CN111739783A - Atmospheric pressure electric arc ion source for small mass spectrometer and detection method thereof - Google Patents
Atmospheric pressure electric arc ion source for small mass spectrometer and detection method thereof Download PDFInfo
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- CN111739783A CN111739783A CN202010467900.2A CN202010467900A CN111739783A CN 111739783 A CN111739783 A CN 111739783A CN 202010467900 A CN202010467900 A CN 202010467900A CN 111739783 A CN111739783 A CN 111739783A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/12—Ion sources; Ion guns using an arc discharge, e.g. of the duoplasmatron type
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- 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
- G01N27/68—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 using electric discharge to ionise a gas
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Abstract
The invention discloses an atmospheric pressure electric arc ion source for a small-sized mass spectrometer and a detection method thereof, wherein the ion source comprises an ion source main body and a power supply, wherein the power supply comprises a power supply main body and a connecting lead and is used for providing electric energy for the ion source main body; the ion source main body comprises a discharge electrode, an insulating shell and an insulating protector; the discharge electrode is used for generating discharge arc, the insulating shell is wrapped outside the discharge electrode and does not wrap the two ends of the discharge electrode, and the insulating shell is used for preventing the discharge electrode at the wrapped position from discharging; the discharge electrodes include a first discharge electrode and a second discharge electrode; one end of the discharge electrode is connected with the power supply main body through a connecting lead, and insulation protection is arranged at the connection part of the discharge electrode; the other end of the discharge electrode discharges between the first discharge electrode and the second discharge electrode to generate a discharge arc. The ion source does not need a complex air inlet pipeline and can work discontinuously or continuously under the atmospheric pressure condition directly.
Description
Technical Field
The invention relates to the technical field of mass spectrometer analysis, in particular to an atmospheric pressure electric arc ion source for a small mass spectrometer and a detection method thereof.
Background
Mass spectrometers, which are among the most sensitive analytical chemical instruments at present, assay samples primarily by detecting their mass-to-nuclear ratio (m/z). Compared with a laboratory mass spectrometer with a large volume, the small mass spectrometer is very suitable for outdoor real-time field detection. Small mass spectrometers have made tremendous progress in design and application over the last decade. The in-situ ionization technology is an important factor for the design of the small mass spectrometer, does not need a complicated laboratory sample preparation process, does not need a specific vacuum condition, simplifies the sample ionization process, and can accelerate the field detection speed of the small mass spectrometer.
The detection of surface traces is an important field of application of small-sized mass spectrometers, such as the detection of explosives on passengers in airports, the screening of food exceeding toxic substances in food markets and supermarkets, and the like. Compared with an ion source mode with other mechanisms, the in-situ ionization designed based on the plasma principle is very suitable for detecting surface solid samples. However, such ion sources are not currently in widespread use because: firstly, an ion source based on a plasma principle usually needs to be introduced with inert gases such as helium and nitrogen at a certain flow rate, and the gases are not suitable for being carried by a small mass spectrometer on site, because the high-pressure gases are dangerous when being used carelessly, and a gas cylinder cannot ensure that the small mass spectrometer is used for a long time; secondly, different from a large-scale mass spectrometer, a small-scale mass spectrometer generally adopts a sample introduction mode of a discontinuous sample introduction interface (DAPI), and most of in-situ ionization based on plasma design is continuous at present, and the in-situ ionization can not be better combined with the small-scale mass spectrometer, so that the problems of sample waste and the like can be caused.
Disclosure of Invention
The present invention is directed to solving, at least to some extent, one of the technical problems in the related art.
To this end, it is an object of the present invention to provide an atmospheric pressure electric arc ion source for a compact mass spectrometer that can operate at atmospheric pressure without the need for an inert gas to generate the plasma.
Another object of the present invention is to provide a detection method.
In order to achieve the above object, an embodiment of an aspect of the present invention provides an atmospheric pressure electric arc ion source for a compact mass spectrometer, including: an ion source body and a power supply;
the power supply comprises a power supply main body and a connecting lead, and is used for providing electric energy for the ion source main body;
the ion source main body comprises a discharge electrode, an insulating shell and an insulating protector; the discharge electrode is used for generating discharge arc, the insulating shell is wrapped outside the discharge electrode and does not wrap the two ends of the discharge electrode, and the insulating shell is used for preventing the discharge electrode at the wrapped position from discharging;
the discharge electrodes include a first discharge electrode and a second discharge electrode;
one end of the discharge electrode is connected with the power supply main body through the connecting lead, and the insulation protection is arranged at the connection position of the discharge electrode;
the other end of the discharge electrode discharges between the first discharge electrode and the second discharge electrode to generate a discharge arc.
