CA3023926A1 - Apparatus and method of operation of a sample introduction system to a chemical analyzer - Google Patents
Apparatus and method of operation of a sample introduction system to a chemical analyzer Download PDFInfo
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- CA3023926A1 CA3023926A1 CA3023926A CA3023926A CA3023926A1 CA 3023926 A1 CA3023926 A1 CA 3023926A1 CA 3023926 A CA3023926 A CA 3023926A CA 3023926 A CA3023926 A CA 3023926A CA 3023926 A1 CA3023926 A1 CA 3023926A1
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating 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
- G01N27/626—Investigating 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 heat to ionise a gas
- G01N27/628—Investigating 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 heat to ionise a gas and a beam of energy, e.g. laser enhanced ionisation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/8813—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample biological materials
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
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- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Electrochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Optics & Photonics (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention includes a chamber into which a sample is placed through a port or an orifice, a means to heat the sample, and a port or an orifice that is in fluid communication with a chemical analyzer. The invention may also include a port or orifice that is in fluid communication with a means to evacuate the sample chamber to a pressure below that of the surrounding atmosphere. The invention may also include one or more apparatus to substantially eliminate fluid communication between the sample chamber and at least one of the atmosphere, the means to evacuate the chamber, and the mass analyzer. Further, the invention includes an apparatus for transferring thermal energy to a sample. The apparatus for transferring thermal energy to the sample is chosen to substantially heat only the sample that is placed in the chamber. The invention may include optical components to cause ionization of chemical species and associated optical components for transferring the ionized chemical species to a desired location.
Description
Field of the Invention This invention relates generally to the field of sample introduction systems for chemical detectors and analyzers, and more specifically to the apparatus and method of operation of a thermal desorber for releasing chemicals from a narcotic or biological sample under reduced pressure into a mass analyzer for determining the nature of the chemicals present in the sample.
The invention includes a chamber into which a sample is placed through a port or an orifice, a means to heat the sample, and a port or an orifice that is in fluid communication with a chemical analyzer. The invention may also include a port or orifice that is in fluid communication with a means to evacuate the sample chamber to a pressure below that of the surrounding atmosphere. The invention may also include one or more apparatus to substantially eliminate fluid communication between the sample chamber and at least one of the atmosphere, the means to evacuate the chamber, and the mass analyzer. Further, the invention includes an apparatus for transferring thermal energy to a sample. The apparatus for transferring thermal energy to the sample is chosen to substantially heat only the sample that is placed in the chamber.
The invention includes numerous advantages over the prior art. First, the invention provides for a reduced pressure in the sample chamber which enables chemicals to undergo a phase transition from a solid or liquid form to a vapour form, thus be released from a sample in a vapour form, at a temperature that is lower than the temperature at which the same chemical will undergo a transition to the vapour phase at standard atmospheric pressure, which is understood by those skilled in the art to be 101.3 kPa (kilopascals) and referred to as the "boiling point". The reduced temperature of this desorption allows those skilled in the art to choose from a wider variety of materials and apparatus.
Further, the invention provides for a means to heat substantially on the sample, which substantially eliminates the requirement to heat the sample of chamber, or a substantial portion thereof, in order to heat the sample to a temperature at which desired chemicals will be released from the sample.
.. This further relaxes the burden on designers of sample introduction systems to choose materials that will withstand the elevated temperatures required for desorption.
It is also desired to provide for a sample introductiots system that responds in a little time as reasonably possible to changes in the temperature applied to the sample. The invention described here requires less power to operate and heats a volume of material substantially less than the volume CA 3023926 2018-11-13 , - _ of the sample introduction system, hence will provide for rapid heating and cooling compared to the prior art.
A further advantage to the apparatus and method described herein over the prior art is that it provides for embodiments where chemicals desorbed from the sample at a substantially similar temperature may be separated according to the retention time in a capillary providing a means for fluid communication between the sample chamber and the mass analyzer.
In addition to the foregoing, the invention provides for a method of operation whereby the temperature of the sample is controlled such that the operator of the sample introduction system can choose which temperature is applied to the sample, and the rate at which the temperature changes as a function of time, known as the "temperature profile." By operating the sample introduction system in a manner such that the temperature of the sample follows a temperature profile chosen by the operator, the chemicals with different boiling points wilt be desorbed from the sample at different times. This method of operation provides an advantage over prior art by allowing chemicals with different boiling points to be analyzed in the mass analyzer substantially independently.
Description of Prior Art It is known in the prior art that the use of a reduced pressure vacuum environment can be provided to desorb a chemical sample into a chemical analyzer. An embodiment is taught by Yasuhiro in JP11287743 which describes a vacuum tank coupled to a mass analyzer, wherein the vacuum tank is a hotplate that heats a sample attracted electrostatically to the surface of the hotplate in order to desorb an analyte from the surface for analysis by a chemical analyzer. With respect to the invention described here, Yasuhiro does not teach the use of an external heat source, specifically an optical heat source, transferred into the vacuum tank but rather relies on a hotplate contained within the vacuum tank. One skilled in the art, when reducing the teaching of Yasuhiro to practice, would be prevented from controlling substantially only the temperature of the sample, which can cause temperature variations throughout the volume of the sample, requires more power to operate the heater, and may lead to a plurality of chemicals being desorbed from the sample which may be convoluted by the chemical analyzer. Further, Yasuhiro does not teach the use of a conduit between the vacuum tank and the chemical analyzer. One skilled in the art, when reducing the teaching of Yasuhiro to practice, would be unable to control the pressure in the vacuum tank separately from the pressure in the mass analyzer. Further to the limitation of Yasuhiro's teaching on pressure, the embodiment does not provide for a separate apparatus to reduce the pressure in the vacuum tank to a desired pressure. When applied to the invention described here, the practitioner would be unable to control the pressure in the sample chamber in order to cause the boiling point of chemicals within the sample to be reduced to a desirable temperature.
