CN211125573U - Low-frequency radio-frequency glow discharge ionization device - Google Patents
Low-frequency radio-frequency glow discharge ionization device Download PDFInfo
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- CN211125573U CN211125573U CN201922272923.3U CN201922272923U CN211125573U CN 211125573 U CN211125573 U CN 211125573U CN 201922272923 U CN201922272923 U CN 201922272923U CN 211125573 U CN211125573 U CN 211125573U
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Abstract
The utility model discloses a low-frequency radio frequency glow discharge ionization device, which comprises an ionization source shell with an ionization chamber, a sample introduction unit and an auxiliary air inlet unit; the sample introduction unit comprises a metal sample introduction pipe and a heating cylinder sleeved with the sample introduction pipe, a heating rod is arranged in the heating cylinder, the sample introduction pipe is inserted into the ionization cavity, and an analyte outlet used for being connected with the mass spectrometer is formed in one end, opposite to the sample introduction pipe, of the ionization source shell; the ionization chamber is internally provided with an ionization source and an electrode plate group capable of exciting an electric field, and charged analyte ions move from the end of the sample introduction pipe to the direction of the analyte outlet under the guidance of the electric field; the auxiliary gas inlet unit comprises a gas inlet pipe and a heating device for heating gas in the gas inlet pipe, and the gas inlet pipe is inserted into the ionization cavity from one end of the sampling pipe. The method has the characteristics of wide detection application range, high ionization efficiency, high detection sensitivity, low requirement on vacuum degree and capability of detecting volatile liquid samples.
Description
Technical Field
The utility model relates to a mass spectrometry analysis detects the field, especially relates to a low frequency radio frequency glow discharge ionization device.
Background
According to the definition of the world health organization, the volatile organic compound refers to a class of organic compounds which have a saturated vapor pressure of more than 133.3Pa at room temperature, a boiling point range of 50-250 ℃ and exist in the air in the form of vapor at room temperature. The main sources of volatile organic compounds are building materials, interior decoration materials, living and office supplies, outdoor industrial waste gas, automobile exhaust, photochemical smog and the like. Many of the volatile organic compounds are carcinogenic, teratogenic, mutagenic, and pose a threat to environmental safety and human survival and proliferation. When the concentration of volatile organic compounds in indoor air is too high, acute poisoning is easily caused, and mild people have symptoms such as headache, dizziness, cough, nausea, vomiting and the like, and severe people can cause convulsion, coma or memory deterioration.
The detection method of volatile organic compounds commonly used in China mainly comprises a chromatography method, a spectrometry method and a mass spectrometry method, and specifically comprises a gas chromatography-flame ionization detection method, a Fourier infrared spectrometry method, a photoionization detection method and a gas chromatography-mass spectrometry combined method.
The gas chromatography-flame ionization detection technology has response to most volatile organic compounds, is equal-carbon response, and is suitable for monitoring the total amount of the volatile organic compounds.
The Fourier infrared detection technology has wide detection spectrum range, can simultaneously detect the content of characteristic components of various volatile organic compounds, has quick determination, no damage to samples, small using amount, simple and convenient operation and higher analysis sensitivity.
The photoionization detector method has weak response to low-carbon saturated hydrocarbon, inconsistent response factors and easy pollution on the surface of the detector, and is not suitable for online monitoring of volatile organic compounds of a pollution source.
The gas chromatography-mass spectrometry combined method has the advantages of high separation and resolution capability of gas chromatography and rapid simultaneous qualitative and quantitative analysis of mass spectra, and is the most common volatile organic compound detection method at present.
For samples with uncomplicated matrixes, the mass spectrometer can also be used alone for detecting volatile organic compounds for the purpose of simplifying the instrument. At present, the ionization sources commonly used for detecting volatile organic compounds by a mass spectrometer mainly comprise an electron bombardment source and an ultraviolet light ionization source, and the two ionization sources can also be used as interfaces of a gas chromatography-mass spectrometer.
