WO2012063796A1 - 分析装置及び分析方法 - Google Patents
分析装置及び分析方法 Download PDFInfo
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- WO2012063796A1 WO2012063796A1 PCT/JP2011/075666 JP2011075666W WO2012063796A1 WO 2012063796 A1 WO2012063796 A1 WO 2012063796A1 JP 2011075666 W JP2011075666 W JP 2011075666W WO 2012063796 A1 WO2012063796 A1 WO 2012063796A1
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- air supply
- sample
- fine particle
- particulate collection
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Images
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
- H01J49/0422—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for gaseous samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2211—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling with cyclones
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/0027—Methods for using particle spectrometers
- H01J49/0036—Step by step routines describing the handling of the data generated during a measurement
-
- 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
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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
- H01J49/0459—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for solid samples
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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
- H01J49/0468—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N2001/028—Sampling from a surface, swabbing, vaporising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/0057—Warfare agents or explosives
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Definitions
- the present invention relates to an analysis apparatus and an analysis method for collecting and analyzing fine particles.
- Patent Document 1 discloses a method of collecting floating dust in a clean room with a cyclone and measuring the number with a counter.
- Patent Document 2 JP 2009-31227 A discloses a method of measuring the weight of airborne particles collected by collecting them on a tape-like filter.
- Patent Document 3 discloses a method of collecting sampled fine particles with an inertial impactor, heating the collection part to evaporate the fine particles, and analyzing with a mass spectrometer. .
- Patent Document 4 describes an explosive detection apparatus using a mass spectrometer. The explosive vapor leaked from the package is collected by a sampling probe, ionized using a negative corona discharge, and detected using a mass spectrometer to determine the presence or absence of a dangerous substance.
- JP-A-7-6729 Patent Document 5
- explosive particles are collected by a cyclone on a disk-shaped or tape-shaped filter, moved to another position, and the collected explosive particles are heated and evaporated.
- a method of analyzing with an ion mobility analyzer is disclosed.
- Japanese Patent Laid-Open No. 3-87629 Patent Document 6 describes a portal-type explosive detection device. Put the subject in a booth-shaped room with walls on the top and bottom and left and right, and blow air from the left and right. This air causes explosive particles adhering to the subject to rise. Furthermore, explosive particles are sucked from a suction port on the ceiling with a large-capacity suction pump and adsorbed by a filter provided on the rotating body. The rotating body is rotated to move the filter to the analysis unit, and the adsorbed explosive fine particles are evaporated by heating and analyzed by an ion mobility analyzer.
- JP 2000-35383 A JP 2009-31227 A JP 2005-91118 A JP 2000-28579 A Japanese Patent Laid-Open No. 7-6729 Japanese Patent Laid-Open No. 3-87629
- Patent Document 1 cannot identify a component of floating dust.
- the technique described in Patent Document 2 cannot identify components of suspended particles.
- the technique described in Patent Document 3 requires adsorption and heating processes of the collection unit, and cannot perform mass analysis of the components of the fine particles continuously. In the case of continuous measurement, a method of alternately operating two inertial impactors is also described, but a space for two is required, and it is difficult to reduce the size.
- fine particles are adsorbed inside the valve, and the valve needs to be cleaned. Therefore, when the valve is used for a long time, a long maintenance time is required.
- Patent Document 4 requires that the explosive vapor leaked from the luggage be collected by a sampling probe.
- Destructive military explosives and explosives, industrial explosives used at construction sites, etc. use stable materials for safe operation, so there are many materials with relatively low vapor pressure. Therefore, it is necessary to collect and analyze as fine particles rather than collecting steam.
- Patent Document 5 requires adsorption and heating processes and cannot perform continuous real-time analysis.
- Patent Document 6 requires adsorption and heating processes and cannot perform continuous real-time analysis. Further, since the suction is performed from the suction port by a large-capacity suction pump, not only explosive fine particles but also dust etc. are sucked together to cause clogging of the filter, and long-term operation is difficult. Furthermore, there is a problem that the vapor generated from the explosive fine particles is diluted by a large volume of suction.
- the conventional explosive detection device as in Patent Document 6 is considered for the purpose of inspecting a relatively small number of people mainly on the premise of operation at an airport or an important facility.
- a mass transit system that is used in large quantities by passengers at stations, etc.
- there is a high throughput that can be inspected in a short time and a reduction in the false alarm rate that the detector reacts without having explosives.
- careful baggage inspection by an inspector is required, which affects the throughput. Therefore, when a false alarm occurs, quick inspection is difficult.
- the present invention provides an analyzer that analyzes in real time while continuously collecting and concentrating fine particles.
- fine particles having a specific particle size can be collected in the collection unit.
- the collected fine particles are evaporated by heating the collection unit.
- sucking this vapor from the back surface of the collection part, ionizing it, and analyzing it with a highly sensitive and highly selective mass spectrometer it becomes possible to specify the components of the fine particles.
- by collecting the fine particles concentrated by the cyclone phenomenon in the collection unit and separating the large volume suction for collecting the fine particles and the suction for analysis sent to the mass spectrometer in the collection unit It is possible to reduce the effect of dilution by suction.
- the analyzer of the present invention includes, as an example, an authentication unit having a surface for bringing an authentication object close thereto, and an air supply that peels off the gas and / or fine particles of the detection target substance that is attached to the authentication object by sending an air flow along the authentication part.
- the suction section for sucking the gas and / or particulates of the detection target substance separated from the authentication target
- the particulate collection section for concentrating and collecting the sample of the suctioned detection target substance
- An ion source unit that introduces and ionizes a sample of the target substance
- a mass analysis unit that performs mass analysis of ions generated in the ion source unit
- a control unit that controls the ion source unit and the mass analysis unit
- a detection target material The database unit that holds the derived mass spectrum data, the mass analysis result of the sample by the mass analyzer unit, and the mass spectrum data held in the database unit are collated to determine the presence or absence of the detection target substance Comprising a tough, a display unit for displaying the determination result of the determining unit.
- FIG. 5 is a view showing an example in which an air supply unit for separating fine particles, an air supply unit for cleaning, and an intake unit for sucking fine particles having a lid are provided, and a coarse mesh filter is installed between the cover for the intake unit and the intake unit. is there. It is a figure which shows an example of the internal structure of the analyzer by this invention.
- FIG. 1 is a schematic diagram showing an example of the analyzer according to the present embodiment, and shows an example incorporated in an automatic ticket gate 50 such as a station.
- automatic ticket gates at stations, etc. they are built into security gates installed at entrances and exits of facilities, boarding gates such as airports and ships, gates of baggage inspection areas and baggage inspection areas, entrance / exit ticket gates of amusement facilities, etc. You can also.
- the analysis apparatus 1 is provided with an authentication unit 4 having an authentication surface 3 for making an authentication object 2 close and authenticating.
- the authentication object 2 is, for example, an IC card, a mobile phone, a ticket, a living body part such as a hand, a finger, or an eye.
- An air supply unit 5 that sends an air flow along the authentication surface 3 is provided, and gas and / or fine particles that are detection target substances attached to the authentication target 2 are peeled off.
- the air supply control unit 7 controls the flow rate or flow velocity, injection pressure, temperature, injection time, injection timing, and the like of the air supply unit 5.
- the gas and / or fine particles of the detection target substance that has been peeled off are sucked by the intake section 6.
- the sucked fine particles of the detection target substance are concentrated and collected by the fine particle collecting unit 10.
- the particulate collection unit 10 collects particulates of the detection target substance with high efficiency using a cyclone phenomenon. Even if the particulate collection unit 10 sucks a large volume from the intake unit 6, it can collect only the particulates of the detection target substance having a specific particle size, and the sample of the detection target substance is diluted by the suction airflow. Can be prevented.
- the particulate collection unit 10 controls operations such as a suction flow rate, a flow rate, a temperature, and an operation sequence by the particulate collection control unit 15.
- the detection target substance collected by the particulate collection unit 10 is ionized by the ion source unit 21.
- the ionized ions are subjected to mass analysis by the mass analyzer 23.
- the ion source unit 21 and the mass analysis unit 23 control the temperature, voltage, and operation sequence by the control unit 24 to acquire mass spectrum data.
- Mass spectrum data derived from the substance to be detected is held in the mass database unit 26, and the determination unit 25 collates the mass analysis result of the sample by the mass analysis unit 23 with the mass spectrum data held in the mass database unit 26.
- the presence or absence of the detection target substance is determined.
- FIG. 2 is a diagram showing an example of the internal configuration of the analyzer according to the present embodiment.
- the analysis apparatus 1 includes an authentication unit 4 including an authentication surface 3 for authenticating the authentication target 2 and includes an authentication acquisition unit.
- the authentication surface 3 may be arranged horizontally or may be inclined.
- the authentication surface 3 may be transparent or mesh-shaped, and may have a shape through which not only radio waves but also light and air current pass from the authentication unit 4.
- the authentication data when the authentication object 2 is authenticated is checked against an external or internal authentication database.
- the air supply part 5 and the air intake part 6 are arranged so that the authentication surface 3 is in between. From the air supply unit 5, when the authentication target 2 approaches the authentication surface 3 by sending an air flow along the authentication surface 3, the air supply hits the authentication target 2 and is attached to the authentication target 2.
- the sample gas is generated by the gas and / or fine particles, or the gas and / or fine particles of the detection target substance are peeled off.
- the wind generated from the air supply unit 5 for separating the gas and / or fine particles of the detection target substance may be continuous, intermittent, irregular, or sudden. Thereby, the gas and / or fine particles of the detection target substance peeled from the authentication target 2 are transferred to the intake section 6.
- This airflow is an airflow that prevents the turbulent flow from preventing the gas and fine particles from being detected without being inhaled. It is desirable to supply air in parallel to the authentication surface 3. That is, an airflow that does not hit the authentication surface 3 is desirable to prevent turbulent flow.
- An air supply control unit 7 that controls the air supply unit 5 is connected to the air supply unit 5.
- the air supply control unit 7 controls the driving of the air supply unit 5 such as the flow rate or flow velocity, the injection pressure, the temperature, the injection time, and the injection timing.
- the air supply unit 5 is a sensor that detects that a person, a hand, a finger, or the like is approaching, or a sensor that detects that a person has passed, even if the air supply unit 5 constantly supplies air or drives in synchronization with authentication. It may be driven when an external sensor such as As an example, after receiving the authentication start signal, an injection pressure of 0.05 MPa, an average flow velocity of 49 meters / second on the authentication surface 3, an injection time of 0.1 second, and a pause time of 0. A 5-second pause was performed 10 times in succession.
- a coarse mesh filter 8 is provided in the intake portion 6 to prevent large dust from entering and a finger from being put into the intake portion 6.
