WO2012158052A1 - Ion mobility spectrometer chamber - Google Patents

Ion mobility spectrometer chamber Download PDF

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Publication number
WO2012158052A1
WO2012158052A1 PCT/PL2012/000033 PL2012000033W WO2012158052A1 WO 2012158052 A1 WO2012158052 A1 WO 2012158052A1 PL 2012000033 W PL2012000033 W PL 2012000033W WO 2012158052 A1 WO2012158052 A1 WO 2012158052A1
Authority
WO
WIPO (PCT)
Prior art keywords
electrodes
chamber
ceramic plates
gas
ionizer
Prior art date
Application number
PCT/PL2012/000033
Other languages
French (fr)
Inventor
Małgorzata JAKUBOWSKA
Wiestaw GALLEWICZ
Michał CEREMUGA
Mirosław MAZIEJUK
Original Assignee
Wojskowy Instytut Chemii I Radiometrii
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.)
Filing date
Publication date
Application filed by Wojskowy Instytut Chemii I Radiometrii filed Critical Wojskowy Instytut Chemii I Radiometrii
Priority to DE112012002128.2T priority Critical patent/DE112012002128T5/en
Priority to EP12741397.9A priority patent/EP2710362B1/en
Priority to CN201280023269.0A priority patent/CN103534589A/en
Priority to GB1319844.5A priority patent/GB2504884A/en
Priority to US14/117,627 priority patent/US9354201B2/en
Publication of WO2012158052A1 publication Critical patent/WO2012158052A1/en
Priority to FI20135985A priority patent/FI20135985L/en

Links

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
    • G01N27/622Ion mobility spectrometry
    • G01N27/624Differential mobility spectrometry [DMS]; Field asymmetric-waveform ion mobility spectrometry [FAIMS]

