CN110828282B - Ion source device for liquid chromatogram and ion mobility spectrometry and application - Google Patents
Ion source device for liquid chromatogram and ion mobility spectrometry and application Download PDFInfo
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- CN110828282B CN110828282B CN201911117846.2A CN201911117846A CN110828282B CN 110828282 B CN110828282 B CN 110828282B CN 201911117846 A CN201911117846 A CN 201911117846A CN 110828282 B CN110828282 B CN 110828282B
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- 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
- G01N27/622—Ion mobility spectrometry
- G01N27/624—Differential mobility spectrometry [DMS]; Field asymmetric-waveform ion mobility spectrometry [FAIMS]
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Abstract
The invention relates to an ion source device for combining liquid chromatogram and ion mobility spectrometry, wherein the ion source adopts a structure that a hollow discharge needle and an annular discharge counter electrode are coaxially arranged; the outer wall surface of the discharge needle is wound with a heating wire or a heating belt, and a mobile phase flowing out of the liquid chromatographic column is vaporized into gas after entering the hollow discharge needle, and then enters a discharge area to be ionized into ions; the cylindrical ion focusing electrode and the annular ion leading-out electrode are respectively arranged on the two axial sides of the discharge counter electrode, ions generated in a discharge area are focused into a beam along the axial direction of the discharge needle and are efficiently transmitted into an ion mobility spectrum for separation and detection; more than 2 air outlets which are uniformly distributed on the same radial section are arranged on the inner bottom surface of the sealing end of the cylindrical ion focusing electrode, one path of scavenging air reversely sweeps a discharge area through a middle through hole of the ion leading-out electrode and the discharge counter electrode, and unreacted neutral molecules in the ion source are rapidly taken out of the ion source through the air outlets, so that the interference of the background of the mobile phase solvent is reduced.
Description
Technical Field
The invention relates to an ion source device for combining liquid chromatogram and ion mobility spectrometry, in particular to a discharge ion source device for realizing synchronous vaporization and ionization of a mobile phase flowing out of a liquid chromatogram column in an ionization source.
Background
Ion Mobility Spectrometry (IMS) is a gas-phase ion separation detection technology that emerged in the early 70 s of the 20 th century. Compared with a mass spectrum technology, the ion resolution capability of the IMS is weaker; however, the IMS has the advantages of high sensitivity, working at atmospheric pressure, portability of instruments, and the like. At present, the IMS plays an important role in the fields of environmental pollution, food safety, and biomedical research, in addition to playing a role as a mainstream technology in the fields of explosives, drug field screening, and public safety, in combination with gas chromatography and liquid chromatography.
In the liquid chromatography and ion mobility spectrometry combined technology, the separation and detection of the ion mobility spectrometry can be carried out only by converting a mobile phase flowing out of a liquid chromatography column into gas-phase ions. At present, techniques capable of converting a mobile phase flowing out of a liquid chromatography column into gas phase ions with high efficiency mainly include thermal spray ionization (US4902891, US4960991), atmospheric pressure photoionization (US6534765), electrospray ionization (US20030160166, US20120228490, CN100601586, CN105719935), and the like. Among them, thermal spray ionization is an ionization technique which is very important in the early development of LC-MS. Thermal spray ionization requires the addition of large amounts of salts and the like to the chromatographic mobile phase, causes extremely severe matrix ionization suppression effects, and has fewer target species that can be detected, and has very few applications after the development of electrospray ionization technology is mature. Atmospheric pressure photoionization is usually combined with an in-source atomization technology, has a complex structure and is mainly used for liquid chromatography-mass spectrometry. In addition, most of the solvents used in the liquid chromatography mobile phase are easy to generate background interference in a photoionization source, the ionization mechanism is very complex, and the sensitivity is not high. At present, the combination of liquid chromatography and ion mobility spectrometry mainly adopts ESI technology. However, the use of ESI in ion mobility spectrometry is often accompanied by problems such as difficulty in desolvation, instability in spraying, and easy clogging of an electrospray needle, which results in low detection sensitivity of a target and poor stability of an instrument.