- a wire mesh (opening 0.5 mm, porosity 50%) was used as an example.
- the coarse mesh filter 8 can be replaced, and when it is clogged with dust, it can be cleaned and reused or replaced with a new one.
- the gas and / or fine particles of the detection target substance sucked from the intake portion 6 are introduced into the fine particle collecting portion 10 through the suction pipe 9.
- the suction pipe 9 is heated by a pipe heater 11 to prevent gas and fine particles from being adsorbed inside the pipe.
- the piping heater 11 was heated at 120 ° C.
- the suction pipe 9 and the pipe heater 11 may be made as short as possible or eliminated, and the particulate collection unit 10 and the suction unit 6 may be directly connected.
- the particulate collection unit 10 includes a conical particulate concentration unit 12, a large-capacity suction pump 13, a particulate collection filter unit 14, a particulate collection control unit 15, and an adsorption preventer 16.
- the large-capacity suction pump 13 performs suction at a flow rate of 40 meters / minute, for example. Due to this suction, a cyclone phenomenon occurs inside the conical fine particle concentrating portion 12. For example, fine particles having a particle size of 5 ⁇ m or more are collected by the fine particle collecting filter portion 14 provided in the small radius portion of the fine particle concentrating portion 12. The other airflow is discharged by the large-capacity suction pump 13.
- the large-capacity suction pump 13 can control the flow rate or flow rate by the particulate collection control unit 15.
- the large-capacity suction pump 13 may be operated at all times or can be synchronized with the operation of the air supply unit 5.
- the adsorption preventer 16 is heated and / or vibrated by a heater to prevent the fine particles from being adsorbed inside the fine particle concentrating unit 12.
- a vibration motor for applying vibration, an ultrasonic vibrator, an eccentric motor, a vibration motor, or the like may be used.
- Explosive fine particles usually have a particle size of 5 ⁇ m or more and 100 ⁇ m or less, so it is preferable to collect fine particles of this particle size.
- the inner surfaces of the intake section 6, the suction pipe 9, the conical fine particle concentrating section 12, etc. may be made of Teflon or coated with Teflon. Fine particles of trimethylenetrinitroamine (RDX) and trinitrotoluene (TNT), which are the main components of plastic explosives, are negatively charged. Since Teflon is also negatively charged, the negatively charged explosive fine particles are repelled and difficult to adsorb.
- RDX trimethylenetrinitroamine
- TNT trinitrotoluene
- the particulate collection filter 14 is wound around a filter winding unit 78b and a filter feeding unit 78a.
- the filter winding unit 78b (or the filter feed unit 78a can also be controlled) is controlled by the particulate collection control unit 15.
- the particulate collection filter 14 is heated by the collection filter heating unit 18, but not only the particulates of the component to be detected but also the particulates of the contaminating components adhere and become dirty with time.
- the mass analyzer 23 measures the mass spectrum continuously and continuously in real time, and can detect this time change of dirt.
- the background threshold value (BG threshold value) is used as the dirt threshold value. When this value is exceeded, the particulate collection filter 14 is wound once by the control of the particulate collection control unit 15 to clean the clean surface. Expose.
- the particulate collection filter 14 As the particulate collection filter 14, a ribbon-shaped object having a filtration accuracy of 50 ⁇ m, a width of 10 mm, and a thickness of 0.5 mm was used. In addition to the ribbon shape, a plate shape, a twisted rope shape, a disk shape, or a loop shape may be used. Even when the detection target substance is detected, the next measurement can be quickly performed by winding up the particulate collection filter 14 to bring out a clean surface.
- the fine particle collecting filter 14 may be made of stainless steel wire, metal fiber, heat resistant fiber (for example, Conex), glass fiber, or the like.
- a detector pipe 17 is connected to the surface on the back side of the particulate collection filter section 14 (opposite side of the particulate concentration section 12).
- the particulate adsorbed on the particulate collection filter unit 14 is heated by the collection filter heating unit 18.
- heating was performed at 230 ° C.
- the heated microparticles are vaporized, and the gasified sample is introduced into the ion source unit 21 by the suction pump 22 via the detector pipe 17.
- the suction pump 22 performs suction at a flow rate of 2.0 liters / minute.
- the detection pipe 17 is heated by a detection pipe heater 19 to prevent gas from being adsorbed inside the pipe.
- the detection pipe heater 19 was heated to 120 ° C.
- the detection pipe 17 and the detection pipe heater 19 may be as short as possible, or may be eliminated and the particulate collection filter unit 14 and the ion source unit 21 may be directly connected.
- the detection pipe 17 is provided with a fine mesh filter 20 to prevent the ion source part 21 from being contaminated with fine particles not gasified by the fine particle collecting filter part 14.
- a fine mesh filter 20 for example, a stainless steel wire filter or a sintered body filter having a filtration accuracy of 50 ⁇ m may be used.
- the fine mesh filter 20 can be cleaned and reused as needed, or replaced with a new one.
- the ion source unit 21 can be an atmospheric pressure chemical ionization source using negative corona discharge or positive corona discharge described in, for example, Japanese Patent Application Laid-Open No. 2000-28579.
- the ion generation method may be other methods such as irradiation with a radiation source, irradiation with electrons or light, laser light, Penning discharge, glow discharge, barrier discharge, electrospray, or the like.
- the ions generated from the sample by the ion source unit 21 are subjected to mass analysis by the mass analysis unit 23.
- the mass spectrometer 23 for example, a wire type linear ion trap mass spectrometer can be used.
- Mass spectrometry methods include linear ion trap mass spectrometer, quadrupole ion trap mass spectrometer, quadrupole filter mass spectrometer, triple quadrupole mass spectrometer, time-of-flight mass spectrometer, and magnetic field mass spectrometry. Other methods such as metering and ion mobility may be used.
- the signal obtained by the mass analyzer 23 is measured by the controller 24 as a mass spectrum.
- the peak of the mass number of the sample is extracted from this mass spectrum.
- the mass database unit 26 holds information including standard mass spectrometry data necessary for identifying a sample.
- the retained information includes the value of the mass-to-charge ratio (m / z) obtained by dividing the ion mass number m by the ion valence z and the relative intensity.
- the mass spectrum measured by the mass analysis unit 23 is sent to the determination unit 25 and subjected to data processing such as collation with the data read from the mass database unit 26 to specify the sample.
- FIG. 3 is an explanatory diagram showing an example of information held by the mass database unit 26.
- the mass database unit 26 includes a component substance of a sample that is a detection target substance, a type of positive ion detection or negative ion detection, a type of mass analysis (MS) or tandem analysis (MSMS), and a sample of the detection target substance Ion mass-to-charge ratio, range of mass-to-charge ratio, threshold value for detection, background threshold value for performing cleaning, etc. (BG threshold value), AND or OR with ions derived from other samples to be detected Or information such as whether to take NOT with ions derived from contaminant components.
- MS mass analysis
- MSMS tandem analysis
- BG threshold value threshold value
- information such as whether to take NOT with ions derived from contaminant components.
- the presence / absence of the sample as the specified detection target substance and / or the result of mass spectrometry is displayed on the display unit 27.
- the display unit 27 turns on a red lamp when a sample that is a detection target substance is detected, turns on a blue lamp when it is not detected, and turns on a yellow lamp when it is near the threshold.
- the display method of the result is not limited to the lighting of the lamp, but it is sufficient that the operator can recognize the presence or absence of detection by changing the display state of the entire screen or a part of the display unit 27. You may alert
- the display unit 27 may be displayed on a remote monitoring center by network communication or the like without being displayed on the apparatus main body.
- FIG. 4 is a diagram illustrating an example of a processing procedure for detecting a detection target substance according to the present embodiment.
- Authentication of the authentication target 2 is started, or the hand of the detection target is detected by the sensor (S11).
- the processing is divided into analysis processing (S12 to S14) and authentication processing (S17 to S19).
- analysis processing S12 to S14
- authentication processing S17 to S19
- the gas and / or fine particles of the detection target substance are peeled off from the authentication target 2 or the hand by the air flow flowing on the authentication surface 3, and from the intake part Suction is performed (S12).
- the sucked gas and / or fine particles of the detection target substance are concentrated by the fine particle collecting unit 10, and the mass spectrum of the detection target substance is analyzed by the mass analysis unit 23 (S13).
- the analysis result is collated with the database of the mass database unit 26 to determine the presence or absence of the detection target substance (S14).
- a detection target substance is detected, an alarm is issued, detection is displayed, and passage is not permitted (S15).
- a sound or light may be emitted as an alarm, or a security officer may be contacted. Also, control such as closing the open / close gate may be performed. If the detection target substance is not detected, passage is permitted by comparing with the authentication result (S16).
- the authentication object 2 is authenticated or a hand or the like is detected by the sensor (S11).
- Authentication data of authentication object 2 is acquired (S17).
- the authentication data is not used, for example, when only the inspection is performed by holding the hand over the authentication surface 3, the time when the hand is held over the authentication surface 3 is measured (S17).
- the authentication time specified time
- a determination is made by comparing with an authentication database registered in advance (S18). If they do not match, an alarm is displayed to prompt re-authentication and disallow passage (S20).
- the sensor detection time is measured (S19).
- the specified time for the sensor detection time is, for example, 2 seconds or more. If it is only held for 1 second, even if it is authenticated, it is shorter than the specified time, so an alarm is displayed and re-authentication is urged and passage is not permitted (S20).
- the passage is permitted by collating with the analysis result (S16).
- FIG. 5 is a schematic diagram showing an example of the mass spectrometer of the present embodiment.
- a wire-type linear ion trap mass spectrometer is used for the mass analyzer.
- the ion source unit 21 primary ions are generated by corona discharge in the atmosphere, and the sample is ionized using a chemical reaction between the primary ions and the sample.
- a needle electrode 28 is disposed in the ion source 21, and a high voltage is applied between the ion source 21 and the extraction electrode 29, and a corona discharge is generated near the tip of the needle electrode 28. For example, a voltage of 5 kV was applied for positive ionization and ⁇ 4 kV was applied for negative ionization.
- the ion of the ionized sample passes through the first pore electrode 30a, the first differential exhaust portion 31a, the second pore exhaust electrode 30b, the second differential exhaust portion 31b, and the third pore electrode 30c. It is introduced into the ion trap part 34 of 31c.
- differential exhaust is used.
- Vacuum pumps 32a and 32b were used for differential exhaust. One vacuum pump 32b can evacuate two places.
- the vacuum pump 32a was also used as a roughing pump for the vacuum pump 32b.
- the differential pumping method may be another method such as using a vacuum pump individually.
- the pore diameter of each pore is, for example, 0.12 mm inner diameter and 10 mm length for the first pore electrode 30a, 0.5 mm inner diameter for the second pore electrode 30b, and the third pore electrode 30c.