Mullock, in US 2005/0109932 Al, teaches the use of a sorbent trap to collect analyte from an air sample; where the pressure in the body of the trap is reduced to a pressure that is lower than atmospheric pressure prior to activating a heater to desorb the collected analyte into a mass spectrometer. In contrast, the invention described here does not require the use of a trap to collect analyte prior to desorbing the analyte into the chemical analyzer. Further, Mullock does not teach the method of reducing the pressure in the trap body in a controlled manner to modify the chemical properties of an analyte or plurality of analytes, such as the boiling point, to a desired level.
Similar to Mullock, Rafferty in CA 2,824,525 teaches an apparatus and method of operating an apparatus to thermally desorb a sample from a sample collector into a mass spectrometer. In one of the embodiments taught, an infrared source is provided to heat the sample collector in order to desorb analytes into a vapour phase. With respect to the invention described here, Rafferty et. al.
does not teach the use of an optical source and a light pipe that is in optical communication with the sample chamber. A practitioner implementing the embodiment disclosed by Rafferty et. al. would not realize the benefit of heating substantially only the sample.
In regards to the apparatus and method for heating a sample, Kashima et. al.
U52004/0124352 Al teaches an embodiment of an apparatus for desorbing a sample by applying heat with an optical source in the infrared wavelength range, that is contained within an atmospheric pressure ion source.
With respect to the invention described here, the embodiment of Kashima et.
al. does not provide for an apparatus or method to reduce the pressure in the atmospheric pressure ion source prior to activating the infrared source. Further, Kashima et. al. requires that analytes be collected on a clean wiping member and does not provide for a means to introduce a sample without such a collector.
Further, with respect to the invention described here, Kashima et. al. teaches a method of heating the sample as quickly as possible to achieve a high concentration of analyte to be introduced to the mass spectrometer. In contrast, the invention described here allows for heat to be applied in a controlled manner, that when coupled with the controlled pressure reduction of the sample chamber, allows a practitioner to release chemicals from a sample in a desired manner.
Whitehouse et. al., in CA 2,837,478, teaches the use of an optical source in an atmospheric pressure ion source that includes means to sense the type, size, physical features and position of each sample introduced. Whitehouse et. al. does not teach the use of said means to measure the mass of a sample during the operation of the apparatus. Further, Whitehouse et. al. does not teach the method of operation where the optical source is used to heat the sample but rather limits the use of the optical source to ionizing the chemical species released from the sample holder. With respect to the invention disclosed here, a practitioner implementing the embodiment of Whitehouse et. al. would not have the means to extract information from the sample concerning the amount of concentration of analytes in the sample. Further, Whitehouse et. al. does not teach an embodiment of an apparatus or method to heat the sample.
References Cited:
1. Yasuhiro; JP 11,287,743; Thermal Desorbing/Analyzing Chamber for Wafer Process Monitor
The invention includes a chamber into which a sample is placed through a port or an orifice, a means to heat the sample, and a port or an orifice that is in fluid communication with a chemical analyzer. The invention may also include a port or orifice that is in fluid communication with a means to evacuate the sample chamber to a pressure below that of the surrounding atmosphere. The invention may also include one or more apparatus to substantially eliminate fluid communication between the sample chamber and at least one of the atmosphere, the means to evacuate the chamber, and the mass analyzer. Further, the invention includes an apparatus for transferring thermal energy to a sample. The apparatus for transferring thermal energy to the sample is chosen to substantially heat only the sample that is placed in the chamber.
The invention includes numerous advantages over the prior art. First, the invention provides for a reduced pressure in the sample chamber which enables chemicals to undergo a phase transition from a solid or liquid form to a vapour form, thus be released from a sample in a vapour form, at a temperature that is lower than the temperature at which the same chemical will undergo a transition to the vapour phase at standard atmospheric pressure, which is understood by those skilled in the art to be 101.3 kPa (kilopascals) and referred to as the "boiling point". The reduced temperature of this desorption allows those skilled in the art to choose from a wider variety of materials and apparatus.
Further, the invention provides for a means to heat substantially on the sample, which substantially eliminates the requirement to heat the sample of chamber, or a substantial portion thereof, in order to heat the sample to a temperature at which desired chemicals will be released from the sample.
.. This further relaxes the burden on designers of sample introduction systems to choose materials that will withstand the elevated temperatures required for desorption.
It is also desired to provide for a sample introductiots system that responds in a little time as reasonably possible to changes in the temperature applied to the sample. The invention described here requires less power to operate and heats a volume of material substantially less than the volume CA 3023926 2018-11-13 , - _ of the sample introduction system, hence will provide for rapid heating and cooling compared to the prior art.
A further advantage to the apparatus and method described herein over the prior art is that it provides for embodiments where chemicals desorbed from the sample at a substantially similar temperature may be separated according to the retention time in a capillary providing a means for fluid communication between the sample chamber and the mass analyzer.
In addition to the foregoing, the invention provides for a method of operation whereby the temperature of the sample is controlled such that the operator of the sample introduction system can choose which temperature is applied to the sample, and the rate at which the temperature changes as a function of time, known as the "temperature profile." By operating the sample introduction system in a manner such that the temperature of the sample follows a temperature profile chosen by the operator, the chemicals with different boiling points wilt be desorbed from the sample at different times. This method of operation provides an advantage over prior art by allowing chemicals with different boiling points to be analyzed in the mass analyzer substantially independently.