The atmospheric pressure electric arc ion source for the small-sized mass spectrometer of the embodiment of the invention belongs to an in-situ ionization ion source based on a plasma principle, and the ionization mode is as follows: through spark thermal desorption and ionization of a sample to be detected between the discharge electrodes, a complex air inlet pipeline is not needed, the sample can directly work discontinuously or continuously under the atmospheric pressure condition, inert gas is not needed to generate plasma, the sample can be detected for multiple times, and a reliable detection result is obtained.
In addition, the atmospheric pressure electric arc ion source for a miniature mass spectrometer according to the above embodiment of the present invention may also have the following additional technical features:
in one embodiment of the present invention, the discharge electrode is a conductive material including a wire, a metal sheet, and a metal block.
In one embodiment of the present invention, the material of the discharge electrode includes platinum, copper and gold.
In one embodiment of the invention, the diameter range of the discharge end of the discharge electrode is greater than or equal to 0.01mm and less than or equal to 20 mm.
In one embodiment of the invention, the power source is pulsed high voltage alternating current or continuous high voltage alternating current.
In one embodiment of the invention, the voltage of the power supply is greater than 500V.
In one embodiment of the present invention, the insulating housing material includes ceramic, silicon and marble.
In one embodiment of the present invention, the discharge voltage and power are adjusted by adjusting a distance between the first discharge electrode and the second discharge electrode.
In one embodiment of the invention, the ion source directly detects the wiped sample surface, and the detection result is obtained by a mass spectrometer.
In order to achieve the above object, another embodiment of the present invention provides a detection method, which uses the above atmospheric pressure electric arc ion source, including the following steps:
wiping the surface of a sample to be tested by using test paper;
electrifying an ion source, and directly detecting the wiper on the surface of the test paper through the ion source;
ionizing the wiper to form charged particles, and sending the charged particles to a sample inlet of a miniature mass spectrometer;
and generating a mass spectrogram through the miniature mass spectrometer, and completing the detection of the surface of the sample to be detected.
The detection method provided by the embodiment of the invention utilizes the atmospheric pressure electric arc ion source, not only can work in the atmosphere and does not need inert gas to generate plasma, but also needs a discontinuous ionization mode, so that a small mass spectrometer can detect a sample for multiple times to obtain a reliable detection result.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing 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 diagram of an atmospheric pressure electric arc ion source for a compact mass spectrometer according to one embodiment of the present invention;
FIG. 2 is a cross-sectional view of an atmospheric pressure electric arc ion source insulator housing and discharge electrode in accordance with one embodiment of the present invention;
FIG. 3 is a schematic diagram of a detection method using an atmospheric pressure arc ion source according to one embodiment of the present invention;
FIG. 4 is a first class diagram of mass spectrum of atmospheric pressure arc ion source for detecting atrazine, a tomato surface pesticide, according to one embodiment of the invention;
FIG. 5 is a second mass spectrum diagram of an atmospheric pressure arc ion source for detecting atrazine, a tomato surface pesticide, according to an embodiment of the invention;
FIG. 6 is a graph of discharge electrode distance versus breakdown voltage for arcing according to one embodiment of the present invention;
FIG. 7 is a graph of discharge electrode distance versus breakdown power for arcing according to one embodiment of the present invention;
FIG. 8 is a flow chart of a method for detection using an atmospheric pressure arc ion source, in accordance with one embodiment of the present invention.
Reference numerals: 10-ion source body, 20-power supply, 101-discharge electrode, 1011-first discharge electrode, 1012-second discharge electrode, 102-insulating shell, 103 discharge spark, 104-insulating protection, 201-power supply body, 202-connecting lead, 301-mass spectrometer interface, 302-detection test paper and 303-charged particles.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the drawings are illustrative and intended to be illustrative of the invention and are not to be construed as limiting the invention.
An atmospheric pressure electric arc ion source for a compact mass spectrometer and a detection method thereof proposed according to an embodiment of the present invention are described below with reference to the accompanying drawings.
The ion source is an important component of a mass spectrometer, and the function of the ion source is to ionize a sample to be tested.
Fig. 1 is a schematic diagram of an atmospheric pressure electric arc ion source for a compact mass spectrometer according to one embodiment of the present invention.