- the pores had an inner diameter of 1.2 mm.
- the hole diameter of the pores depends on the displacement of the vacuum pump.
- An ion guide 33 is installed in the second differential exhaust part 31b. Instead of the ion guide, an ion lens or the like may be used. Further, an ion guide, an ion lens, or the like may be installed in the first differential exhaust part 31a, the second differential exhaust part 31b, and the high vacuum part 31c. It is desirable to heat the ion source section 21, the first pore electrode 30a, and the second pore electrode 30b in order to prevent dirt and the like from adhering to the inside.
- the ion trap section 34 includes an inlet end electrode 35a, an outlet end electrode 35b, a quadrupole rod electrode 36, an excitation electrode 37 inserted in a gap between the quadrupole rod electrodes 36, a trap wire electrode 38a, and an extraction wire electrode 38b. Is done.
- a buffer gas necessary for ion trap and ion dissociation is supplied from a buffer gas supply source 41 to the ion trap unit 34.
- helium gas is used in this embodiment, air, argon, nitrogen, or the like may be used.
- Ions introduced into the ion trap section 34 are trapped in the trap region 39 by the electrostatic potential between the axial entrance end electrode 35a and the trap wire electrode 38a and the quadrupole potential by the quadrupole rod electrode 36 in the radial direction. Is done.
- an AC voltage is applied to the excitation electrode 37 inserted between the quadrupole rod electrodes 36, only ions of a specific m / z are resonantly excited in the direction of the excitation electrode 37, and the axis is generated by the extraction electric field formed by the extraction wire electrode 38b. Discharged in the direction. This specific m / z ion is detected by the detector 40.
- a mass spectrum is obtained by discharging the ions of an arbitrary m / z by controlling the resonance condition and the voltage of each electrode by the control unit 24.
- the measurement of the mass spectrum once is possible in 100 milliseconds, for example. It is also possible to measure positive ions and negative ions alternately. Specifically, for example, after measuring positive ions in 0.5 seconds, each electrode is switched to negative ion detection at high speed to measure negative ions in 0.5 seconds, and each electrode is again positive ion at high speed. Switch to detection and measure positive ions. By repeating this, the mass spectrum of positive ions and the mass spectrum of negative ions are measured. As a result, the mass spectrum of both positive and negative ions can be measured in 1 second. The switching speed can be further increased.
- a plurality of spectra such as a mass spectrum having a different mass range and a normal mass spectrum and a tandem mass spectrum can be measured. Switching between these measurement modes and continuous measurement are performed under the control of the control unit 24.
- the measured mass spectrum is sent to the determination unit 25 and subjected to data processing such as collation with the information in the mass database of the sample to be detected read from the mass database unit 26, and the sample to be detected Is specified.
- the presence / absence of the specified sample gas and / or the result of mass spectrometry is displayed on the display unit 27.
- a wire-type linear ion trap mass spectrometer is used for the mass analysis unit, but the ion trap unit 34 can be used for other mass analysis methods such as a linear trap, a quadrupole ion trap, a quadrupole filter, and ion mobility. Good.
- Trinitrotoluene which is a typical material for military explosive components, was measured with the analyzer of this example.
- FIG. 6 is a diagram showing an example of a mass spectrum of trinitrotoluene measured by the analyzer of this example.
- silica gel fine particles having a particle diameter of 20 to 30 ⁇ m and containing trinitrotoluene were used.
- Several micrograms of this sample was attached to the IC card to be authenticated. The IC card is touched on the authentication surface of the analyzer of the present embodiment for authentication, and the sample attached to the IC card is peeled off, sucked in the suction part, and concentrated and collected in the particulate collection part.
- ionization was performed in the ionization section, and analysis was performed in the mass spectrometry section.
- the negative ion detection for example, the intake part, the pipe heater, and the fine particle concentration part were heated to 120 ° C.
- the collection filter heating part was heated to 200 ° C.
- the detection pipe heater, the ion source part, and the first pore electrode were heated to 120 ° C.
- the molecular weight (M) of trinitrotoluene is 227.
- 210 is detected at the same time, and if trinitrotoluene is detected, the possibility of false alarms is reduced.
- detection of trimethylenetrinitroamine, dinitrotoluene, cyclotetramethylenetetranitramine, pentaerythritol pen slit, hydrogen peroxide, etc. was also confirmed by negative ion detection.
- detection of triacetone tripoxide, hexamethylenetripoxide diamine, etc. was also confirmed by positive ion detection.
- tandem mass spectrometry can further increase the selectivity and reduce the false alarm rate.
- FIG. 7 is a diagram illustrating an example of a processing procedure for cleaning the particulate collection filter unit.
- the background (BG) of the sample is sucked from the particulate collection filter section through the detection pipe (S21).
- the aspirated background is ionized and the mass spectrum is analyzed by the mass analyzer (S22).
- the analysis result is collated with the database of the mass database unit, and it is determined whether the background exceeds or exceeds the BG threshold value due to impurities or the like (S23).
- the particulate collection filter section is contaminated with impurities, the background exceeds the BG threshold, so that the clean surface is exposed by winding a predetermined amount of the filter under the control of the particulate collection control section of the particulate collection filter section.
- the background is not allowed to exceed the BG threshold value due to foreign matters (S24).
- FIG. 8 is a diagram showing an example in which the signal intensity change in the background (BG) and the particulate collection filter are subjected to a clean surface treatment.
- the BG signal intensity tends to increase. Conversely, it may decrease with time, but this is an effect of cleaning the particulate collection filter by heating or the like.
- the BG signal intensity exceeds the BG threshold value described in the mass database, the particulate collection filter unit is made a clean surface. Along with this, the BG signal intensity rapidly decreases.
- the filter surface is made clean only when the BG threshold is exceeded or when the detection target substance is detected by the clean surface processing of the particulate collection filter unit, so it can be used for a long time with a small amount of filter. Therefore, the maintenance frequency can be reduced.
- the fine particle collecting unit collects the fine particles using a plurality of fine particle concentrating units. By using this method, it becomes possible to control the particle diameter of the detection target substance while controlling the particle diameter.
- FIG. 9 is a schematic diagram showing an example of a particle collecting unit using a large rotation particle concentration unit and a small rotation particle concentration unit.
- the particulate collection unit 10 is provided with a conical large rotating particulate concentrating portion 51 having a large rotation radius and a conical small rotating particulate concentrating portion 52 having a small rotation radius in the cyclone phenomenon.
- the small rotating particle concentrating unit 52 is connected in series to the downstream side of the large rotating particle concentrating unit 51.
- the detection target substance gas and / or fine particles sucked from the intake portion 6 are first introduced into the large conical large rotation fine particle concentrating portion 51 via the suction pipe 9.
- a cyclone phenomenon with a large rotation radius occurs inside the large rotating fine particle concentrating portion 51.
- fine particles having a particle size exceeding 100 ⁇ m are collected on the bottom surface of the large rotating fine particle concentrating portion 51, and other particle sizes of 100 ⁇ m or less.
- the fine particles are sent to the next small conical small rotating fine particle concentrating unit 52.
- a cyclone phenomenon with a small rotation radius occurs inside the small rotating particle concentrating unit 52, and for example, particles having a particle size of 100 ⁇ m or less and 5 ⁇ m or more are collected by the particle collecting filter unit 14. Particles having a particle diameter of less than 5 ⁇ m and airflow are sucked by the large-capacity suction pump 13.
- the particulate matter of the detection target substance having a particle size of 100 ⁇ m or less and 5 ⁇ m or more collected by the particulate collection filter unit 14 is heated and vaporized by the collection filter heating unit 18, and the vaporized sample is introduced into the ion source unit 21 for ionization. To do.
- the ionized ions are subjected to mass analysis by the mass analyzer 23 to detect the presence or absence of the detection target substance in the sample.
- the large rotation particle concentration unit 51 can prevent the particle collection filter 14 from being clogged by collecting relatively large particles, particularly dust or dust. These dust and dust are collected on the bottom surface of the large rotating particle concentrating unit 51. Therefore, dust and dust can be periodically discarded by making the bottom surface easy to open.
- FIG. 10 is a schematic view showing an example of a particle collecting unit using a large rotation particle concentration unit and a plurality of small rotation particle concentration units.
- the fine particle collecting unit 10 includes two conical large rotating particle concentrating units 53 having a large rotation radius and two conical small rotating particle concentrating units having a small rotation radius in the cyclone phenomenon, that is, a first small rotating particle concentrating unit. 54a and a second small rotating particle concentrating part 54b are provided.
- the arrangement may be such that the first small rotating particle concentrating unit 54a and the second small rotating particle concentrating unit 54b are arranged around the particle collecting filter unit 14.
- the first small rotating particle concentrating part 54 a and the second small rotating particle concentrating part 54 b are sucked by the large capacity suction pump 13.
- the gas and / or fine particles of the detection target substance sucked from the intake portion 6 are first introduced into the large conical large rotation fine particle concentrating portion 53 via the suction pipe 9.
- a cyclone phenomenon with a large rotation radius occurs inside the large rotating fine particle concentrating portion 53.
- fine particles having a particle size exceeding 100 ⁇ m are collected on the bottom surface of the large rotating fine particle concentrating portion 53, and other particle sizes of 100 ⁇ m or less.
- the fine particles are sent to the next small conical first small rotating particle concentrating unit 54a and second small rotating particle concentrating unit 54b.
- a cyclone phenomenon with a small rotation radius occurs inside the first small rotating particle concentrating unit 54a and the second small rotating particle concentrating unit 54b.
- particles having a particle size of 100 ⁇ m or less and 5 ⁇ m or more are captured by the particle collecting filter unit 14. Be collected. Particles having a particle diameter of less than 5 ⁇ m and airflow are sucked by the large-capacity suction pump 13.
- the particulate matter of the detection target substance having a particle size of 100 ⁇ m or less and 5 ⁇ m or more collected by the particulate collection filter unit 14 is heated and vaporized by the collection filter heating unit 18, and the vaporized sample is introduced into the ion source unit 21 for ionization. To do.
- the ionized ions are subjected to mass analysis by the mass analyzer 23 to detect the presence or absence of the detection target substance in the sample.
- the conical first small rotating particle concentrating portion 54a and the second small rotating particle concentrating portion 54b have the same size.
- the particle diameters to be concentrated can be controlled.
- the particle size to concentrate can be controlled also by making the flow velocity or flow volume to attract
- both the radius of rotation and the flow velocity or flow rate to be sucked may be changed. It is also possible to collect fine particles having a smaller particle diameter by installing a fine particle concentrating unit having a smaller rotation radius next to the first small rotating fine particle concentrating portion 54a and the second small rotating fine particle concentrating portion 54b. It is.