The ionization efficiency of the electron bombardment source is high, the sensitivity is high, and abundant structural information can be provided, but the sample must be gasified and is not suitable for the sample which is difficult to volatilize and has poor thermal stability, and the spectrum is complex and difficult to resolve.
The ultraviolet ionization source can enable organic molecules with ionization energy lower than photon energy to generate soft ionization, mainly generates molecular ions, is combined with the mass spectrometer to detect high molecular ion response signals, basically generates no fragment ions, and can realize real-time online monitoring and qualitative and quantitative analysis of volatile organic compounds. However, the light window material of the ultraviolet ionization source limits the energy of photons which can be emitted, and has poor luminous flux and stability, large volume and high manufacturing cost.
The utility model discloses metal ion in low frequency radio frequency glow discharge ionization source can detect characteristic composition, organic solvent and the water of multiple volatile organic compounds simultaneously, and it is wider to have the detection range of application, and ionization efficiency is high, and detectivity is high, requires lower characteristics to the vacuum. Compared with the common discharge frequency of glow discharge of 13.56M, the utility model discloses 1-5M's discharge frequency energy consumption is low, the interference is little and simple structure, the low price.
SUMMERY OF THE UTILITY MODEL
The utility model discloses aim at solving one of the technical problem that exists among the prior art at least. Therefore, the utility model provides a low frequency radio frequency glow discharge ionization device has the detection range of application wider, and ionization efficiency is high, and detectivity is high, requires lower characteristics to the vacuum.
The utility model adopts the technical proposal that: a low-frequency radio frequency glow discharge ionization device comprises an ionization source shell with an ionization cavity, a sample introduction unit and an auxiliary air inlet unit;
the sample introduction unit comprises a metal sample introduction pipe and a heating cylinder sleeved with the sample introduction pipe, a heating rod is arranged in the heating cylinder, the sample introduction pipe is inserted into the ionization cavity, and an analyte outlet used for being connected with the mass spectrometer is formed in one end, opposite to the sample introduction pipe, of the ionization source shell;
the ionization chamber is internally provided with an ionization source and an electrode plate group capable of exciting an electric field, and charged analyte ions move from the end of the sample introduction pipe to the direction of the analyte outlet under the guidance of the electric field;
the auxiliary gas inlet unit comprises a gas inlet pipe and a heating device for heating gas in the gas inlet pipe, and the gas inlet pipe is inserted into the ionization cavity from one end of the sampling pipe.
Further optimize, the ionization source includes that the multiunit is established cylinder pole in the ionization chamber, the cylinder pole sets up to analyte export direction along advancing the appearance pipe, the multiunit the cylinder pole encloses into a cylindrical ionization region, every group the cylinder pole is established ties in turn by conducting block and insulating piece and forms, and is adjacent all communicate through paster electric capacity and paster resistance between the conducting block, the conducting block at cylinder pole both ends links to each other with radio frequency power supply and exerts different direct current voltage, and advances the voltage of the conducting block of appearance pipe end and is higher than the conducting block voltage of analyte exit end.
Further optimize, the electrode plate group comprises positive electrode plate and negative electrode plate that relative setting constitutes, positive electrode plate is located the one end of advancing the appearance pipe, negative electrode plate is located the one end of analyte export, direct current voltage is all applyed to positive electrode plate and negative electrode plate, and the direct current voltage on the positive electrode plate is higher than the voltage of negative electrode plate.
Further preferably, the conducting block and the insulating sheet are formed by connecting insulating fixing rods in series, and two ends of each insulating fixing rod are respectively connected with the positive electrode plate and the negative electrode plate.
Further preferably, the analyte outlet is arranged in the middle of the negative electrode plate and is a conical hole.
Further preferably, a vacuum pumping hole is formed in the ionization source shell, and a vacuum gauge is connected to the vacuum pumping hole.
Further optimize, the heating rod is the ceramic heating rod, the ceramic heating rod by wrap up in the heating barrel.