Description of Prior Art It is known in the prior art that the use of a reduced pressure vacuum environment can be provided to desorb a chemical sample into a chemical analyzer. An embodiment is taught by Yasuhiro in JP11287743 which describes a vacuum tank coupled to a mass analyzer, wherein the vacuum tank is a hotplate that heats a sample attracted electrostatically to the surface of the hotplate in order to desorb an analyte from the surface for analysis by a chemical analyzer. With respect to the invention described here, Yasuhiro does not teach the use of an external heat source, specifically an optical heat source, transferred into the vacuum tank but rather relies on a hotplate contained within the vacuum tank. One skilled in the art, when reducing the teaching of Yasuhiro to practice, would be prevented from controlling substantially only the temperature of the sample, which can cause temperature variations throughout the volume of the sample, requires more power to operate the heater, and may lead to a plurality of chemicals being desorbed from the sample which may be convoluted by the chemical analyzer. Further, Yasuhiro does not teach the use of a conduit between the vacuum tank and the chemical analyzer. One skilled in the art, when reducing the teaching of Yasuhiro to practice, would be unable to control the pressure in the vacuum tank separately from the pressure in the mass analyzer. Further to the limitation of Yasuhiro's teaching on pressure, the embodiment does not provide for a separate apparatus to reduce the pressure in the vacuum tank to a desired pressure. When applied to the invention described here, the practitioner would be unable to control the pressure in the sample chamber in order to cause the boiling point of chemicals within the sample to be reduced to a desirable temperature.
Mullock, in US 2005/0109932 Al, teaches the use of a sorbent trap to collect analyte from an air sample; where the pressure in the body of the trap is reduced to a pressure that is lower than atmospheric pressure prior to activating a heater to desorb the collected analyte into a mass spectrometer. In contrast, the invention described here does not require the use of a trap to collect analyte prior to desorbing the analyte into the chemical analyzer. Further, Mullock does not teach the method of reducing the pressure in the trap body in a controlled manner to modify the chemical properties of an analyte or plurality of analytes, such as the boiling point, to a desired level.
Similar to Mullock, Rafferty in CA 2,824,525 teaches an apparatus and method of operating an apparatus to thermally desorb a sample from a sample collector into a mass spectrometer. In one of the embodiments taught, an infrared source is provided to heat the sample collector in order to desorb analytes into a vapour phase. With respect to the invention described here, Rafferty et. al.
does not teach the use of an optical source and a light pipe that is in optical communication with the sample chamber. A practitioner implementing the embodiment disclosed by Rafferty et. al. would not realize the benefit of heating substantially only the sample.
In regards to the apparatus and method for heating a sample, Kashima et. al.
U52004/0124352 Al teaches an embodiment of an apparatus for desorbing a sample by applying heat with an optical source in the infrared wavelength range, that is contained within an atmospheric pressure ion source.
With respect to the invention described here, the embodiment of Kashima et.
al. does not provide for an apparatus or method to reduce the pressure in the atmospheric pressure ion source prior to activating the infrared source. Further, Kashima et. al. requires that analytes be collected on a clean wiping member and does not provide for a means to introduce a sample without such a collector.
Further, with respect to the invention described here, Kashima et. al. teaches a method of heating the sample as quickly as possible to achieve a high concentration of analyte to be introduced to the mass spectrometer. In contrast, the invention described here allows for heat to be applied in a controlled manner, that when coupled with the controlled pressure reduction of the sample chamber, allows a practitioner to release chemicals from a sample in a desired manner.
Whitehouse et. al., in CA 2,837,478, teaches the use of an optical source in an atmospheric pressure ion source that includes means to sense the type, size, physical features and position of each sample introduced. Whitehouse et. al. does not teach the use of said means to measure the mass of a sample during the operation of the apparatus. Further, Whitehouse et. al. does not teach the method of operation where the optical source is used to heat the sample but rather limits the use of the optical source to ionizing the chemical species released from the sample holder. With respect to the invention disclosed here, a practitioner implementing the embodiment of Whitehouse et. al. would not have the means to extract information from the sample concerning the amount of concentration of analytes in the sample. Further, Whitehouse et. al. does not teach an embodiment of an apparatus or method to heat the sample.
References Cited:
1. Yasuhiro; JP 11,287,743; Thermal Desorbing/Analyzing Chamber for Wafer Process Monitor
2. Mullock et. al.; US 2005/0109932A1; Gas Concentration
3. Rafferty et. al.; CA 2,824,525; Evacuating a Sample Chamber
4. Kashima et. al.; US 2004/0124352 Al; Method and Apparatus for Detecting Dangerous Substance
5. Whitehouse et. al.; CA 2,837,478; Direct Sample Analysis Ion Source References Considered but not Cited:
1. Hughley et. al.; US 6,707,035 B2; Sample introduction interface for analytical processing of a sample placed on a substrate 2. Ishikawa et. al.; US 2006/0226358 Al; Detection method and detection device of special drugs 3. Muneishi et. al.; US 2009/0293647 Al; Sample Holder, Sample Suction Device Using the Same, and Sample Processing Method 4. Luke et. al.; CA 2503807; Desorber 5. Wu; US 2011/0283776 Al; Chemical sampling and multi-function detection methods and apparatus
1. Hughley et. al.; US 6,707,035 B2; Sample introduction interface for analytical processing of a sample placed on a substrate 2. Ishikawa et. al.; US 2006/0226358 Al; Detection method and detection device of special drugs 3. Muneishi et. al.; US 2009/0293647 Al; Sample Holder, Sample Suction Device Using the Same, and Sample Processing Method 4. Luke et. al.; CA 2503807; Desorber 5. Wu; US 2011/0283776 Al; Chemical sampling and multi-function detection methods and apparatus
6. Tovena-Pecault; US 8,291,777 B2; Devices for sampling and confining chemical contaminations, associated transport device and application to the transport of chemical samples to a chemical analysis unit
7. Chutjian; US 5,256,874; Gridded electron reversal ionizer
8. Wade et. al.; NZ 537,372; Sample extraction system
9. Jewett et. al.; Exhaust gas analyzer having pressure and temperature compensation; US
3,958,122
3,958,122
10. Nelson et. al.; US 4,663,961; System for remote chemical analysis
11. Ward et. al.; US 7,554,096 B2; Ion sources, systems and methods
12. Ward et. al.; US 7,557,359 B2; Ion sources, systems and methods Brief Description of the Drawings Figure 1 is a plot of the desorption temperature of Linalool as a function of applied pressure.
