CN102263006A - Mass spectrometry ion source apparatus based on heat auxiliary glow discharge and ionization analysis method thereof - Google Patents
Mass spectrometry ion source apparatus based on heat auxiliary glow discharge and ionization analysis method thereof Download PDFInfo
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- CN102263006A CN102263006A CN201110177040XA CN201110177040A CN102263006A CN 102263006 A CN102263006 A CN 102263006A CN 201110177040X A CN201110177040X A CN 201110177040XA CN 201110177040 A CN201110177040 A CN 201110177040A CN 102263006 A CN102263006 A CN 102263006A
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Abstract
The invention discloses a mass spectrometry ion source apparatus based on heat auxiliary glow discharge and an ionization analysis method thereof. The apparatus comprises: a glow discharge apparatus and a heating device. The glow discharge apparatus comprises: a closed tubular cavity and a needle electrode which passes through the tubular cavity. The needle electrode extends out of two ends of the tubular cavity. A narrow pipe is sleeved on the needle electrode which is arranged out of one end of the tubular cavity. The narrow pipe forms seal connection with the tubular cavity. A ring cavity is arranged between the narrow pipe and the needle electrode and is communicated with an inner cavity of the tubular cavity. An end of the narrow pipe sleeved on the needle electrode is an outlet of a plasma torch. A carrier gas inlet is arranged on a side wall of the tubular cavity. A grounding electrode is arranged on the end of the tubular cavity, wherein the end is close to the plasma torch outlet. There is space between a free end of the grounding electrode and the plasma torch outlet. And there is space between the heating device and the plasma torch outlet.
Description
Technical field
The present invention relates to a kind of mass ion source device and ionization analytical method thereof, belong to analytical chemistry molecularization ionization techniques field based on the auxiliary glow discharge of heat.
Background technology
Along with the actual needs of the development and the macromolecule industry of material science, macromolecular material is carried out rapid analysis detect particularly important.Can be sensitive, fast, also become pressing for of macromolecular material analysis field without any need for the detection method of sample pretreatment.
Mass spectrometer all plays an important role at aspects such as scientific research, medical treatment, productions as one of the sensitiveest known and analytical instrument that range of application is the widest, also is to be used to one of effective tool of analyzing macromolecular material.Ionization source is mass spectrometric important component part, and ion source commonly used has electron impact ionization source (EI), chemical ionization source (CI), fast atom bombardment source (FAB), glow discharge (GD), electron spray ionisation source (ESI), ground substance assistant laser to resolve ion source (MALDI) etc.These ion sources of different nature can obtain various forms of quasi-molecular ions or its fragment ion at different samples according to different requirements.Yet all need to keep certain vacuum degree during the work of these ion sources, and analyzed sample need carry out loaded down with trivial details preprocessing process, therefore, be difficult for realizing to target components continuously, monitoring and high throughput analysis in real time.Need certain vacuum condition as the glow discharge method, make the device design become complicated, improved operating cost, in addition, the electrode of glow discharge directly contacts with sample, need clean electrode, could guarantee the repeatability of experiment.
Recently, desorption electro-spray ionization (DESI), the directly development of real-time analysis (DART) plasma technology are for realizing that direct rapid analysis provides possibility to the sample that is left intact under the atmospheric pressure.But the gas of employed ionizing solvent of DESI and high flow rate, not only cost is high but also can cause certain pollution to environment.Though DART has saved solvent, but need the ionized gas of high-tension electricity and high flow rate, and need gas-heating apparatus, be difficult for realizing the miniaturization of instrument.In addition, DESI and DART are the ionization sources of comparison " soft ", thereby it is detected to be difficult to make the high molecular polymer molecule with HMW to enter gas phase formation ion, and therefore, these two kinds of technology also have certain limitation in the application aspect the macromolecular material analysis.
Summary of the invention
The purpose of this invention is to provide a kind of mass ion source device and ionization analytical method thereof based on the auxiliary glow discharge of heat, can be implemented under the atmospheric pressure, with testing sample especially macromolecular material molecular ionization, to carrying out detecting real-time without any pretreated sample.