In 2012, m.t.jafari (anal. chem.84,10077) reported a gas chromatography and ion mobility spectrometry setup based on a discharge ion source. The hollow stainless steel capillary tube is used as a discharge needle, and the effluent of the gas chromatographic column is directly conveyed to a discharge area through a cavity of the discharge needle for ionization, so that the detection sensitivity is greatly improved, but the gas chromatographic column is not suitable for liquid sample detection.
The invention constructs a discharge ion source, realizes the in-source synchronous vaporization and ionization of a liquid sample, and effectively solves the problems of matrix ionization inhibition, difficult desolvation, easy blockage of a spray needle and the like when an electrospray ion source is adopted in the combined use of liquid chromatogram and ion mobility spectrometry. Meanwhile, the ion source device adopts an electrode structure design of high-efficiency ion focusing and ion transmission, and has high detection sensitivity; and an electric discharge area reverse purging mode is adopted, so that unreacted neutral molecules in the ion source are quickly removed, and the interference of the background of the liquid chromatography mobile phase solvent is reduced.
The invention content is as follows:
the invention aims to provide a high-efficiency discharge ion source device which combines liquid chromatogram and ion mobility spectrometry and solves the problems of matrix ionization inhibition, difficulty in desolvation, easiness in blockage of a spray needle and the like when an electrospray ion source is adopted in the combination of the liquid chromatogram and the ion mobility spectrometry.
In order to achieve the purpose, the invention adopts the technical scheme that:
an ion source device for the combination of liquid chromatogram and ion mobility spectrometry comprises a discharge needle, a cylindrical ion focusing electrode, a discharge counter electrode and an ion extraction electrode;
the discharge needle is a discharge needle with an axial through hole, the cylindrical ion focusing electrode is a cylindrical barrel with a closed left end and an open right end, the left side bottom surface inside the barrel is hemispherical, the hemispherical bottom surface is coaxial with the barrel, the through hole is formed in the hemispherical bottom surface along the axis direction, one end of the tip of the discharge needle penetrates through the through hole and extends into the barrel, the other end of the tip of the discharge needle is positioned outside the barrel, an electric heating wire or an electric heating belt is wound on the outer wall surface of the discharge needle positioned outside the barrel, and an insulating layer is arranged between the outer wall surface of the discharge needle and the electric heating wire; the hemispherical bottom surface is provided with through holes as air outlets, and the air outlets are more than 2 and are uniformly distributed along the same radial section of the hemispherical bottom surface.
Two parallel discharge counter electrodes and two parallel ion extraction electrodes are arranged in the cylindrical ion focusing electrode, the plate surfaces of the flat discharge counter electrodes and the ion extraction electrodes are vertical to the axis of the cylinder, the discharge counter electrodes are positioned between the discharge needles and the ion extraction electrodes, through holes are respectively arranged in the middle parts of the discharge counter electrodes and the ion extraction electrodes, and the through holes in the middle parts of the discharge counter electrodes and the ion extraction electrodes are coaxial with the discharge needles;
the peripheral edges of the plate bodies of the discharge counter electrode and the ion extraction electrode are hermetically connected with the inner wall surface of the cylindrical ion focusing electrode through an insulator.
The ion extraction electrode, the discharge counter electrode, the cylindrical ion focusing electrode and the hollow discharge needle are applied with direct current voltages with the same polarity and sequentially increased voltage values.
One end of the needle tip of the discharge needle passes through the through hole and extends to the middle part of the cylinder body after passing through the hemispherical bottom surface.
An insulating sleeve serving as an insulating layer is sleeved on the outer wall surface of the discharge needle, an electric heating wire or an electric heating belt is wound on the outer wall surface of the insulating sleeve, and the electric heating wire or the electric heating belt is electrically connected with an external power supply; the left end of the cylindrical ion focusing electrode is provided with a heat insulation block body, the heat insulation block body is hermetically connected with the outer wall surface of the left end of the cylindrical ion focusing electrode, meanwhile, the heat insulation block body seals a through hole of the hemispherical bottom surface through which the discharge needle passes, and the discharge needle passes through the heat insulation block body and then extends into the cylinder; the outer wall surface of the insulating sleeve is wound with an electric heating wire or an electric heating belt which is arranged in the heat insulation block.