Figure 2 is an exemplar embodiment of the invention.
Figure 3 is an exemplar of an embodiment of the invention using an optical source to heat the sample.
Figure 4 is an exemplar embodiment of the invention that provides for a first reflective surface and a second absorptive surface.
Figure 5 is an exemplar embodiment of the invention that provides for a capillary between the sample chamber and the mass analyzer.
Figure 6 is an exemplar embodiment of the invention that provides for a capillary between the sample chamber and the mass analyzer, wherein the capillary is configured to operate as a chromatographic column.
Summary of the Invention The invention pertains to a sample introduction system apparatus that is configured to release, by transforming the chemical from a solid or a liquid phase into a vapour phase, at least one chemical from a sample, which may be comprised of at least a biological organism, a manufactured pharmaceutical, or a naturally occurring matrix. The invention also provides for a means of operating the sample introduction apparatus to cause the temperature of the sample to be raised to a temperature above the ambient temperature while minimizing the increase in the temperature of the apparatus or the components that comprise the apparatus. Further, the operation of the apparatus provides for a means to reduce the pressure of the ambient environment within the sample chamber in order to transform the chemical in the sample into a vapour phase at a temperature that is lower than the boiling point of the sample at standard atmospheric pressure. The configuration of the invention is chosen to provide a means to introduce the sample directly into the chamber of the sample introduction system without the need to collected the sample on coupon, swab, or other such matrix that are known to those skilled in the art.
The relationship between the temperature at which a material is transformed from a liquid or solid phase into the vapour phase and the pressure at which the transformation takes place is known to those skilled in the art at the Clausius-Clapeyron Relation, and is typically presented in the form:
(¨P1) AH ( 1 1) In where:
Pi is a pressure at one state, P2 is a pressure at a state different from Pi, Ti is the boiling point of the materials at the pressure Pi, Ti is the boiling point of the material at the pressure P2, is the latent heat of vaporization of the material, and R is the Universal Gas Constant.
An exemplar plot of the desorption temperature as a function of the ambient pressure is shown in .. Figure 1 for Linalool (Molecular formula: C10H180, CAS Registry Number: 78-70-6), a common chemical found in cannabis samples that contributes to the taste and smell of the sample. Linalool has a boiling point of 198.8 C when held at standard atmosphere (760 Torr) and latest heat of vaporization of 65 kJIkmol. Using this information, and with knowledge of the Clausius-Clepeyron Relation, those skilled in the art would recognize that the desorption temperature is a function of temperature according to:
Applied Desorption Pressure Temperature (Torr) ( C) 1E-05 -47.8 1E-04 -31.8 1E-03 -13.4 1E-02 8.11 1E-01 33.5 1E+00 63.9 1E+01 101.0 1E+02 147.4 1E+03 206.7 Examination of this information and with respect to Figure 1, those skilled in the art would recognize that Linalool, a chemical that boils at 198.8 C when at standard pressure (760 Torr) will boil at a temperature substantially equal to 100 C when the pressure is reduced to 10 Torr. It is also recognized that this choice of chemical, its chemical properties, pressures, and temperatures are exemplars only and those skilled in the art would recognize that other chemicals, temperatures, and pressures could be operated upon using substantially the same analysis without changing the scope of this invention.
In one embodiment of the invention, and with respect to Figure 2, a sample chamber (2) is provided that is substantially airtight and includes a plurality of ports: a sample introduction port (2) that is in fluid communication with the sample chamber through an orifice or conduit (3), a port that is in fluid communication with a mass analyzer or chemical detector (4) through a conduit (5), and a port that is in fluid communication with an apparatus (6) through a conduit (7) for reducing the pressure in the sample chamber. Fluid communication between the sample chamber and one or more of the conduits may be controlled or substantially eliminated by providing chokes or valves (6, 7.5, and 8).
A fixture (9) is provided to place the sample (10) in the sample chamber. The fixture includes an apparatus (11) to measure the mass of the sample and communicate the mass information through an electrical path (12). Further, an apparatus (13) to provide thermal energy to the sample (10) is provided.
It would be recognized by those skilled in the art that conduits (3), (5), and (7) may be comprised of a capillary, channel, tube, pipe, or other such apparatus for fluid communication without altering the scope of this invention. It would also be recognized by those skilled in the art that the apparatus (6) for reducing the pressure in the chamber (1) may be comprised of a pump, a turbo pump, a getter pump, or a combination of pumps without altering the scope of this invention.
Further, those skilled .. in the art would recognize that the chemical detector (4) may consist of a mass spectrometer, a Raman spectrometer, an ion mobility spectrometer, or other type of apparatus to measure the nature of chemicals in a sample without altering the scope of this invention.
Finally, those skilled in the art would recognize that the heat source (13) may be comprised of a Joule heater, a Peltier heater, an infrared heater, or other apparatus that generates heat in the sample (10) in the proximity of the .. sample.
J
In another embodiment of the invention, and with respect to Figure 3, the heat source (13) is replaced by an optical lamp (14) that is placed outside of the sample chamber (1). The optical source (14) is in optical communication with the sample (10) through a light guide (15). The optical source (14) is chosen to provide emitted light at a wavelength that causes the temperature of sample (10) to be increased. Examples of optical sources include infrared (IR), near-infrared (NIR), ultraviolet (UV), and ultraviolet-visible (UV-VIS). Those skilled in the art would recognize that other varieties of optical sources may be provided without changing the scope of this invention. Examples of the light guide (15) include optical fibres, glass rods, lens(es), or light pipes.
Those skilled in the art would recognize that a light guide (15) made of an appropriate material such as quartz, silica, or acrylic would provide a sufficient quantity of light to be guided into the sample chamber with minimal losses. Further, the light guide (15) is configured to focus substantially all of the light on the sample (10) by choosing an appropriate divergence angle, a, (16) of the light emitted from the guide.
