CN109887830B - Double-region chemical ionization source for mass spectrum - Google Patents
Double-region chemical ionization source for mass spectrum Download PDFInfo
- Publication number
- CN109887830B CN109887830B CN201711272689.3A CN201711272689A CN109887830B CN 109887830 B CN109887830 B CN 109887830B CN 201711272689 A CN201711272689 A CN 201711272689A CN 109887830 B CN109887830 B CN 109887830B
- Authority
- CN
- China
- Prior art keywords
- sample
- detected
- focusing electrode
- ionization
- reagent
- Prior art date
- Legal status (The legal status 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 status listed.)
- Active
Links
Images
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Electron Tubes For Measurement (AREA)
Abstract
The invention relates to an ionization source, in particular to a double-region chemical ionization source for mass spectrum. In the invention, a reagent ion generating cavity and a sample ionization cavity to be detected are designed into a double-region structure, reagent gas is ionized in the reagent ion generating cavity, neutral molecules and metastable molecules of the reagent gas are directly discharged out of the cavity through a tail gas pipeline, charged particles enter the sample ionization cavity to be detected through a transmission channel to interact with the molecules of the sample to be detected to form target ions, and enter a mass spectrometer to be detected under the action of a specific electric field to realize detection. The invention has the unique and main advantages that the design of the double-area structure ensures that neutral molecules and metastable-state molecules cannot enter the ionization cavity of the sample to be detected, and a pure reaction environment is maintained to avoid interfering the detection of target ions.
Description
Technical Field
The invention relates to an ionization source, in particular to a double-region chemical ionization source for mass spectrum. The design of the double-region structure ensures that neutral molecules and metastable-state molecules cannot enter the ionization cavity of the sample to be detected, and a pure reaction environment is kept to avoid interfering the detection of target ions.
Background
The ionization source is an important component of the TOFMS and is one of the most important factors affecting the sensitivity of mass spectrometry. Generally, different types of ionization sources have different ionization efficiencies due to the difference of the working principle of the ionization sources. Current sources commonly used today include photo-ionization sources and chemical ionization sources: the photoionization source ionizes an analyte by utilizing the collision of photons with the analyte, a common vacuum ultraviolet lamp generates photons, inert gas is filled in the lamp, and photons with different energies can be obtained by selecting different gases. The chemical ionization source may be divided into two steps, a first step to generate reagent ions, and a second step to ionize the reagent ions by collisions with analyte molecules. The reagent ion is an ion generated by collision of a photon or electron with some reagent gas which is relatively easily ionized and easily subjected to a reaction such as charge transfer, and the commonly used reagent ion is NO3 -、O2 -、H3O+、NO+Etc., organic dibromomethane, etc. also exist as reagent ionsOne of the main issues in chemical ionization source design is how to ensure a chemical reaction environment without any impurities (anal. chem.2016,88, 5028-.
Based on the conventional ionization source, the penmen introduces a back-blowing gas and tail gas pipe design, utilizes the effect of the back-blowing gas to discharge neutral gas molecules out of an ionization region, avoids the interference of ionization, ensures that charged reagent ions and sample ions react under the environment without any impurities to obtain pure product characteristic ions, and applies for a national invention patent (CN 105632870B).
The invention is continuously improved on the basis, neutral gas molecules such as metastable state molecules and the like are thoroughly prevented from entering the ionization cavity of the sample to be detected, a pure ionization environment is kept, and the detection of target ions is prevented from being interfered.
Disclosure of Invention
The invention aims to provide a double-region chemical ionization source which is more accurate and efficient and is used for mass spectrometry, neutral molecules and metastable-state molecules can be ensured not to enter an ionization cavity of a sample to be detected, a pure reaction environment is maintained, and the detection of target ions is prevented from being interfered.
