CN109307706B - Organic matter detection device and detection method of double-focusing chemical ionization mass spectrum - Google Patents
Organic matter detection device and detection method of double-focusing chemical ionization mass spectrum Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 63
- 239000005416 organic matter Substances 0.000 title claims abstract description 19
- 238000000170 chemical ionisation mass spectrum Methods 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 113
- 150000002500 ions Chemical class 0.000 claims abstract description 94
- 238000001819 mass spectrum Methods 0.000 claims abstract description 68
- 239000002131 composite material Substances 0.000 claims abstract description 12
- 230000005684 electric field Effects 0.000 claims description 19
- 230000007704 transition Effects 0.000 claims description 15
- 230000009471 action Effects 0.000 claims description 7
- 238000000262 chemical ionisation mass spectrometry Methods 0.000 claims description 6
- 238000002347 injection Methods 0.000 claims description 6
- 239000007924 injection Substances 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 238000000451 chemical ionisation Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 3
- 230000000694 effects Effects 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000009977 dual effect Effects 0.000 claims 3
- 230000007547 defect Effects 0.000 abstract 1
- 239000012855 volatile organic compound Substances 0.000 description 11
- 238000006276 transfer reaction Methods 0.000 description 8
- 230000035945 sensitivity Effects 0.000 description 7
- 238000001184 proton transfer reaction mass spectrometry Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000004252 FT/ICR mass spectrometry Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005040 ion trap Methods 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000001196 time-of-flight mass spectrum Methods 0.000 description 1
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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
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Abstract
The invention relates to an organic matter detection device and a detection method of a double-focusing chemical ionization mass spectrum, comprising a discharge ion source, a source drift tube and a reaction tube with gradually smaller inner diameters, a mass spectrum detection system, an alternating current-direct current composite power supply and the like; the detection method of the invention realizes double focusing of the chemically ionized parent ions and product ions through the ion focusing source drift tube and the ion focusing reaction tube, and realizes on-line high-sensitivity detection of the ions through the mass spectrum detection system. The invention makes up the defect of low ion guiding efficiency in the conventional source drift tube and the reaction tube by double focusing ion guiding reaction and mass spectrum detection. The invention can realize the efficient focusing guide of ions, thereby realizing the high-sensitivity on-line mass spectrum detection of organic matters.
Description
Technical Field
The invention belongs to the field of analysis and detection, and particularly relates to a device and a method for detecting Volatile Organic Compounds (VOCs) by double-focusing chemical ionization mass spectrometry.
Background
The proton transfer reaction mass spectrometry technology is a newly developed chemical ionization mass spectrometry technology based on ion-molecule reaction, and is usually used for preparing parent ion H of ion-molecule reaction by water vapor discharge 3 O + Then the parent ion H is led through the small hole between the ion source and the reaction tube 3 O + Introducing into a reaction tube, wherein the volatile organic compounds M and H to be detected can be introduced into the reaction tube 3 O + Ion-molecule reaction occurs and is ionized into MH + 。MH + And finally can be detected by mass spectrum to obtain molecular weight information and concentration information. The technology has the advantages of high sensitivity, quick response, soft ionization, no need of calibration and the like, and is more and more paid attention to the field of monitoring and analyzing volatile organic compounds in recent years.
Although proton transfer reaction mass spectrometry is the most sensitive chemical ionization mass spectrometry technology for detecting volatile organic compounds at present, the technology itself still has the points of further improvement and improvement, such as that parent ions and product ions in a reaction tube can be scattered off-axis, so that the ions cannot be completely guided into a transition cavity and a mass spectrometry cavity, and thus the detection sensitivity is affected, so Wang Yujie et al (Wang Yujie, proton transfer reaction mass spectrometry technology and application to medical material detection research, doctor paper of the national academy of sciences of China, 2011) propose to introduce an ion funnel concept into the reaction tube, and improve the detection sensitivity. However, a small hole is also connected between the discharge ion source and the reaction tube for transporting the parent ion H 3 O + If the pore diameter of the small hole is enlarged, air in the reaction tube easily flows back to the discharge ion source to participate in discharge, a large amount of impurity ions are generated, the ion-molecule reaction in the reaction tube is complicated, and the small hole between the discharge ion source and the reaction tube also limits the effective entry of parent ions into the reaction tube. Therefore, the parent ions prepared in the discharge ion source are introduced into the reaction more, and the high-efficiency focusing guide of the ions in the reaction tube is maintained, so that the sensitivity of the proton transfer reaction mass spectrum can be further improved.