A kind of mass ion source device based on the auxiliary glow discharge of heat provided by the invention comprises glow discharge device and heater; Described glow discharge device comprises the tubular housing of sealing and runs through the pin electrode of this tubular housing that described pin electrode stretches out from the two ends of described tubular housing; Be located on the outer pin electrode of described tubular housing one end and be arranged with tubule, described tubule and described tubular housing are for being tightly connected; Be provided with ring cavity between described tubule and the described pin electrode, described ring cavity communicates with the inner chamber of described tubular housing; The end of sheathed described tubule is the plasma torch outlet on the described pin electrode; The sidewall of described tubular housing is provided with carrier gas inlet; The end of nearly described plasma torch outlet is provided with grounding electrode on the described tubular housing, is provided with spacing between the free-end of described grounding electrode and the outlet of described plasma torch; Be provided with spacing between described heater and the outlet of described plasma torch.
In the above-mentioned mass ion source device, the material of described tubular housing can be polytetrafluoroethylene, bakelite or other synthetic resin; The material of described pin electrode, grounding electrode and tubule is stainless steel, gold or platinum.
In the above-mentioned mass ion source device, the diameter of described pin electrode and grounding electrode all can be 0.25mm-0.75mm; The internal diameter of described tubule can be 0.5mm-1.0mm, and external diameter can be 1.0mm-1.5mm.
In the above-mentioned mass ion source device, described heater comprises metal bar and the sample stage of being located on the described metal bar; The material of described metal bar and described sample stage all can be thermal conductivity preferably in the metals such as stainless steel, iron, copper and silver any one.
In the above-mentioned mass ion source device, the spacing between the free-end of described grounding electrode and the outlet of described plasma torch can be 0.3cm-0.5cm; Spacing between described heater and the outlet of described plasma torch can be 0.5cm-1.5cm, as 0.5cm, 1.0cm or 1.5cm; Angle can be 0-30 °, as 30 °.
The present invention also provides and has utilized above-mentioned ion source device to carry out the method that ionization is analyzed, and comprises the steps: to place sample to be analyzed on the described sample stage and heat; One end of described pin electrode is linked to each other with power supply, carrier gas is fed to described tubular housing from described carrier gas inlet; Connect described power supply, then in mass spectrometer, obtain the mass spectrum information of testing sample.
In the above-mentioned method, described carrier gas can be in helium, argon gas, nitrogen and the neon any; The flow velocity of described carrier gas can be 0.5L/min-2.0L/min, as 1.0L/min, 1.5L/min or 2.0L/min.
In the above-mentioned method, the spacing between described mass spectrometric thief hatch and the described glow discharge device can be 1.0cm-2.0cm, as 1.0cm, 1.5cm or 2.0cm.
In the above-mentioned method, described testing sample can be heated to 100 ℃-150 ℃, as 100 ℃ or 130 ℃; The temperature of described mass spectrometric thief hatch can be 100 ℃-350 ℃, as 275 ℃ or 300 ℃.
In the above-mentioned method, described power source voltage can be 2000V-3500V, as 2000V, 3000V or 3500V.
In the above-mentioned method, described analytic sample to be measured can be macromolecular material, specifically can be copolymerized macromolecule material or polyamino polymer material.
Use mass ion source device provided by the invention carry out ionization analytical method can be to sample especially macromolecular material under atmospheric pressure, synthesized polymer material as homopolymerization and copolymerization is directly analyzed fast, and need not any sample pretreatment process.Can detect the thermal degradation product of synthesized polymer material by tandem mass spectrum, comprise monomeric unit and other molecular fragments etc., can obtain the abundant chemical composition information of sample, thereby can be used for structural analysis homopolymerization and copolymerized macromolecule material.This method has high flux, characteristics such as high sensitivity, and abundant information can be provided, in polymer science, have good application prospects.
Description of drawings
Fig. 1 is the structural representation that the heat of the embodiment of the invention 1 is assisted the mass ion source device of glow discharge; Among the figure, each mark is as follows: 1 tubular housing, 2 pin electrodes, 3 grounding electrodes, 4 tubules, 5 carrier gas inlets, the outlet of 6 plasma torches, 7 stainless steel bars, 8 sample stage.
Fig. 2 is the mass spectrogram of polyethylene (PE).
Fig. 3 is the mass spectrogram of polystyrene (PS).
Fig. 4 is the mass spectrogram of polyformaldehyde (POM).
Fig. 5 is the mass spectrogram of poly butylene succinate (PBS).