In a further embodiment of the invention, and with respect to Figure 4, the sample chamber (1) .. contains an inner surface that is comprised of a least two properties. A
first surface (17) that is located substantially on the opposite side of the sample chamber (1) is configured to reflect light emitted from the light guide (15) at wavelength, or wavelengths, substantially similar that emitted by the light source (14). A second surface (18) that is located substantially opposite to the first surface is configured to absorb light emitted from the light guide (15) at wavelength, or .. wavelengths, substantially similar that emitted by the light source (14).
The configuration of the light guide (15), first reflective surface (17), and second absorptive surface (18) may be chosen such that the path of light (19) emitted from light guide (14) is reflected (20) by the first surface (17) and is absorbed by the second surface (18).
In a further embodiment of the invention, and with respect to Figure 5, the sample chamber (1) is in fluid communication with the chemical analyzer (4) through a capillary (21) where the length of the capillary (22) is substantially longer than the inner diameter of the capillary (23). Further to the embodiment in Figure 5, Figure 6 provides an embodiment where the capillary column (21) is sufficiently long to be configured to operate as a chromatographic column. An exemplar embodiment is to provide a capillary 5 in in length with an inner diameter of 100 pm. Those skilled in the art would recognize that other lengths and inner diameters of columns may be chosen without altering the scope of the invention disclosed here. Addition, this embodiment provides for a =
capillary temperature control (24) apparatus that is configured to operate substantially the entire column at a desired temperature.
Figure 12 describes a further embodiment of the invention described here. In this embodiment, optical source (13) is chosen such that it emits a wavelength or plurality of wavelengths to provide thermal energy to heat the sample, 10, as well as ionization energy to cause chemicals released from the sample, 10, to be ionized with an electrical charge. The method of causing ionization with an optical means is well described in the literature and is commonly known to those skilled in the art as photoionization. Ion optical apparatus are provided and configured to focus, apparatus 5.4, and guide, apparatus 5.5, ions substantially into the mass analyzer, 4. The ion optical apparatus may include, but are not limited to, one of a combination of Einzel lenses, octopoles, hexapoles, quadrupoles, orifices, or skimmers.
Figure 14 provides for a further embodiment wherein a plurality of optical sources, apparatus 14 and apparatus 14.5, each of which may be comprised Of a plurality of optical sources, are provided.
Optical source, 14 is configured to provide optical energy to desorb chemicals from sample, 10;
optical source 14.5 is configured to provide optical energy to cause ionization of the chemical substantially at the exit of fluid conduit, 21, which may be comprised of apparatus described in preceding embodiments of the invention described here.
A further embodiment to cause ionization of the chemicals released from the sample, 10, is provided in Figure 13. In the embodiment described here, optical source, 14, is comprised of a plurality of optical sources that are configured to provide optical energy at a plurality of wavelengths to cause heating of the sample, 10, and ionization of the desorbed chemicals. Light guide, 15, is comprised of a plurality of guides configured to transfer optical energy from the plurality of optical sources into the sample chamber, 1.
A method of operating the invention disclosed herein is provided, and with respect to Figure 7, where a sample contains at least one of a chemical whose properties include a boiling point, Ti, and a pressure Pi, is placed in the sample chamber (1) of Figures 2 ¨ 6. It is desired to desorb at least one chemical from the sample at a temperature less than 7'1. In this exemplar method, the pressure in the sample chamber (1) is reduced by pump (6) of Figures 1 ¨2 by removing ambient vapours, such as but not limited to, air present in the interior of sample chamber (1) via conduit (7), to a pressure, P2, where the boiling point of the chemical or chemicals desired to be released is reduced to a temperature, T2, less than temperature, Ti. Heating apparatus (13) is activated to raise the temperature of the sample (10) to at least the temperature Ti causing the chemical or chemicals to be desorbed from the sample (10). The chemical desorbed from the sample (10) is transferred to the mass analyzer (4) through conduit (5) for analysis. Those skilled in the art would recognize that the mass analyzer (4) may be operated to reveal desirable information about the chemical or chemicals released such as, but not limited to, their mass spectrum, optical desorption spectrum, or mobility.
A further method of operating the invention described herein involves a sample (10) that contains at least two chemicals that are desired to be analyzed and, with respect to Figure 8, that the chemicals possess chemical properties where the nature of the relationship between desorption temperature and pressure is different from one another. The first chemical, Chemical A, possesses chemical properties such that the boiling point at a pressure, Pi, is given by temperature Ti; and a second chemical, Chemical B, possesses chemical properties such the boiling point at a pressure, Pi, is given by a temperature that is different from temperature Ti. Further, Chemical A, possesses chemical properties such that the boiling point at a pressure, P2, is given by temperature T2; and a second chemical, Chemical B, possesses chemical properties such the boiling point at a pressure, P2, is given by a temperature T2'. In the mode of operation provided here, and with respect to Figure 9a, a pressure in sample chamber (10) is first reduced to a pressure P2 from pressure Pi at a time to.
After the desired pressure, P2, is achieved, the temperature is increased to a temperature, Ti, from temperature To at a time ti as demonstrated in Figure 9b. Temperature Ti is chosen to desorb chemical A, the evolution of which is monitored on mass analyzer (4) as demonstrated in Figure 9c.
At a later time, t2, the temperature of the sample (10) is increased to a temperature Ti which is greater than temperature T2 and corresponds to the temperature at which Chemical B is desorbed at pressure P2.