Disclosure of Invention
The technical solution of the invention is as follows: the organic matter detection device and the detection method of the double-focusing chemical ionization mass spectrum are provided, and parent ion H is prepared through the discharge ion source 3 O + 、CH 5 + Or NH 4 + And the active ions are used as reactive ions, and under the action of an electric field in a focusing type source drift tube and a reaction tube, the efficient focusing and guiding of the parent ions and the product ions are realized, and the high-sensitivity online mass spectrum detection of the volatile organic compounds in the atmosphere is realized.
The technical solution of the invention is as follows: an organic matter detection device of a double-focusing chemical ionization mass spectrum comprises a discharge ion source 1, a source drift tube 2 with an electrode with gradually smaller inner diameter, a reaction tube 3 with the electrode with gradually smaller inner diameter, a mass spectrum detection system 4 and an alternating current-direct current composite power supply 5; the outlet of the discharge ion source 1 is coaxially communicated with the inlet of the source drift tube 2, and the outlet of the source drift tube 2 is communicated with the inlet of the reaction tube 3 through an axle center hole; the outlet of the reaction tube 3 is coaxially communicated with the inlet of the mass spectrum detection system 4; the alternating current-direct current composite power supply 5 is respectively connected with the discharge ion source 1, the source drift tube 2 and the reaction tube 3 through leads. The source drift tube 2 comprises a plurality of source drift tube electrodes 6 with gradually reduced inner diameters and a plurality of source drift tube insulating gaskets 7, and the plurality of source drift tube insulating gaskets 7 are separated among the plurality of source drift tube electrodes 6 with gradually reduced inner diameters; the reaction tube 3 comprises a plurality of reaction tube electrodes 8 with gradually reduced inner diameters, a plurality of reaction tube insulating gaskets 9 and a sample injection electrode 10, wherein the plurality of reaction tube insulating gaskets 9 are separated among the plurality of reaction tube electrodes 8 with gradually reduced inner diameters; the sample injection electrode 10 is an inlet electrode at the top end of the reaction tube 3.
The air pressure ranges in the source drift tube 2 and the reaction tube 3 are 60 Pa-500 Pa, and the effective electric field ranges from 10V/cm to 700V/cm.
The discharge ion source 1 comprises a gas source 11 and a discharge cavity 12, and the gas source 11 is connected with the discharge cavity 12 through a gas pipeline; the pressure in the discharge chamber 12 is in the range of 5Pa to 200Pa.
The mass spectrum detection system 4 comprises a transition cavity 13, a mass spectrum cavity 14, a vacuum pump group 15 and an ion detection mass spectrum 16; the transition cavity 13 is communicated with the mass spectrum cavity 14 through a coaxial small hole; the vacuum pump set 15 is communicated with the transition cavity 13 and the mass spectrum cavity 14 through gas path pipelines; ion detection mass spectrum 16 is located within the cavity of mass spectrum cavity 14.
The inner diameter of the electrode at the front section of the source drift tube 2 is larger than the inner diameter of the discharge cavity 12, no small hole shielding exists between the electrode and the discharge cavity, and the diameter of a small hole communicated between the source drift tube 2 and the reaction tube 3 is 1-20 mm; the diameter range of the small hole communicated between the reaction tube 3 and the mass spectrum detection system 4 is 0.1 mm-5 mm; the diameter of the small hole communicated between the transition cavity 13 and the mass spectrum cavity 14 is 0.1 mm-5 mm.
The air source 11 is water vapor, methane gas or ammonia gas, and the air flow of the air source 11 is 0.5 ml/min-40 ml/min.
The detection method of the invention comprises the following steps: the parent ions prepared by the discharge ion source 1 are focused and guided under the action of a radio frequency electric field in the source drift tube 2 with the gradually smaller inner diameter of the electrode, are injected into the reaction tube 3 with the gradually smaller inner diameter of the electrode through the small hole between the source drift tube 2 and the reaction tube 3, are sucked into the organic matter to be detected of the reaction tube 3, and undergo chemical ionization reaction in the reaction tube 3 to obtain product ions of the organic matter to be detected; the product ions are focused and guided under the action of the radio frequency electric field in the reaction tube 3, pass through the small hole communicated between the reaction tube 3 and the mass spectrum detection system 4, and enter the mass spectrum detection system 4 to be detected. The high-efficiency transmission of the parent ions and the product ions is realized through the double focusing guidance of the source drift tube and the reaction tube, so that the high-sensitivity on-line mass spectrum detection of the volatile organic compounds in the atmosphere is realized.