- FIG. 11 is a diagram showing an example of a particulate collection unit using the particulate concentration intake section and the particulate concentration section.
- the particulate collection unit 10 is provided with a conical particulate concentrating intake portion 55 having a large rotation radius in the cyclone phenomenon.
- a conical small rotating particulate concentrating portion 56 having a smaller rotational radius than the particulate concentration intake portion 55 is provided. Is provided.
- a coarse mesh filter 57 is attached to the fine particle concentration intake section 55 to prevent large dust from entering and a finger from entering the fine particle concentration intake section 55.
- the fine particle concentration intake section 55 has a conical shape with a large radius, and a cyclone phenomenon with a large rotation radius occurs. Due to this cyclone phenomenon, for example, fine particles having a particle size exceeding 100 ⁇ m are collected on the bottom surface of the fine particle concentration intake portion 55. The other fine particles having a particle size of 100 ⁇ m or less are sent to the next small conical small rotating fine particle concentrating unit 56.
- a cyclone phenomenon with a small rotation radius occurs inside the small rotating particle concentrating unit 56, and for example, particles having a particle size of 100 ⁇ m or less and 5 ⁇ m or more are collected by the particle collecting filter unit 14. Particles having a particle diameter of less than 5 ⁇ m and airflow are sucked by the large-capacity suction pump 13.
- the particulate matter of the detection target substance having a particle size of 100 ⁇ m or less and 5 ⁇ m or more collected by the particulate collection filter unit 14 is heated and vaporized by the collection filter heating unit 18, and the vaporized sample is introduced into the ion source unit 21 for ionization. To do.
- the ionized ions are subjected to mass analysis by the mass analyzer 23 to detect the presence or absence of the detection target substance in the sample.
- the particle collection filter 14 can be prevented from being clogged. These dust and dust are collected on the bottom surface of the fine particle concentration intake section 55. Therefore, dust and dust can be periodically discarded by making the bottom surface easy to open.
- the device can be made compact by setting the rotation radius of the fine particle concentrating intake section 55 to a half circumference.
- FIG. 12 is a schematic diagram showing an example of an analyzer using a gas suction inlet, a particulate suction suction section, and a particulate collection section.
- air currents such as gas and steam are diluted.
- air stream such as gas and vapor can be detected in a state of being attached to other fine particles.
- a gas suction inlet 58 for sucking an air current such as gas and vapor a fine particle suction air intake 59 for sucking both an air current such as fine particles, gas and steam, and a particle collecting portion 10 are provided.
- a fine mesh filter 60 is provided in the gas suction portion 58 so that fine particles and the like are not sucked.
- Air currents such as gas and vapor sucked by the gas suction intake section 58 are introduced into the ion source section 21 through the gas suction pipe 61 and ionized.
- the ionized ions are subjected to mass analysis by the mass analyzer 23 to detect the presence or absence of the detection target substance in the sample.
- the suction pump 22 performs suction at a flow rate of 4.0 liters / minute.
- the gas suction pipe 61 has a flow rate of 2.0 liters / minute
- the detector pipe 17 has a flow rate of 2.0 liters / minute.
- the gas suction pipe 61 is heated by the gas suction pipe heater 62 to prevent the gas from being adsorbed into the pipe.
- the gas suction pipe heater 62 was heated at 70 ° C. For example, since triacetone triperoxide is decomposed by heat, the heating temperature is set low.
- the gas suction part 58 and the particulate suction part 59 are arranged separately, but an intake port may be provided inside the particulate suction part 59 or vice versa.
- the gas suction pipe 61 is preferably as short as possible in order to prevent the gas from adsorbing inside.
- FIG. 13 is a schematic diagram showing an example of collecting particles from the lower part of the gate.
- the gate 70 incorporates an authentication unit 4 having an authentication surface 3, an air supply unit 5 and an air supply control unit 7.
- a grating 72 is provided on the floor through which the subject 71 passes.
- a lower intake part 73 is installed under the grating 72 and sucks fine particles adhering to the shoes and clothes of the subject 71. It is preferable that the size of the grating 72 and the lower intake portion 73 is such a length that the subject 71 proceeds while the subject 2 is authenticated by the authentication unit 4 and can be identified.
- the air supply unit 5 sends an air flow to the subject 71.
- the air flow may be continuous, intermittent, irregular, or sudden, as long as the attached fine particles can be efficiently peeled off.
- the position of the air supply part 4 should just be a position which can peel the microparticles
- the peeled fine particles are concentrated in the fine particle collecting unit 10 and collected in a fine particle collecting filter, and the sample vaporized by heating is introduced into the ion source unit 21 from the back side of the fine particle collecting filter and ionized.
- the ionized ions are subjected to mass analysis by the mass analysis unit 23, and the presence or absence of the detection target substance in the collected fine particles is detected.
- the particulate collection unit 10 the ion source unit 21, the mass analysis unit 23, and the like, those described in the above embodiments can be appropriately employed.
- airflow may be applied at the timing when the subject 71 passes by a human sensor or the like, and the fine particles attached to the shoes and clothes of the subject 71 may be peeled off.
- FIG. 14 shows an example of collecting particles from the lower part of the gate, and is a view seen from the front.
- the gate 74 is installed on the opposite side of the gate 70 and the subject 71.
- the fine particles adhering to the subject 71 may be peeled off by applying airflow from both the gate 70 and the opposite gate 74.
- the air supply unit 5 may be installed only in the gate 70 or only in the opposite gate 74.
- the authentication surface 3 is provided on the gate 70 on the right hand side of the subject 71, but may be installed on the opposite gate 74 on the left hand side.
- a plurality of gates may be arranged.
- FIG. 15 shows an example of collecting particles from the side of the gate, and is a schematic view seen from the front.
- the air supply unit 5 is installed in the gate 70, and the air intake unit 76 is installed in the opposite gate 74.
- the intake portion 76 is covered with a protective mesh 75.
- the particulate collection unit 10 is connected to the intake unit 76.
- an ion source unit, a mass analysis unit, and the like are not shown, they are built in the opposite gate 74.
- the gate in which the air supply unit 5 and the intake unit 76 are built may be reversed.
- the airflow generated from the air supply unit may be slit-shaped.
- a plurality of air supply units may be arranged vertically or horizontally.
- fine particles can be peeled only by one subject 71.
- the airflow should be laminar. Further, by making the airflow flow in one direction, there is an advantage that the space cleaning effect and the subject 71 can be specified. Further, the fine particles may be peeled from the whole body by flowing an air flow in a downward flow from the upper surface or the ceiling. Instead of using the authentication unit 4, airflow may be applied at the timing when the subject 71 passes by a human sensor or the like, and the fine particles attached to the shoes and clothes of the subject 71 may be peeled off.
- FIG. 16 is a schematic diagram showing an example in which fine particles are peeled off from an authentication target by applying an air flow from the back of the authentication surface.
- the authentication surface 3 is formed in a mesh shape, and a hole that does not affect the antenna of the authentication unit 4 is formed in the center of the authentication unit 4 or at an arbitrary place.
- air is supplied from the lower air supply unit 77 through this hole, and the gas and / or fine particles attached to the authentication target 2 are peeled off.
- the airflow from the air supply unit 5 is applied at the timing of separation.
- the fine particles are sucked into the intake section 6 by the airflow of the air supply section 5.
- the airflow of the air supply unit 5 may be constantly supplied, or may be operated when authenticated or in synchronization with the operation of the lower air supply unit 77. Further, instead of using the air supply unit 5, only the lower air supply unit 77 may be used to separate the fine particles from the authentication target 2 and to suck the suction unit 6.
- FIG. 17 is a diagram illustrating an example of an operation sequence of the lower air supply unit and the air supply unit.
- the gas attached to the authentication target 2 is injected through the hole from the lower air supply unit 77 with an injection pressure of 0.05 MPa and an injection time of 0.1 seconds. / Or fine particles are peeled off.
- the gas and / or fine particles injected from the air supply unit 5 with an injection pressure of 0.05 MPa and an injection time of 0.1 second and separated by the lower air supply unit 77 are taken into the intake unit. 6 to suck. This operation is repeated, for example, five times.
- authentication is started and repeated until the end.
- timing which starts injection is not illustrated in FIG. 17, you may start when external sensors, such as a sensor which detects that an authentication object, a person, a hand, a finger, etc. approached.
- FIG. 18 is a schematic diagram illustrating an example of an analyzer that includes an air supply unit for separating fine particles and an air supply unit for cleaning, and uses an intake unit for sucking particles and a particle concentration unit.
- the analysis apparatus 1 includes an authentication unit 4 including an authentication surface 3 for authenticating the authentication target 2 and includes an authentication acquisition unit.
- the authentication surface 3 may be arranged horizontally or may be inclined.
- the authentication surface 3 may be transparent or mesh-shaped, and may have a shape through which not only radio waves but also light and air current pass from the authentication unit 4.
- the authentication data when the authentication object 2 is authenticated is checked against an external or internal authentication database.
- An air supply unit 5 and an air intake unit 6 are arranged so that the authentication surface 3 is in between.
- a cleaning air supply unit 105a is disposed on the air supply unit 6 side.
- the air supply unit 5 From the air supply unit 5, when the authentication target 2 approaches the authentication surface 3 by sending an air flow along the authentication surface 3, the air supply hits the authentication target 2 and is attached to the authentication target 2.
- the sample gas is generated by the gas and / or fine particles, or the gas and / or fine particles of the detection target substance are peeled off.
- the wind generated from the air supply unit 5 for separating the gas and / or fine particles of the detection target substance may be continuous, intermittent, irregular, or sudden. Thereby, the gas and / or fine particles of the detection target substance peeled from the authentication target 2 are transferred to the intake section 6.
- This airflow is an airflow that prevents the turbulent flow from preventing the gas and fine particles from being detected without being inhaled. It is desirable to supply air in parallel to the authentication surface 3. That is, an airflow that does not hit the authentication surface 3 is desirable to prevent turbulent flow. Moreover, you may use for the air supply part 5 what built in the ion generator for adhesion and removal of dust.
- the cleaning air supply unit 105a is used to clean the gas and / or fine particles of the detection target substance that has been peeled off from the authentication target 2 and reattached to the authentication surface 3 by jetting an air flow onto the authentication surface 3. .
- the air supply unit 5 and the air supply unit 105a for cleaning are connected to the air supply unit 5 and the cleaning air supply unit 105a.
- the air supply control unit 7 controls the driving of the air supply unit 5 and the cleaning air supply unit 105a, and controls the flow rate or flow velocity, injection pressure, temperature, injection time, injection timing, and the like.