In order to achieve the above purpose, the invention adopts the technical scheme that:
a two district chemical ionization sources for mass spectrum, including the sample ionization chamber that awaits measuring, reagent ion produce the chamber, characterized by:
the sample ionization chamber to be detected is a cylindrical barrel A;
a cylindrical barrel B is coaxially sleeved outside the sample ionization cavity to be detected, and a reagent ion generation cavity is formed between the outer wall surface of the cylindrical barrel A and the inner wall surface of the cylindrical barrel B; the reagent ion generating cavity and the sample ionization cavity to be detected form a double-region arrangement, so that neutral molecules and metastable-state molecules in the reagent gas are prevented from entering the sample ionization cavity to be detected to interfere the detection of target ions;
a repulsion electrode, a plate-shaped focusing electrode A with a through hole in the middle, a plate-shaped focusing electrode B with a through hole in the middle, a plate-shaped focusing electrode C with a through hole in the middle, a plate-shaped focusing electrode D with a through hole in the middle and a differential electrode with a through hole in the middle are sequentially arranged in the ionization cavity of the sample to be detected from left to right;
the diameters of the focusing electrode A, the focusing electrode B, the focusing electrode C, the focusing electrode D and the central through hole of the differential electrode are reduced in sequence;
a through hole serving as a transmission channel is formed in the side wall surface of the cylindrical barrel A between the repulsion electrode and the focusing electrode A;
a sample inlet tube of a sample to be detected extends into a space between the repulsion electrode and the focusing electrode A through the side wall surface of the ionization chamber of the sample to be detected and the through hole arranged in the middle of the repulsion electrode in sequence;
and a reagent gas inlet connected with the reagent gas sampling pipe, an ionization source placing port and a tail gas outlet connected with a tail gas pipeline are respectively arranged on the side wall of the cylindrical barrel B.
One end of the sample inlet pipe for the sample to be detected extends into the ionization cavity of the sample to be detected, and the other end of the sample inlet pipe for the sample to be detected is connected with the sample to be detected;
one end of the reagent gas sample inlet pipe extends into the reagent ion generating cavity, and the other end of the reagent gas sample inlet pipe is connected with the reagent gas; one end of the tail gas pipeline extends into the reagent ion generating cavity, and the other end of the tail gas pipeline is connected with the tail gas collecting device through the air extracting valve.
The ionization source is arranged facing the transmission channel and is used for ionizing the reagent gas and the sample to be detected to generate charged particles;
the reagent gas enters the reagent ion generation cavity through the gas sample inlet pipe, charged reagent ions are generated under the action of the ionization source, and the charged reagent ions enter the sample ionization cavity to be detected through the transmission channel;
the sample to be detected enters the ionization cavity of the sample to be detected through the sample inlet pipe of the sample to be detected, and the sample to be detected interacts with the charged reagent ions under the action of the ionization source to obtain target ions of the sample to be detected;
and applying a certain electric field to the repulsion electrode, the focusing electrode A, the focusing electrode B, the focusing electrode C, the focusing electrode D and the differential electrode, and enabling ions of the sample to be detected to enter the mass spectrometer under the action of the electric field to realize detection and analysis.
And a gradient direct current electric field or a radio frequency electric field is arranged on the focusing electrode A, the focusing electrode B, the focusing electrode C and the focusing electrode D and is used for controlling the movement of target ions of the sample to be detected.
The ionization source is set as a photo ionization source or a discharge ionization source;
a through hole is formed in the side wall of the cylindrical barrel A at the right end of the differential electrode far away from the focusing electrode D, and a mass spectrometer is arranged outside the through hole;
the mass spectrometer is a time-of-flight mass spectrometer or a quadrupole mass spectrometer.
In the ionization source, reagent gas is ionized in a reagent ion generation cavity, neutral molecules and metastable molecules of the reagent gas are directly discharged out of the cavity through a tail gas pipeline, charged particles enter a sample ionization cavity to be detected through a transmission channel and interact with the sample molecules to be detected to form target ions, and the target ions enter a mass spectrometer under the action of a specific electric field to realize detection. The design of the double-region structure ensures that neutral molecules and metastable-state molecules cannot enter the ionization cavity of the sample to be detected, and a pure reaction environment is kept to avoid interfering the detection of target ions.
Drawings
Fig. 1 is a schematic structural diagram of a sample injection system of atmospheric pressure time-of-flight mass spectrometry of the present invention.
Detailed Description
Fig. 1 is a schematic structural diagram of the present invention. The invention relates to a double-region chemical ionization source for mass spectrum, which consists of a sample ionization cavity 1 to be detected and a reagent ion generation cavity 2.