Definitions

  • This invention relates to a FAIMS (Field Asymmetric Ion Mobility Spectrometry) spectrometer chamber, a device intended to detect chemical contamination.
  • FAIMS Field Asymmetric Ion Mobility Spectrometry
  • Modern spectrometer scanners detect and identify most organic substances regarded as highly toxic.
  • highly toxic chemicals chemical weapons and toxic industrial materials
  • IMS technology ion mobility spectrometry
  • These are typically classical spectrometers operating at a temperature of about 50°C, with high sensitivity, but not very high resolution, which in practice leads to false alarms.
  • the indicator after ' detecting chemical contamination, generates a warning signal, i.e. it activates a beep and light or sends a signal to activate user-defined devices, such as ventilation devices or alarm systems.
  • the number of false alarms should be as low as possible, as this undermines confidence in the contamination detection system and may cause the unnecessary implementation of emergency procedures.
  • the IMS detector chamber is divided into two areas. The first is the area from the semi-permeable membrane to the injection grid, in which ionization takes place by a ⁇ - or a-radioactive source, the second is the drift area - from the injection grid to the collecting electrode.
  • a high voltage generally 1.5 kV to 3 kV
  • the field is thus shaped so that the ions from the ionization area move in straight lines to the collecting electrode.
  • Most gaseous substances have different rates of mobility, so the transit time of the ions through the drift area varies, allowing for their identification.
  • FAIMS technology is based on the phenomenon of the segregation of ions passing through the detector.
  • the FAIMS detector is constructed of ceramic plates opposite each other to which high voltage is applied at high frequencies. Under the influence of the electric field created within the detector segregation takes place at the collecting electrode.
  • the observed segregation of ions in the gas flowing through results from their varying mobility in fields of greater and lesser intensity.
  • the mobility of the ions is dependent on mass, the charge of the ion and the velocity of the gas flow.
  • the structure of the hybrid FAIMS-1MS system is based on using the FAIMS spectrometer as the first step, but without the collecting electrode. It works on a principle similar to an ion trap. After passing through the ionization source, ions of the analyzed gas pass into the ion trap, formed of two rectangular plates parallel to one another. Between the covers a high intensity field of over 10,000 [V/m] is applied. Thanks to the fact that the mobility of the ions is dependent on the electric field, ion separation can be achieved, since the electric field in the ion trap can be shaped such that only selected ions reach the collecting electrode.
  • FAIMS spectrometers are approximately 10 times as sensitive, furthermore, they permit the separation of gaseous substances such as acetone, benzene and toluene, which to date have not been differentiated by classical IMS spectrometers, even those with high resolution.
  • the aim of the invention was to develop a chamber in which the drawbacks of current devices have been eliminated.
  • the essence of the FAIMS ion mobility spectrometer chamber in this invention comprising an inlet and outlet for the analyzed gas, heating resistors, a gas flow ionizer, FAIMS detector and ionic current collecting electrodes, where the FAIMS detector comprises two electrodes separated by a gap, to which a high voltage high frequency current is connected, is that the heating resistors, the ionizer electrodes, the detector electrodes and the collecting electrodes, as well as the conducting contacts, are applied in the form of layers of precious metals on ceramic plates.
  • the heating resistors are located on the outer surface of the ceramic plates, in the form of a resistive layer of ruthenium dioxide.
  • the top and bottom ceramic plate On the inner surfaces of the top and bottom ceramic plate, sequentially, starting from the inlet of the gas into the chamber, there are gas ionizer electrodes in the form of layers of radioactive nickel, HV and collecting electrodes in the form of layers of gold.
  • the conducting contacts are made of a palladium-silver layer.
  • edge contacts On the side edges of the ceramic plates there are edge contacts that are made of layers of silver.
  • Such a chamber has high repeatability of dimensions, permitting stable gas flow, mechanical rigidity, excellent thermal conductivity and high temperature stability of gas flow, resulting in the analyzed gas being of the same temperature throughout the chamber and the ability to produce a very strong electric field inside.
  • the use of layers of precious metals on the electrodes and detection surfaces fully protects the instrument from corrosion and enables long-term, stable operation, without any changes in parameters.
  • FIG. 1 shows a perspective view of the chamber
  • Figure 2 - a view of the outer surface of the top plate
  • Figure 3 - a view of the inner surface of the top plate, identical to the view of the inner surface of the bottom plate.
  • the spectrometer chamber with the inlet 1 and outlet 2 of the analyzed gas is constructed from four ceramic plates, the top plate 3, the bottom plate 4 and two interstitial plates 5 and 6, ensuring the air-tightness of the chamber and a constant distance between the top and bottom plates.
  • the ceramic plates are made of 96% AI2O3 alumina.
  • the top and bottom plates have a thickness of 1 /40", and the interstitial plates - 1 / 100".
  • the heating resistor 7 constitutes a resistive layer of ruthenium dioxide paste, applied onto the ceramic plate. Above the resistor there is an electronic plate with an amplifier 9.
  • the ionizer electrode in the form of a layer of radioactive Ni 63, is applied on a base of gold paste applied to the ceramic plate. Both the HV electrodes and the collecting electrodes are made of gold past.
  • the conducting contacts . 13, 14 and 15 are made of palladium-silver paste and the edge contacts 16 are made of silver paste.
  • the two plates are bonded together with the interstitial plates 5 and 6 with low-melting sealing glass 7 at a temperature of 560° to 620° at a pressure of 8N to 12N, obtaining a monolithic, sealed chamber of a shape in accordance with the assumptions.

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  • Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (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

The invention concerns a FAIMS ion mobility spectrometer chamber, characterized by a high repeatability of dimensions, permitting stable gas flow, mechanical rigidity, excellent thermal conductivity and high temperature stability of gas flow. The essence of the chamber is that the heating resistor (7), the ionizer electrodes (10), the HV detector electrodes (11) and the collecting electrodes (12), as well as the conducting contacts (13, 14, 15), are applied in the form of layers of precious metals on ceramic plates (3,4). The heating resistor (7) is located on the outer surface of the top (3) and bottom (4) ceramic plate in the form of a resistive layer of ruthenium dioxide. On the inner surface of each of the top (3) and bottom (4) ceramic plates, sequentially, starting from the gas inlet ( 1J to the chamber, there are gas ionizer electrodes (10) in the form of a layer of radioactive nickel, HV electrodes (11) and collecting electrodes ( 12), in the form of layers of gold. The conducting contacts (13, 14, 15) are made of a palladium-silver layer, whereas on the edge surfaces of the ceramic plates there are edge contacts (16), which are made of silver paste.