The ion source device is used as an ion source of an ion mobility spectrum, and an ion extraction electrode is used as a top electrode of an ionization area of the ion mobility spectrum; one end of a discharge needle through hole positioned outside the cylindrical ion focusing electrode is connected with the mobile phase outlet end of the liquid chromatogram column, and the liquid chromatogram and the ion mobility spectrometry are used together.
When the device for combining the liquid chromatogram and the ion mobility spectrometry works, the flow velocity of a mobile phase of the liquid chromatogram is between 0.1 and 1000 mu L/min (preferably 100 to 300 mu L/min); the temperature of the heating wire or the heating belt (3) is adjustable between 100 ℃ and 600 ℃ (preferably 250 ℃ to 400 ℃); and the floating gas in the ion mobility spectrometry is used as purge gas and flows out of the combined device from the gas outlet of the ion focusing cylinder after passing through the ion leading-out electrode and the discharge counter electrode middle through hole.
The invention has the advantages that:
the discharge ion source device disclosed by the invention is simple in structure, and effectively solves the problems of matrix ionization inhibition, difficulty in desolvation, easiness in blockage of a spray needle and the like when an electrospray ion source is adopted in the combined use of liquid chromatography and ion mobility spectrometry in a mode of synchronously vaporizing and ionizing in the source. Meanwhile, the ion source device adopts an electrode structure design of high-efficiency ion focusing and ion transmission, and has high detection sensitivity; and an electric discharge area reverse purging mode is adopted, so that unreacted neutral molecules in the ion source are quickly removed, and the interference of the background of the liquid chromatography mobile phase solvent is reduced.
The invention is described in further detail below with reference to the accompanying drawings:
description of the drawings:
FIG. 1 shows a liquid chromatogram and ion mobility spectrometry combined device constructed based on the discharge ion source disclosed by the invention. Wherein: (1) a hollow discharge needle; (2) a quartz glass sleeve; (3) a nickel-chromium heating wire; (4) a ceramic insulation block; (5) a cylindrical ion focusing electrode; (6) an annular discharge counter electrode; (7) an annular ion extraction electrode; (8) an air outlet; (9) bleaching; (10) an ionization region; (11) Tyndall-Powell type ion gate; (12) an ion transfer region; (13) an ion receiving electrode; (14) a liquid chromatograph.
FIG. 2, using trioctylamine, cocaine, tributylamine, ephedrine, n-butylamine, and diethylamine to prepare a mixed sample with a concentration of 10ng/mL, and a solvent is methanol; 10 μ L of the mixed sample formed a two-dimensional response profile in the combination set.
FIG. 3 is a schematic representation of the structure of the present invention in a combined liquid chromatography and ion mobility spectrometry apparatus. Wherein: (1) a hollow discharge needle; (2) a quartz glass sleeve; (3) a nickel-chromium heating wire; (4) a ceramic insulation block; (5) a cylindrical ion focusing electrode; (6) an annular discharge counter electrode; (7) an annular ion extraction electrode; (8) an air outlet; (9) and (4) floating gas.
The specific implementation mode is as follows:
example 1
The device for combining liquid chromatography and ion mobility spectrometry constructed based on the discharge ion source disclosed by the invention is shown in figure 1.
