WO2012012657A2 - Appareils d'admission d'analyse de substrat, instruments d'analyse de substrat et procédés d'analyse de substrat - Google Patents

Appareils d'admission d'analyse de substrat, instruments d'analyse de substrat et procédés d'analyse de substrat Download PDF

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Publication number
WO2012012657A2
WO2012012657A2 PCT/US2011/044886 US2011044886W WO2012012657A2 WO 2012012657 A2 WO2012012657 A2 WO 2012012657A2 US 2011044886 W US2011044886 W US 2011044886W WO 2012012657 A2 WO2012012657 A2 WO 2012012657A2
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WO
WIPO (PCT)
Prior art keywords
substrate
component
compartment
analysis
sampling
Prior art date
Application number
PCT/US2011/044886
Other languages
English (en)
Other versions
WO2012012657A3 (fr
Inventor
Jeffrey J. Corpstein
Tri Le
Jason Springston
Garth E. Patterson
Original Assignee
Griffin Analytical Technologies, L.L.C.
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 Griffin Analytical Technologies, L.L.C. filed Critical Griffin Analytical Technologies, L.L.C.
Publication of WO2012012657A2 publication Critical patent/WO2012012657A2/fr
Publication of WO2012012657A3 publication Critical patent/WO2012012657A3/fr

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Classifications

    • 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
    • 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
    • H01J49/0404—Capillaries used for transferring samples or ions
    • 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
    • H01J49/0409—Sample holders or containers
    • 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
    • H01J49/049—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 with means for applying heat to desorb the sample; Evaporation