The sample ionization chamber 1 to be tested is a cylindrical barrel A;
a cylindrical barrel B is coaxially sleeved outside the sample ionization chamber 1 to be detected, and a reagent ion generation chamber 2 is formed between the outer wall surface of the cylindrical barrel A and the inner wall surface of the cylindrical barrel B; the reagent ion generating cavity 2 and the sample ionization cavity 1 to be detected form a double-area arrangement, so that neutral molecules and metastable-state molecules in the reagent gas are prevented from entering the sample ionization cavity 1 to be detected to interfere the detection of target ions;
a repulsion electrode 11, a plate-shaped focusing electrode A12 with a through hole in the middle, a plate-shaped focusing electrode B13 with a through hole in the middle, a plate-shaped focusing electrode C14 with a through hole in the middle, a plate-shaped focusing electrode D15 with a through hole in the middle and a differential electrode 16 with a through hole in the middle are sequentially arranged in the sample ionization chamber 1 to be detected from left to right;
the diameters of central through holes of the focusing electrode A12, the focusing electrode B13, the focusing electrode C14, the focusing electrode D15 and the differential electrode 16 are sequentially reduced;
a through hole as a transmission channel 8 is arranged on the side wall surface of the cylindrical cylinder A between the repulsion electrode 11 and the focusing electrode A12;
a sample inlet tube 18 of a sample to be detected extends into a space between the repulsion electrode 11 and the focusing electrode A12 through the side wall surface of the ionization chamber 1 of the sample to be detected and a through hole arranged in the middle of the repulsion electrode 11 in sequence;
a reagent gas inlet connected with the reagent gas sampling pipe 5, an ionization source 17 placing port and a tail gas outlet connected with the tail gas pipeline 10 are respectively arranged on the side wall of the cylindrical barrel B.
One end of the sample inlet pipe 18 for the sample to be tested extends into the ionization chamber 1 for the sample to be tested, and the other end is connected with the sample 6 for the sample to be tested;
one end of the reagent gas sample inlet pipe 5 extends into the reagent ion generating cavity 2, and the other end is connected with the reagent gas 4; one end of a tail gas pipeline 10 extends into the reagent ion generating cavity 2, and the other end of the tail gas pipeline is connected with a tail gas collecting device 7 through an air extraction valve 9.
The ionization source 17 is arranged facing the transmission channel 8 and is used for ionizing the reagent gas and the sample to be detected to generate charged particles;
the reagent gas 4 enters the reagent ion generating cavity 2 through the gas sampling tube 5, and generates charged reagent ions under the action of the ionization source 17, and the charged reagent ions enter the sample ionization cavity 1 to be detected through the transmission channel 8;
the sample 6 to be detected enters the ionization chamber 1 of the sample to be detected through the sample inlet tube 18 of the sample to be detected, and the sample 6 to be detected interacts with the charged reagent ions under the action of the ionization source 17 to obtain target ions of the sample to be detected;
a certain electric field is applied to the repulsion electrode 11, the focusing electrode a 12, the focusing electrode B13, the focusing electrode C14, the focusing electrode D15 and the differential electrode 16, and the ions of the sample to be detected enter the mass spectrometer 3 under the action of the electric field to realize detection and analysis.
And a gradient direct current electric field or a radio frequency electric field is arranged on the focusing electrode A12, the focusing electrode B13, the focusing electrode C14 and the focusing electrode D15 and is used for controlling the movement of target ions of the sample to be detected.
The ionization source 17 is set as a photo ionization source or a discharge ionization source;
a through hole is formed in the side wall of the cylindrical barrel A at the right end of the differential electrode 16 far away from the focusing electrode D15, and a mass spectrometer 3 is arranged outside the through hole;
the mass spectrometer 3 is a time-of-flight mass spectrometer or a quadrupole mass spectrometer.