Embodiment
Employed experimental technique is conventional method if no special instructions among the following embodiment.
Used material, reagent etc. if no special instructions, all can obtain from commercial channels among the following embodiment.
Following embodiment 2-5 all adopts linear ion trap mass spectrometer (LTQ-XL) to carry out collection analysis.
The mass ion source device based on the auxiliary glow discharge of heat of present embodiment comprises glow discharge device and heater; Glow discharge device comprises the tubular housing 1 and the stainless pin electrode 2 that runs through this tubular housing 1 of sealing, and the material of tubular housing 1 is a polytetrafluoroethylene, and stainless pin electrode 2 stretches out from the two ends of tubular housing 1; The diameter of stainless pin electrode 2 is 0.5mm; Be located on the outer stainless pin electrode 2 of tubular housing 1 one ends and be arranged with stainless steel tubule 4, this stainless steel tubule 4 and tubular housing 1 are for being tightly connected; The internal diameter of stainless steel tubule 4 is 0.75mm, and external diameter is 1.5mm; The ring cavity (not shown) that forms between stainless steel tubule 4 and the stainless pin electrode 2 communicates with the inner chamber of tubular housing 1, and the plasma of generation flows out from this ring cavity in the tubular housing 1; The end of sheathed stainless steel tubule 4 is plasma torch outlet 6 on the stainless pin electrode 2; The sidewall of tubular housing 1 is provided with carrier gas inlet 5, and carrier gas feeds to this tubular housing 1 from this carrier gas inlet 5; The end of nearly plasma torch outlet 6 is provided with grounding electrode 3 on the tubular housing 1, and the diameter of grounding electrode 3 is 0.5mm; Spacing between the free-end of grounding electrode 3 and the plasma torch outlet 6 is 0.3cm; Heater comprises stainless steel bar 7 and the stainless steel sample stage of being located on this stainless steel bar 78; Spacing between this heater and the plasma torch outlet 6 is 0.5cm, and angle is 30 °.
In the above-mentioned ion source device, the material of tubular housing 1 also can be bakelite or other synthetic resin; The material of pin electrode 2, grounding electrode 3 and tubule 4 also can be gold or platinum; The internal diameter of pin electrode 2 and grounding electrode 3 can be regulated in 0.25mm-0.75mm; The internal diameter of tubule 4 can be regulated in 0.5mm-1.0mm, and external diameter can be regulated in 1.0mm-1.5mm; The material of metal bar 7 and sample stage 8 also can be thermal conductivity metals such as iron, copper, silver preferably.
The Mass Spectrometer Method of embodiment 2, polyethylene (PE)
Utilize the mass ion source device of embodiment 1 to carry out mass spectral analysis, concrete grammar is as follows: polyethylene (PE) solid particle is placed on the specimen heating holder 8, continue to be heated to 130 ℃, polyethylene particle generation thermal degradation, use argon gas as carrier gas, controlling its flow velocity is 2.0L/min, apply the high pressure of 3000V to an end of pin electrode 2, distance between outlet 6 of metering needle electrode plasma torch and the specimen heating holder 8 is 0.5cm, angle is 30 °, glow discharge device is 2cm apart from the distance of mass spectrometric thief hatch, mass spectrometric thief hatch temperature is controlled to be 275 ℃, polyethylene specimen is detected, mass spectral analysis figure as shown in Figure 2, the mass signal peak in the mass spectrogram is the fragment ion that contains different carbon chain lengths.
