation, which is manifested in the form of the time dependence of the recorded ion current.

To prevent debris from entering the drift region ionized molecules in the drift tube 14 by means of the air pump arranged the buffer gas stream 19, which creates a kind of gas valve on the boundary of the region of ionization and drift region.

The air, which forms the buffer gas flow passes through the cartridges with molecular sieves 20, which provide cleaning and reduce the content of water vapor. For the organization of the buffer and sampling of gas streams using non-aggressive gases (N2Not, Ar and others).

One of the most important characteristics of the drift tube 14 is resolution, which which is defined as

,

where tdthe time drift of the ion packet, Δt is the width of the signal of the ion current on the half-amplitude.

The value of resolution is at the level of R=45, which ensures reliable separation of the signals of the ion current, relevant, in particular, various explosives.

The sensitivity of the drift tube 14 is not less than 10-14g/cm3. The assessment is based on the experimental results on the detection of RDX vapor when multiphoton ionization.

The spectrum of positive ions RDX and plastid C31-E with their ionization laser radiation with λ=266 nm and detection using drift tube 14 is presented in figure 5.

Registration system and signal processing ion current includes a reservoir 15, which is placed at the exit of the drift tube 14, a high-current amplifier 18, a personal computer with a built - in CPU and software, as well as the clock generator for ADC Board.

At the end of the movement in the drift tube 14 ions into the collector 15, which is directly connected to the input current (electrometric) of the amplifier 18. The sensitivity of this system allows you to boost the signal of the ion current at 100 f.

The frequency range of the signal amplification up to 3 kHz provides amplification ion is th current without distorting its temporal characteristics.

The signal from the current amplifier 18 is fed to the input of the ADC Board of a personal computer, through which it is possible to observe in real time, and to produce a record for further processing.

As the device operates on time-of-flight principle, for monitoring and recording the ion current signal provided by the synchronization of the laser pulse with the beginning of the timebase Board ADC. This electrical signal synchronized with the laser unit served by the pulse generator, and then to the sync input of the ADC Board.

In the field of nanostructured surface of a solid target 5 form an electric field of not less than 100 V/cm and record the range of ion mobility.

The lower limit value of the electric field strength in the area of nanostructured surface is determined by the effective beginning of the collection of generated ions to 100%.

The upper limit is caused by the occurrence of corona discharge and destruction of the surface. When increasing the field strength in the case of registration of negative ions, there is an increasing process of laser desorption or ionization and sharp, up to 5-6 times the amplitude and up to 10 times the square of the increase in the detected signal of the ion current.

1. A device for obtaining and analyzing ions of the analyte, containing the its target with nanostructured surface, means for sending to the target analyte, the laser, the means for selecting ions of the analyte, characterized in that the means for directing to the target analyte and a means for selecting ions of the analyte are 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 end of the drift tube collector is connected to the amplifier, the amplifier output connected to the computer input.

2. A device for obtaining and analyzing ions of the analyte according to claim 1, wherein the drift tube is made in the form of ring electrodes separated by dielectric rings.

3. A device for obtaining and analyzing ions of the analyte according to claim 1, characterized in that the node input samples provided with the insulator, inside of which is a metal Cup with a grid and heating element.

4. A device for obtaining and analyzing ions of the analyte according to claim 1, characterized in that the laser is performed pulse-periodic, one of the outputs of the laser through the synchronizer is connected to the input of the of the computer.

5. A device for obtaining and analyzing ions of the analyte according to claim 1, characterized in that the target is equipped with a host of control.

 

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