Description

Ion mobility spectrometer chamber
This invention relates to a FAIMS (Field Asymmetric Ion Mobility Spectrometry) spectrometer chamber, a device intended to detect chemical contamination.
Modern spectrometer scanners detect and identify most organic substances regarded as highly toxic. Currently, the detection of highly toxic chemicals (chemical weapons and toxic industrial materials) is performed by detectors based on IMS technology (ion mobility spectrometry) . These are typically classical spectrometers operating at a temperature of about 50°C, with high sensitivity, but not very high resolution, which in practice leads to false alarms. The indicator, after ' detecting chemical contamination, generates a warning signal, i.e. it activates a beep and light or sends a signal to activate user-defined devices, such as ventilation devices or alarm systems. The number of false alarms should be as low as possible, as this undermines confidence in the contamination detection system and may cause the unnecessary implementation of emergency procedures.
The IMS detector chamber is divided into two areas. The first is the area from the semi-permeable membrane to the injection grid, in which ionization takes place by a β- or a-radioactive source, the second is the drift area - from the injection grid to the collecting electrode. A high voltage (generally 1.5 kV to 3 kV) is applied to the grid in front of the radioactive source, while the metal rings from the source to the collecting electrode have ever lower potentials. The field is thus shaped so that the ions from the ionization area move in straight lines to the collecting electrode. Most gaseous substances have different rates of mobility, so the transit time of the ions through the drift area varies, allowing for their identification.
Currently there is much research being carried out into the improvement of the properties of devices used to detect contamination. One solution is the coupling of the classical ion mobility spectrometer with a spectrometer with a high intensity, high frequency transverse field - FAIMS in a cascade sequence. FAIMS technology is based on the phenomenon of the segregation of ions passing through the detector. The FAIMS detector is constructed of ceramic plates opposite each other to which high voltage is applied at high frequencies. Under the influence of the electric field created within the detector segregation takes place at the collecting electrode. The observed segregation of ions in the gas flowing through results from their varying mobility in fields of greater and lesser intensity. The mobility of the ions is dependent on mass, the charge of the ion and the velocity of the gas flow. Under the influence of an alternating electric field applied to the electrodes, ions whose mobility does not fulfil the conditions of stable flow through the detector are captured. Considering the dependence of the mobility of the ions from the particles migrating through the active interior of the spectrometer on the value of the compensated field, we are dealing with a type of ion filter. The structure of the hybrid FAIMS-1MS system is based on using the FAIMS spectrometer as the first step, but without the collecting electrode. It works on a principle similar to an ion trap. After passing through the ionization source, ions of the analyzed gas pass into the ion trap, formed of two rectangular plates parallel to one another. Between the covers a high intensity field of over 10,000 [V/m] is applied. Thanks to the fact that the mobility of the ions is dependent on the electric field, ion separation can be achieved, since the electric field in the ion trap can be shaped such that only selected ions reach the collecting electrode.
FAIMS spectrometers are approximately 10 times as sensitive, furthermore, they permit the separation of gaseous substances such as acetone, benzene and toluene, which to date have not been differentiated by classical IMS spectrometers, even those with high resolution.
An important factor in the operating of FAIMS spectrometers, omitted in scientific reports or patent descriptions, is the temperature stability of the gas flow. The temperature of the gas has a significant effect on the mobility of the ions, thus it has an effect on the location of the electrical peaks arising from different gaseous substances. The construction of such closed chambers in glass systems is known, allowing for high purity in the chamber, but unfortunately such systems do not ensure the appropriate temperature stability of the gas flow.
The aim of the invention was to develop a chamber in which the drawbacks of current devices have been eliminated.
The essence of the FAIMS ion mobility spectrometer chamber in this invention, comprising an inlet and outlet for the analyzed gas, heating resistors, a gas flow ionizer, FAIMS detector and ionic current collecting electrodes, where the FAIMS detector comprises two electrodes separated by a gap, to which a high voltage high frequency current is connected, is that the heating resistors, the ionizer electrodes, the detector electrodes and the collecting electrodes, as well as the conducting contacts, are applied in the form of layers of precious metals on ceramic plates. The heating resistors are located on the outer surface of the ceramic plates, in the form of a resistive layer of ruthenium dioxide. On the inner surfaces of the top and bottom ceramic plate, sequentially, starting from the inlet of the gas into the chamber, there are gas ionizer electrodes in the form of layers of radioactive nickel, HV and collecting electrodes in the form of layers of gold. The conducting contacts are made of a palladium-silver layer. On the side edges of the ceramic plates there are edge contacts that are made of layers of silver.
Such a chamber has high repeatability of dimensions, permitting stable gas flow, mechanical rigidity, excellent thermal conductivity and high temperature stability of gas flow, resulting in the analyzed gas being of the same temperature throughout the chamber and the ability to produce a very strong electric field inside. The use of layers of precious metals on the electrodes and detection surfaces fully protects the instrument from corrosion and enables long-term, stable operation, without any changes in parameters.
The chamber is shown in an example of the realization of this invention in the drawings where Figure 1 shows a perspective view of the chamber, Figure 2 - a view of the outer surface of the top plate, and Figure 3 - a view of the inner surface of the top plate, identical to the view of the inner surface of the bottom plate.
The spectrometer chamber with the inlet 1 and outlet 2 of the analyzed gas is constructed from four ceramic plates, the top plate 3, the bottom plate 4 and two interstitial plates 5 and 6, ensuring the air-tightness of the chamber and a constant distance between the top and bottom plates. The ceramic plates are made of 96% AI2O3 alumina. The top and bottom plates have a thickness of 1 /40", and the interstitial plates - 1 / 100". On the outer surface of each of the top 3 and bottom 4 ceramic plates, there is a heating resistor 7 and temperature sensor 8. The heating resistor 7 constitutes a resistive layer of ruthenium dioxide paste, applied onto the ceramic plate. Above the resistor there is an electronic plate with an amplifier 9.
On each of the top 3 and bottom 4 ceramic plates on their inner surfaces there are, sequentially, starting from the gas inlet: ionizer electrodes 10, HV electrodes H and collecting electrodes 12. The ionizer electrode, in the form of a layer of radioactive Ni 63, is applied on a base of gold paste applied to the ceramic plate. Both the HV electrodes and the collecting electrodes are made of gold past. The conducting contacts .13, 14 and 15 are made of palladium-silver paste and the edge contacts 16 are made of silver paste. After applying the above features onto the top plate 3 and the bottom plate 4, the two plates are bonded together with the interstitial plates 5 and 6 with low-melting sealing glass 7 at a temperature of 560° to 620° at a pressure of 8N to 12N, obtaining a monolithic, sealed chamber of a shape in accordance with the assumptions.