Further preferably, a sealing sleeve is arranged outside the heating cylinder and is fixedly connected to the ionization source shell through the sealing sleeve.
Further optimize, the intake pipe is copper material can effectively conduct heat, and to the difference that detects the sample, can choose not to apply gas or apply different gas and assist the effective ionization of the sample that needs measuring of heating help.
Further preferably, the ionization source shell is a stainless steel body, and ground potential is applied.
Further optimizing, the number of the cylindrical rods is four.
According to the utility model discloses low frequency radio frequency glow discharge ionization device has following beneficial effect at least:
1. the detection range is wide, the device can be used as an independent glow discharge ionization source to be used with a mass spectrometer for detecting volatile gas samples and liquid samples, and can also be used as an interface of a chromatograph and a mass spectrometer;
2. the ionization efficiency is high, and a heating rod can be used for heating a sample to be analyzed, so that the sample to be analyzed can be more easily subjected to dissociation and ionization, and the sensitivity of a detection signal can be improved;
3. the requirement on the vacuum degree is low;
4. volatile gas detectable samples can also be detected as liquid samples.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
fig. 1 is a schematic plan structure diagram of a low-frequency radio frequency glow discharge ionization device according to an embodiment of the present invention.
Detailed Description
Reference will now be made in detail to the embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below with reference to the drawings are exemplary only for the purpose of explaining the present invention, and should not be construed as limiting the present invention.
In the description of the present invention, it should be understood that the orientation or positional relationship indicated with respect to the orientation description, such as up, down, front, rear, left, right, etc., is based on the orientation or positional relationship shown in the drawings, and is only for convenience of description and simplification of description, and does not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
In the description of the present invention, a plurality of means are one or more, a plurality of means are two or more, and the terms greater than, less than, exceeding, etc. are understood as not including the number, and the terms greater than, less than, within, etc. are understood as including the number. If the first and second are described for the purpose of distinguishing technical features, they are not to be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated or implicitly indicating the precedence of the technical features indicated.
In the description of the present invention, unless there is an explicit limitation, the words such as setting, installation, connection, etc. should be understood in a broad sense, and those skilled in the art can reasonably determine the specific meanings of the above words in combination with the specific contents of the technical solution.
Referring to the schematic plane structure diagram of the low-frequency radio frequency glow discharge ionization device shown in fig. 1, the low-frequency radio frequency glow discharge ionization device is characterized in that: comprises an ionization source housing 100 with an ionization chamber 110, a sample introduction unit 200 and an auxiliary air intake unit 300;
the sample introduction unit 200 comprises a metal type sample introduction tube 210 and a heating cylinder 220 sleeved with the sample introduction tube 210, a heating rod 230 is arranged in the heating cylinder 220, the sample introduction tube 210 is inserted into the ionization chamber 110, and an analyte outlet 120 for connecting with a mass spectrometer is arranged at one end, opposite to the sample introduction tube 210, of the ionization source shell 100;
an ionization source and an electrode plate group capable of exciting an electric field are arranged in the ionization cavity 110, and charged analyte ions move from the end of the sample introduction pipe to the direction of an analyte outlet under the guidance of the electric field;
the auxiliary gas inlet unit 300 includes a gas inlet pipe 310 and a heating device 320 for heating gas in the gas inlet pipe 310, and the gas inlet pipe 310 is inserted into the ionization chamber 110 from one end of the sample introduction pipe 210. The heating device 320 is a heating resistor, and the heating resistor is closely attached to the outside of the air inlet pipe 310 and used for heating the auxiliary gas, so that the auxiliary gas is easier to assist in ionization. The whole auxiliary air inlet unit is fixed on the ionization source shell 100 through a fixing sleeve.
When the low-frequency radio frequency glow discharge ionization device is used as a glow discharge ionization source and is used with a mass spectrum to detect a volatile gas sample, the volatile gas sample enters through the sample inlet pipe 210. The ceramic heating rod 230 generates heat and conducts the heat to the sample inlet pipe 210 through the stainless steel heating cylinder, so that the volatile gas sample is heated and is easier to decompose and ionize.
