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CN-122000268-A - Dirty carbon collaborative monitoring mass spectrum ionization device and method

CN122000268ACN 122000268 ACN122000268 ACN 122000268ACN-122000268-A

Abstract

The invention relates to the technical field of mass spectrometers, in particular to a device and a method for cooperatively monitoring mass spectrum ionization by using waste carbon. The device comprises a high-pressure photo-induced chemical ionization cavity and a low-pressure photoelectron ionization cavity, wherein an ion transmission module and an ion converging reaction electrode group are arranged in the high-pressure photo-induced chemical ionization cavity, organic product ions are generated in the high-pressure photo-induced chemical ionization cavity and transmitted into the low-pressure photoelectron ionization cavity through a differential electrode, an electron transmission module, an ion converging multipole rod group and an ion extraction electrode are arranged in the low-pressure photoelectron ionization cavity, and inorganic product ions and organic product ions are generated in the low-pressure photoelectron ionization cavity and transmitted to a mass analyzer through the ion extraction electrode for detection. According to the invention, the cascade connection of the ion sources under two different working pressures is realized through vacuum difference, so that the ionization detection of the two ionization sources can be obtained by single sample injection of a sample, the analysis coverage of a mass spectrometer instrument is greatly improved, and the application field is widened.

Inventors

  • JIANG JICHUN
  • HUA LEI
  • REN MEIHUI
  • FAN ZHIGANG
  • YANG MING
  • LI HAIYANG

Assignees

  • 中国科学院大连化学物理研究所

Dates

Publication Date
20260508
Application Date
20241105

Claims (10)