A method of operation involving chemicals that desorb at substantially the same temperature, and utilizes the long capillary column disclosed in the configuration of Figure 6, is provided. A first chemical, Chemical A, possesses chemical properties such that the boiling point at a pressure, P2, is given by temperature T2; and a second chemical, Chemical A', possesses chemical properties such that the boiling point at a pressure, P2, is given by a temperature substantially equal to Ti. In the mode of operation provided here, and with respect to Figure 10a, a pressure in sample chamber (10) is first reduced to a pressure P2 from pressure Pi at a time to. After the desired pressure, P2, is achieved, the temperature is increased to a temperature, T2, from temperature To at a time ti as demonstrated in Figure 9b. Temperature T2 is chosen to desorb both Chemical A
and Chemical B.
The temperature of the capillary is then increased from a temperature Tc,/ to a temperature Tc,2', which may be linear, as provided in Figure 10c, or according to a temperature profile that is known to those skilled in the art. It is also recognized that more than two chemicals may be desorbed and separated in the capillary (21) at each temperature applied to the sample (10), a plurality of sample temperatures may be also be employed, which each temperature desorbing a plurality of chemicals, and that a plurality of chemicals may be separated by the capillary (21).
A method of operation is provided for embodiments that include an optical source for causing ionization of the chemicals desorbed from sample, 10. In these embodiments, examples of which are provided in Figure 12, Figure 13, and Figure 14, the optical source(s) to provide for ionization of the desorbed chemicals is operated in conjunction with the optical source(s) provided for desorption of the chemicals from the sample, 10. Signals are applied to the ion optical apparatus, examples of which are provided by apparatus 5.4 and 5.5 in Figure 12 and Figure 13 according to methods that are known to those skilled in the art.
Figure 2 is an exemplar embodiment of the invention.
Figure 3 is an exemplar of an embodiment of the invention using an optical source to heat the sample.
Figure 4 is an exemplar embodiment of the invention that provides for a first reflective surface and a second absorptive surface.
Figure 5 is an exemplar embodiment of the invention that provides for a capillary between the sample chamber and the mass analyzer.
Figure 6 is an exemplar embodiment of the invention that provides for a capillary between the sample chamber and the mass analyzer, wherein the capillary is configured to operate as a chromatographic column.
Summary of the Invention The invention pertains to a sample introduction system apparatus that is configured to release, by transforming the chemical from a solid or a liquid phase into a vapour phase, at least one chemical from a sample, which may be comprised of at least a biological organism, a manufactured pharmaceutical, or a naturally occurring matrix. The invention also provides for a means of operating the sample introduction apparatus to cause the temperature of the sample to be raised to a temperature above the ambient temperature while minimizing the increase in the temperature of the apparatus or the components that comprise the apparatus. Further, the operation of the apparatus provides for a means to reduce the pressure of the ambient environment within the sample chamber in order to transform the chemical in the sample into a vapour phase at a temperature that is lower than the boiling point of the sample at standard atmospheric pressure. The configuration of the invention is chosen to provide a means to introduce the sample directly into the chamber of the sample introduction system without the need to collected the sample on coupon, swab, or other such matrix that are known to those skilled in the art.
The relationship between the temperature at which a material is transformed from a liquid or solid phase into the vapour phase and the pressure at which the transformation takes place is known to those skilled in the art at the Clausius-Clapeyron Relation, and is typically presented in the form:
(¨P1) AH ( 1 1) In where:
Pi is a pressure at one state, P2 is a pressure at a state different from Pi, Ti is the boiling point of the materials at the pressure Pi, Ti is the boiling point of the material at the pressure P2, is the latent heat of vaporization of the material, and R is the Universal Gas Constant.
An exemplar plot of the desorption temperature as a function of the ambient pressure is shown in .. Figure 1 for Linalool (Molecular formula: C10H180, CAS Registry Number: 78-70-6), a common chemical found in cannabis samples that contributes to the taste and smell of the sample. Linalool has a boiling point of 198.8 C when held at standard atmosphere (760 Torr) and latest heat of vaporization of 65 kJIkmol. Using this information, and with knowledge of the Clausius-Clepeyron Relation, those skilled in the art would recognize that the desorption temperature is a function of temperature according to:
Applied Desorption Pressure Temperature (Torr) ( C) 1E-05 -47.8 1E-04 -31.8 1E-03 -13.4 1E-02 8.11 1E-01 33.5 1E+00 63.9 1E+01 101.0 1E+02 147.4 1E+03 206.7 Examination of this information and with respect to Figure 1, those skilled in the art would recognize that Linalool, a chemical that boils at 198.8 C when at standard pressure (760 Torr) will boil at a temperature substantially equal to 100 C when the pressure is reduced to 10 Torr. It is also recognized that this choice of chemical, its chemical properties, pressures, and temperatures are exemplars only and those skilled in the art would recognize that other chemicals, temperatures, and pressures could be operated upon using substantially the same analysis without changing the scope of this invention.
In one embodiment of the invention, and with respect to Figure 2, a sample chamber (2) is provided that is substantially airtight and includes a plurality of ports: a sample introduction port (2) that is in fluid communication with the sample chamber through an orifice or conduit (3), a port that is in fluid communication with a mass analyzer or chemical detector (4) through a conduit (5), and a port that is in fluid communication with an apparatus (6) through a conduit (7) for reducing the pressure in the sample chamber. Fluid communication between the sample chamber and one or more of the conduits may be controlled or substantially eliminated by providing chokes or valves (6, 7.5, and 8).
A fixture (9) is provided to place the sample (10) in the sample chamber. The fixture includes an apparatus (11) to measure the mass of the sample and communicate the mass information through an electrical path (12). Further, an apparatus (13) to provide thermal energy to the sample (10) is provided.
It would be recognized by those skilled in the art that conduits (3), (5), and (7) may be comprised of a capillary, channel, tube, pipe, or other such apparatus for fluid communication without altering the scope of this invention. It would also be recognized by those skilled in the art that the apparatus (6) for reducing the pressure in the chamber (1) may be comprised of a pump, a turbo pump, a getter pump, or a combination of pumps without altering the scope of this invention.