Definitions

  • the present disclosure relates to analytical instruments and methods.
  • Particular embodiments of the disclosu relate to sampli ng components of analytical instruments as well as sampling techniques such as substrate analysis inlet apparatuses, substrate analysis instruments, and substrate analysis methods. I n particular applications the substrates are sampling swabs.
  • swab analytical system One piece of analytical instrumentation utilized by security person nel is the swab analytical system .
  • a swab is a substrate that is utilized and contacted with a person , a person's clothi ng, or a person's personal item. After being contacted , the swab can then be analyzed for compounds of concern.
  • the present disclosure provides analytical instrumentation, analytical methods, mass spectrometry instrumentation, and mass spectrometry methods.
  • E mbodi ments of the disclosure provide i nstru ments and/or methods that may be utilized in conjunction with swab analytical tech niques. DESCRIPTION OF THE DRAWINGS
  • Fig. 1 is an analytical instrument according to an embodiment.
  • Fig.2 is an exemplary swab according to an embodiment.
  • Fig. 3 is a component of an analytical instrument according to an embodiment.
  • Fig. 4 is a component of an analytical instrument according to an embodiment.
  • Fig. 5 is a component of an analytical instrument according to an embodiment.
  • Fig. 6 is a component of an analytical instrument according to an embodiment.
  • Fig. 7 is a component of an analytical instrument according to an embodiment.
  • Fig. 8 is a component of an analytical instrument according to an embodiment.
  • Fig. 9 is another view of the component of Fig. 8 according to an embodiment.
  • Fig. 10 is another view of the component of Fig. 8 according to an embodiment.
  • Fig. 11 is a component of an analytical instrument according to an embodiment.
  • Fig. 12 is data acquired utilizing the analytical instrument using analytical methods according to an embodiment.
  • Fig . 1 3 is data acquired utilizing analytical methods according to an embodi ment.
  • an analytical instrument 1 0 that includes a sample i ntroduction component 1 2 coupled to an analysis component 1 3.
  • analysis component 1 3 may be configured to perform all manner of i nstru mental analysis.
  • Such instrumental analysis can include one or both of qualitative and/or quantitative analysis.
  • Example instru mentation can include but is not limited to optical spectroscopy, ultraviolet/visible spectroscopy, near infrared absorption spectroscopy, fluorescence, phosphorescence, and/or chemilu mi nescence detection , atomic spectroscopy such as flame or electrothermal atomization, emission spectroscopy such as plasma, arc, and/or spark atomization, infrared absorption spectroscopy, Raman spectroscopy, N M R spectroscopy, X-ray spectroscopy, Radiochemical methods, mass spectrometry, chromatog raphic analytical techniques such as gas and/or liquid chromatog raphy and/or combi nations of the above.
  • optical spectroscopy ultraviolet/visible spectroscopy, near infrared absorption spectroscopy, fluorescence, phosphorescence, and/or chemilu mi nescence detection
  • atomic spectroscopy such as flame or electrothermal atomization
  • emission spectroscopy such as plasma
  • analysis component 1 3 can be configured to perform gas chromatography/mass spectrometry.
  • Component 1 3 can include sample preparation component 1 4, mass separation component 1 6, and detection component 1 8.
  • Example component 1 3 can include sample inlet, ion source, mass separator, detector, and processing and control components.
  • Example mass spectrometry assembly configu rations can house one or more of the ion source, mass separator, and detector components withi n an analysis chamber.
  • the mass spectrometry analysis chamber can be maintai ned below atmospheric pressure, while typical mass spectrometry analysis chambers are maintained under high vacuum while restricting the flow of contaminants into the analysis chamber to as few as practically possible.
  • Components 1 3 can be configured as described in U nited States
  • i nstrument 1 0 can be configured to receive sample into sample component 1 4.
  • Sample analysis can be performed according to exemplary aspects described below.
  • components 1 2 can be operationally connected to component 1 4 which can be operationally connected to component 1 6 which can be operationally connected to component 1 8.
  • These general components can be operationally con nected to processi ng and control device components.
  • Example embodi ments provide for the use of components 1 3 to perform mass spectrometry.
  • Components 1 3 can be operationally connected as shown in Fig. 1 or operationally connected in other configu rations enabling mass spectrometry operations. Fu rther, other arrangements includi ng more or less or alternative components are possible.
  • Sample inlet component 1 2 can be configu red to introduce an amount of sample into assembly 1 0 (Fig . 1 ) for analysis. Depending upon the sample, sample inlet component 1 2 may be configu red to prepare the sample for ionization . I n some aspects, sample inlet component 1 2 may be combi ned with component 1 4.
  • Sample i nlet component 1 2 can be configured as a sampling substrate analysis inlet apparatus configured to receive a swab for analysis of the swab. Referri ng to Fig. 2, swab 20 is shown that includes an upper face 22 and a lower face 24. I n practice, upper face 22 can be applied to a person or personal item and then provided to the instrument for analysis.
  • upper face 22 may i nclude analytes of interest.
  • Swab 20 can be a cellulose fabric substrate, for example.