The heated volatile organic compounds then enter the ionization chamber 110 where they are dissociated and ionized by the ionization source to form charged analyte ions. The charged analyte ions are directed to the analyte outlet 120 by the action of the electric field formed between the electrode plate sets for detection in the mass analyser. The ceramic heating rod is used for heating a sample to be analyzed, so that the sample to be analyzed is easier to decompose and ionize, and the sensitivity of a detection signal can be improved.
When the low frequency radio frequency glow discharge ionization device of this application detects volatile liquid sample, can let in nitrogen gas or inert gas and await measuring volatile liquid sample and sweep, then with the hose will await measuring the export of volatile liquid sample splendid attire household utensils with the utility model discloses the sample inlet pipe 210 links to each other, gets into in the ionization chamber 110 afterwards.
The utility model discloses some non-volatile liquid sample of detection also, liquid sample directly lets in into the appearance pipe 210 and advances the appearance, applys the direct current voltage that is greater than 200V on appearance pipe 210 and in order to help its ionization.
The utility model discloses a set up the gas sample that heating rod 220 can heat the intraductal on advancing appearance pipe 210 for the gas sample is getting into ionization chamber 110 ionization more easily, improves the sensitivity of detected signal, has reduced the demand to the vacuum.
In this embodiment, the ionization source includes a plurality of sets of cylindrical rods 400 disposed in the ionization chamber 110, the cylindrical rods 400 are disposed along a direction from the sample inlet tube to the analyte outlet, a cylindrical ionization region is defined by the plurality of sets of cylindrical rods 400, each set of cylindrical rods 400 is formed by alternately connecting conductive blocks 410 and insulating sheets 420 in series, adjacent conductive blocks 410 are communicated with each other through a patch capacitor 500 and a patch resistor 600, the conductive blocks 410 at two ends of the cylindrical rods 400 are connected with a radio frequency power supply and are applied with different dc voltages, and the voltage of the conductive block 410 at the sample inlet tube 210 end is higher than the voltage of the conductive block 410 at the analyte outlet 120 end.
The conductive blocks 410 on the cylindrical rod 400 are connected with a low-frequency radio frequency power supply, the radio frequency is adjustable within 1-5M, and the radio frequency electricity between the adjacent conductive blocks 410 is conducted through the patch capacitor 500.
The rightmost conductive block 410 on the cylindrical rod 400 is applied with a dc voltage of about 150V, the leftmost conductive block 410 on the rod is applied with a dc voltage of about 80V, and the dc current between the adjacent conductive blocks is conducted through the chip resistor 600.
The sample is ionized in a cylindrical region surrounded by sets of cylindrical rods 400. Compare in glow discharge frequency 13.56M commonly used, the utility model discloses 1-5M's discharge frequency energy consumption is low, and low radio frequency can make the ionization source little to external interference, reduces impurity peak and consumes energy fewly.
In this embodiment, the electrode plate set comprises two oppositely disposed positive electrode plates 710 and negative electrode plates 720, the positive electrode plates 710 are located at one end of the sample inlet tube, the negative electrode plates 720 are located at one end of the analyte outlet tube, the positive electrode plates 710 and the negative electrode plates 720 both apply a dc voltage, and the dc voltage on the positive electrode plates 710 is higher than the voltage of the negative electrode plates 720.
Wherein, the positive electrode plate 710 applies a dc voltage of about 200V, the negative electrode plate 720 applies a dc voltage of about 50V, which is lower than the voltage on the positive electrode plate 710, an electric field is formed between the positive electrode plate 710 and the negative electrode plate 720, and under the guidance of the electric field, the ions to be analyzed are transported from one end of the sampling tube to one end of the analyte outlet, and enter the mass spectrometer for analysis and detection.
In this embodiment, the electrode plate 710 and the negative electrode plate 720 are both stainless steel plates, and the two stainless steel plates are fixed on the ionization source casing 100 by a teflon fixing block.