The Mass Spectrometer Method of embodiment 3, polystyrene (PS)
Utilize the mass ion source device of embodiment 1 to carry out mass spectral analysis, concrete grammar is as follows: polystyrene (PS) solid particle is placed on the specimen heating holder 8, continue to be heated to 130 ℃, granules of polystyrene generation thermal degradation, use argon gas as carrier gas, its flow velocity is 1.0L/min, apply the high pressure of 3500V to an end of pin electrode 2, distance between outlet 6 of metering needle electrode plasma torch and the specimen heating holder 8 is 1.0cm, angle is 30 °, and glow discharge device is 1.5cm apart from the distance of mass spectrometric thief hatch, and Zhi Pu Yi Alto thief hatch temperature is controlled to be 275 ℃, polyethylene specimen is detected, and mass spectral analysis figure as shown in Figure 3; As can see from Figure 3, the monomeric unit of polystyrene and some other fragment ions are detected.With mass-to-charge ratio m/z among the figure 91.25,105.17,117.17 3 stronger corresponding ions of mass spectra peak of signal are respectively C
7H
7 +, C
8H
9 +, C
9H
9 +
The Mass Spectrometer Method of embodiment 4, polyformaldehyde (POM)
Utilize the mass ion source device of embodiment 1 to carry out mass spectral analysis, concrete grammar is as follows: polyformaldehyde (POM) solid is placed on the specimen heating holder 8, continue to be heated to 100 ℃, polyformaldehyde solid generation thermal degradation, use argon gas as carrier gas, its flow velocity is 1.5L/min, apply the high pressure of 2000V to an end of pin electrode 2, distance between outlet 6 of metering needle electrode plasma torch and the specimen heating holder 8 is 1.5cm, angle is 30 °, and glow discharge device is 1cm apart from the distance of mass spectrometric thief hatch, and mass spectrometric thief hatch temperature is controlled to be 275 ℃, the polyformaldehyde sample is detected, and mass spectral analysis figure as shown in Figure 4.Three characteristic peaks are that 31,45 and 89 places occur in mass-to-charge ratio respectively in the mass spectrogram, the corresponding with it fragment ion [CH that respectively does for oneself
3O]
+, [C
2H
5O]
+[C
3H
4O
3]
+Wherein molecular weight is that 31 mass spectra peak is the quasi-molecular ion peak of polyformaldehyde monomeric unit.
The Mass Spectrometer Method of embodiment 5, poly butylene succinate (PBS)
Utilize the mass ion source device of embodiment 1 to carry out mass spectral analysis, concrete grammar is as follows: poly butylene succinate (PBS) solid is placed on the specimen heating holder 8, continue to be heated to 130 ℃, polyethylene solid generation thermal degradation, use argon gas as carrier gas, its flow velocity is 2.0L/min, apply the high pressure of 3000V to an end of pin electrode 2, distance between outlet 6 of metering needle electrode plasma torch and the specimen heating holder 8 is 0.5cm, angle is 30 °, and glow discharge device is 2cm apart from the distance of mass spectrometric thief hatch, and mass spectrometric thief hatch temperature is controlled to be 300 ℃, the poly butylene succinate sample is detected, and mass spectral analysis figure as shown in Figure 5; Mass spectrogram has provided relevant poly butylene succinate fragment ion information.
By the foregoing description as can be known, the auxiliary glow discharge mass spectrometry ion source device of heat provided by the invention not only can be analyzed the polyamino polymer material, also can be used to analyze the copolymerized macromolecule material.
Claims (10)
1. mass ion source device based on the auxiliary glow discharge of heat, it is characterized in that: described device comprises glow discharge device and heater; Described glow discharge device comprises the tubular housing of sealing and runs through the pin electrode of this tubular housing that described pin electrode stretches out from the two ends of described tubular housing; Be located on the outer pin electrode of described tubular housing one end and be arranged with tubule, described tubule and described tubular housing are for being tightly connected; Be provided with ring cavity between described tubule and the described pin electrode, described ring cavity communicates with the inner chamber of described tubular housing; The end of sheathed described tubule is the plasma torch outlet on the described pin electrode; The sidewall of described tubular housing is provided with carrier gas inlet; The end of nearly described plasma torch outlet is provided with grounding electrode on the described tubular housing, is provided with spacing between the free-end of described grounding electrode and the outlet of described plasma torch; Be provided with spacing between described heater and the outlet of described plasma torch.
2. ion source device according to claim 1 is characterized in that: the material of described tubular housing is polytetrafluoroethylene or bakelite; The material of described pin electrode, grounding electrode and tubule is stainless steel, gold or platinum.
3. ion source device according to claim 1 and 2 is characterized in that: the diameter of described pin electrode and grounding electrode is 0.25mm-0.75mm; The internal diameter of described tubule is 0.5mm-1.0mm, and external diameter is 1.0mm-1.5mm.
4. according to arbitrary described ion source device among the claim 1-3, it is characterized in that: described heater comprises metal bar and the sample stage of being located on the described metal bar; The material of described metal bar and described sample stage is stainless steel, iron, copper or silver.