Claims

Patent claim
A ion mobility spectrometer chamber, FAIMS type, with an inlet and outlet for the analyzed gas, a heating resistor, an ionizer of the gas flowing through, a FAIMS detector and electrodes collecting ionic current, where the FAIMS detector comprises two electrodes separated by a gap, to which a high voltage, high frequency current is connected, characterized in that the heating resistor (7) , the ionizer electrodes ( 10) , the HV detector electrodes ( 1 1) and the collecting electrodes (12) , as well as the conducting contacts (13, 14, 15) , are applied in the form of layers of precious metals on ceramic plates (3,4) , where the heating resistor (7) is located on the outer surface of the top (3) and bottom (4) ceramic plate in the form of a resistive layer of ruthenium dioxide, on the inner surface of each of the top (3) and bottom (4) ceramic plates, sequentially, starting from the gas inlet (1) to the chamber, there are gas ionizer electrodes ( 10) in the form of a layer of radioactive nickel, HV electrodes ( 1 1) and collecting electrodes ( 12) in the form of layers of gold, and the conducting contacts ( 13, 14, 15) are made of a palladium-silver layer, whereas on the edge surfaces of the ceramic plates there are edge contacts ( 16) , which are made of silver layer.
PCT/PL2012/000033 2011-05-17 2012-05-16 Ion mobility spectrometer chamber WO2012158052A1 (en)