Claims (6)
1. The utility model provides a two district chemical ionization sources for mass spectrum, includes sample ionization chamber (1) that awaits measuring, reagent ion production chamber (2), its characterized in that:
the sample ionization chamber (1) to be tested is a cylindrical barrel A;
a cylindrical barrel B is coaxially sleeved outside the sample ionization cavity (1) to be detected, and a reagent ion generation cavity (2) is formed between the outer wall surface of the cylindrical barrel A and the inner wall surface of the cylindrical barrel B; the reagent ion generating cavity (2) and the sample ionization cavity (1) to be detected form a double-area arrangement, so that neutral molecules and metastable molecules in reagent gas are prevented from entering the sample ionization cavity (1) to be detected to interfere the detection of target ions;
a repulsion electrode (11), a plate-shaped focusing electrode A (12) with a through hole in the middle, a plate-shaped focusing electrode B (13) with a through hole in the middle, a plate-shaped focusing electrode C (14) with a through hole in the middle, a plate-shaped focusing electrode D (15) with a through hole in the middle and a differential electrode (16) with a through hole in the middle are sequentially arranged in the sample ionization chamber (1) to be detected from left to right;
the diameters of central through holes of the focusing electrode A (12), the focusing electrode B (13), the focusing electrode C (14), the focusing electrode D (15) and the differential electrode (16) are reduced in sequence;
a through hole as a transmission channel (8) is arranged on the side wall surface of the cylindrical barrel A between the repulsion electrode (11) and the focusing electrode A (12);
a sample inlet pipe (18) of a sample to be detected extends into a space between the repulsion electrode (11) and the focusing electrode A (12) through a through hole formed in the side wall surface of the ionization chamber (1) of the sample to be detected and the middle part of the repulsion electrode (11) in sequence;
a reagent gas inlet connected with the reagent gas sampling pipe (5), an ionization source (17) placing port and a tail gas outlet connected with the tail gas pipeline (10) are respectively arranged on the side wall of the cylindrical barrel body B;
the ionization source (17) is arranged facing the transmission channel (8) and is used for ionizing the reagent gas and the sample to be detected to generate charged particles;
the reagent gas (4) enters the reagent ion generating cavity (2) through the gas sampling tube (5), and generates charged reagent ions under the action of the ionization source (17), and the charged reagent ions enter the sample ionization cavity (1) to be detected through the transmission channel (8);
the sample (6) to be detected enters the ionization cavity (1) of the sample to be detected through the sample inlet tube (18) of the sample to be detected, and the sample (6) to be detected interacts with the charged reagent ions under the action of the ionization source (17) to obtain target ions of the sample to be detected.
2. The dual-region chemical ionization source for mass spectrometry of claim 1, wherein:
one end of the sample inlet pipe (18) for the sample to be detected extends into the ionization cavity (1) for the sample to be detected, and the other end is connected with the sample (6) for the sample to be detected;
one end of the reagent gas sample inlet pipe (5) extends into the reagent ion generating cavity (2), and the other end is connected with the reagent gas (4); one end of a tail gas pipeline (10) extends into the reagent ion generating cavity (2), and the other end of the tail gas pipeline is connected with a tail gas collecting device (7) through an air extraction valve (9).
3. The dual-region chemical ionization source for mass spectrometry of claim 1, wherein:
and applying a certain electric field to the repulsion electrode (11), the focusing electrode A (12), the focusing electrode B (13), the focusing electrode C (14), the focusing electrode D (15) and the differential electrode (16), and enabling the ions of the sample to be detected to enter the mass spectrometer (3) under the action of the electric field to realize detection and analysis.
4. The dual-region chemical ionization source for mass spectrometry of claim 1 or 3, wherein:
and a gradient direct current electric field or a radio frequency electric field is arranged on the focusing electrode A (12), the focusing electrode B (13), the focusing electrode C (14) and the focusing electrode D (15) and is used for controlling the movement of target ions of the sample to be detected.
5. The dual-region chemical ionization source for mass spectrometry of claim 1 or 3, wherein:
the ionization source (17) is provided as a photo-ionization source or a discharge ionization source.