- the air supply unit 5 operates with an air supply unit start signal. Even if this air supply unit start signal is generated in synchronization with the authentication, an external sensor such as a sensor that detects that an authentication target, a person, a hand, or a finger is approaching, or a sensor that detects that a person has passed It may occur when reacting.
- FIG. 19 is a diagram illustrating an example of an operation sequence of the air supply unit for particle separation and the air supply unit for cleaning.
- the air supply unit 5 after receiving the air supply unit start signal, the air supply unit 5 alternately and continuously performs injection with an injection pressure of 0.05 MPa, an injection time of 0.1 seconds, and a pause of a pause time of 0.1 seconds. Repeat 5 times. Thereafter, the cleaning air feeding unit 105a sprayed with an ejection pressure of 0.05 MPa and an ejection time of 1 second.
- the jet from the cleaning air supply unit 105a may be intermittent operation similar to that of the air supply unit 5, or may be supplied continuously, irregularly, or suddenly.
- the cleaning air supply unit 105a a device incorporating an ion generator may be used in order to attach and remove dust.
- the ejection from the cleaning air supply unit 105a may be always performed after the air supply unit 5 for separating fine particles is operated. Or you may operate after the air supply part 5 operate
- the air supply section 5 and the cleaning air supply section 105a may be combined to be one unit. In this case, the angle for fine particle peeling and the cleaning angle are changed mechanically or electrically to cope with it.
- two nozzles having an opening / closing mechanism set at an angle for fine particle peeling and an angle for cleaning may be used in one unit. The fine particle peeling and cleaning may be performed simultaneously.
- a coarse mesh filter 8 is provided in the intake portion 6 to prevent large dust from entering and a finger from being put into the intake portion 6.
- a wire mesh (opening 0.5 mm, porosity 50%) was used as an example.
- the coarse mesh filter 8 can be replaced, and when it is clogged with dust, it can be cleaned and reused or replaced with a new one.
- the gas and / or fine particles of the detection target substance sucked from the intake portion 6 are introduced into the fine particle collecting portion 10 through the suction pipe 9.
- the suction pipe 9 may be made as short as possible or eliminated, and the particulate collection unit 10 and the suction unit 6 may be directly connected.
- the particulate collection unit 10 includes a conical particulate concentration unit 12, a large-capacity suction pump 13, a particulate collection filter unit 14, and a particulate collection control unit 15.
- the large-capacity suction pump 13 performs suction at a flow rate of 40 meters / minute, for example. Due to this suction, a cyclone phenomenon occurs inside the conical fine particle concentrating portion 12.
- fine particles having a particle size of 5 ⁇ m or more are collected by the fine particle collecting filter portion 14 provided in the small radius portion of the fine particle concentrating portion 12.
- the other airflow is discharged by the large-capacity suction pump 13.
- the large-capacity suction pump 13 can control the flow rate or flow rate by the particulate collection control unit 15.
- the large-capacity suction pump 13 may be operated constantly, or can be operated in synchronization with the operation of the air supply unit 5. In addition, control that is normally performed in a stopped state or with a small amount of suction may be performed.
- the output of the large-capacity suction pump 13 is operated at about 20% (the flow rate of about 5 meters / second at the inlet of the fine particle concentrating unit 12) during the pause, and synchronized with the operation of the air supply unit 5,
- By operating at about 80% (the flow rate of about 7-8 meters / second at the inlet of the fine particle concentrating unit 12), which is the output of the large-capacity suction pump 13 that can collect the most fine particles it is possible to collect fine particles more efficiently It becomes.
- the output of the large-capacity suction pump 13 at about 100% (flow rate of about 10 meters / second at the inlet of the fine particle concentrating unit 12).
- the filter 20 may become dirty and the frequency of replacement and cleaning may increase, such a situation can be prevented. Similarly, if it becomes dirty, the background noise increases, so that the detection sensitivity may be lowered. Since the flow velocity at the inlet of the fine particle concentrating portion 12 varies depending on the long diameter and length of the cone of the fine particle concentrating portion 12, an optimum shape is used.
- Explosive fine particles usually have a particle size of 5 ⁇ m or more and 100 ⁇ m or less, so it is preferable to collect fine particles of this particle size.
- the inner surfaces of the intake portion 6, the suction pipe 9, the conical fine particle concentrating portion 12 and the like may be made of Teflon or coated with Teflon. Fine particles of trimethylenetrinitroamine (RDX) and trinitrotoluene (TNT), which are the main components of plastic explosives, are negatively charged. Since Teflon is also negatively charged, the negatively charged explosive fine particles are repelled and difficult to adsorb.
- RDX trimethylenetrinitroamine
- TNT trinitrotoluene
- the particulate collection filter 14 is wound around a filter winding unit 78b and a filter feeding unit 78a.
- the filter winding unit 78b (or the filter feed unit 78a can also be controlled) is controlled by the particulate collection control unit 15.
- the particulate collection filter 14 is heated by the collection filter heating unit 18, but not only the particulates of the component to be detected but also the particulates of the contaminating components adhere and become dirty with time.
- the mass analyzer 23 measures the mass spectrum continuously and continuously in real time, and can detect this time change of dirt.
- the background threshold value (BG threshold value) is used as the stain threshold value. If this value is exceeded, the particulate collection filter 14 is wound up only once by the control of the particulate collection control unit 15 to clean the surface. To expose.
- the particulate collection filter 14 As the particulate collection filter 14, a ribbon-shaped object having a filtration accuracy of 50 ⁇ m, a width of 10 mm, and a thickness of 0.5 mm was used. In addition to the ribbon shape, a plate shape, a twisted rope shape, a disk shape, or a loop shape may be used. Even when the detection target substance is detected, the next measurement can be quickly performed by winding up the particulate collection filter 14 to bring out a clean surface.
- the fine particle collecting filter 14 may be made of stainless steel wire, metal fiber, heat resistant fiber (for example, Conex), glass fiber, or the like.
- a detector pipe 17 is connected to the surface on the back side of the particulate collection filter section 14 (opposite side of the particulate concentration section 12).
- the particulate adsorbed on the particulate collection filter unit 14 is heated by the collection filter heating unit 18.
- heating was performed at 230 ° C.
- the heated microparticles are vaporized, and the gasified sample is introduced into the ion source unit 21 by the suction pump 22 via the detector pipe 17.
- the suction pump 22 sucks at a flow rate of 0.5 liter / min.
- the detection pipe 17 is heated by a detection pipe heater 19 to prevent gas from being adsorbed inside the pipe.
- the detection pipe heater 19 was heated to 180 ° C.
- the detection pipe 17 and the detection pipe heater 19 may be as short as possible, or may be eliminated and the particulate collection filter unit 14 and the ion source unit 21 may be directly connected.
- the detection pipe 17 is provided with a fine mesh filter 20 to prevent the ion source part 21 from being contaminated with fine particles not gasified by the fine particle collecting filter part 14.
- a fine mesh filter 20 for example, a stainless steel wire filter or a sintered body filter having a filtration accuracy of 1 ⁇ m may be used.
- the fine mesh filter 20 can be cleaned and reused as needed, or replaced with a new one.
- the ion source unit 21 can be an atmospheric pressure chemical ionization source using negative corona discharge or positive corona discharge described in, for example, Japanese Patent Application Laid-Open No. 2000-28579.
- the ion generation method may be other methods such as irradiation with a radiation source, irradiation with electrons or light, laser light, Penning discharge, glow discharge, barrier discharge, electrospray, or the like.
- the ions generated from the sample by the ion source unit 21 are subjected to mass analysis by the mass analysis unit 23.
- the mass spectrometer 23 for example, a wire type linear ion trap mass spectrometer can be used.
- Mass spectrometry methods include linear ion trap mass spectrometer, quadrupole ion trap mass spectrometer, quadrupole filter mass spectrometer, triple quadrupole mass spectrometer, time-of-flight mass spectrometer, and magnetic field mass spectrometry. Other methods such as metering and ion mobility may be used.
- the signal obtained by the mass analyzer 23 is measured by the controller 24 as a mass spectrum.
- the peak of the mass number of the sample is extracted from this mass spectrum.
- the mass database unit 26 holds information including standard mass spectrometry data necessary for identifying a sample.
- the retained information includes the value of the mass-to-charge ratio (m / z) obtained by dividing the ion mass number m by the ion valence z and the relative intensity.
- the mass spectrum measured by the mass analysis unit 23 is sent to the determination unit 25 and subjected to data processing such as collation with the data read from the mass database unit 26 to specify the sample.
- Trinitrotoluene and trimethylenetrinitroamine which are representative materials for military explosive components, were measured with the analyzer of this example.
- FIG. 20 shows an example in which trinitrotoluene (TNT) and trimethylenetrinitroamine (RDX) are detected by changing the heating temperature of the collection filter heating unit.
- TNT trinitrotoluene
- RDX trimethylenetrinitroamine
- silica gel fine particles having a particle diameter of 20 to 30 ⁇ m containing trinitrotoluene and trimethylenetrinitroamine were used.
- Several micrograms of this sample was attached to the IC card to be authenticated.
- the molecular weight (M) of trimethylenetrinitroamine is 222.
- trimethylenetrinitroamine Since trimethylenetrinitroamine has a lower vapor pressure than trinitrotoluene, it re-adsorbs and desorbs in the piping and arrives at the ion source unit 21 and is detected with a delay.
- the heating temperature of the collection filter heating unit 18 was in the range of 180 ° C. to 300 ° C., detection of both trinitrotoluene and trimethylenetrinitroamine within 3 seconds could be confirmed.
- detection of dinitrotoluene, cyclotetramethylenetetranitramine, pentaerythritol tetrapentanitrate, hydrogen peroxide, etc. was confirmed by negative ion detection.
- detection of triacetone tripoxide, hexamethylenetripoxide diamine, etc. was confirmed by positive ion detection.
- FIG. 21 shows an example in which the separation recovery rate of trinitrotoluene (TNT) was evaluated by changing the inlet flow rate of the fine particle concentrating portion.
- TNT trinitrotoluene
- silica gel fine particles having a particle diameter of 20 to 30 ⁇ m and containing trinitrotoluene were used.
- Several micrograms of this sample was attached to the IC card to be authenticated. The IC card is touched on the authentication surface of the analyzer of the present embodiment for authentication, and the sample adhering to the IC card is peeled off, sucked by the suction unit 6 and concentrated by the fine particle concentration unit 12 and collected.
- the collection filter heating unit 18 was heated to 200 ° C.
- the detection pipe heater 19 the ion source unit 21, and the first pore electrode were heated to 180 ° C.
- the same amount as the amount attached to the IC card was taken as 100% when the signal was directly put into the particulate collection filter unit 14, and the ratio of the signal amount when collected by the particulate concentration unit 12 was taken as the separation recovery rate. .
