CN112986370A - Mass spectrum detection method for trace volatile components - Google Patents
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- CN112986370A CN112986370A CN201911283131.4A CN201911283131A CN112986370A CN 112986370 A CN112986370 A CN 112986370A CN 201911283131 A CN201911283131 A CN 201911283131A CN 112986370 A CN112986370 A CN 112986370A
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- 238000001514 detection method Methods 0.000 title claims abstract description 50
- 238000001819 mass spectrum Methods 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000004458 analytical method Methods 0.000 claims abstract description 11
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 9
- 125000004122 cyclic group Chemical group 0.000 claims abstract description 4
- 239000003570 air Substances 0.000 claims description 70
- 239000007789 gas Substances 0.000 claims description 54
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 239000012159 carrier gas Substances 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000002485 combustion reaction Methods 0.000 claims description 3
- 238000000855 fermentation Methods 0.000 claims description 3
- 230000004151 fermentation Effects 0.000 claims description 3
- 239000003546 flue gas Substances 0.000 claims description 3
- 239000001307 helium Substances 0.000 claims description 3
- 229910052734 helium Inorganic materials 0.000 claims description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 3
- 238000005040 ion trap Methods 0.000 claims description 3
- 230000004060 metabolic process Effects 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims 1
- 239000007924 injection Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 2
- 238000011002 quantification Methods 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 4
- 238000004451 qualitative analysis Methods 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000035945 sensitivity Effects 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/24—Suction devices
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Abstract
The invention relates to the field of chemical analysis, in particular to a mass spectrometry detection method for trace volatile components. The mass spectrum detection method of the trace volatile components is used for detecting the volatile components of which the volatile quantity V1 of a sample to be detected generated by a sample generating device is less than the sample inlet quantity V2 of a mass spectrometer; a detection process comprising a sample gas collection stage S1, a mass spectrometer detection stage S2, an air bag emptying stage S3 and an air bag emptying stage S4 in that order; each stage of the cyclic work realizes the high-efficiency mass spectrum detection and analysis of trace volatile components. The method has the remarkable advantages of simplicity and convenience in operation, rapidness in detection, accuracy in quantification and the like, meets the field detection requirements of various trace volatile components, and has a wide application prospect.
Description
Technical Field
The invention belongs to the field of chemical analysis, relates to a mass spectrum detection method, and particularly relates to a mass spectrum detection method for trace volatile components.
Background
The mass spectrometry technology has been widely used in many fields such as process analysis, environmental detection, material science, biomedicine, life science, etc. because of its advantages such as accurate qualitative and quantitative analysis ability, high resolution, high sensitivity, etc. With the gradual expansion of mass spectrum application scenes, more and more application occasions put higher requirements on mass spectrum detection methods. For some special application scenes, the volatilization amount of a sample to be detected is very weak, and the sample introduction standard of a mass spectrum is difficult to achieve, and how to realize accurate and efficient detection and analysis of the sample to be detected under the harsh detection condition is very important. The detection method provided by the invention mainly aims at the process of detection of the volatility less than the sample volume of the mass spectrometer, and realizes collection and detection of trace volatile components and accurate qualitative and quantitative analysis by automatically switching the working flow of the detection system.
Disclosure of Invention
The invention aims to provide an accurate and efficient mass spectrometry detection method for trace volatile components.