The conductive block 410 and the insulating sheet 420 are formed by connecting insulating fixing bars 430 in series, and both ends of the insulating fixing bars 430 are connected to the positive electrode plate 710 and the negative electrode plate 720, respectively.
In this embodiment, the conductive blocks 410 and the insulating sheets 420 are formed by serially connecting teflon fixing rods, the number of the cylindrical rods 400 is six, and four groups are formed to surround a cylindrical area, two ends of the cylindrical rods 400 are connected with the stainless steel plate, and the insulating sheets 420 are connected to achieve the insulating connection.
In this embodiment, the analyte outlet 120 opens in the middle of the negative electrode plate 720, and the analyte outlet 120 is a conical bore. The conical hole is located in the middle of the negative electrode plate 720 and in the ionization region surrounded by the four sets of cylindrical rods 400. The ionized analyte enters the mass spectrometer from the conical hole for analysis.
The ionization source housing 100 is provided with a vacuum pumping port 130, and the vacuum pumping port 130 is connected with a vacuum gauge 131. The ionization source enclosure 100 is provided with a vacuum pumping port 130 to maintain the pressure of the entire ionization chamber 110 at about 50 Pa. The vacuum pumping port 130 is further connected to a vacuum gauge 131 for measuring low vacuum, which is used for monitoring the pressure in the ionization chamber in real time.
The ionization efficiency is better when the vacuum degree of the volatile gas sample is maintained at about 1-60Pa, and the ionization efficiency is better when the vacuum degree of the liquid sample is maintained at about 100 Pa.
The heating cartridge 220 is externally provided with a sealing sleeve 240 and is fixedly connected to the ionization source housing 100 through the sealing sleeve 240. The sealing sleeve 240 is made of a polytetrafluoroethylene insulating material, so that heat can be effectively insulated and external interference can be shielded.
The sample inlet pipe 210 is made of stainless steel and is used for introducing a sample to be measured. The sample inlet tube may also apply a voltage higher than 200V to aid in ionization of the liquid sample, depending on the sample being tested.
The ionization source enclosure 100 is a stainless steel body and is applied to ground potential. To improve the sensitivity of detection and reduce quenching of analyte ions by collisions with background gas, the entire ionization chamber 110 is sealed with an ionization source enclosure 100.
The ionization source housing 100 is used for sealing the ionization chamber 110 and shielding the external interference to the radio frequency discharge in the ionization chamber 110, and is made of stainless steel material and applied with ground potential.
The utility model discloses not only expanded the range of application of glow discharge ionization source, its detection method who allies oneself with the mass spectrograph jointly can detect the characteristic composition of multiple volatile organic compounds simultaneously moreover, has the detection range of application wide, and the energy consumption is low, the interference is little, require lower, the higher and simple structure low price characteristics of sensitivity to the vacuum. The ionization source can be used to detect volatile organic liquid samples by purging and to directly detect metal ions in some non-volatile liquid samples.
Of course, the present invention is not limited to the above-mentioned embodiments, and those skilled in the art can make equivalent modifications or substitutions without departing from the spirit of the present invention, and such equivalent modifications or substitutions are included in the scope defined by the claims of the present application.
Claims (10)
1. A low frequency radio frequency glow discharge ionization apparatus characterized by: comprises an ionization source shell (100) with an ionization cavity (110), a sample introduction unit (200) and an auxiliary air inlet unit (300);
the sample introduction unit (200) comprises a metal type sample introduction tube (210) and a heating cylinder (220) sleeved with the sample introduction tube (210), a heating rod (230) is arranged in the heating cylinder (220), the sample introduction tube (210) is inserted into the ionization chamber (110), and an analyte outlet (120) used for being connected with a mass spectrometer is arranged at one end, opposite to the sample introduction tube (210), of the ionization source shell (100);
an ionization source and an electrode plate group capable of exciting an electric field are arranged in the ionization cavity (110), and charged analyte ions move towards an analyte outlet from the end of the sample introduction pipe under the guidance of the electric field;
the auxiliary gas inlet unit (300) comprises a gas inlet pipe (310) and a heating device (320) for heating gas in the gas inlet pipe (310), wherein the gas inlet pipe (310) is inserted into the ionization chamber (110) from one end of a sample inlet pipe (210).