- the separation recovery rate is high. In this range, a fine particle sample containing trinitrotoluene having a particle diameter of 20 to 30 ⁇ m is efficiently collected. It was confirmed that it could be recovered.
- FIG. 22 is an example in which the separation recovery rate of trinitrotoluene (TNT) was evaluated by changing the injection pressure of the air supply section.
- TNT trinitrotoluene
- the injection with an injection time of 0.1 second and the pause with a pause time of 0.1 second were alternately and continuously performed 5 times.
- a spray recovery of 0.05 to 0.1 MPa is advantageous because the peel recovery rate is high.
- FIG. 23 is an example in which the separation recovery rate of trinitrotoluene (TNT) was evaluated by changing the injection time of the air supply unit.
- TNT trinitrotoluene
- a pause with an injection pressure of 0.05 MPa and a pause time of 0.1 seconds was alternately and continuously performed 5 times.
- the spraying time is 0.1 to 0.2 seconds, which is advantageous because the peel recovery rate is high.
- FIG. 24 is an example in which the jet separation rate of trinitrotoluene (TNT) was evaluated by changing the number of jets of the air supply section. Injection with an injection pressure of 0.05 MPa and an injection time of 0.1 seconds was made 5 times at intervals of 5 seconds. Assuming that the fine particle sample is peeled 100% from the surface of the IC card by spraying the air supply section 5 times, the spray peeling rate in one spray was determined from the signal intensity. The spray peeling rate was about 70% for the first injection, about 20% for the second injection, and about 5% for the third to fifth times. Accordingly, although about 70% can be peeled by one injection, it is advantageous that more fine particle samples can be peeled from the IC card by increasing the number of continuous injections.
- TNT trinitrotoluene
- FIG. 25 is an example in which the separation recovery rate of trinitrotoluene (TNT) was evaluated by changing the pause time of the air supply unit. Injection with an injection pressure of 0.05 MPa and an injection time of 0.1 seconds was made 5 times. When the resting time of the air supply unit 5 is sprayed at intervals of 5 seconds, not all fine particle samples have been peeled off from the IC card surface by the first peeling, but the resting time should be 0.1 seconds or less. Thus, it was confirmed that all fine particle samples could be peeled off and the signal intensity was increased.
- TNT trinitrotoluene
- the fine particles attached to various positions can be obtained by spraying the air supply section 5 multiple times. This increases the probability that the sample will be exposed to wind, and is advantageous in that the peel recovery rate is increased.
- FIG. 26 is a schematic diagram showing an example in which the cleaning air supply section is installed on the side of the suction section for suctioning fine particles.
- An air supply unit 5 and an air intake unit 6 are arranged so that the authentication surface 3 is in between.
- a cleaning air supply unit 105 a is disposed on the side of the intake unit 6.
- the cleaning air supply unit 105a is used to clean the gas and / or fine particles of the detection target material that has been peeled off from the authentication target 2 and reattached to the authentication surface 3 by injecting an airflow onto the authentication surface 3.
- the cleaning air supply unit 105a By disposing the cleaning air supply unit 105a on the side of the intake unit 6, the gas and / or fine particles of the detection target substance reattached to the authentication surface 3 are prevented from entering the intake unit 6 during cleaning. It is possible to prevent contamination.
- the air supply unit 5 and the air supply unit 105a for cleaning are connected to the air supply unit 5 and the cleaning air supply unit 105a.
- the air supply control unit 7 controls driving of the air supply unit 5 and the cleaning air supply unit 105a to control the flow rate or flow velocity, injection pressure, temperature, injection time, injection timing, and the like.
- the air supply unit 5 operates with an air supply unit start signal. Even if this air supply unit start signal is generated in synchronization with the authentication, an external sensor such as a sensor that detects that an authentication target, a person, a hand, or a finger is approaching, or a sensor that detects that a person has passed It may occur when reacting.
- an injection pressure of 0.05 MPa, an injection of an injection time of 0.1 seconds, and a pause of a pause time of 0.1 seconds are alternately continuously performed. 5 times.
- the cleaning air feeding unit 105a sprayed with an ejection pressure of 0.05 MPa and an ejection time of 1 second.
- the jet from the cleaning air supply unit 105a may be intermittent operation similar to that of the air supply unit 5, or may be continuous, irregular, or sudden wind.
- the jet from the cleaning air supply unit 105a may be operated after the air supply unit 5 for separating fine particles is operated, or may be operated after the air supply unit 5 is operated a certain number of times, or for a certain period of time. It may be operated periodically such as at intervals. Further, when a detection target substance is detected, the detection target substance may be operated until no detection target substance is detected.
- FIG. 27 is a diagram showing an example of the air supply unit for separating fine particles, the air intake unit for sucking fine particles, and the air supply unit for cleaning as viewed from above.
- a plurality of air supply units for cleaning are installed on the side surface on the side of the intake unit for sucking fine particles.
- the air supply unit 5 for separating fine particles is installed in the air supply unit cover 110.
- the cleaning air supply parts 105 a and 105 b and the suction part 6 for sucking the fine particles are installed in the suction part cover 111.
- two cleaning air supply units are used, but three or more may be used. In the case of one, it is desirable that only the cleaning air supply unit 105a is used, and the cleaning jet is performed farther than the direction of human movement.
- there is an advantage that the height of the intake portion cover 111 can be reduced by installing the cleaning air supply portions 105 a and 105 b on the side surface of the intake portion 6.
- FIG. 28 is a schematic view showing an example provided with an air supply unit for removing fine particles, an air supply unit for cleaning, and an intake unit for sucking fine particles having a lid.
- the air intake lid 106 which is a lid for the air intake
- the air intake lid 106 is closed during cleaning to prevent contamination of the air intake 6, and the dust intake lid 106 is closed during detection non-operation. It can prevent dirt and garbage from entering.
- the intake section lid 106 may be mechanically or electrically opened and closed, and may be opened and closed forward and backward or opened and closed.
- the air intake control unit 7 controls opening and closing of the air intake unit lid 106.
- the cleaning air supply unit 105a may be disposed on the intake unit 6 side.
- FIG. 29 is a diagram illustrating an example of an operation sequence of the air supply unit for separating fine particles, the air intake unit lid, and the air supply unit for cleaning.
- the intake unit lid 106 is opened, and from the air supply unit 5, an injection with an injection pressure of 0.05 MPa, an injection time of 0.1 seconds, and a pause of 0.1 seconds with a pause time Are performed five times in succession.
- the intake unit cover 106 is closed after a certain time. For example, the intake cover 106 is closed after 5 seconds.
- the cleaning air feeding unit 105a sprayed with an ejection pressure of 0.05 MPa and an ejection time of 1 second.
- the ejection from the cleaning air supply unit 105a may be an intermittent operation similar to that of the air supply unit 5. Alternatively, it may be a continuous, irregular or sudden wind. The ejection from the cleaning air supply unit 105a may be always performed after the air supply unit 5 for separating fine particles is operated. Alternatively, the air supply unit 5 may be operated periodically after a certain number of operations or at regular intervals. Further, when a detection target substance is detected, the detection target substance may be operated until no detection target substance is detected.
- FIG. 30 is a diagram showing an example of a fine particle peeling air supply unit, a plurality of cleaning air supply units, and a fine particle suction intake unit having a lid as viewed from above.
- the air supply unit 5 for separating fine particles and the plurality of cleaning air supply units 105 a and 105 b are installed in the air supply unit cover 110.
- the suction part 6 for sucking fine particles having the suction part cover 106 as a cover for the suction part is installed in the suction part cover 111.
- two cleaning air supply units are used, but three or more may be used. In the case of one, it is desirable to use only the cleaning air supply part 105a and perform the cleaning jet farther than the direction of human movement.
- FIG. 31 shows an example in which an air supply unit for removing fine particles, an air supply unit for cleaning, and an intake unit for suctioning fine particles having a lid are provided, and a coarse mesh filter is installed between the cover for the intake unit and the intake unit.
- the coarse mesh filter 8 is arranged inside the air intake lid 106, and the intake air lid 106 is closed for non-detection to prevent clogging of the coarse mesh filter 8 due to dust and dirt from the surroundings. It becomes possible.
- a net for preventing pinching of hands, fingers, IC cards and the like may be provided in front of the air intake cover 106.
- the analyzer 1 controls the auxiliary air supply unit 78 that injects an airflow onto the inner surface of the suction pipe 9 toward the fine particle concentration unit 12 on the track of the suction pipe 9 and the auxiliary air supply unit 78.
- An auxiliary air supply control unit 79 is provided.
- the auxiliary air supply unit 78 of the present embodiment is disposed at a position where the airflow is jetted to a portion where the trajectory of the suction pipe 9 changes in the horizontal direction. Below, the effect obtained by providing the auxiliary air supply part 78 and the auxiliary air supply control part 79 in the analyzer 1 is demonstrated.
- the inventors detect the trinitrotoluene explosive from the authentication object 2 by the analyzer 1 of the first embodiment, and then blow an air flow to the intake portion 6 while generating a cyclone phenomenon inside the fine particle concentration unit 12.
- the presence or absence of the trinitrotoluene explosive collected in the particulate collection filter unit 14 was inspected. As a result of the inspection, it was confirmed that the trinitrotoluene explosive was collected in the particulate collection filter unit 14. From this result, it was found that trinitrotoluene explosive particles remain inside the suction pipe 9 from which the trinitrotoluene explosive was once collected.
- the explosive fine particles adhering to the inner wall of the suction pipe 9 may be peeled off and captured by the fine particle collecting filter unit 14. Conceivable. In this case, the explosive fine particles are not attached to the authentication target 2, but the determination unit 25 detects the explosive, which causes a false detection. Therefore, in the analyzer 1, it turned out that the self-cleaning function in the suction piping 9 is an indispensable function.
- the analyzer 1 of the present embodiment can automatically clean the suction pipe 9 without human intervention, and can further inspect the cleaning effect quantitatively.
- the self-cleaning by the analyzer 1 of this embodiment is performed according to the following procedure. This will be described with reference to FIG.
- the sample fine particles peeled off from the authentication target 2 are detected and sucked (S25), and the mass spectrum of the sample fine particles is measured (S26).
- the signal intensity of the mass spectrum of the sample particulate is compared with the determination threshold (S27).
- the determination unit 25 determines that the signal intensity of the mass spectrum of the sample fine particle has exceeded the determination threshold value
- the determination unit 25 displays it on the display unit 27 to notify the inspector.
- the analyzer 1 is in a state of waiting for an instruction to start the self-cleaning step 80.
- the execution instruction of the self-cleaning process 80 is selected by the inspector, the normal inspection process is stopped and a predetermined self-cleaning process 80 is started.