Further, those skilled .. in the art would recognize that the chemical detector (4) may consist of a mass spectrometer, a Raman spectrometer, an ion mobility spectrometer, or other type of apparatus to measure the nature of chemicals in a sample without altering the scope of this invention.
Finally, those skilled in the art would recognize that the heat source (13) may be comprised of a Joule heater, a Peltier heater, an infrared heater, or other apparatus that generates heat in the sample (10) in the proximity of the .. sample.
J
In another embodiment of the invention, and with respect to Figure 3, the heat source (13) is replaced by an optical lamp (14) that is placed outside of the sample chamber (1). The optical source (14) is in optical communication with the sample (10) through a light guide (15). The optical source (14) is chosen to provide emitted light at a wavelength that causes the temperature of sample (10) to be increased. Examples of optical sources include infrared (IR), near-infrared (NIR), ultraviolet (UV), and ultraviolet-visible (UV-VIS). Those skilled in the art would recognize that other varieties of optical sources may be provided without changing the scope of this invention. Examples of the light guide (15) include optical fibres, glass rods, lens(es), or light pipes.
Those skilled in the art would recognize that a light guide (15) made of an appropriate material such as quartz, silica, or acrylic would provide a sufficient quantity of light to be guided into the sample chamber with minimal losses. Further, the light guide (15) is configured to focus substantially all of the light on the sample (10) by choosing an appropriate divergence angle, a, (16) of the light emitted from the guide.
In a further embodiment of the invention, and with respect to Figure 4, the sample chamber (1) .. contains an inner surface that is comprised of a least two properties. A
first surface (17) that is located substantially on the opposite side of the sample chamber (1) is configured to reflect light emitted from the light guide (15) at wavelength, or wavelengths, substantially similar that emitted by the light source (14). A second surface (18) that is located substantially opposite to the first surface is configured to absorb light emitted from the light guide (15) at wavelength, or .. wavelengths, substantially similar that emitted by the light source (14).
The configuration of the light guide (15), first reflective surface (17), and second absorptive surface (18) may be chosen such that the path of light (19) emitted from light guide (14) is reflected (20) by the first surface (17) and is absorbed by the second surface (18).
In a further embodiment of the invention, and with respect to Figure 5, the sample chamber (1) is in fluid communication with the chemical analyzer (4) through a capillary (21) where the length of the capillary (22) is substantially longer than the inner diameter of the capillary (23). Further to the embodiment in Figure 5, Figure 6 provides an embodiment where the capillary column (21) is sufficiently long to be configured to operate as a chromatographic column. An exemplar embodiment is to provide a capillary 5 in in length with an inner diameter of 100 pm. Those skilled in the art would recognize that other lengths and inner diameters of columns may be chosen without altering the scope of the invention disclosed here. Addition, this embodiment provides for a =
capillary temperature control (24) apparatus that is configured to operate substantially the entire column at a desired temperature.
Figure 12 describes a further embodiment of the invention described here. In this embodiment, optical source (13) is chosen such that it emits a wavelength or plurality of wavelengths to provide thermal energy to heat the sample, 10, as well as ionization energy to cause chemicals released from the sample, 10, to be ionized with an electrical charge. The method of causing ionization with an optical means is well described in the literature and is commonly known to those skilled in the art as photoionization. Ion optical apparatus are provided and configured to focus, apparatus 5.4, and guide, apparatus 5.5, ions substantially into the mass analyzer, 4. The ion optical apparatus may include, but are not limited to, one of a combination of Einzel lenses, octopoles, hexapoles, quadrupoles, orifices, or skimmers.
Figure 14 provides for a further embodiment wherein a plurality of optical sources, apparatus 14 and apparatus 14.5, each of which may be comprised Of a plurality of optical sources, are provided.
Optical source, 14 is configured to provide optical energy to desorb chemicals from sample, 10;
optical source 14.5 is configured to provide optical energy to cause ionization of the chemical substantially at the exit of fluid conduit, 21, which may be comprised of apparatus described in preceding embodiments of the invention described here.
A further embodiment to cause ionization of the chemicals released from the sample, 10, is provided in Figure 13. In the embodiment described here, optical source, 14, is comprised of a plurality of optical sources that are configured to provide optical energy at a plurality of wavelengths to cause heating of the sample, 10, and ionization of the desorbed chemicals. Light guide, 15, is comprised of a plurality of guides configured to transfer optical energy from the plurality of optical sources into the sample chamber, 1.
A method of operating the invention disclosed herein is provided, and with respect to Figure 7, where a sample contains at least one of a chemical whose properties include a boiling point, Ti, and a pressure Pi, is placed in the sample chamber (1) of Figures 2 ¨ 6. It is desired to desorb at least one chemical from the sample at a temperature less than 7'1. In this exemplar method, the pressure in the sample chamber (1) is reduced by pump (6) of Figures 1 ¨2 by removing ambient vapours, such as but not limited to, air present in the interior of sample chamber (1) via conduit (7), to a pressure, P2, where the boiling point of the chemical or chemicals desired to be released is reduced to a temperature, T2, less than temperature, Ti. Heating apparatus (13) is activated to raise the temperature of the sample (10) to at least the temperature Ti causing the chemical or chemicals to be desorbed from the sample (10). The chemical desorbed from the sample (10) is transferred to the mass analyzer (4) through conduit (5) for analysis. Those skilled in the art would recognize that the mass analyzer (4) may be operated to reveal desirable information about the chemical or chemicals released such as, but not limited to, their mass spectrum, optical desorption spectrum, or mobility.
A further method of operating the invention described herein involves a sample (10) that contains at least two chemicals that are desired to be analyzed and, with respect to Figure 8, that the chemicals possess chemical properties where the nature of the relationship between desorption temperature and pressure is different from one another. The first chemical, Chemical A, possesses chemical properties such that the boiling point at a pressure, Pi, is given by temperature Ti; and a second chemical, Chemical B, possesses chemical properties such the boiling point at a pressure, Pi, is given by a temperature that is different from temperature Ti. Further, Chemical A, possesses chemical properties such that the boiling point at a pressure, P2, is given by temperature T2; and a second chemical, Chemical B, possesses chemical properties such the boiling point at a pressure, P2, is given by a temperature T2'. In the mode of operation provided here, and with respect to Figure 9a, a pressure in sample chamber (10) is first reduced to a pressure P2 from pressure Pi at a time to.
