WO2006028402A1 - Tete d'analyse destinee a la detection dans le gaz de substances sous forme de micro-impuretes - Google Patents

Tete d'analyse destinee a la detection dans le gaz de substances sous forme de micro-impuretes Download PDF

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Publication number
WO2006028402A1
WO2006028402A1 PCT/RU2005/000290 RU2005000290W WO2006028402A1 WO 2006028402 A1 WO2006028402 A1 WO 2006028402A1 RU 2005000290 W RU2005000290 W RU 2005000290W WO 2006028402 A1 WO2006028402 A1 WO 2006028402A1
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WIPO (PCT)
Prior art keywords
drift
gap
channel
ion
additional
Prior art date
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PCT/RU2005/000290
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English (en)
Russian (ru)
Inventor
Yuri Petrovich Gorbachev
Vladimir Vladimirovich Ionov
Yuri Nikolaevich Kolomiec
Original Assignee
Yuri Petrovich Gorbachev
Vladimir Vladimirovich Ionov
Yuri Nikolaevich Kolomiec
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Application filed by Yuri Petrovich Gorbachev, Vladimir Vladimirovich Ionov, Yuri Nikolaevich Kolomiec filed Critical Yuri Petrovich Gorbachev
Publication of WO2006028402A1 publication Critical patent/WO2006028402A1/fr

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Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/64Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber
    • G01N27/66Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber and measuring current or voltage