The hollow discharge needle (1) of the discharge ion source is a stainless steel capillary tube with the outer diameter of 1/16inch, the inner diameter of 100 mu m and the length of 80mm, one end of the hollow discharge needle keeps the section flush, and the other end of the hollow discharge needle is sharpened in a 45-degree inclined plane; the cylindrical ion focusing electrode (5) is a stainless steel electrode with the outer diameter of 40mm and the length of 35mm, the radius of the hemispherical inner bottom surface of the sealing end of the stainless steel electrode is 15mm, and a through hole with the diameter of 5mm is axially formed in the sealing end of the stainless steel electrode, so that the hollow discharge needle (1) is ensured to be mutually insulated when penetrating along the axis of the cylindrical ion focusing electrode (5); 4 through holes with the diameter of 5mm, namely air outlets (8), are uniformly distributed on the hemispherical inner bottom surface at the sealing end of the cylindrical ion focusing electrode (5) along the radial section at the spherical radius 1/2 and are used as outlets of reverse purge gas in a discharge area; the discharge counter electrode (6) is a tungsten steel electrode with the outer diameter of 40mm, the inner diameter of 6mm and the thickness of 1mm, and the axial distance between the tip of the hollow discharge needle (1) and the discharge counter electrode (6) is 5 mm; the ion extraction electrode (7) is a stainless steel electrode with the outer diameter of 40mm, the inner diameter of 6mm and the thickness of 1mm, and the axial distance between the ion extraction electrode (7) and the discharge counter electrode (6) is 5 mm. The cylindrical ion focusing electrode (5), the discharge counter electrode (6) and the ion extraction electrode (7) are sequentially coaxially and hermetically matched through a tetrafluoro insulating ring with the outer diameter of 40mm, the inner diameter of 30mm and the thickness of 5 mm.
The outer wall surface of the part of the hollow discharge needle (1) which does not penetrate into the cylindrical ion focusing electrode (5) is sleeved with a quartz glass sleeve (2) with the outer diameter of 4mm, the inner diameter of 1/16inch and the length of 30 mm; a spiral nichrome heating wire (3) with the axial length of 20mm is wound on the outer wall surface of the quartz glass sleeve (2), and the resistance value is 5 omega; a ceramic heat insulation block body (4) with the outer diameter of 40mm and the length of 35mm is arranged at the left end of the cylindrical ion focusing electrode (5), the ceramic heat insulation block body (4) is hermetically connected with the outer wall surface of the left end of the cylindrical ion focusing electrode (5), and the hemispherical bottom surface is sealed at a through hole through which the hollow discharge needle (1) passes; the discharge needle (1) penetrates through the ceramic heat insulation block body (4) and then extends into the cylindrical ion focusing electrode (5); the insulating sleeve (2) and the nickel-chromium heating wire (3) on the outer wall surface of the discharge needle (1) are arranged in the ceramic heat-insulating block body (4).
The ionization region of the ion mobility spectrometry is a hollow cavity with the outer diameter of 40mm, the inner diameter of 30mm and the length of 20 mm; the ion gate is a Tyndall-Powell type ion gate, and has an outer diameter of 40mm and a thickness of 1 mm; the ion migration zone is a hollow cavity with the outer diameter of 40mm, the inner diameter of 30mm and the length of 60 mm; the liquid chromatograph (14) is any commercially available liquid chromatograph.
When the discharge ion source is used as the ion source of the ion mobility spectrometry, the ion extraction electrode (7) is used as the top electrode of the ionization region (2) of the ion mobility spectrometry; one end of a through hole of the discharge needle (1) positioned outside the cylindrical ion focusing electrode (5) is connected with the chromatographic column mobile phase outlet end of the liquid chromatogram (14) through a standard chromatographic accessory, and the liquid chromatogram (14) is used together with the ion mobility spectrometry.
When the device for combining the liquid chromatogram and the ion mobility spectrometry works, the nickel-chromium heating wire (3) is powered by an isolation power supply with a high withstand voltage value, and the temperature is kept between 250 and 400 ℃; a uniform electric field is kept in an ionization region (10) and an ion migration region (12) of the ion mobility spectrometry; the ion extraction electrode (7), the discharge counter electrode (6), the cylindrical ion focusing electrode (5) and the hollow discharge needle (1) are applied with direct current voltages with the same polarity and sequentially increased voltage values.