Compared with the prior art, the invention has the following differences and advantages:
(1) In proton transfer reaction mass spectrometry, as sample air is prevented from entering a discharge ion source to participate in discharge, the discharge ion source is connected with a reaction tube through a small hole, however, parent ions generated by the discharge ion source are not easy to enter the reaction tube through the small hole; in addition, because a certain reaction air pressure is needed in the reaction tube, and the mass spectrum cavity needs low-air pressure mass spectrum to work, the tail end of the reaction tube can only guide ions through the current-limiting small hole, so that parent ions and product ions in the reaction tube are not easy to exit the reaction tube through the small hole. This reduces the intensity of the ion signal detected by mass spectrometry, impairing the detection sensitivity. According to the invention, the ion focusing source drift tube is added between the discharge ion source and the reaction tube, the ion focusing reaction tube is adopted in the reaction tube, so that double focusing of parent ions and product ions at different stages is realized, the efficiency of the ions passing through two small holes is improved, the detection sensitivity is further improved, and the high-sensitivity detection of the chemical ionization mass spectrum similar to the proton transfer reaction mass spectrum on volatile organic matters is realized. The invention mainly comprises a discharge ion source, a source drift tube and a reaction tube with gradually smaller inner diameter of an electrode, a transition cavity, a mass spectrum cavity, a transition cavity molecular pump, a mass spectrum cavity molecular pump, a backing pump, an alternating current-direct current composite power supply, a sample inlet, an ion detection mass spectrum, an air source and the like. The source drift tube and the reaction tube adopt electrode structures with gradually smaller inner diameters and are connected with an alternating current-direct current composite power supply in a connection mode different from the prior art.
(2) The innovation of the invention is that: the source drift tube and the reaction tube with the gradually-reduced inner diameters of the electrodes are simultaneously connected with an alternating current-direct current composite power supply, the alternating current-direct current composite power supply can simultaneously form a focusing electric field in the source drift tube and the reaction tube with the gradually-reduced inner diameters of the electrodes, and off-axis ions can be focused to an axle center area after passing through the source drift tube and the reaction tube, so that the ions can more easily pass through two small holes in front of and behind the reaction tube. Compared with the existing conventional proton transfer reaction mass spectrum, the invention has the greatest advantages that more parent ions can be focused to enter the reaction tube to participate in the reaction, more parent ions and product ions can be improved to fly out of the reaction tube and detected by the rear-end mass spectrum, so that the detection of volatile organic compounds is more sensitive.
Drawings
FIG. 1 is a schematic diagram of a device for detecting volatile organic compounds in a dual-focus chemical ionization mass spectrum according to the present invention;
FIG. 2 is a mass spectrum of a comparative experiment of a radio frequency electric field modulation reaction tube and a conventional direct current electric field reaction tube.
Detailed Description
As shown in fig. 1, an embodiment of a volatile organic compound detection device for dual-focusing chemical ionization mass spectrometry according to the present invention includes: the device comprises a discharge ion source 1, a source drift tube 2 with the electrode inner diameter gradually becoming smaller, a reaction tube 3 with the electrode inner diameter gradually becoming smaller, a mass spectrum detection system 4 and an alternating current-direct current composite power supply 5; the outlet of the discharge ion source 1 is coaxially communicated with the inlet of the source drift tube 2, and the outlet of the source drift tube 2 is communicated with the inlet of the reaction tube 3 through an axle center hole; the outlet of the reaction tube 3 is coaxially communicated with the inlet of the mass spectrum detection system 4; the alternating current-direct current composite power supply 5 is respectively connected with the discharge ion source 1, the source drift tube 2 and the reaction tube 3 through leads. The source drift tube 2 comprises a plurality of source drift tube electrodes 6 with gradually reduced inner diameters and a plurality of source drift tube insulating gaskets 7, and the plurality of source drift tube insulating gaskets 7 are separated among the plurality of source drift tube electrodes 6 with gradually reduced inner diameters; the reaction tube 3 comprises a plurality of reaction tube electrodes 8 with gradually reduced inner diameters, a plurality of reaction tube insulating gaskets 9 and a sample injection electrode 10, wherein the plurality of reaction tube insulating gaskets 9 are separated among the plurality of reaction tube electrodes 8 with gradually reduced inner diameters; the sample injection electrode 10 is an inlet electrode at the top end of the reaction tube 3. The discharge ion source 1 comprises a gas source 11 and a discharge cavity 12, and the gas source 11 is connected with the discharge cavity 12 through a gas pipeline; the mass spectrum detection system 4 comprises a transition cavity 13, a mass spectrum cavity 14, a vacuum pump group 15 and an ion detection mass spectrum 16; the transition cavity 13 is communicated with the mass spectrum cavity 14 through a coaxial small hole; the vacuum pump set 15 is communicated with the transition cavity 13 and the mass spectrum cavity 14 through gas path pipelines; ion detection mass spectrum 16 is located within the cavity of mass spectrum cavity 14. The inner diameter of the electrode at the front section of the source drift tube 2 is larger than that of the discharge cavity 12, and no small hole is reserved between the electrode and the discharge cavity.