Definitions

  • Analytical head for detecting trace substances in gases
  • the invention relates to the field of gas analysis and can be used to determine microimpurities of substances in gases when solving environmental monitoring problems, detecting accidental emissions of toxic substances at work, controlling the atmosphere of a work area in enterprises associated with harmful working conditions, and searching for hidden explosive and narcotic substances during operational activities by special services or customs inspection at control passages.
  • the invention can also be used in gas chromatography as a sensitive detector with controlled selectivity.
  • a device based on ion mobility spectrometry [see TX. Whoptop, R.V. Narrgptop. Rarid multivariate Georgiaurve resolutiop arrlied to idptifivictiop schreibf exposiv réelles bu iop mobilitu sotrotometra.
  • Apalutisa Shimisa Assa 434 (2001) 269-282,] consists of a sequentially placed sample inlet chamber, an ionization chamber with an ionization source introduced into it (radioactive, corona discharge, ultraviolet radiation, etc.), a drift tube containing a series of electrodes for creating a longitudinal electric field, and a collector electrode.
  • the device operates as follows.
  • the ion mixture is separated into individual components during the drift in the stream of purified air and is recorded by the collector.
  • the SIP spectrum is the dependence of the ion current on the drift time t d . Each type of ion is recorded as an ion peak.
  • the value of t d is inversely proportional to the coefficient of mobility of the ion Ko, which in turn is determined by its charge, is
  • SPIP devices which are based on the dependence of the increment of the ion mobility coefficient on the electric field strength, and are devoid of the main disadvantages of SIP.
  • SPIP uses the fact that in strong electric fields (E), the ion mobility is not constant, and the drift velocity (V) is determined by the expression [see I.A. Buryakov, Yu.N. Kolomiets, V.B. Luppu. Journal of Analytical Chemistry, 2001, Volume 56, N ° 4, p. 381- 385.]:
  • V K o ⁇ (l + ⁇ (E)) ⁇ E, where Ko is the ion mobility coefficient in a weak field (EVN ⁇ 1x10 " V-cm, N is the gas density), ⁇ (E) is the field-dependent increment of the coefficient mobility.
  • the SPIP consists of a sequentially placed sample input chamber, an ionization chamber with an ionization source (radioactive, corona discharge, etc.) introduced into it, an ion separation device made in the form of an extended drift gap between two electrodes, and an ion collection system, which includes a collector electrode connected
  • the electrodes of the drift gap are fed the sum of a constant (Ui) and periodic asymmetric in polarity (U 2 (t)) electrical voltage. After ionization of impurities, the mixture of ions is fed into the drift gap by a continuous stream. The process of separation of ions into components occurs across the gas flow under the action of a periodic strong asymmetric in polarity strong electric field E 2 (t). Ions, rapidly oscillating, drift with an average velocity V, characteristic of each component and proportional to ⁇ . This drift is compensated by the constant electric field Ei created by the voltage Ui.
  • a device based on SPIP consisting of a housing having an input for connecting to the external environment and an outlet, an ion separation device located inside the housing and made in the form of a drift gap formed by electrodes located opposite each other connected to sources of constant compensating and variable asymmetric voltages, an ionization source located near the drift gap and connected to the input for ionization of the sample and the ion collection system located behind the drift electrodes romezhutka.
  • the device operates as follows. The analyzed mixture of impurities is sucked through the inlet using a pump
  • This device does not meet the requirements of the task due to a number of serious drawbacks.
  • the device has low sensitivity due to the large loss of ions that occur when they exit the drift gap. This is primarily due to the fact that ions are removed by gas flow through an annular gap or holes in one of the drift gap electrodes in the direction opposite to their drift under the action of a separating periodic asymmetric voltage. As a result, a stagnant zone is created at the outlet openings, which leads to an increase in the concentration of ions and space charge, which enhances their losses due to spurious processes of diffusion and drift to the walls of the drift gap.
  • the organization of the exit of ions through the wall of one of the electrodes of the drift gap leads to the inevitable emergence of the so-called “dead” non-blown zones with a near-zero transport flow. In such zones, the diffusion losses of the analyzed ions increase many times.
  • the device does not meet the requirements of portability due to problems arising in the organization of proper isolation between the drift gap and the ion collection system. This is due to the fact that the collecting electrode of the ion collection system is located directly at the exit of the drift gap and is connected to the highly sensitive input of the electrometric amplifier of the recording circuit. The presence in the outlet of the drift gap of a high-voltage periodic voltage (amplitude 2 - 5 kB and frequency 140 - 220 kHz) creates a significant
  • Replacement sheet a decaying signal, increasing the noise background of the amplifier by several orders of magnitude. To reduce it, it is necessary to significantly reduce the width of the exit slit and the diameter of the outlet openings, which leads to a significant increase in the gas-dynamic resistance of the entire analytical channel, and requires the use of more powerful pumps to maintain the proper transport flow in the drift gap. As a result of this, the weight and size characteristics of the entire product become unacceptably large for a portable device.
  • an analytical head for the detection of vapors of explosives [see WO 99/02981, MKI: G01N27 / 62, 1999], operating on the basis of SPIP and including a flow channel containing a sequentially placed ionization chamber, an ion separation device made in the form of a drift gap formed by coaxially located central and external electrodes connected to sources of constant compensating and variable asymmetric voltages and an ion collection system made in the form of a ring electrode mounted at the output of the drift gap.
  • the ion is released by the transport stream not through the electrode wall, but along the axis of the drift gap, in the direction perpendicular to the ion drift under the influence of an asymmetric alternating voltage.
  • the causes leading to the formation of stagnant and “dead” not blown zones in the ion exit region and, consequently, related losses are eliminated.
  • the main disadvantage of this device is the low sensitivity caused by the lack of effective isolation between the drift gap and the ion collection system.
  • An object of the present invention is to increase the detection sensitivity of trace substances in a gas.
  • the specified task in the analytical head for detecting microimpurities of substances in gases including a flow channel containing sequentially located ionization chamber, consisting of an inlet pipe through which the analyzed gas and an ionization source introduced into it, an ion separation device for mobility, made in the form of a drift gap formed by coaxially located central and external electrodes connected to sources of constant compensating and variable asymmetric voltages, and the ion collection system, it is decided that between the drift gap and the ion collection system coaxially with the drift gap there is an additional flow channel made of an electrically conductive material and connected to an external electrode, while the input of the additional channel is connected to the output of the drift gap, the output of the additional channel is connected to the input of the ion collection system, and the length of the additional channel is selected from the condition of eliminating the influence of a penetrating variable asymmetric drift voltage th gap on the ion collection system.
  • the specified execution of the analytical head allows you to eliminate the influence of high-voltage alternating voltage of the drift gap on the ion collection system and thereby significantly increase its sensitivity.
  • Fig. 1 shows an analytical head with a conical additional flow channel.
  • Figure 2 presents the analytical head with a cylindrical additional flow channel.
  • the analytical head includes: 1 - inlet pipe, 2 - ionization source ( ⁇ source 63 Ni), 3 - drift gap formed between the central electrode 4 and the external electrode 5, 6 and 7 - sources of respectively constant compensating and variable asymmetric voltages, 8 - additional flow channel, 9 - ion collection system.
  • the analytical head works as follows.
  • the analyzed gas with the help of a pump (not shown in the figure) enters through the inlet pipe 1 into the ionization chamber 2, where the impurities contained in the gas are ionized using a ⁇ -source.
  • the impurity ions are carried along with the analyzed gas into the drift gap 3, during movement along which the process of separation of ions into components occurs due to their drift across the gas flow under the action of a superposition of constant compensating (V 1 ) and periodic high-voltage (V 2 ( t)) stresses.
  • V 1 constant compensating
  • V 2 ( t) periodic high-voltage
  • Replacement sheet the flow channel 8, passing through which they enter the ion collection system 9, where they are captured by the collector electrode using the electric field acting in it.
  • the presence of an extended additional flow channel from the conducting material between the drift gap and the working area of the ion collection system carries out their spatial separation, providing reliable shielding of the highly sensitive collector from the action of an alternating high-voltage voltage.
  • the sufficiency of the length of the additional channel is determined experimentally from the condition that there is no change in the level of the noise signal of the electrometric amplifier after switching on a high-voltage alternating voltage-asymmetric separation voltage of the drift gap.
  • the alternating electric field acting at the output of the drift gap almost completely attenuates along the length of the additional channel, without appreciably affecting the ion collection system and, accordingly, without reducing the sensitivity of the electrometric amplifier.
  • the smooth gas-dynamic articulation of the additional channel with the drift gap and the ion collection system completely eliminate the occurrence of stagnant and “dead” zones, as well as disturbing turbulences, thereby minimizing the parasitic processes of the diffusion of recorded ions on the channel walls and their loss.
  • the cylindrical geometry of the drift gap of the analytical head creates a focusing effect, consisting in the localization of ions mainly near the average radius of the channel of the drift gap.
  • the additional channel By changing the shape of the additional flow channel, you can change the characteristics of the analytical head, achieving the desired properties of the device.
  • the additional channel should be in the form of a cylindrical gap. In this case, there is a decrease in the capacity of the ion collection system and the entire analytical head, which allows, on the one hand, to increase the speed of the electrometric signal recording circuit, and on the other hand, to reduce the total consumption of the device.
  • a laboratory model of the device was made on the basis of an analytical head with parameters: inlet pipe 12 mm long and 9.4 mm in diameter, drift gap 40.8 mm long, central electrode diameter 5 mm, external electrode diameter 9.4 mm.
  • a tritium source in the form of a ring of foil 2 mm wide served as an ionizer.
  • An alternating voltage asymmetric in polarity with an amplitude of 4.5 kB and a frequency of 170 kHz was applied to the central electrode of the drift gap.
  • the flow of the analyzed gas was ZOOml / min, the weight of the entire device was 1.8 kg, consumption - 15W.
  • THT 2,4,6-trinitrotolol vapor
  • the survey was carried out without violating the integrity of the envelope envelope.
  • THT pairs were detected after 2.5 months of holding the envelope at a temperature of 20 0 C.
  • Using the same head with both a cylindrical and conical additional channels made it possible to detect THT pairs within a day after the TNT was inserted into the envelope.
  • the time of recording the THT signal at the head with a conical additional channel was 1 - Zsec., Then the use of the cylindrical shape of the additional channel made it possible to reduce it to 0.5 - 0.7 sec.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Toxicology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