  • Swab 20 is shown havi ng a substantially rectangular perimeter.
  • Other configurations of swab 20 are contemplated , i ncluding but not li mited to circular configurations.
  • analytes 31 can be removed from swab 20 and passed th rough a conduit coupling sample introduction component 1 2 to the remainder of instrument 1 0 as defined as preparation, separation , and detection components 1 3.
  • a compartment 30 can be defined to receive swab 20. Compartment 30 can have walls and upper portion 31 and lower portion 32. Within upper portion 31 can be openi ng 56 configured to receive analytes 31 and/or carrier gas and provide same to instrument 1 0.
  • lower component 32 can be represented as
  • lower component 32a can have a heating component 40 that provides a heightened temperatu re to substrate 20, thereby facilitating the removal of analytes from swab 20.
  • this heating component can be configu red to be heated electrically and the temperatu re gauged by a thermal couple.
  • upper component 31 can include openi ngs 52 to facilitate the transfer of carrier gas across surface 22 of substrate 20.
  • 31 can include openings 52 at the periphery or peri meter of component 32 that facilitates the flow of carrier gas across surface 22 to an intake 56 centrally located over substrate 20.
  • the carrier gas can be air, nitrogen , heliu m, oxygen, and/or hyd rogen, for example.
  • the lower surface of component 31 can define a wall of a substrate receiving compartment and this wall can defi ne openings 52, for example.
  • These openi ngs can be i n fluid com munication with a space defi ned by the compartment.
  • These openings can be configured to provide the carrier gas to with the compartment.
  • these openings 52 can be placed and/or arranged around a peri meter of the lower surface of component 31 , that peri meter being consistent with the peri meter of a swab to be analyzed.
  • this peri meter may be defined as a square.
  • this perimeter may be defined as a ci rcle.
  • the upper component 31 may be configured to include heating elements 60 proxi mate i ntake 61 as well as diffuser block 62.
  • carrier gas may be provided throug h opening 61 where it is heated by heati ng element 60 which also heats diffuser block 62.
  • the carrier gas entering 61 can diffuse through diffuser block 62 prior to enteri ng openi ngs 52, for example as shown and described in Fig . 5.
  • Block 62 can occupy a recess within component 31 for example.
  • component 31 may include openings to facilitate flow of carrier gas to one or both of a sample pump and/or instrumentation 1 3.
  • carrier gas may enter openi ng 56 and proceed to sample pump 70 in one direction , or proceed to instrument 72 in another alternative di rection.
  • Carrier gas can enter 56 and then proceed to i nstru ment 1 3 via 72 or sample pump via 70.
  • Openi ng 56 can be a portion of a conduit, the conduit extending to a bifurcated portion extendi ng the conduit i nto at least two portions. The bifurcated portion can be within the wall of the compartment defined by lower portion of component 31 , for example.
  • conduit withi n component 31 can be bifurcated at portion 74, for example. Where, for example, the distance 70 i n relation to 56 is greater, sample concentration to openi ng 72 i n instrument 1 3 is increased ; where it is lesser, sample concentration to instrument 1 3 is less.
  • an input apparatus 80 that includes a heated diffuser component comprised by components 84, 90, and 82, as well as analyte collection component 82 and analyte transfer component 82.
  • Component 82 defines openings configured to provide carrier gas and additional openi ngs configured to receive analytes and conduits withi n component 82 to transfer analytes to an i nstru ment.
  • the diffuser component includes heater block 84 defi ning a recess to receive porous material 90. Heater block 84 also i ncludes heating elements 86. These heati ng elements can be placed within heater block 84 proxi mate carrier gas i nlet 88.
  • Porous material 90 can be configured as diffusion discs that may be placed within the recess of heater block 84 shown , and then above a support block 82 which is configu red to receive an O ring 92 to facilitate the coupling of heater block 84 and support block 82.
  • support block 82 includes peripheral openi ngs 96 to facilitate the flow of carrier gas across a substrate which is configu red to be received within recess 98 defining at least a portion of a substrate compartment.
  • an underside view of component 82 is shown that demonstrates the flow of carrier gas through peripheral openings 96 across a substrate to facilitate the gathering of analytes to i ntake 1 1 0.
  • I ntake 1 1 0 is i n fluid com mu nication with split flow 1 00 and sample flow 1 1 2.
  • This configuration can define the analyte collection component of the apparatus.
  • support block 82 is coupled to heater block 84 having carrier gas 88 directed thereto. As shown, gas is diffused and passes through opening 96 which passes across substrate 20 to enter sample inlet 110 which is in fluid communication with split flow 100 and instrument conduit 112. This configuration can define the sample transfer component of the apparatus.
  • the apparatus can be coupled to mass analysis component as described and referenced herein.
  • component 80 can include a lower insulated block 114 configured to surround lower block 112 that includes a recess configured to include heater element 116.
  • swab 20 can be placed over heater element 116 within a recess defined by upper block 82 and lower block 112 to facilitate the transfer of components from swab 20 to instrument 13.