FIG. 2 is a cross-sectional view of an insulating housing and discharge electrode of an atmospheric pressure electric arc ion source in accordance with one embodiment of the present invention.
As shown in fig. 1 and 2, the atmospheric pressure electric arc ion source for a compact mass spectrometer includes: an ion source body 10 and a power supply 20.
The ion source body comprises a discharge electrode 101, an insulating shell 102 and an insulating protection 104, wherein a discharge spark 103 is generated between the discharge electrodes, and the insulating protection 104.
The discharge electrode 101 is used for generating a discharge arc, the insulating casing 102 is wrapped outside the discharge electrode 101 and does not wrap the two ends of the discharge electrode, and the insulating casing 102 is used for preventing the discharge electrode at the wrapped position from discharging.
The insulating housing 102 has high insulation to prevent the high voltage wires from being broken down, and may be made of ceramic, silicon, marble, or the like.
The power supply 20 is used to provide the voltage required for ionization of the ion source. The ion source can directly detect the wiped sample surface, and the result is quickly obtained by combining with a small-sized mass spectrometer.
The discharge electrode 101 includes a first discharge electrode 1011 and a second discharge electrode 1012, wherein the discharge electrode is a conductive material, and the conductive material may be other conductive materials such as a metal wire, a metal sheet, and a metal block. The metal material may be platinum, copper, gold, or the like. As shown in fig. 1 and 2, the discharge electrode is two wires.
The discharge electrode 101 can break down air at the tip to generate an arc without being largely decomposed during the discharge process, and the diameter (or thickness) of the discharge end of the discharge electrode ranges from 0.01mm to 20 mm.
The insulating housing 102 does not wrap both ends of the discharge electrode, and a discharge spark 103 is generated at the non-wrapped tip of the discharge electrode 101; the insulating case 102 is fitted over the discharge electrode 101 for preventing sparks from being generated at positions other than the tip.
The power supply 20 includes a power supply main body 201 and a connection wire 202; the power supply main body 201 is used for supplying pulse alternating current or continuous alternating current; the connecting wire is used for connecting the power supply main body 201 and the discharge electrode 101, and an insulation protection 104 is arranged at the connection part of the discharge electrode and the power supply 20 and used for preventing discharge at the connection part of the discharge electrode 101 and the power supply 20.
In an embodiment of the present invention, the discharge power source of the ion source is a pulsed high voltage alternating current or a continuous high voltage alternating current, and the voltage of the high voltage is usually greater than 500V.
It will be appreciated that because the manner in which the ion source generates ions is relatively intense, the sample need not be in direct contact with the plasma arc. At the same time, compared to other ion sources, the plasma generated by the arc is very intense and close to the sample, and no additional gas flow is required to blow the plasma into the mass spectrometer. Therefore, a complex air inlet pipeline is not needed, in addition, the small mass spectrometer adopts a discontinuous sample inlet interface, so that the air suction quantity of the sample inlet is larger, the introduction of a sample is facilitated, and the ionization mode can also be directly operated discontinuously or continuously under the atmospheric pressure condition.
As shown in fig. 3, the process of ion source operation is illustrated. The ion source can directly detect solid particles on the surface of a sample by a wiping method. Wiping a sample with test paper, ionizing the sample on the test paper through a novel arc ion source, and then allowing the ionized charged object to be detected to enter a sample inlet of a small mass spectrometer to rapidly obtain a mass spectrogram.
Specifically, firstly, the test paper 302 is used for wiping the surface to be tested, then the ion source can directly detect the wiper on the surface of the test paper 302, the wiper is ionized to form charged particles 303, the charged particles enter the mass spectrometer interface 301, and finally a mass spectrogram is formed, so that the object to be tested on the surface of the sample is tested. FIGS. 4 and 5 are views showing wiping of 1ng/mm of the surface of actual tomato samples by the method of FIG. 32The first-level diagram and the second-level diagram of the mass spectrum are obtained by the pesticide atrazine.
As shown in fig. 6 and 7, the relationship between the discharge electrode distance and the breakdown voltage and the breakdown power, which are the minimum voltage and power at which an electric spark is generated, is shown. The user can confirm required discharge voltage and power according to the distance between the discharge electrode (can be the wire), and when voltage is less than the breakdown value, the ion source can not produce the spark, can not carry out normal work.