L'invention appartient au domaine de l'analyse de gaz et peut s'utiliser pour déterminer dans le gaz des substances sous forme de micro-impuretés, y compris les substances toxiques, explosives ou narcotiques. Selon l'invention, la tête d'analyse comprend un canal d'écoulement destiné à l'amenée de gaz analysé, constitué d'une chambre d'ionisation avec une source d'ionisation, d'un dispositif de répartition d'ions en fonction de leur mobilité, qui se présente comme un intervalle de dérive, et d'un système de collecte d'ions, le tout disposé en série. Les électrodes sont reliées à une source de courant continu de compensation et à une source de courant alternatif asymétrique. La tête comprend également un canal d'écoulement supplémentaire, disposé entre l'intervalle de dérive et le système de collecte d'ions coaxialement avec l'intervalle de dérive. Le canal supplémentaire est fait d'un matériau conducteur et est relié avec une électrode externe. La longueur du canal supplémentaire est choisie de manière à ne pas permettre au courant alternatif asymétrique de l'intervalle de dérive d'agir sur le système de collecte d'ions.
PCT/RU2005/000290 2004-09-01 2005-05-30 Tete d'analyse destinee a la detection dans le gaz de substances sous forme de micro-impuretes WO2006028402A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
RU2004126269/28A RU2265832C1 (ru) 2004-09-01 2004-09-01 Аналитическая головка для обнаружения микропримесей веществ в газах
RU2004126269 2004-09-01