6. The dual-region chemical ionization source for mass spectrometry of claim 1, wherein:
a through hole is formed in the side wall of a cylindrical barrel A at the right end of a differential electrode (16) far away from a focusing electrode D (15), and a mass spectrometer (3) is arranged outside the through hole;
the mass spectrometer (3) is a time-of-flight mass spectrometer or a quadrupole mass spectrometer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711272689.3A CN109887830B (en) | 2017-12-06 | 2017-12-06 | Double-region chemical ionization source for mass spectrum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711272689.3A CN109887830B (en) | 2017-12-06 | 2017-12-06 | Double-region chemical ionization source for mass spectrum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109887830A CN109887830A (en) | 2019-06-14 |
| CN109887830B true CN109887830B (en) | 2020-05-05 |
Family
ID=66923194
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711272689.3A Active CN109887830B (en) | 2017-12-06 | 2017-12-06 | Double-region chemical ionization source for mass spectrum |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109887830B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101660133A (en) * | 2008-07-24 | 2010-03-03 | 希捷科技有限公司 | Two-zone ion beam carbon deposition |
| CN102479661A (en) * | 2010-11-30 | 2012-05-30 | 中国科学院大连化学物理研究所 | Composite ionization source of vacuum ultraviolet photoionization and chemical ionization used in mass spectrometry |
| CN105206499A (en) * | 2015-10-14 | 2015-12-30 | 中国烟草总公司郑州烟草研究院 | Two-area reverse airflow atmospheric pressure chemical ionization source |
-
2017
- 2017-12-06 CN CN201711272689.3A patent/CN109887830B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101660133A (en) * | 2008-07-24 | 2010-03-03 | 希捷科技有限公司 | Two-zone ion beam carbon deposition |
| CN102479661A (en) * | 2010-11-30 | 2012-05-30 | 中国科学院大连化学物理研究所 | Composite ionization source of vacuum ultraviolet photoionization and chemical ionization used in mass spectrometry |
| CN105206499A (en) * | 2015-10-14 | 2015-12-30 | 中国烟草总公司郑州烟草研究院 | Two-area reverse airflow atmospheric pressure chemical ionization source |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109887830A (en) | 2019-06-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US10109471B1 (en) | Ion funnel for efficient transmission of low mass-to-charge ratio ions with reduced gas flow at the exit | |
| CN101281165B (en) | Method and apparatus for ionizing mass spectrographic analysis sample | |
| CN108538700B (en) | Proton transfer reaction ion source, mass spectrometer and detection method thereof | |
| CN105632870A (en) | Atmospheric pressure chemical ionization source for mass spectrum | |
| CN109643636B (en) | Low temperature plasma probe with auxiliary heating gas jet | |
| CN106876243A (en) | One kind aids in low pressure vacuum ultraviolet light ionization source for mass spectrographic reagent molecule | |
| CN208256615U (en) | A kind of Proton-Transfer Reactions ion source and mass spectrograph | |
| CN103094050A (en) | Sensitive glow discharge direct ionization method and device thereof | |
| CN103165390A (en) | Ozone modified beta radioactive ion source and application thereof | |
| CN109887824A (en) | A kind of mass spectrograph and Mass Spectrometry detection method | |
| CN111199862B (en) | Capillary micro-area ionization source | |
| CN109887830B (en) | Double-region chemical ionization source for mass spectrum | |
| CN105719937A (en) | High-efficiency VUV photo ionization source for ionic migration spectrum | |
| CN103776893A (en) | Ionic migration spectrometer of dielectric barrier discharging ionization source | |
| CN108493091B (en) | High-electron-utilization-rate low-energy ionization device, mass spectrum system and method | |
| CN213042872U (en) | Time-of-flight mass spectrometer reaction chamber | |
| CN102683152B (en) | A kind of proton translocation mass ion source | |
| CN105655227B (en) | A kind of effectively ionized source of dielectric barrier discharge and its application | |
| CN112201561A (en) | Time-of-flight mass spectrometer reaction chamber | |
| CN111243935A (en) | Ion mobility spectrometer of dielectric barrier discharge ionization source | |
| CN210722952U (en) | Composite ionization source device for mass spectrometry | |
| CN108091546B (en) | Discharge gas assisted windowless radio frequency lamp mass spectrum ionization source | |
| CN216747541U (en) | Ion-molecule reaction selection control measuring device based on ion mobility spectrometry | |
| CN117711909B (en) | Non-uniform field ionizer and ion focusing method | |
| CN112951703B (en) | Heatable VUV photoionization source |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |