CN110993480B - A low frequency radio frequency glow discharge ionization device - Google Patents
A low frequency radio frequency glow discharge ionization device Download PDFInfo
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Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
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- H01J49/10—Ion sources; Ion guns
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- Physics & Mathematics (AREA)
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Abstract
本发明公开了一种低频射频辉光放电电离装置，包括具有电离腔的电离源外壳、进样单元和辅助进气单元；所述进样单元包括金属型的进样管、套装所述进样管的加热筒，所述加热筒内设有加热棒，所述进样管插入电离腔内，所述电离源外壳正对进样管的一端设有用于和质谱仪相连的分析物出口；所述电离腔内设有电离源和能够激发电场的电极板组，带电分析物离子在电场引导下由进样管端朝分析物出口方向运动；所述辅助进气单元包括进气管和用于加热所述进气管内气体的加热装置，所述进气管从进样管的一端插入所述电离腔内。具有检测应用范围较广，电离效率高，检测灵敏度高，对真空度要求较低及可检测挥发性液体样品的特点。
The invention discloses a low-frequency radio frequency glow discharge ionization device, comprising an ionization source housing with an ionization chamber, a sampling unit and an auxiliary air intake unit; the sampling unit comprises a metal sampling tube, a heating cylinder sleeved with the sampling tube, a heating rod is arranged in the heating cylinder, the sampling tube is inserted into the ionization chamber, and the end of the ionization source housing facing the sampling tube is provided with an analyte outlet for connecting with a mass spectrometer; the ionization chamber is provided with an ionization source and an electrode plate group capable of exciting an electric field, and the charged analyte ions move from the end of the sampling tube toward the analyte outlet under the guidance of the electric field; the auxiliary air intake unit comprises an air intake pipe and a heating device for heating the gas in the air intake pipe, and the air intake pipe is inserted into the ionization chamber from one end of the sampling tube. The device has the characteristics of a wide range of detection applications, high ionization efficiency, high detection sensitivity, low vacuum requirements, and the ability to detect volatile liquid samples.
Description
Technical Field
The invention relates to the field of mass spectrometry analysis and detection, in particular to a low-frequency radio-frequency glow discharge ionization device.
Background
According to the definition of the world health organization, volatile organic compounds are understood to be those which have a saturation vapor pressure of more than 133.3Pa at room temperature, a boiling point in the range from 50 to 250℃and are present in the air in vapor form 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 environmentally safe and pose a threat to human survival. When the concentration of the volatile organic compounds in indoor air is too high, acute poisoning is easy to cause, headache, dizziness, cough, nausea, vomiting and other symptoms occur to light people, and convulsion, coma or memory decline can be caused to heavy people.
The detection method of the volatile organic compounds commonly used in China mainly comprises a chromatography method, a spectrometry method and a mass spectrometry method, and particularly 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 is responsive to most volatile organic compounds, is equal-carbon responsive, and is suitable for monitoring the total amount of the volatile organic compounds.
The Fourier infrared detection technology has wide detection spectrum range, can detect the characteristic component content of various volatile organic compounds simultaneously, has quick measurement, does not destroy samples, has less consumption, is simple and convenient to operate and has higher analysis sensitivity.
The photoionization detector method has weak response to low-carbon saturated hydrocarbon, inconsistent response factors, and easily polluted detector surfaces, and is not suitable for on-line monitoring of pollution source volatile organic compounds.
The gas chromatography-mass spectrometry has the advantages of high separation and resolution of gas chromatography and rapid simultaneous qualitative and quantitative analysis of mass spectrum, and is the most common volatile organic compound detection method at present.
For samples with uncomplicated matrix, the mass spectrometer can be used alone to detect volatile organic compounds for the purpose of simplifying the instrument. The ionization sources commonly used for detecting volatile organic compounds by mass spectrometers at present mainly comprise an electron bombardment source and an ultraviolet ionization source, and the two ionization sources can also be used as interfaces of gas chromatograph-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 complicated spectrum resolution of the spectrogram has certain difficulty.
The ultraviolet light ionization source can enable organic matter molecules with ionization energy lower than photon energy to generate soft ionization, mainly generates molecular ions, has high molecular ion response signals detected by combining the ultraviolet light ionization source with a mass spectrum analyzer, basically generates no fragment ions, and can realize real-time online monitoring and qualitative and quantitative analysis of volatile organic matters. However, the energy of photons which can be emitted is limited by the light window material of the ultraviolet ionization source, the luminous flux and the stability are poor, the volume is large and the manufacturing cost is high.
The low-frequency radio-frequency glow discharge ionization source can detect the characteristic components of various volatile organic compounds, organic solvents and metal ions in water simultaneously, and has the characteristics of wide detection application range, high ionization efficiency, high detection sensitivity and low requirement on vacuum degree. Compared with the common discharge frequency of 13.56M in glow discharge, the discharge frequency of 1-5M in the invention has the advantages of low energy consumption, small interference, simple structure and low price.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides a low-frequency radio-frequency glow discharge ionization device which has the characteristics of wider detection application range, high ionization efficiency, high detection sensitivity and lower requirement on vacuum degree.
The invention adopts the technical scheme that the low-frequency radio-frequency glow discharge ionization device comprises an ionization source shell with an ionization cavity, a sample injection unit and an auxiliary air inlet unit;
the sample injection unit comprises a metal sample injection tube and a heating cylinder sleeved with the sample injection tube, a heating rod is arranged in the heating cylinder, the sample injection tube is inserted into the ionization cavity, and one end of the ionization source shell, which is opposite to the sample injection tube, is provided with an analyte outlet which is used for being connected with the mass spectrometer;
An ionization source and an electrode plate group capable of exciting an electric field are arranged in the ionization cavity, and charged analyte ions move towards an analyte outlet from a sample injection pipe end under the guidance of the electric field;
the auxiliary air inlet unit comprises an air inlet pipe and a heating device for heating air in the air inlet pipe, and the air inlet pipe is inserted into the ionization cavity from one end of the sample inlet pipe.
Further preferably, the ionization source comprises a plurality of groups of cylindrical rods arranged in the ionization cavity, the cylindrical rods are arranged along the direction from the sample inlet pipe to the analyte outlet, a plurality of groups of cylindrical rods enclose a cylindrical ionization area, each group of cylindrical rods is formed by alternately connecting conductive blocks and insulating sheets in series, adjacent conductive blocks are communicated through a patch capacitor and a patch resistor, the conductive blocks at two ends of the cylindrical rods are connected with a radio-frequency power supply and are applied with different direct-current voltages, and the voltage of the conductive blocks at the end of the sample inlet pipe is higher than that of the conductive blocks at the outlet end of the analyte.
Further preferably, the electrode plate group comprises a positive electrode plate and a negative electrode plate which are oppositely arranged, the positive electrode plate is positioned at one end of the sample inlet tube, the negative electrode plate is positioned at one end of the analyte outlet, direct-current voltage is applied to the positive electrode plate and the negative electrode plate, and the direct-current voltage on the positive electrode plate is higher than the voltage of the negative electrode plate.
Further preferably, the conductive 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 formed in the middle of the negative electrode plate, and the analyte outlet is a conical hole.
Further preferably, the ionization source shell is provided with a vacuum extraction opening, and the vacuum extraction opening is connected with a vacuum gauge.
Further preferably, the heating rod is a ceramic heating rod, and the ceramic heating rod is wrapped in the heating cylinder.
Further preferably, the heating cylinder is externally provided with a sealing sleeve and is fixedly connected to the ionization source shell through the sealing sleeve.
Further optimizing, the intake pipe is copper material and can effectively conduct heat, and according to the difference of detection samples, gas can be selected to be not applied or different gases can be applied, and heating is assisted to help the effective ionization of the samples to be detected.
Further preferably, the ionization source housing is a stainless steel body and a ground potential is applied.
Further preferably, the number of the cylindrical rods is four.
The low-frequency radio-frequency glow discharge ionization device provided by the embodiment of the invention has at least the following beneficial effects:
1. The detection range is wide, and the device can be used for detecting volatile gas samples and liquid samples by being used as an independent glow discharge ionization source and a mass spectrometer, 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 is easier to decompose and ionize, and the sensitivity of a detection signal can be improved;
3. The vacuum degree requirement is low;
4. volatile gas samples may be detected as well as liquid samples.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
fig. 1 is a schematic plan view of a low-frequency rf glow discharge ionization apparatus according to an embodiment of the present invention.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative only and are not to be construed as limiting the invention.
In the description of the present invention, it should be understood that references to orientation descriptions such as upper, lower, front, rear, left, right, etc. are based on the orientation or positional relationship shown in the drawings, are merely for convenience of description of the present invention and to simplify the description, and do not indicate or imply that the apparatus or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus should not be construed as limiting the present invention.
In the description of the present invention, a number means one or more, a number means two or more, and greater than, less than, exceeding, etc. are understood to not include the present number, and above, below, within, etc. are understood to include the present number. The description of the first and second is for the purpose of distinguishing between technical features only and should not be construed 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 explicitly defined otherwise, terms such as arrangement, installation, connection, etc. should be construed broadly and the specific meaning of the terms in the present invention can be reasonably determined by a person skilled in the art in combination with the specific contents of the technical scheme.