  1. 1. The device is characterized by comprising a high-pressure photo-chemical ionization cavity (14) and a low-pressure photoelectron ionization cavity (11), which are all operated under vacuum and realize vacuum difference through a flat differential electrode (5) with a hole in the middle; The ion converging reaction electrode group (4) is used for carrying out chemical reaction ionization on the ions and trace organic compound components in sample gas molecules to generate organic product ions, and the organic product ions pass through the differential electrode (5) to be transmitted into the low-pressure photoelectron ionization cavity (11); The low-pressure photoelectron ionization chamber (11) is internally provided with an electron transmission module, an ion convergence multipole rod group (8) and an ion extraction electrode (10) in sequence, wherein the electron transmission module is used for generating photoelectrons and generating inorganic product ions by collision of the photoelectrons with inorganic components in gas molecules of a sample, the ion convergence multipole rod group (8) is used for transmitting the inorganic product ions and the organic product ions through a central hole of the ion extraction electrode (10) to a mass analyzer (9) for detection, and vacuum difference is realized between the low-pressure photoelectron ionization chamber (11) and the mass analyzer (9) through the ion extraction electrode (10).
  2. 2. The device for the collaborative monitoring of mass spectrum ionization of carbon pollutants according to claim 1, wherein the ion transmission module comprises a first vacuum ultraviolet light source (1), an axial ion extraction electrode (2) and an axial electron extraction electrode (3) which are sequentially arranged at intervals along a light path, wherein a reagent gas sample injection pipeline (16) is led in between the first vacuum ultraviolet light source (1) and the axial ion extraction electrode (2), a sample gas sample injection pipeline (15) is led in between the axial electron extraction electrode (3) and the ion convergence reaction electrode group (4), the first vacuum ultraviolet light source (1) is used for generating photons to carry out direct photoionization or photoelectron ionization on the reagent gas, and generated ions are led out into the ion convergence reaction electrode group (4) under the action of the axial ion extraction electrode (2) and the axial electron extraction electrode (3).
  3. 3. The carbon-contaminated co-monitoring mass spectrum ionization device according to claim 2, wherein the axial ion extraction electrode (2) and the axial electron extraction electrode (3) are both flat plate structures with through holes in the center, and the center holes are coaxial; The ion convergence reaction electrode group (4) comprises more than two convergence electrodes (13) which are parallel and are arranged at intervals, the convergence electrodes (13) are of a flat plate structure with through holes at the center, and the central holes among the convergence electrodes are coaxial.
  4. 4. A carbon-contaminated co-monitoring mass spectrum ionization device according to claim 3, wherein the ion convergence reaction electrode group (4) is a uniform electrostatic field ion convergence reaction region composed of the same plurality of convergence electrodes (13), or the ion convergence reaction electrode group (4) is an electrostatic field or radio frequency field ion convergence reaction region composed of a plurality of convergence electrodes (13) whose inner diameters are sequentially reduced.
  5. 5. The carbon-contaminated co-monitoring mass spectrum ionization device according to claim 2, wherein the inner diameters of the reagent gas sample introduction pipeline (16) and the sample gas sample introduction pipeline (15) are 0.1-2mm, and the flow rate is 1-100mL/min.
  6. 6. The carbon-contaminated co-monitoring mass spectrum ionization device according to claim 2, wherein the electron transmission module comprises a second vacuum ultraviolet light source (6), a vertical electron accelerating electrode (7) and a vertical electron extracting electrode (12) which are sequentially arranged along the direction perpendicular to the axis of the differential electrode (5), wherein the vertical electron accelerating electrode (7) and the vertical electron extracting electrode (12) are equidistantly arranged at two sides of the axis of the differential electrode (5), the vertical electron extracting electrode (12) is irradiated by light emitted by the second vacuum ultraviolet light source (6) to generate photoelectrons, and the photoelectrons are accelerated and collide with inorganic components in gas molecules of a sample under the action of an electric field between the vertical electron accelerating electrode (7) and the vertical electron extracting electrode (12) to generate inorganic product ions.
  7. 7. The device for the collaborative monitoring of mass spectrum ionization by carbon contamination according to claim 6, wherein the vertical electron accelerating electrode (7) is of a flat plate structure with a through hole in the center, the central through hole is coaxial with the light outlet hole of the second vacuum ultraviolet light source (6), and the vertical electron extracting electrode (12) is of a flat plate structure and is arranged below the vertical electron accelerating electrode (7) in parallel.
  8. 8. The device for the carbon-contaminated co-monitoring mass spectrum ionization according to claim 1, wherein the ion convergence multipole rod group (8) is composed of radio frequency multipole rods, the central axis of the ion convergence multipole rod group (8) coincides with the central axis of the differential electrode (5), and the ion extraction electrode (10) is of a flat plate structure with a through hole in the center.
  9. 9. The device according to claim 1, wherein the working pressure range of the high-pressure photo-electrochemical ionization chamber (14) is 10Pa-5000 Pa, and the working pressure range of the low-pressure photo-electrochemical ionization chamber (11) is 0.01Pa-10 Pa.
  10. 10. A method for ionization of a carbon-contaminated co-monitoring mass spectrum, characterized in that the method is realized by the device for ionization of a carbon-contaminated co-monitoring mass spectrum according to claim 6, and comprises the following steps: The method comprises the steps of 1) introducing reagent gas and sample gas into a high-pressure photo-induced chemical ionization cavity (14), directly photo-ionizing or photoelectron ionizing the reagent gas by photons generated by a first vacuum ultraviolet light source (1), leading out generated ions to an ion convergence reaction electrode group (4) under the action of an axial ion leading-out electrode (2) and an axial electron leading-out electrode (3), carrying out chemical reaction ionization with trace organic compound components in introduced sample gas molecules to generate organic product ions, and transmitting the organic product ions into a low-pressure photoelectron ionization cavity (11) through a central hole of a differential electrode (5) under the action of the ion convergence reaction electrode group (4); 2) The inorganic components which are not ionized in the sample gas pass through the center hole of the differential electrode (5) under the action of vacuum differential action and enter the low-pressure photoelectron ionization cavity (11), the light emitted by the second vacuum ultraviolet light source (6) irradiates the vertical electron extraction electrode (12) to generate photoelectrons, the photoelectrons are accelerated and collide with the inorganic component sample under the action of an electric field between the vertical electron acceleration electrode (7) and the vertical electron extraction electrode (12) to generate inorganic product ions, and the inorganic product ions and the organic product ions entering the low-pressure photoelectron ionization cavity (11) pass through the center hole of the ion extraction electrode (10) together under the action of the ion converging multipole rod group (8) and are transmitted into the mass analyzer (9) for detection.