5. according to arbitrary described ion source device among the claim 1-4, it is characterized in that: the spacing between the free-end of described grounding electrode and the outlet of described plasma torch is 0.3cm-0.5cm; Spacing between described heater and the outlet of described plasma torch is 0.5cm-1.5cm, and angle is 0-30 °.
6. utilize the method that arbitrary described ion source device carries out the ionization analysis among the claim 1-5, comprise the steps: to place sample to be analyzed on the described sample stage and heat; One end of described pin electrode is linked to each other with power supply, carrier gas is fed to described tubular housing from described carrier gas inlet; Connect described power supply, then in mass spectrometer, obtain the mass spectrum information of testing sample.
7. method according to claim 6 is characterized in that: described carrier gas be in helium, argon gas, nitrogen and the neon any; The flow velocity of described carrier gas is 0.5L/min-2.0L/min.
8. according to claim 6 or 7 described methods, it is characterized in that: distance is 1.0cm-2.0cm between between described mass spectrometric thief hatch and the described glow discharge device.
9. according to arbitrary described method among the claim 6-8, it is characterized in that: described testing sample is heated to 100 ℃-150 ℃; The temperature of described mass spectrometric thief hatch is 100 ℃-350 ℃.
10. according to arbitrary described method among the claim 6-9, it is characterized in that: described power source voltage is 2000V-3500V; Described sample to be analyzed is a macromolecular material.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107004551A (en) * | 2014-12-16 | 2017-08-01 | 卡尔蔡司Smt有限责任公司 | Ionization apparatus and the mass spectrograph comprising ionization apparatus |
| CN109690296A (en) * | 2016-09-08 | 2019-04-26 | 阿格尼丝·奥布肖斯卡 | The equipment and its application method that element for analyzing fluid sample forms |
| CN113035686A (en) * | 2021-03-03 | 2021-06-25 | 桂林电子科技大学 | Ion source, FAIMS device and method for improving resolution and sensitivity of FAIMS device |
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| US20090039251A1 (en) * | 2007-08-09 | 2009-02-12 | Agilent Technologies, Inc. | Mass spectrometer |
| CN101510493A (en) * | 2008-11-18 | 2009-08-19 | 清华大学 | Method and ion source for direct ionization of sample of low-temperature plasma |
| CN201348623Y (en) * | 2008-12-29 | 2009-11-18 | 东华理工大学 | Neutral desorption device and neutral desorption electron-spray ionization extraction mass spectrography system |
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Patent Citations (3)
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| US20090039251A1 (en) * | 2007-08-09 | 2009-02-12 | Agilent Technologies, Inc. | Mass spectrometer |
| CN101510493A (en) * | 2008-11-18 | 2009-08-19 | 清华大学 | Method and ion source for direct ionization of sample of low-temperature plasma |
| CN201348623Y (en) * | 2008-12-29 | 2009-11-18 | 东华理工大学 | Neutral desorption device and neutral desorption electron-spray ionization extraction mass spectrography system |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107004551A (en) * | 2014-12-16 | 2017-08-01 | 卡尔蔡司Smt有限责任公司 | Ionization apparatus and the mass spectrograph comprising ionization apparatus |
| CN107004551B (en) * | 2014-12-16 | 2018-09-25 | 卡尔蔡司Smt有限责任公司 | Ionization apparatus and mass spectrograph comprising ionization apparatus |
| US10236169B2 (en) | 2014-12-16 | 2019-03-19 | Carl Zeiss Smt Gmbh | Ionization device with mass spectrometer therewith |
| CN109690296A (en) * | 2016-09-08 | 2019-04-26 | 阿格尼丝·奥布肖斯卡 | The equipment and its application method that element for analyzing fluid sample forms |
| CN109690296B (en) * | 2016-09-08 | 2021-10-08 | 阿格尼丝·奥布肖斯卡 | Apparatus for analyzing elemental composition of liquid sample and method of use thereof |
| CN113035686A (en) * | 2021-03-03 | 2021-06-25 | 桂林电子科技大学 | Ion source, FAIMS device and method for improving resolution and sensitivity of FAIMS device |
| CN113035686B (en) * | 2021-03-03 | 2023-06-16 | 桂林电子科技大学 | Ion source, FAIMS device and method for improving resolution and sensitivity of FAIMS device |
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