After a mobile phase flowing out of a chromatographic column of the liquid chromatogram (14) enters the hollow discharge needle (1), the mobile phase is heated and quickly vaporized and ionized into ions in a discharge area; the cylindrical ion focusing electrode (5) and the ion extraction electrode (7) focus and shape ions and efficiently transmit the ions to an ion mobility spectrum for separation and detection, so that a spectrogram of ion intensity corresponding to migration time is formed. The drift gas (9) of the ion mobility spectrometry sweeps a discharge area through an ion leading-out electrode (7) and a through hole in the middle of a discharge counter electrode (6), and neutral molecules in an ionization area are taken out through an air outlet (8) of a cylindrical ion focusing electrode (5).
Example 2
In the combined apparatus disclosed in example 1, the liquid chromatograph (14) was a Jasco PU-1580 coupled to a Waters C18 column (5 μm,4.6X100mm, XTerra)TM) The mobile phase is 1:4 methanol water solution, and the flow rate is 200 mu L/min; the electric field intensity of an ionization region (10) and an ion migration region (12) of an ion mobility spectrum is set to be 250V/cm, and the opening time of an ion gate is set to be 200 mu s; the voltage values of the ion extraction electrode (7), the discharge counter electrode (6), the cylindrical ion focusing electrode (5) and the hollow discharge needle (1) are sequentially set to be 2200V, 2700V, 3200V and 6200V; the temperature of the nickel-chromium heating wire is controlled at 300 ℃.
A two-dimensional response spectrogram formed by 10 mu L of a mixed sample in a combined device is shown in figure 2 by using a mixed sample with the concentration of 10ng/mL of trioctylamine, cocaine, tributylamine, ephedrine, n-butylamine and diethylamine and a solvent of methanol.
Claims (9)
1. An ion source apparatus for use in conjunction with liquid chromatography and ion mobility spectrometry, comprising: comprises a discharge needle (1), a cylindrical ion focusing electrode (5), a discharge counter electrode (6) and an ion extraction electrode (7);
the discharge needle (1) is a discharge needle with an axial through hole, the cylindrical ion focusing electrode (5) is a cylindrical barrel with a closed left end and an open right end, the left bottom surface inside the barrel is hemispherical, the hemispherical bottom surface is coaxial with the barrel, a through hole is formed in the hemispherical bottom surface along the axis direction, one end of the needle point of the discharge needle (1) penetrates through the through hole and extends into the barrel, the other end of the needle point is positioned outside the barrel, an electric heating wire or an electric heating belt (3) is wound on the outer wall surface of the discharge needle positioned outside the barrel, and an insulating layer is arranged between the outer wall surface of the discharge needle and the electric heating wire or the electric heating belt; a through hole serving as an air outlet (8) is formed in the hemispherical bottom surface;
a discharge counter electrode (6) and an ion extraction electrode (7) which are arranged in parallel at intervals are arranged in the cylindrical ion focusing electrode (5), the plate surfaces of the flat discharge counter electrode (6) and the ion extraction electrode (7) are vertical to the axis of the cylinder, the discharge counter electrode (6) is positioned between the discharge needle (1) and the ion extraction electrode (7), through holes are respectively formed in the middle parts of the discharge counter electrode (6) and the ion extraction electrode (7), and the through holes in the middle parts of the discharge counter electrode (6) and the ion extraction electrode (7) are coaxial with the discharge needle (1);
the peripheral edges of the plate bodies of the discharge counter electrode (6) and the ion extraction electrode (7) are hermetically connected with the inner wall surface of the cylindrical ion focusing electrode (5) through an insulator;
the ion extraction electrode (7), the discharge counter electrode (6), the cylindrical ion focusing electrode (5) and the hollow discharge needle (1) are applied with direct current voltages with the same polarity and sequentially increased voltage values.
2. The apparatus of claim 1, wherein: one end of the needle tip of the discharge needle (1) passes through the through hole and extends to the middle part of the cylinder body after passing through the hemispherical bottom surface.
3. The apparatus of claim 1, wherein:
an insulating sleeve (2) serving as an insulating layer is sleeved on the outer wall surface of the discharge needle (1), an electric heating wire or an electric heating belt (3) is wound on the outer wall surface of the insulating sleeve (2), and the electric heating wire or the electric heating belt (3) is electrically connected with an external power supply.