  • analysis methods of the present disclosure can include preheating the carrier gas and applying the gas to the substrate from about the outer edge(s) of the substrate toward an opening over a central portion of the substrate.
  • the substrate can be a circular swab, and the applying being around the edges of the swab.
  • Methods can also include receiving analyte and carrier gas from within a substrate compartment and splitting the applied carrier gas to provide a portion of the gas to an analysis component.
  • the analyzing the gas can be performed in sub atmospheric conditions.
  • a chamber can house components 13 such as sample preparation component 14, separation component 16, and detector component 18.
  • Component 14 can be configured, according to example embodiments, to receive sample directly or, in other example embodiments, to receive sample from component 12.
  • Component 14 can be configured to convert portions or an entirety of sample into analyte ions in one example. This conversion can include the bombardment of sample with electrons, ions, molecules, and/or photons. This conversion can also be performed by thermal or electrical energy.
  • Component 14 may utilize, for example, electron ionization (El, typically suitable for the gas phase ionization), photo ionization (PI), chemical ionization, and/or collisio nally activated disassociation.
  • El electron ionization
  • PI photo ionization
  • PI chemical ionization
  • collisio nally activated disassociation For example in PI, the photo energy can be varied to vary the internal energy of the sample.
  • sample can be energized under atmospheric pressure and potentials applied can be varied to cause varying degrees of dissociation. Potentials applied can be varied to cause varying degrees of dissociation as described in International Application Publication No. WO/2004/097352 published November 11, 2004, entitled “Instrumentation, Articles of Manufacture, and Analysis Methods", the entirety of which is incorporated by reference herein.
  • exemplary ion source components include those described in United States Patent No, 7,361,890 issued April 22, 2008, entitled “Analytical Instruments, Assembl
  • Mass separator component 16 can include one or more of linear quadrupoles, triple quadrupoles, quadrupole ion traps (Paul), cylindrical ion traps, linear ion traps, rectilinear ion traps, ion cyclotron resonance, quadrupole ion trap/time-of-flight mass spectrometers, or other structures. Mass separator component 16 can also include focusing lenses as well as tandem mass separator components such as tandem ion traps or ion traps and quadrupoles in tandem. In one implementation at least one of multiple tandem mass separator components can be an ion trap.
  • Exemplary mass separators i n include those described i n I nternational Patent Application Publication No. WO/2004/051 225 published June 1 7, 2004, entitled "Processes for Designi ng Mass Separators and Ion Traps, Methods for Producing Mass Separators and Ion Traps, Mass Spectrometers, Ion Traps, and Methods for Analyzi ng Samples", the entirety of which is incorporated by reference herei n.
  • Tandem mass separator components can be placed in series or parallel.
  • tandem mass separator components can receive ions from the same ion sou rce component.
  • the tandem mass separator components may have the same or different geometric parameters.
  • the tandem mass separator components may also receive analyte ions from the same or multiple ion source components. Analytes may proceed to detector component 1 8.
  • Example detector components include electron multipliers, Faraday cup collectors, photog raphic and scintillation-type detectors.
  • Example detector components also include those described i n U nited States Patent No. 7, 1 61 , 1 42 issued January 9, 2007, entitled "Portable Mass Spectrometers", the entirety of which is i ncorporated by reference herein .
  • the prog ression of mass spectrometry analysis from component 1 2 to detector component 1 8 can be controlled and monitored by a processi ng and control device components (not shown) . Acquisition and generation of data can be facilitated with the same or different processi ng and control device component.
  • Example processi ng and control device components can be a computer or mini-computer or other appropriate ci rcuitry that is capable of controlling i nstru ment components. This control can include, for example, the specific application of voltages to component 1 4 and mass separator component 1 6, as well as the introduction of sample via sample inlet component 1 2 and may further include determi ning , stori ng and ulti mately displaying mass spectra recorded from detector component 1 8.
  • Processi ng and control device components can contain data acquisition and searching software.
  • data acquisition and searching software can be configu red to perform data acquisition and searching that i ncludes the programmed acquisition of total analyte count.
  • data acquisition and searching parameters can include methods for correlating the amount of analytes generated to predetermine programs for acquiring data.
  • Exemplary configu rations of processing and control components include those described in I nternational Patent Application Publication No. WO/2005/024594 published March 1 7, 2005, entitled "Analysis Device Operational Methods and Analysis Device Programming Methods", the entirety of which is incorporated by reference herein .
  • Referri ng to Figs. 1 2 and 1 3 example data is as shown utilizing the inlets, apparatuses, instruments, and methods of present disclosure. This data is mass spectral data acqui red from analysis of "doped" swabs.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)