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WO2006028402A1 true WO2006028402A1 (fr) 2006-03-16

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105527335A (zh) * 2016-02-02 2016-04-27 中国科学院电子学研究所 光离子化检测器

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008018811A1 (fr) * 2006-08-08 2008-02-14 Yuri Petrovich Gorbachev Tête analytique servant à détecter des micro-impuretés de substances dans des gaz
RU2444007C1 (ru) * 2010-11-29 2012-02-27 Федеральное государственное унитарное предприятие "Научно-исследовательский технологический институт имени А.П. Александрова" Устройство для одновременного разделения положительных и отрицательных ионов
RU2460067C1 (ru) * 2011-04-20 2012-08-27 Учреждение Российской академии наук Институт металлургии и материаловедения им. А.А. Байкова РАН Способ обнаружения взрывчатых веществ
CA2885713C (fr) 2012-09-24 2021-01-19 Smiths Detection - Watford Limited Generateur de vapeur a la demande
CN104678055B (zh) * 2013-11-28 2016-06-29 旭月(北京)科技有限公司 一种通过生物体离子分子流速判别气体安全性的方法

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1412447A1 (ru) * 1986-11-03 1998-06-20 И.А. Буряков Дрейф-спектрометр для обнаружения микропримесей веществ в газах
WO1999002981A1 (fr) * 1997-07-07 1999-01-21 Aktsionernoe Obschestvo Otkrytogo Tipa 'institut Prikladnoi Fiziki' Tete d'analyse permettant de deceler la presence de vapeurs de substances explosives

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU1412447A1 (ru) * 1986-11-03 1998-06-20 И.А. Буряков Дрейф-спектрометр для обнаружения микропримесей веществ в газах
WO1999002981A1 (fr) * 1997-07-07 1999-01-21 Aktsionernoe Obschestvo Otkrytogo Tipa 'institut Prikladnoi Fiziki' Tete d'analyse permettant de deceler la presence de vapeurs de substances explosives

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105527335A (zh) * 2016-02-02 2016-04-27 中国科学院电子学研究所 光离子化检测器

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