In summary, the ion source belongs to an in-situ ionization ion source based on the plasma principle, and the ionization method is as follows: the advantage of this ion source over other ion sources, which desorb and ionize the sample to be measured by the spark heat between the discharge electrodes, is that no complex gas inlet line is required, since the arc generates a plasma that is very intense and close to the sample, and no additional gas flow is required to blow the plasma into the mass spectrometer. In addition, the small-sized mass spectrometer adopts a discontinuous sample inlet, so that the gas suction amount of the sample inlet is larger, the introduction of a sample is facilitated, and the ionization mode can also be directly operated discontinuously or continuously under the atmospheric pressure condition.
Next, a detection method proposed according to an embodiment of the present invention is described with reference to the drawings.
FIG. 8 is a flow chart of a method for detection using an atmospheric pressure arc ion source, in accordance with one embodiment of the present invention.
As shown in fig. 8, the detection method includes the steps of:
and S1, wiping the surface of the sample to be tested by using the test paper.
And S2, electrifying the ion source, and directly detecting the wipes on the test paper surface through the ion source.
And S3, ionizing the wiper to form charged particles, and sending the charged particles to a sample inlet of the miniature mass spectrometer.
And S4, generating a mass spectrogram through a miniature mass spectrometer, and completing the detection of the surface of the sample to be tested.
It should be noted that the foregoing explanation of the embodiment of the atmospheric pressure arc ion source also applies to the method of this embodiment, and the details are not repeated here.
According to the detection method provided by the embodiment of the invention, the sample is wiped by using the test paper, the sample on the test paper is ionized by the novel arc ion source, and then the ionized charged object to be detected enters the sample inlet of the miniature mass spectrometer, so that the mass spectrogram is rapidly obtained. Can be directly operated discontinuously or continuously under the atmospheric pressure condition, and does not need inert gas to generate plasma.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. An atmospheric pressure electric arc ion source for a miniature mass spectrometer comprising: an ion source body and a power supply;
the power supply comprises a power supply main body and a connecting lead, and is used for providing electric energy for the ion source main body;
the ion source main body comprises a discharge electrode, an insulating shell and an insulating protector; the discharge electrode is used for generating discharge arc, the insulating shell is wrapped outside the discharge electrode and does not wrap the two ends of the discharge electrode, and the insulating shell is used for preventing the discharge electrode at the wrapped position from discharging;
the discharge electrodes include a first discharge electrode and a second discharge electrode;
one end of the discharge electrode is connected with the power supply main body through the connecting lead, and the insulation protection is arranged at the connection position of the discharge electrode;
the other end of the discharge electrode discharges between the first discharge electrode and the second discharge electrode to generate a discharge arc.
2. The atmospheric pressure electric arc ion source for a miniature mass spectrometer of claim 1 wherein said discharge electrode is a conductive material comprising a wire, a metal sheet and a metal block.
3. The atmospheric pressure electric arc ion source for a miniature mass spectrometer of claim 2 wherein the material of said discharge electrode comprises platinum, copper and gold.
4. The atmospheric pressure electric arc ion source for a miniature mass spectrometer as defined in claim 1, wherein said discharge electrode discharge end has a diameter in the range of 0.01mm or more and 20mm or less.
5. The atmospheric pressure electric arc ion source for a miniature mass spectrometer of claim 1 wherein said power supply is pulsed high voltage alternating current or continuous high voltage alternating current.
6. The atmospheric pressure electric arc ion source for a miniature mass spectrometer of claim 5 wherein the voltage of said power supply is greater than 500V.
7. The atmospheric pressure electric arc ion source for a miniature mass spectrometer of claim 1 wherein said insulating housing material comprises ceramic, silicon and marble.
8. The atmospheric pressure electric arc ion source for a compact mass spectrometer of claim 1, wherein discharge voltage and power are adjusted by adjusting a distance of the first discharge electrode and the second discharge electrode.
9. The atmospheric pressure electric arc ion source for a miniature mass spectrometer of claims 1-8 wherein said ion source directly detects the wiped sample surface and the detection results are obtained by the mass spectrometer.
10. A method of detection using the atmospheric pressure electric arc ion source of claim 1, comprising the steps of:
wiping the surface of a sample to be tested by using test paper;
electrifying an ion source, and directly detecting the wiper on the surface of the test paper through the ion source;
ionizing the wiper to form charged particles, and sending the charged particles to a sample inlet of a miniature mass spectrometer;
and generating a mass spectrogram through the miniature mass spectrometer, and completing the detection of the surface of the sample to be detected.
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