Abstract

L'invention concerne des admissions, des appareils, des instruments et des procédés d'analyse de substrat d'échantillon pouvant comprendre ou utiliser un élément diffuseur chauffé et/ou un élément de collecte de substance destinée à être analysée et/ou un élément de transfert de substance destinée à être analysée.
PCT/US2011/044886 2010-07-21 2011-07-21 Appareils d'admission d'analyse de substrat, instruments d'analyse de substrat et procédés d'analyse de substrat WO2012012657A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US36647210P 2010-07-21 2010-07-21
US61/366,472 2010-07-21

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WO2012012657A2 true WO2012012657A2 (fr) 2012-01-26
WO2012012657A3 WO2012012657A3 (fr) 2012-05-03

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102891062A (zh) * 2012-09-18 2013-01-23 昆山禾信质谱技术有限公司 一种用于质谱仪的膜加热进样装置

Citations (6)

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Publication number Priority date Publication date Assignee Title
WO2004051225A2 (fr) 2002-12-02 2004-06-17 Griffin Analytical Technologies, Inc. Processus pour concevoir des separateurs de masse et des pieges a ions, procedes pour produire des separateurs de masse et des pieges a ions, spectrometres de masse, pieges a ions et procedes pour analyser des echantillons
WO2004097352A2 (fr) 2003-04-25 2004-11-11 Griffin Analytical Technologies, Inc. Appareillage, articles manufactures et methodes d'analyse
WO2005024594A2 (fr) 2003-09-04 2005-03-17 Griffin Analytical Technologies, Inc. Methodes d'utilisation et de programmation d'un instrument d'analyse
US7161142B1 (en) 2003-09-05 2007-01-09 Griffin Analytical Technologies Portable mass spectrometers
US20070258861A1 (en) 2004-06-15 2007-11-08 Barket Dennis Jr Analytical Instruments, Assemblies, and Methods
US7361890B2 (en) 2004-07-02 2008-04-22 Griffin Analytical Technologies, Inc. Analytical instruments, assemblies, and methods

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US5859375A (en) * 1996-04-03 1999-01-12 Barringer Research Limited Apparatus for and method of collecting trace samples for analysis
MX2009000099A (es) * 2006-06-29 2009-02-13 Separation Systems Inc Metodo y sistema para caracterizacion fisica y quimica de muestras complejas.
JP2008139130A (ja) * 2006-12-01 2008-06-19 Hitachi Ltd リアルタイム分析装置及び方法
DE102008059112A1 (de) * 2008-11-26 2010-06-17 Eads Deutschland Gmbh Probensammler und Probensammeleinrichtung für eine Analyseeinrichtung sowie Verfahren zu dessen Betrieb

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004051225A2 (fr) 2002-12-02 2004-06-17 Griffin Analytical Technologies, Inc. Processus pour concevoir des separateurs de masse et des pieges a ions, procedes pour produire des separateurs de masse et des pieges a ions, spectrometres de masse, pieges a ions et procedes pour analyser des echantillons
WO2004097352A2 (fr) 2003-04-25 2004-11-11 Griffin Analytical Technologies, Inc. Appareillage, articles manufactures et methodes d'analyse
WO2005024594A2 (fr) 2003-09-04 2005-03-17 Griffin Analytical Technologies, Inc. Methodes d'utilisation et de programmation d'un instrument d'analyse
US7161142B1 (en) 2003-09-05 2007-01-09 Griffin Analytical Technologies Portable mass spectrometers
US20070258861A1 (en) 2004-06-15 2007-11-08 Barket Dennis Jr Analytical Instruments, Assemblies, and Methods
US7361890B2 (en) 2004-07-02 2008-04-22 Griffin Analytical Technologies, Inc. Analytical instruments, assemblies, and methods

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102891062A (zh) * 2012-09-18 2013-01-23 昆山禾信质谱技术有限公司 一种用于质谱仪的膜加热进样装置

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