Description

Dirty carbon collaborative monitoring mass spectrum ionization device and method Technical Field The invention relates to the technical field of mass spectrometers, in particular to a device and a method for cooperatively monitoring mass spectrum ionization by using waste carbon. Background The smoke pollution carbon comprises VOCs, NH 3、CO2 and the like which are controlled in an important way in the important industry, has the characteristics of complex background matrix, various types, large concentration range, obvious property difference and the like, the VOCs are main precursors generated by ozone (O 3) and secondary organic particles (SOA), the NH 3 is an important precursor of secondary inorganic ammonium salt, the ammonia escape can influence the light radiation intensity and exacerbate the photochemical pollution of the atmosphere, and the CO 2 is used as a bulk representative of greenhouse gas and can cause the global warming and other series of climate changes. The high coverage, high sensitivity and high accuracy monitoring of the components such as VOCs, NH 3, CO 2 and the like in the flue gas are the precondition of the atmosphere combined pollution trace cause and treatment. However, the commonly adopted FT I R and other spectroscopic techniques have complex system component cross interference, which affects the accuracy of measurement. Although GC-MS is a gold standard for analysis and detection, the analysis period is long, the flow is complex, and the method is not suitable for the requirement of long-term continuous monitoring of the carbon in the flue gas. The online mass spectrum has the characteristics of high analysis speed and high sensitivity, but ionization coverage and accurate identification capability of the prior art can not meet the requirement of collaborative monitoring of the carbon pollution. The related patent related to photoelectron ionization and chemical ionization is that the gas pressure controlled photoelectron ionization and chemical ionization switching system and method is disclosed in 2023, 8 and 25 of Shandong university through the retrieval of patent and paper. The pressure of the ionization source is regulated and controlled through flow switching and center aperture switching, so that the photoelectron ionization of the mass spectrum under low pressure and the chemical ionization under medium pressure are realized. However, the switching mode is complicated, flow, aperture and other regulation and control are needed, real-time regulation and control are difficult to realize, and the switching mode cannot be applied to the cooperative monitoring of the atmospheric pollution and carbon. Therefore, a method for cooperatively monitoring mass spectrum ionization by using polluted carbon is needed to be developed so as to realize simultaneous measurement of trace organic matters, CO 2 and other inorganic components. Disclosure of Invention Aiming at the problems existing in the prior art, the invention aims to provide a pollution and carbon cooperative monitoring mass spectrum ionization device so as to solve the problem of cooperative monitoring of organic pollutants, inorganic components such as CO 2 and the like. In order to achieve the above purpose, the present invention adopts the following technical scheme: The invention provides a mass spectrum ionization device for cooperatively monitoring carbon pollution, which comprises a high-pressure photo-chemical ionization cavity and a low-pressure photoelectron ionization cavity which are all operated under vacuum and realize vacuum difference through a flat differential electrode with a hole in the middle; The ion convergence reaction electrode group is used for carrying out chemical reaction ionization on the ions and trace organic compound components in sample gas molecules to generate organic product ions and enabling the organic product ions to pass through the differential electrode and be transmitted into the low-pressure photoelectron ionization cavity; The ion converging multipole rod group is used for transmitting inorganic product ions and organic product ions through a central hole of the ion extraction electrode to the mass analyzer for detection, and vacuum difference is realized between the low-pressure photoelectron ionization chamber and the mass analyzer through the ion extraction electrode. The ion transmission module comprises a first vacuum ultraviolet light source, an axial ion extraction electrode and an axial electron extraction electrode which are sequentially arranged at intervals along a light path, wherein a reagent gas sample injection pipeline is introduced between the first vacuum ultraviolet light source and the axial ion extraction electrode, a sample gas sample injection pipeline is introduced between the axial electron extraction electrode and the ion convergence reaction electrode group, the first vacuum ultraviolet light source is used for generating photons to directly pho