Referring to a schematic plan structure 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 by comprising an ionization source housing 100 with an ionization cavity 110, a sample introduction unit 200 and an auxiliary air inlet unit 300;
The sample injection unit 200 comprises a metal sample injection tube 210 and a heating cylinder 220 sleeved with the sample injection tube 210, a heating rod 230 is arranged in the heating cylinder 220, the sample injection tube 210 is inserted into the ionization cavity 110, and one end of the ionization source housing 100, which is opposite to the sample injection tube 210, is provided with an analyte outlet 120 for connecting with a mass spectrometer;
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 a sample injection pipe end under the guidance of the electric field;
The auxiliary air intake unit 300 includes an air intake pipe 310 and a heating device 320 for heating air in the air intake pipe 310, and the air intake 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 is used for heating the auxiliary gas, so that the auxiliary gas is easier to assist ionization. The entire auxiliary air intake unit is secured to the ionization source housing 100 by a retaining sleeve.
When the low-frequency radio-frequency glow discharge ionization device is used as a glow discharge ionization source and is used for detecting a volatile gas sample in combination with mass spectrometry, the volatile gas sample enters through the sampling tube 210. The ceramic heating rod 230 heats the sample feeding tube 210 through the conduction of the stainless steel heating cylinder, so that the volatile gas sample is heated and is more easily decomposed and ionized.
The heated volatile organic compounds then enter ionization chamber 110 where they are dissociated by the ionization source to form charged analyte ions. The action of the electric field formed by the charged analyte ions between the electrode plate groups is directed to the analyte outlet 120 for detection into the mass spectrometer. 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 detection signals can be improved.
When the low-frequency radio-frequency glow discharge ionization device detects the volatile liquid sample, nitrogen or inert gas can be introduced into the volatile liquid sample to be detected for purging, and then the outlet of the volatile liquid sample containing vessel to be detected is connected with the sample inlet tube 210 by a hose and then enters the ionization cavity 110.
The invention can also detect some non-volatile liquid samples, the liquid samples are directly introduced into the sample inlet pipe 210 for sample introduction, and a direct current voltage of more than 200V is applied to the sample inlet pipe 210 to assist ionization of the liquid samples.
According to the invention, the heating rod 220 is arranged on the sample injection pipe 210, so that the gas sample in the heating pipe can be ionized more easily when entering the ionization cavity 110, the sensitivity of a detection signal is improved, and the requirement on vacuum degree is reduced.
In this embodiment, the ionization source includes a plurality of groups of cylindrical rods 400 disposed in the ionization chamber 110, the cylindrical rods 400 are disposed along the direction from the sample inlet tube to the analyte outlet, the plurality of groups of cylindrical rods 400 enclose a cylindrical ionization region, each group of cylindrical rods 400 is formed by alternately connecting conductive blocks 410 and insulating sheets 420 in series, the adjacent conductive blocks 410 are all connected through the chip capacitor 500 and the chip resistor 600, the conductive blocks 410 at two ends of the cylindrical rods 400 are connected with a radio frequency power supply and apply different direct current voltages, and the voltage of the conductive blocks 410 at the end of the sample inlet tube 210 is higher than the voltage of the conductive blocks 410 at the end of the analyte outlet 120.
The conductive blocks 410 on the cylindrical rod 400 are connected with a low-frequency radio-frequency power supply, the radio-frequency is adjustable between 1M and 5M, and radio-frequency electricity between adjacent conductive blocks 410 is conducted through the patch capacitor 500.
The rightmost conductive block 410 on the cylindrical rod 400 applies a dc voltage of about 150V, the leftmost conductive block 410 on the rod applies a dc voltage of about 80V, and the dc between adjacent conductive blocks is conducted through the chip resistor 600.
The sample is ionized in a cylindrical region surrounded by a plurality of sets of cylindrical rods 400. Compared with the common discharge frequency of 13.56M in glow discharge, the discharge frequency of 1-5M in the invention has low energy consumption, and the low radio frequency can lead the ionization source to have small interference to the outside, reduce impurity peaks and have low energy consumption.
In this embodiment, the electrode plate group comprises two positive electrode plates 710 and negative electrode plates 720 which are oppositely arranged, the positive electrode plates 710 are positioned at one end of the sample tube, the negative electrode plates 720 are positioned at one end of the analyte outlet, the positive electrode plates 710 and the negative electrode plates 720 are both applied with direct current voltage, and the direct current 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 ions to be analyzed are transmitted from one end of the sample inlet tube to one end of the analyte outlet under the guidance of the electric field, and enter the mass spectrometer for analysis detection.