- the self-cleaning step 80 is performed according to the procedure shown in FIG.
- the large-capacity suction pump is driven to generate a cyclone phenomenon inside the fine particle concentration unit 12 (S28).
- an air flow is injected from the auxiliary air supply unit 78 into the suction pipe 9 (S29).
- the air flow to be injected has an injection time of 0.5 seconds and an injection pressure of 0.4 Mpa.
- the sample fine particles remaining in the suction pipe 9 and the fine particle collection unit 10 are peeled off by the air flow from the auxiliary air supply unit 78, and the mass spectrum is measured (S30).
- the unit 25 compares with the determination threshold value. As a result of the comparison, when the determination unit 25 determines that there is no explosive, the normal inspection process is resumed. When it is determined that there is explosive, the self-cleaning process 80 is started again.
- the position of the arrow shown in the figure indicates the timing at which the airflow is ejected from the auxiliary air supply unit 78.
- the reason why the air flow injection period from the auxiliary air supply unit 78 is not uniform is that the air injection is performed manually.
- a mass spectrum derived from trinitrotoluene is obtained from the sample fine particles by the mass analyzing unit 23.
- the self-cleaning step 80 is repeatedly performed until the mass spectrum signal intensity derived from trinitrotoluene is sufficiently smaller than the determination threshold in the mass analyzer 23.
- the self-cleaning step 80 when the self-cleaning step 80 was repeated seven times, it was confirmed that the signal derived from trinitrotoluene disappeared from the sample particulates collected in the particulate collection unit 10. Therefore, according to the present embodiment, it was shown that the self-cleaning can be completed in 7 seconds even if the air flow injection period from the auxiliary air supply unit 78 is 1 second.
- the suction pipe 9 is cleaned without contamination by humans, and the configuration of the intake unit 6 and the particulate collection unit 10 is provided. It can be performed automatically and in a short time without damaging the parts.
- the cleanliness of the suction pipe 9 after cleaning is determined by the determination unit 25, the effect of cleaning can be quantitatively confirmed. Therefore, erroneous detection may be performed even in the inspection after detecting the explosive component. No. Note that the self-cleaning effect need not be measured every self-cleaning. By measuring the effect of self-cleaning when a predetermined number of self-cleaning operations are completed, the time required for self-cleaning can be further shortened.
- the sample particulates separated from the authentication target 2 are efficiently collected by the fine particle collection filter unit 14. Can be transported to.
- FIG. 35 is a diagram showing an example of timing for injecting airflow from the air supply unit 5 and the auxiliary air supply unit 78 in time series in a normal inspection according to the detection processing procedure described above.
- the inventors have found from experimental results that in order to peel sample fine particles from the authentication object 2, it can also be realized by irradiating the authentication object 2 with the pulsed airflow a plurality of times.
- the operation of injecting the airflow from the air supply unit 5 and the auxiliary air supply unit 78 for 0.1 second and stopping for 0.1 second is repeated five times.
- the jet pressure of the air flow was 0.05 MPa.
- the explosive fine particles can be detected even from the authentication target 2 to which a small amount of explosive fine particles that cannot be detected by the analyzer 1 that does not include the auxiliary air supply unit 78 are attached.
- the analyzer 1 with high sensitivity and few false detections can be realized.
- the air flow is injected from the auxiliary air supply unit 78 after the injection of the air supply unit 5, but the air flow is simultaneously injected from the air supply unit 5 and the auxiliary air supply unit 78 as shown in FIG. Also good.
- the inspection is performed at the injection timing shown in FIG. Similar effects can be obtained.
- the jetting time of the airflow jetted from the auxiliary air feeding unit 78 is 0.1 seconds, but it may be jetted continuously.
- FIG. 37 is a diagram showing an example of timing for injecting airflow from the air supply unit 5 and the auxiliary air supply unit 78 in time series in a normal inspection according to the above-described detection processing procedure.
- a continuous air flow is injected from the auxiliary air supply unit 78 in synchronization with the air flow injected from the air supply unit 5.
- the airflow from the auxiliary air supply unit 78 is stopped, which is the same as the case where the inspection is performed at the injection timing shown in FIG. The effect of can be obtained.
- the airflow injection time from the auxiliary air supply unit 78 is 1 second, but the same effect can be obtained even if the airflow injection time from the auxiliary air supply unit 78 is 1 second or longer.
- the auxiliary air supply unit 78 again injects the airflow after the background during mass spectrum measurement becomes lower than the BG threshold. Control may be performed by the air control unit 79.
- the signal strength of the explosive component may be near the determination threshold for determining the presence or absence of the explosive component. In such a case, it is difficult to determine, which is one of the causes of erroneous detection.
- the air supply air is supplied from the auxiliary air supply unit 78 into the suction pipe 9 after the normal inspection in which the air flow is not injected from the auxiliary air supply unit.
- the sample fine particles peeled off from the same authentication object 2 remaining inside can be inspected twice. That is, when the signal intensity of the explosive component is obtained in the vicinity of the determination threshold value in both inspections, it is possible to reduce false detection by determining that there is an explosive component.
- the auxiliary air supply part 78 is provided only in the suction pipe 9, but a plurality of auxiliary air supply parts 78 for injecting airflow into the suction pipe 9 and the intake part 6 are arranged. In this case, the same effect as in this embodiment can be obtained.
- this invention is not limited to the above-mentioned Example, Various modifications are included.
- the above-described embodiments have been described in detail for easy understanding of the present invention, and are not necessarily limited to those having all the configurations described.
- a part of the configuration of one embodiment can be replaced with the configuration of another embodiment, and the configuration of another embodiment can be added to the configuration of one embodiment.