The method of the invention is realized as follows: the parent ions prepared by the discharge ion source 1 are focused and guided under the action of a radio frequency electric field in the source drift tube 2 with the gradually smaller inner diameter of the electrode, are injected into the reaction tube 3 with the gradually smaller inner diameter of the electrode through the small hole between the source drift tube 2 and the reaction tube 3, are sucked into the organic matter to be detected of the reaction tube 3, and undergo chemical ionization reaction in the reaction tube 3 to obtain product ions of the organic matter to be detected; the product ions are focused and guided under the action of the radio frequency electric field in the reaction tube 3, pass through the small hole communicated between the reaction tube 3 and the mass spectrum detection system 4, and enter the mass spectrum detection system 4 to be detected. The high-efficiency transmission of the parent ions and the product ions is realized through the double focusing guidance of the source drift tube and the reaction tube, so that the high-sensitivity on-line mass spectrum detection of the volatile organic compounds in the atmosphere is realized.
In order to obtain the high-sensitivity detection effect of chemical ionization, the alternating current-direct current composite power supply 5 comprises a plurality of paths of high-voltage direct current power supply outputs, a source drift tube 2 and a radio frequency power supply output modulated by the electric field of the reaction tube 3; the gas source 11 can be steam, methane gas or ammonia gas, and the like, and the gas flow can be selected within the range of 0.5 ml/min-40 ml/min; the air pressure range in the discharge ion source 1 is 5 Pa-200 Pa; the air pressure in the reaction tube 3 ranges from 60Pa to 500Pa, and the effective electric field formed by the radio frequency electric field and the direct current electric field in the source drift tube and the reaction tube ranges from 10V/cm to 700V/cm.
According to different vacuum system configurations, the diameter of a small hole communicated between the source drift tube 2 and the reaction tube 3 is between 1mm and 20mm, and the diameter of a small hole communicated between the reaction tube 3 and the mass spectrum detection system 4 is between 0.1mm and 5mm; the diameter of the small hole communicated between the transition cavity 13 and the mass spectrum cavity 14 is 0.1 mm-5 mm.
The ion detection mass spectrum 16 may be a detection system such as quadrupole mass spectrum, time-of-flight mass spectrum, ion trap mass spectrum, fourier transform ion cyclotron resonance mass spectrum or magnetic mass spectrum, depending on the ion detection requirements.
FIG. 2 shows the form of H 3 O + The contrast test result of the chemical ionization mass spectrum (namely proton transfer reaction mass spectrum) of the parent ion is that the line graph is that of the double-focusing proton transfer reaction mass spectrum, the gray shadow graph is that of the conventional proton transfer reaction mass spectrum, and the signal sensitivity of the double-focusing proton transfer reaction mass spectrum is greatly improved compared with that of the conventional proton transfer reaction mass spectrum, and the contrast of different substances is enhanced by about 10-100 times.
Portions of this specification, not specifically described herein, are well known in the art.
While the invention has been described with respect to certain preferred embodiments, it will be apparent to those skilled in the art that various changes and substitutions can be made herein without departing from the scope of the invention as defined by the appended claims.