2. The low frequency radio frequency glow discharge ionization apparatus of claim 1 wherein: the ionization source includes that the multiunit is established cylinder pole (400) in ionization chamber (110), cylinder pole (400) are followed sample injection pipe and are set up to analyte export direction, the multiunit cylinder pole (400) enclose into a cylindrical ionization region, every group cylinder pole (400) are established ties in turn by conducting block (410) and insulating piece (420) and are formed, and are adjacent all communicate through paster electric capacity (500) and paster resistance (600) between conducting block (410), conducting block (410) at cylinder pole (400) both ends link to each other with radio frequency power supply and apply different direct current voltage, and the voltage of conducting block (410) of sample injection pipe end is higher than conducting block (410) voltage of analyte exit end.
3. A low frequency radio frequency glow discharge ionization apparatus as claimed in claim 2 wherein: the electrode plate group comprises a positive electrode plate (710) and a negative electrode plate (720) which are oppositely arranged, the positive electrode plate (710) is positioned at one end of the sample inlet pipe, the negative electrode plate (720) is positioned at one end of the analyte outlet, direct current voltage is applied to the positive electrode plate (710) and the negative electrode plate (720), and the direct current voltage on the positive electrode plate (710) is higher than the voltage of the negative electrode plate (720).
4. A low frequency radio frequency glow discharge ionization apparatus as claimed in claim 3 wherein: the conductive block (410) and the insulating sheet (420) are formed by connecting insulating fixing rods (430) in series, and two ends of each insulating fixing rod (430) are respectively connected with the positive electrode plate (710) and the negative electrode plate (720) in an insulating mode.
5. A low frequency radio frequency glow discharge ionization apparatus as claimed in claim 3 or 4 wherein: the analyte outlet (120) is arranged in the middle of the negative electrode plate (720), and the analyte outlet (120) is a conical hole.
6. A low frequency radio frequency glow discharge ionization apparatus as claimed in any one of claims 1 to 4 wherein: the ionization source is characterized in that a vacuum pumping hole (130) is formed in the ionization source shell (100), and a vacuum gauge (131) is connected to the vacuum pumping hole (130).
7. A low frequency radio frequency glow discharge ionization apparatus as claimed in any one of claims 1 to 4 wherein: the heating rod (230) is a ceramic heating rod, and the ceramic heating rod is wrapped in the heating cylinder (220).
8. A low frequency radio frequency glow discharge ionization apparatus as claimed in any one of claims 1 to 4 wherein: and a sealing sleeve (240) is arranged outside the heating cylinder (220) and is fixedly connected to the ionization source shell (100) through the sealing sleeve (240).
9. A low frequency radio frequency glow discharge ionization apparatus as claimed in any one of claims 1 to 4 wherein: the ionization source shell (100) is a stainless steel body and is applied with ground potential.
10. A low frequency radio frequency glow discharge ionization apparatus as claimed in any one of claims 2 to 4 wherein: the number of the cylindrical rods (400) is four.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922272923.3U CN211125573U (en) | 2019-12-16 | 2019-12-16 | Low-frequency radio-frequency glow discharge ionization device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201922272923.3U CN211125573U (en) | 2019-12-16 | 2019-12-16 | Low-frequency radio-frequency glow discharge ionization device |
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| Publication Number | Publication Date |
|---|---|
| CN211125573U true CN211125573U (en) | 2020-07-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201922272923.3U Expired - Fee Related CN211125573U (en) | 2019-12-16 | 2019-12-16 | Low-frequency radio-frequency glow discharge ionization device |
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| CN (1) | CN211125573U (en) |
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- 2019-12-16 CN CN201922272923.3U patent/CN211125573U/en not_active Expired - Fee Related
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