In the present embodiment, the electrode plate 710 and the negative electrode plate 720 are both stainless steel plates, and both stainless steel plates are fixed to the ionization source case 100 by polytetrafluoroethylene fixing blocks.
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 respectively connected with the positive electrode plate 710 and the negative electrode plate 720.
In this embodiment, the conductive block 410 and the insulating sheet 420 are formed by connecting polytetrafluoroethylene fixing rods in series, the number of the cylindrical rods 400 is six, four groups are formed, a cylindrical area is enclosed, two ends of the cylindrical rods 400 are connected with stainless steel plates, and the insulating sheet 420 is connected to achieve the function of insulating connection.
In this embodiment, the analyte outlet 120 is open in the middle of the negative electrode plate 720, and the analyte outlet 120 is a conical hole. The conical hole is located in the middle of the negative electrode plate 720 and in the ionization region enclosed 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 housing 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 also connected with a vacuum gauge 131 for measuring the low vacuum for monitoring the air pressure in the ionization chamber in real time.
Wherein, the vacuum degree of the volatile gas sample is maintained at about 1 Pa to 60Pa, the ionization efficiency is better, and the vacuum degree of the liquid sample is maintained at about 100Pa, and the ionization efficiency is better.
The heating cartridge 220 is externally provided with a sealing sleeve 240 and is fixedly connected to the ionization source housing 100 by the sealing sleeve 240. The sealing sleeve 240 is made of polytetrafluoroethylene insulating material, so that the sealing sleeve can effectively insulate heat and shield external interference.
The sample tube 210 is made of stainless steel and is used for introducing a sample to be tested. The sample introduction tube may also be applied with a voltage higher than 200V for the detection sample to assist ionization of the liquid sample.
The ionization source enclosure 100 is a stainless steel body and is grounded. To increase the sensitivity of detection, the entire ionization chamber 110 is sealed with the ionization source enclosure 100 to reduce quenching by collisions of analyte ions with background gas.
The ionization source housing 100 is used for sealing the ionization chamber 110 and shielding the interference of the outside to the radio frequency discharge in the ionization chamber 110, and is made of stainless steel material and is applied with a ground potential.
The invention not only expands the application range of the glow discharge ionization source, but also can detect the characteristic components of various volatile organic compounds simultaneously by the detection method combined with a mass spectrometer, and has the characteristics of wide detection application range, low energy consumption, small interference, lower requirement on vacuum degree, higher sensitivity, simple structure and low price. The ionization source can be used to detect volatile organic liquid samples by purging and to directly detect metal ions in certain non-volatile liquid samples.
Of course, the present application is not limited to the above-described embodiments, and those skilled in the art can make equivalent modifications or substitutions without departing from the spirit of the present application, and these equivalent modifications or substitutions are included in the scope of the present application as defined in the appended claims.
Claims (7)
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| CN106298428A (en) * | 2016-09-23 | 2017-01-04 | 四川大学 | Microwave Induced Plasma ionic migration spectrometer |
| CN211125573U (en) * | 2019-12-16 | 2020-07-28 | 华南师范大学 | Low-frequency radio-frequency glow discharge ionization device |
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| US6586731B1 (en) * | 1999-04-12 | 2003-07-01 | Mds Inc. | High intensity ion source apparatus for mass spectrometry |
| CN102103970B (en) * | 2011-01-18 | 2013-08-14 | 四川大学 | Microwave plasma generator and proton transfer mass spectrometer |
| CN202167454U (en) * | 2011-07-01 | 2012-03-14 | 上海大学 | A multi-pole proton transfer reaction device |
| CN105632869A (en) * | 2014-11-06 | 2016-06-01 | 中国科学院大连化学物理研究所 | Vacuum ultraviolet light ionization source device based on glow discharge |
| CN104538279B (en) * | 2014-12-25 | 2016-11-30 | 华南师范大学 | A kind of radio frequency glow discharge ionization device |
| CN108091545B (en) * | 2016-11-21 | 2019-11-29 | 中国科学院大连化学物理研究所 | A kind of ultraviolet light ionization source for mass spectral analysis |
| CN108091540B (en) * | 2016-11-21 | 2019-10-25 | 中国科学院大连化学物理研究所 | A radio frequency focusing enhanced vacuum ultraviolet light mass spectrometry ionization source |
| CN109686647B (en) * | 2018-12-12 | 2021-06-29 | 上海裕达实业有限公司 | Multi-stage ion guide and mass spectrometer |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106298428A (en) * | 2016-09-23 | 2017-01-04 | 四川大学 | Microwave Induced Plasma ionic migration spectrometer |
| CN211125573U (en) * | 2019-12-16 | 2020-07-28 | 华南师范大学 | Low-frequency radio-frequency glow discharge ionization device |
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