4. The apparatus of claim 1, wherein: the left end of the cylindrical ion focusing electrode (5) is provided with a heat insulation block (4), the heat insulation block (4) is hermetically connected with the outer wall surface of the left end of the cylindrical ion focusing electrode (5), meanwhile, the heat insulation block (4) seals a through hole of a hemispherical bottom surface through which the discharge needle (1) passes, and the discharge needle (1) passes through the heat insulation block (4) and then extends into the cylinder;
an electric heating wire or an electric heating belt (3) is wound on the outer wall surface of the insulating sleeve (2) and is arranged in the heat insulation block body (4).
5. The apparatus of claim 1, wherein: the air outlets (8) are more than 2 and are uniformly distributed along the same radial section of the hemispherical bottom surface.
6. Use of an ion source apparatus according to any of claims 1 to 5, wherein:
the ion source device of any one of claims 1 to 5 as an ion source for ion mobility spectrometry, wherein the ion extraction electrode (7) is used as a top electrode of an ionization region of the ion mobility spectrometry; one end of a through hole of the discharge needle (1) positioned outside the cylindrical ion focusing electrode (5) is connected with a mobile phase outlet of the liquid chromatogram column, and the liquid chromatogram and the ion mobility spectrometry are used together.
7. Use according to claim 6, characterized in that: the flow rate of a mobile phase of the liquid chromatogram is adjustable between 0.1 and 1000 mu L/min; the temperature of the electric heating wire or the electric heating belt (3) can be adjusted between 100 ℃ and 600 ℃.
8. Use according to claim 7, characterized in that: the flow rate of a mobile phase of the liquid chromatogram is adjustable between 100 and 300 mu L/min; the temperature of the electric heating wire or the electric heating belt (3) is adjustable between 250 and 400 ℃.
9. Use according to claim 6, characterized in that: the floating gas in the ion mobility spectrometry is taken as the purge gas (9) and flows out of the combined device from the gas outlet (8) after passing through the ion leading-out electrode (7) and the through hole in the middle of the discharge counter electrode (6).
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| CN113727508A (en) * | 2020-05-26 | 2021-11-30 | 上海大学 | Novel vacuum microwave plasma ion source |
| CN114334598A (en) * | 2021-12-25 | 2022-04-12 | 广州禾信仪器股份有限公司 | Mass spectrometer, sample ionization platform and ion source thereof |
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| CN105185686A (en) * | 2015-08-31 | 2015-12-23 | 中国科学院电子学研究所 | Ion mobility spectrometry employing electrospray/corona discharge dual-mode ion source |
| CN106855541A (en) * | 2016-11-28 | 2017-06-16 | 大连大学 | A kind of detection means based on micro-fluidic chip Yu Nanoliter electrospray ion mobility spectrometry |
| CN108369889A (en) * | 2015-12-18 | 2018-08-03 | Dh科技发展私人贸易有限公司 | The system minimized for the electric discharge during making ESI operate |
| CN110376323A (en) * | 2019-06-26 | 2019-10-25 | 北京中医药大学东直门医院 | A kind of heating device and heating means of capillary chromatographic column |
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| WO2014146200A1 (en) * | 2013-03-18 | 2014-09-25 | Smiths Detection Montreal Inc. | Ion mobility spectrometry (ims) device with charged material transportation chamber |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105185686A (en) * | 2015-08-31 | 2015-12-23 | 中国科学院电子学研究所 | Ion mobility spectrometry employing electrospray/corona discharge dual-mode ion source |
| CN108369889A (en) * | 2015-12-18 | 2018-08-03 | Dh科技发展私人贸易有限公司 | The system minimized for the electric discharge during making ESI operate |
| CN106855541A (en) * | 2016-11-28 | 2017-06-16 | 大连大学 | A kind of detection means based on micro-fluidic chip Yu Nanoliter electrospray ion mobility spectrometry |
| CN110376323A (en) * | 2019-06-26 | 2019-10-25 | 北京中医药大学东直门医院 | A kind of heating device and heating means of capillary chromatographic column |
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