Claims (7)
1. An organic matter detection device of double focusing type chemical ionization mass spectrum, which is characterized in that: the device comprises a discharge ion source (1), a source drift tube (2) with the inner diameter of an electrode gradually becoming smaller, a reaction tube (3) with the inner diameter of the electrode gradually becoming smaller, a mass spectrum detection system (4) and an alternating current-direct current composite power supply (5); the outlet of the discharge ion source (1) is coaxially communicated with the inlet of the source drift tube (2), and the outlet of the source drift tube (2) is communicated with the inlet of the reaction tube (3) through an axle center hole; the outlet of the reaction tube (3) is coaxially communicated with the inlet of the mass spectrum detection system (4); the alternating current-direct current composite power supply (5) is respectively connected with the discharge ion source (1), the source drift tube (2) and the reaction tube (3) through wires; the source drift tube (2) comprises a plurality of source drift tube electrodes (6) with gradually reduced inner diameters and a plurality of source drift tube insulating gaskets (7), and the plurality of source drift tube insulating gaskets (7) are separated among the plurality of source drift tube electrodes (6) with gradually reduced inner diameters; the reaction tube (3) comprises a plurality of reaction tube electrodes (8) with gradually reduced inner diameters, a plurality of reaction tube insulating gaskets (9) and a sample injection electrode (10), wherein the plurality of reaction tube insulating gaskets (9) are separated among the plurality of reaction tube electrodes (8) with gradually reduced inner diameters; the sample injection electrode (10) is an inlet electrode at the top end of the reaction tube (3);
the parent ions prepared by the discharge ion source (1) are focused and guided under the effect of a radio frequency electric field in a source drift tube (2) with the inner diameter of an electrode gradually becoming smaller, are injected into a reaction tube (3) with the inner diameter of the electrode gradually becoming smaller through a small hole between the source drift tube (2) and the reaction tube (3), are sucked into an organic matter to be detected of the reaction tube (3), and undergo chemical ionization reaction in the reaction tube (3) to obtain product ions of the organic matter to be detected; the product ions are focused and guided under the action of a radio frequency electric field in the reaction tube (3), and pass through the reaction tube (3) to be communicated with the mass spectrum detection system (4);
the air pressure range in the source drift tube (2) is 60 Pa-500 Pa, and the effective electric field range is 10V/cm-700V/cm;
the inner diameter of the electrode at the front section of the source drift tube (2) is larger than that of the discharge cavity (12), no small hole is reserved between the electrode and the discharge cavity, and the diameter of a small hole communicated between the source drift tube (2) and the reaction tube (3) is 1-mm-20 mm.
2. The organic matter detection device of a dual focus chemical ionization mass spectrum according to claim 1, wherein: the air pressure in the reaction tube (3) ranges from 60Pa to 500Pa, and the effective electric field ranges from 10V/cm to 700V/cm.
3. The organic matter detection device of a dual focus chemical ionization mass spectrum according to claim 1, wherein: the discharge ion source (1) comprises an air source (11) and a discharge cavity (12), and the air source (11) is connected with the discharge cavity (12) through an air pipeline; the air pressure in the discharge cavity (12) ranges from 5Pa to 200Pa.
4. The organic matter detection device of a dual focus chemical ionization mass spectrum according to claim 1, wherein: the mass spectrum detection system (4) comprises a transition cavity (13), a mass spectrum cavity (14), a vacuum pump group (15) and an ion detection mass spectrum (16); the transition cavity (13) is communicated with the mass spectrum cavity (14) through a coaxial small hole; the vacuum pump set (15) is communicated with the transition cavity (13) and the mass spectrum cavity (14) through gas path pipelines; an ion detection mass spectrum (16) is located within the cavity of the mass spectrum cavity (14).
5. The device for detecting organic matters by double focusing chemical ionization mass spectrometry according to claim 4, wherein: the diameter range of the small hole communicated between the reaction tube (3) and the mass spectrum detection system (4) is 0.1-mm-5 mm; the diameter of a small hole communicated between the transition cavity (13) and the mass spectrum cavity (14) is 0.1-mm mm.
6. The organic matter detecting device of claim 3, wherein: the air source (11) is water vapor, methane gas or ammonia gas, and the air flow of the air source (11) is 0.5-ml/min-40 ml/min.
7. A method for detecting organic matters by double focusing type chemical ionization mass spectrometry, which uses the organic matter detection device according to claim 1, and is characterized in that the method comprises the following steps:
the parent ions prepared by the discharge ion source (1) are focused and guided under the effect of a radio frequency electric field in a source drift tube (2) with the inner diameter of an electrode gradually becoming smaller, are injected into a reaction tube (3) with the inner diameter of the electrode gradually becoming smaller through a small hole between the source drift tube (2) and the reaction tube (3), are sucked into an organic matter to be detected of the reaction tube (3), and undergo chemical ionization reaction in the reaction tube (3) to obtain product ions of the organic matter to be detected; the product ions are focused and guided under the action of a radio frequency electric field in the reaction tube (3), pass through a small hole communicated between the reaction tube (3) and the mass spectrum detection system (4), and enter the mass spectrum detection system (4) to be detected.
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