Priority Applications (6)

Application Number Priority Date Filing Date Title
DE112012002128.2T DE112012002128T5 (en) 2011-05-17 2012-05-16 Ion mobility spectrometer chamber
EP12741397.9A EP2710362B1 (en) 2011-05-17 2012-05-16 Ion mobility spectrometer chamber
CN201280023269.0A CN103534589A (en) 2011-05-17 2012-05-16 Ion mobility spectrometer chamber
GB1319844.5A GB2504884A (en) 2011-05-17 2012-05-16 Ion mobility spectrometer chamber
US14/117,627 US9354201B2 (en) 2011-05-17 2012-05-16 Ion mobility spectrometer chamber
FI20135985A FI20135985L (en) 2011-05-17 2013-10-02 ION MOBILITY SPECTROMETER CHAMBER

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
PLP-394898 2011-05-17
PL394898A PL218395B1 (en) 2011-05-17 2011-05-17 Ion mobility spectrometer chamber

Publications (1)

Publication Number Publication Date
WO2012158052A1 true WO2012158052A1 (en) 2012-11-22

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PCT/PL2012/000033 WO2012158052A1 (en) 2011-05-17 2012-05-16 Ion mobility spectrometer chamber

Country Status (8)

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US (1) US9354201B2 (en)
EP (1) EP2710362B1 (en)
CN (1) CN103534589A (en)
DE (1) DE112012002128T5 (en)
FI (1) FI20135985L (en)
GB (1) GB2504884A (en)
PL (1) PL218395B1 (en)
WO (1) WO2012158052A1 (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
PL402111A1 (en) 2012-12-18 2014-06-23 Wojskowy Instytut Chemii I Radiometrii Device for diagnosis of contamination based on the ceramic chamber FAIMS type spectrometer or DMS
CN111398097A (en) * 2020-04-02 2020-07-10 西安宏星电子浆料科技股份有限公司 Silver migration testing method of silver conductor slurry for sheet resistor
US20220397552A1 (en) * 2021-06-10 2022-12-15 GP Ionics LLC Molecular identification using field induced fragmentation spectra by reactive stage tandem differential mobility spectrometry

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050133716A1 (en) * 1999-07-21 2005-06-23 Miller Raanan A. Explosives detection using differential ion mobility spectrometry
US7098449B1 (en) * 1999-07-21 2006-08-29 The Charles Stark Draper Laboratory, Inc. Spectrometer chip assembly

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ATE220936T1 (en) * 1998-05-13 2002-08-15 Cygnus Therapeutic Systems COLLECTION DEVICES FOR TRANSDERMAL SAMPLING SYSTEMS
US6495823B1 (en) * 1999-07-21 2002-12-17 The Charles Stark Draper Laboratory, Inc. Micromachined field asymmetric ion mobility filter and detection system
US6815668B2 (en) * 1999-07-21 2004-11-09 The Charles Stark Draper Laboratory, Inc. Method and apparatus for chromatography-high field asymmetric waveform ion mobility spectrometry
US7576320B2 (en) * 2002-02-15 2009-08-18 Implant Sciences Corporation Photoelectric ion source photocathode regeneration system

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050133716A1 (en) * 1999-07-21 2005-06-23 Miller Raanan A. Explosives detection using differential ion mobility spectrometry
US7098449B1 (en) * 1999-07-21 2006-08-29 The Charles Stark Draper Laboratory, Inc. Spectrometer chip assembly

Also Published As

Publication number Publication date
US20160069836A1 (en) 2016-03-10
EP2710362A1 (en) 2014-03-26
GB2504884A (en) 2014-02-12
EP2710362B1 (en) 2016-07-06
DE112012002128T5 (en) 2014-03-06
FI20135985L (en) 2013-10-02
US9354201B2 (en) 2016-05-31
PL218395B1 (en) 2014-11-28
PL394898A1 (en) 2012-11-19
GB201319844D0 (en) 2013-12-25
CN103534589A (en) 2014-01-22

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