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Abstract
Description
以下、本発明の第一の実施の形態について説明する。図1は、本実施形態の分析装置の一例を示す概略図であり、駅などの自動改札機50に内蔵した実施例を示す。駅などの自動改札機以外にも施設等の出入り口に設置するセキュリティゲート、空港や船などの搭乗ゲートや手荷物検査場や預入荷物検査場のゲート、アミューズメント施設等の入退場チケットゲートなどに内蔵することもできる。
以下、本発明の第二の実施の形態について説明する。本実施の形態では、微粒子捕集部において複数の微粒子濃縮部を利用して微粒子を捕集する。この方法を用いることで、検出対象物質の微粒子の粒径をコントロールして捕集することが可能になる。
以下、本発明の第三の実施の形態について説明する。本実施の形態では、分析装置をゲート等に組込む方法の例を説明する。
以下、本発明の第四の実施の形態について説明する。本実施の形態では、認証面をクリーニングする方法の例を説明する。図18は、微粒子剥離用の送気部とクリーニング用の送気部を備え、微粒子吸引用吸気部及び微粒子濃縮部を用いた分析装置の一例を示す模式図である。分析装置1には、認証対象2を認証する認証面3を備えた認証部4があり、認証取得手段を備える。認証面3は水平に配置しても、傾斜させて配置してもよい。認証面3は透明又はメッシュ状でもよく、認証部4から、電波だけでなく光や気流が通る形状でもよい。認証対象2を認証した時の認証データは、外部あるいは内部にある認証データベースと照合し判定を行う。認証面3が間にくるように、送気部5と吸気部6が配置されている。送気部6の側にはクリーニング用送気部105aが配置される。
以下、本発明の第五の実施の形態について説明する。本実施の形態では、クリーニング用の送気部の配置方法の例を説明する。図26は、クリーニング用の送気部が、微粒子吸引用の吸気部側に設置される一例を示す模式図である。認証面3が間にくるように、送気部5と吸気部6が配置されている。吸気部6の側にはクリーニング用送気部105aが配置される。クリーニング用送気部105aは、認証面3に対して気流を噴射させることで、認証対象2から剥離され、認証面3に再付着した検出対象物質のガス及び/又は微粒子をクリーニングするのに使用する。クリーニング用送気部105aを吸気部6側に配置することで、認証面3に再付着した検出対象物質のガス及び/又は微粒子がクリーニング時に吸気部6内に入らないようにし、吸気部6が汚染することを防ぐことができる。
以下、本発明の第六の実施の形態について図32を用いて説明する。
2 認証対象
3 認証面
4 認証部
5 送気部
6 吸気部
7 送気制御部
8 粗メッシュ状フィルタ
9 吸引配管
10 微粒子捕集部
11 配管ヒータ
12 微粒子濃縮部
13 大容量吸引ポンプ
14 微粒子捕集フィルタ部
15 微粒子捕集制御部
16 吸着防止器
17 検出器配管
18 捕集フィルタ加熱部
19 検出配管ヒータ
20 細メッシュ状フィルタ
21 イオン源部
22 吸引ポンプ
23 質量分析部
24 制御部
25 判定部
26 質量データベース部
27 表示部
28 針電極
29 引出電極
30a 第1細孔電極
30b 第2細孔電極
30c 第3細孔電極
31a 第1差動排気部
31b 第2差動排気部
31c 高真空部
32a 真空ポンプ
32b 真空ポンプ
33 イオンガイド
34 イオントラップ部
35a 入口端電極
35b 出口端電極
36 四重極ロッド電極
37 励起電極
38a トラップワイヤー電極
38b 引き出しワイヤー電極
39 トラップ領域
40 検出器
41 バッファーガス供給源
50 自動改札機
51 大回転微粒子濃縮部
52 小回転微粒子濃縮部
53 大回転微粒子濃縮部
54a 第1小回転微粒子濃縮部
54b 第2小回転微粒子濃縮部
55 微粒子濃縮吸気部
56 小回転微粒子濃縮部
57 粗メッシュ状フィルタ
58 ガス吸引用吸気部
59 微粒子吸引用吸気部
60 細メッシュ状フィルタ
61 ガス吸引用配管
62 ガス吸引配管ヒータ
70 ゲート
71 被検者
72 グレーティング
73 下部吸気部
74 反対側ゲート
75 メッシュ
76 側面吸気部
77 下部送気部
78 補助送気部
79 補助送気制御部
80 自己クリーニング工程
105a クリーニング用送気部
105b クリーニング用送気部
106 吸気部蓋
110 送気部カバー
111 吸気部カバー
Claims (33)
- 対象に付着した試料を剥離させる送気部と、
前記対象から剥離した試料を吸引する吸気部と、
前記吸引した試料を濃縮して捕集する微粒子捕集部と、
前記微粒子捕集部から試料を導入してイオン化するイオン源部と、
前記イオン源部で生成されたイオンを質量分析する質量分析部と、
前記イオン源部と前記質量分析部を制御する制御部と、
検出対象物質に由来する質量スペクトルデータを保持するデータベース部と、
前記質量分析部による試料の質量分析結果と前記データベース部に保持された質量スペクトルデータとを照合して前記検出対象物質の有無を判定する判定部と、
を備えることを特徴とする分析装置。 - 請求項1に記載の分析装置において、前記微粒子捕集部に円錐状の微粒子濃縮部を備えることを特徴とする分析装置。
- 請求項1に記載の分析装置において、前記微粒子捕集部に回転半径が大きい円錐状の第1の微粒子濃縮部と、回転半径が前記第1の微粒子濃縮部より小さい第2の微粒子濃縮部とを備え、前記第2の微粒子濃縮部は前記第1の微粒子濃縮部の下流側に直列に接続されていることを特徴とする分析装置。
- 請求項3に記載の分析装置において、前記第2の微粒子濃縮部を複数備えることを特徴とする分析装置。
- 請求項1に記載の分析装置において、前記吸気部に回転半径が大きい円錐状の第1の微粒子濃縮部と、回転半径が前記第1の微粒子濃縮部より小さい第2の微粒子濃縮部とを備え、前記第2の微粒子濃縮部は前記第1の微粒子濃縮部の下流側に直列に接続されていることを特徴とする分析装置。
- 請求項2~5のいずれか1項に記載の分析装置において、前記微粒子濃縮部の小半径部に設けられた微粒子捕集フィルタと、前記微粒子捕集フィルタを加熱する加熱部と、前記微粒子捕集フィルタの裏面を吸引する吸引部とを備え、前記微粒子捕集フィルタの表面に捕集された試料を前記微粒子捕集フィルタの裏面から連続的に吸引して前記イオン源部に導入することを特徴とする分析装置。
- 請求項1~6のいずれか1項に記載の分析装置において、前記データベース部はバックグラウンド閾値を保持し、前記質量分析部によって検出された前記微粒子捕集フィルタのバックグラウンドが前記データベース部に保持されたバックグラウンド閾値を超えたときに前記微粒子捕集フィルタを移動し、清浄面を露出させることを特徴とする分析装置。
- 認証対象を近接させる面を備えた認証部と、
前記認証部に沿って気流を送り前記認証対象に付着した試料を剥離させる送気部と、
前記認証対象から剥離した試料を吸引する吸気部と、
前記吸引した試料を濃縮して捕集する微粒子捕集部と、
前記微粒子捕集部から試料を導入してイオン化するイオン源部と、
前記イオン源部で生成されたイオンを質量分析する質量分析部と、
前記イオン源部と前記質量分析部を制御する制御部と、
検出対象物質に由来する質量スペクトルデータを保持するデータベース部と、
前記質量分析部による試料の質量分析結果と前記データベース部に保持された質量スペクトルデータとを照合して前記検出対象物質の有無を判定する判定部と、
を備えることを特徴とする分析装置。 - 請求項8に記載の分析装置において、前記微粒子捕集部に円錐状の微粒子濃縮部を備えることを特徴とする分析装置。
- 請求項8に記載の分析装置において、前記微粒子捕集部に回転半径が大きい円錐状の第1の微粒子濃縮部と、回転半径が前記第1の微粒子濃縮部より小さい第2の微粒子濃縮部とを備え、前記第2の微粒子濃縮部は前記第1の微粒子濃縮部の下流側に直列に接続されていることを特徴とする分析装置。
- 請求項10に記載の分析装置において、前記第2の微粒子濃縮部を複数備えることを特徴とする分析装置。
- 請求項8に記載の分析装置において、前記吸気部に回転半径が大きい円錐状の第1の微粒子濃縮部と、回転半径が前記第1の微粒子濃縮部より小さい第2の微粒子濃縮部とを備え、前記第2の微粒子濃縮部は前記第1の微粒子濃縮部の下流側に直列に接続されていることを特徴とする分析装置。
- 請求項9~12のいずれか1項に記載の分析装置において、前記微粒子濃縮部の小半径部に設けられた微粒子捕集フィルタと、前記微粒子捕集フィルタを加熱する加熱部と、前記微粒子捕集フィルタの裏面を吸引する吸引部とを備え、前記微粒子捕集フィルタの表面に捕集された試料を前記微粒子捕集フィルタの裏面から連続的に吸引して前記イオン源部に導入することを特徴とする分析装置。
- 請求項8~13のいずれか1項に記載の分析装置において、前記データベース部はバックグラウンド閾値を保持し、前記質量分析部によって検出された前記微粒子捕集フィルタのバックグラウンドが前記データベース部に保持されたバックグラウンド閾値を超えたときに前記微粒子捕集フィルタを移動し、清浄面を露出させることを特徴とする分析装置。
- 請求項8~14のいずれか1項に記載の分析装置において、前記吸気部に、ガス吸引用吸気部と前記ガス吸引用吸気部を前記イオン源部に接続させるガス吸引用配管、及び微粒子用吸気部と前記微粒子吸気部を前記微粒子捕集部に接続させる吸引配管を備えることを特徴とする分析装置。
- 請求項8~15のいずれか1項に記載の分析装置において、前記認証部は孔を有し、当該孔から前記認証対象に気流を送気する第2の送気部を備えることを特徴とする分析装置。
- 請求項8~16のいずれか1項に記載の分析装置において、前記微粒子捕集部が捕集する微粒子は粒径が5~100μmであることを特徴とする分析装置。
- 被検者を通過させるゲートと、
前記ゲートへの被検者の近接を検出する認識部と、
前記ゲートに設けられ、前記ゲートを通過する被検者に気流を送って前記被検者に付着した試料を剥離させる送気部と、
前記ゲートの床面あるいは側面に設けられ、前記送気部による送気によって剥離した試料を吸引する吸気部と、
前記吸引された試料を濃縮して捕集する微粒子捕集部と、
前記微粒子捕集部から試料を導入してイオン化するイオン源部と、
前記イオン源部で生成されたイオンを質量分析する質量分析部と、
前記イオン源部と前記質量分析部を制御する制御部と、
検出対象物質に由来する質量スペクトルデータを保持するデータベース部と、
前記質量分析部による試料の質量分析結果と前記データベース部に保持された質量スペクトルデータとを照合して前記検出対象物質の有無を判定する判定部と、
を備えることを特徴とする分析装置。 - 請求項18に記載の分析装置において、前記微粒子捕集部に設けられた微粒子捕集フィルタと、前記微粒子捕集フィルタを加熱する加熱部と、前記微粒子捕集フィルタの裏面を吸引する吸引部とを備え、前記微粒子捕集フィルタの表面に捕集された試料を前記微粒子捕集フィルタの裏面から連続的に吸引して前記イオン源部に導入することを特徴とする分析装置。
- 請求項18に記載の分析装置において、前記ゲートは第1のゲートと前記第1のゲートと対向する一に設置された第2のゲートからなり、前記送気部は前記第1のゲートに内蔵され、前記吸気部は前記第2のゲートに内蔵され、前記送気部から前記吸気部に向かって層流を形成していることを特徴とする分析装置。
- 近接した認証対象を認証する工程と、
前記認証対象に付着した試料を剥離させる工程と、
剥離した試料を吸引する工程と、
前記吸引された試料を濃縮して捕集し、連続的に試料をイオン化する工程と、
前記イオン化されたイオンを質量分析する工程と、
前記質量分析の結果得られた質量スペクトルとデータベースに保持された検出対象物質に由来する質量スペクトルデータとを照合する工程と、
前記照合結果に基づいて前記検出対象物質の成分物質の存在の有無を判定する工程と、
を有することを特徴とする分析方法。 - 請求項21に記載の分析方法において、
前記吸引された試料をサイクロンの原理によって濃縮して微粒子捕集フィルタの表面に捕集し、前記微粒子捕集フィルタに捕集された試料を加熱して気化し、気化した試料を前記前記微粒子捕集フィルタの裏面から吸引してイオン化することを特徴とする分析方法。 - 請求項1又は8に記載の分析装置において、前記認証部に対して気流を噴射し前記認証部に付着した試料を剥離させるクリーニング用送気部を備えることを特徴とする分析装置。
- 請求項23に記載の分析装置において、前記クリーニング用送気部は前記送気部側に設置されていることを特徴とする分析装置。
- 請求項23に記載の分析装置において、前記クリーニング用送気部は前記吸気部側に設置されていることを特徴とする分析装置。
- 請求項1~20、23~25のいずれか1項に記載の分析装置において、前記吸気部に蓋を備えることを特徴とする分析装置。
- 請求項6、13、19のいずれか1項に記載の分析装置において、前記加熱部の温度が180℃から300℃であることを特徴とする分析装置。
- 請求項1~17、23~25のいずれか1項に記載の分析装置において、前記送気部の噴射圧力が0.05~0.1MPa、噴射時間が0.1~0.2秒であることを特徴とする分析装置。
- 請求項1~17、23~25のいずれか1項に記載の分析装置において、前記送気部の噴射を0.1秒間隔で複数回噴射させることを特徴とする分析装置。
- 請求項1~20のいずれか1項に記載の分析装置において、
前記吸気部と前記微粒子濃縮部を結合する吸引配管を有し、
前記吸引配管の内部に、噴射時間が1秒以下のパルス状の気流を、前記吸引配管の軌道に沿って前記微粒子濃縮部に向かって送る補助送気部と、
前記補助送気部を制御する補助送気制御部とを備えたことを特徴とする分析装置。 - 請求項1~20のいずれか1項に記載の分析装置において、
前記吸気部と前記微粒子濃縮部を結合する吸引配管を有し、
前記吸引配管の内部に、噴射時間が1秒以上の連続状の気流を、前記吸引配管の軌道に沿って前記微粒子濃縮部に向かって送る補助送気部と、
前記補助送気部を制御する補助送気制御部を備えたことを特徴とする分析装置。 - 請求項30又は31に記載の分析装置において、
前記補助送気制御部は、前記送気部から噴射される気流の噴射タイミングに連動して、前記補助送気部から気流を送ることを特徴とする分析装置。 - 請求項30~32のいずれか1項に記載の分析装置において
前記補助送気部は、前記吸引配管の軌道が水平方向に変わる部位に前記気流を送ることを特徴とする分析装置。
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JP5981578B2 (ja) | 2016-08-31 |
US20140151543A1 (en) | 2014-06-05 |
CN105223043A (zh) | 2016-01-06 |
US9040905B2 (en) | 2015-05-26 |
CN105223043B (zh) | 2017-12-19 |
CN103221812A (zh) | 2013-07-24 |
JP5690840B2 (ja) | 2015-03-25 |
CN103221812B (zh) | 2015-11-25 |
JP2015135329A (ja) | 2015-07-27 |
US9214324B2 (en) | 2015-12-15 |
US20150235831A1 (en) | 2015-08-20 |
JPWO2012063796A1 (ja) | 2014-05-12 |
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