After the desired pressure, P2, is achieved, the temperature is increased to a temperature, Ti, from temperature To at a time ti as demonstrated in Figure 9b. Temperature Ti is chosen to desorb chemical A, the evolution of which is monitored on mass analyzer (4) as demonstrated in Figure 9c.
At a later time, t2, the temperature of the sample (10) is increased to a temperature Ti which is greater than temperature T2 and corresponds to the temperature at which Chemical B is desorbed at pressure P2.
A method of operation involving chemicals that desorb at substantially the same temperature, and utilizes the long capillary column disclosed in the configuration of Figure 6, is provided. A first chemical, Chemical A, possesses chemical properties such that the boiling point at a pressure, P2, is given by temperature T2; and a second chemical, Chemical A', possesses chemical properties such that the boiling point at a pressure, P2, is given by a temperature substantially equal to Ti. In the mode of operation provided here, and with respect to Figure 10a, a pressure in sample chamber (10) is first reduced to a pressure P2 from pressure Pi at a time to. After the desired pressure, P2, is achieved, the temperature is increased to a temperature, T2, from temperature To at a time ti as demonstrated in Figure 9b. Temperature T2 is chosen to desorb both Chemical A
and Chemical B.
The temperature of the capillary is then increased from a temperature Tc,/ to a temperature Tc,2', which may be linear, as provided in Figure 10c, or according to a temperature profile that is known to those skilled in the art. It is also recognized that more than two chemicals may be desorbed and separated in the capillary (21) at each temperature applied to the sample (10), a plurality of sample temperatures may be also be employed, which each temperature desorbing a plurality of chemicals, and that a plurality of chemicals may be separated by the capillary (21).
A method of operation is provided for embodiments that include an optical source for causing ionization of the chemicals desorbed from sample, 10. In these embodiments, examples of which are provided in Figure 12, Figure 13, and Figure 14, the optical source(s) to provide for ionization of the desorbed chemicals is operated in conjunction with the optical source(s) provided for desorption of the chemicals from the sample, 10. Signals are applied to the ion optical apparatus, examples of which are provided by apparatus 5.4 and 5.5 in Figure 12 and Figure 13 according to methods that are known to those skilled in the art.
Claims (21)
1. A sample introduction system for introducing a chemical into an chemical analysis component in an instrument that is comprised of a sample chamber capable of operating at a plurality of pressures, and includes a means to control the temperature of the sample.
2. The apparatus of claim 1 where the sample is comprised of a biological sample.
3. The apparatus of claim 1 where the sample is comprised of a pharmaceutical sample.
4. The apparatus of claim 1 where the sample is comprised of a plurality of a biological and a pharmaceutical sample.
5. The apparatus of claim 1 where the temperature of the sample is controlled using an optical light guide and light source.
6. The apparatus of claim 5 where the light source emits light at a wavelength that is capable of increasing the temperature of a sample.
7. The apparatus of claim 6 where the sample chamber contains a first surface that is configured to reflect light at the wavelength of the light source.
8. The apparatus of claim 7 where the sample contains a second surface that configured to absorb light at the wavelength of the light source.
9. The apparatus of claim 1 wherein a plurality of chemicals are released into the chemical analysis instrument.
10. The apparatus of claim 1 where the sample chamber is in fluid communication with the chemical analysis component through a capillary.
11. The apparatus of claim 10 where the sample introduction system includes a means to heat the capillary.
12. The apparatus of claim 11 where the capillary is sufficiently long to narrow to operate as a chromatographic column.
13. The apparatus of claim 1 that contains a plurality of means to control or choke the flow of fluid in our out of the sample chamber.
14. The apparatus of claim 1 that contains an optical source, or plurality of optical sources, to cause ionization of chemicals.
15. The apparatus of claim 14 that contains one or more ion optical apparatus.
16. A method of operating a sample introduction system for introducing a chemical into an chemical analysis component in an instrument that is comprised of a sample chamber capable of operating at a plurality of pressures, and includes a means to control the temperature of the sample, where the sample chamber is operated at a plurality of pressures.
17. The method of claim 16 where the sample introduction system is operated at a first pressure and at a second pressure that is different from the first pressure.
18. The method of claim 17 where the second pressure is chosen to allow at least one chemical from the sample to be desorbed at a temperature that is less than the boiling point of the chemical at standard pressure.
19. The method of claim 18 where a plurality of temperatures of the sample is chosen and applied to desorb a plurality of chemicals from the sample.
20. The method of claim 18 where a temperature profile is applied to a capillary to temporally separate a plurality of chemicals desorbed from the sample at substantially equal sample temperatures.
21. The method of claim 18 where signals are applied to ion optical components to transfer ionized chemical species along a path defined by the ion optical components.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA3023926A CA3023926A1 (en) | 2018-11-13 | 2018-11-13 | Apparatus and method of operation of a sample introduction system to a chemical analyzer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA3023926A CA3023926A1 (en) | 2018-11-13 | 2018-11-13 | Apparatus and method of operation of a sample introduction system to a chemical analyzer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA3023926A1 true CA3023926A1 (en) | 2020-05-13 |
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ID=70728559
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA3023926A Abandoned CA3023926A1 (en) | 2018-11-13 | 2018-11-13 | Apparatus and method of operation of a sample introduction system to a chemical analyzer |
Country Status (1)
| Country | Link |
|---|---|
| CA (1) | CA3023926A1 (en) |
-
2018
- 2018-11-13 CA CA3023926A patent/CA3023926A1/en not_active Abandoned
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