In order to achieve the above purpose, the invention adopts the technical scheme that:
a mass spectrometric detection method for trace volatile components relates to a device which comprises a sample generating device, a sample collecting air bag, an air source, an air pump and a mass spectrometer;
the mass spectrometry detection method of the trace volatile components is used for detecting the volatile components of which the volatile amount V1 of the sample to be detected generated by the sample generation device is less than the sample inlet amount V2 of a mass spectrometer;
a detection process comprising a sample gas collection stage S1, a mass spectrometer detection stage S2, an air bag emptying stage S3 and an air bag emptying stage S4 in that order;
the high-efficiency mass spectrum detection and analysis of trace volatile components are realized through the cyclic work of each stage; the working state and switching of each stage are realized by controlling a two-position three-way valve A, a two-position three-way valve B and a two-position three-way valve C; the inlet end of the air pump is connected with the NC end (normally closed) of the two-position three-way valve C, and the outlet end of the air pump is connected with a tail gas collecting system; the NO end (normally open) of the two-position three-way valve C is connected with the sample inlet of the mass spectrometer (8), and the inlet end of the two-position three-way valve C is connected with the sample collecting air bag; the inlet of the two-position three-way valve A is connected with the sample generating device, the NO end of the two-position three-way valve A is connected with the tail gas collecting system, the NC end of the two-position three-way valve A is connected with the NO end of the two-position three-way valve B, the outlet of the two-position three-way valve B is connected with the sample collecting air bag, and the;
s1: the two-position three-way valve A works in an NC state, the two-position three-way valve B3 works in an NO state, and the two-position three-way valve C works in the NC state; the sample generating device generates sample gas to be detected, the sample gas to be detected sequentially passes through the NC channel of the two-position three-way valve A and the NO channel of the two-position three-way valve B, the air pump is started, the sample gas to be detected is extracted through the NC channel of the two-position three-way valve C, and the sample gas to be detected is promoted to enter the sample collecting air bag; after the sample to be detected reaches the target amount V3, entering a mass spectrometer detection stage S2;
s2: the two-position three-way valve A works in the NO state, the two-position three-way valve B works in the NO state, and the two-position three-way valve C works in the NO state; the sample generating device generates sample gas to be detected and is connected with the tail gas collecting system through an NO channel of the two-position three-way valve A; the air pump is closed, and a sample to be detected collected in the sample collection and gas collection bag enters the mass spectrometer through the NO channel of the two-position three-way valve C for detection and analysis; after the mass spectrometer detection process is finished, entering an air bag emptying stage S3;
s3: the two-position three-way valve A works in an NO state, the two-position three-way valve B works in an NO state, and the two-position three-way valve C works in an NC state; the sample generating device generates sample gas to be detected and is connected with the tail gas collecting system through an NO channel of the two-position three-way valve A; the air pump is started, and under the action of the air pump, the residual sample to be detected in the sample collection gas bag enters the tail gas collection system through the NC channel of the two-position three-way valve C; after the air bag is emptied, the air bag cleaning stage S4 is entered;
s4: the two-position three-way valve A works in an NO state, the two-position three-way valve B works in an NC state, and the two-position three-way valve C works in the NC state; the sample generating device 1 generates sample gas to be detected and is connected with the tail gas collecting system through an NO channel of the two-position three-way valve A; and the air pump is started, and the carrier gas in the gas source enters the sample collecting air bag through the NC channel of the two-position three-way valve B and enters the tail gas collecting system through the NC channel of the two-position three-way valve C under the action of the air pump.
The sample generating device 1 comprises one or more than two sample generating devices in a plurality of fields such as fermentation process, catalytic reaction process, flue gas combustion process, animal and plant metabolic process and the like.
The gas source is one or more than two of high-purity nitrogen, helium, argon or air.
The mass spectrometer is a quadrupole mass spectrometer, an ion trap mass spectrometer, a magnetic mass spectrometer or a time-of-flight mass spectrometer.
The mass spectrum detection method for trace volatile components provided by the invention realizes the collection, qualitative and quantitative analysis of trace volatile components by rapidly switching the working process of the detection system, and can meet the application scene that the volatile amount of a sample to be analyzed is less than the sample amount of a mass spectrometer.
Drawings
Fig. 1 is a schematic structural diagram and a schematic working flow diagram of the sample gas collection stage S1 according to the present invention.
Fig. 2 is a schematic flow diagram of the mass spectrometer detection stage S2 of the present invention.
Fig. 3 is a schematic flow chart of the air bag emptying stage S3 according to the present invention.
Fig. 4 is a schematic flow chart of the air bag emptying stage S4 according to the present invention.
Detailed Description
Fig. 1 is a schematic structural diagram of the present invention. The mass spectrometry method for the rapid detection of the trace volatile components comprises a sample generating device, a sample collecting air bag, an air source, an air pump and a mass spectrometer;
the mass spectrum detection method of the trace volatile components is used for detecting the volatile components of a sample to be detected, which is generated by the sample generating device 1 and has the volatile quantity V1 smaller than the sample inlet quantity V2 of a mass spectrometer 8;
a detection process comprising a sample gas collection stage S1, a mass spectrometer detection stage S2, an air bag emptying stage S3 and an air bag emptying stage S4 in that order;
the high-efficiency mass spectrum detection and analysis of trace volatile components are realized through the cyclic work of each stage; the working state and switching of each stage are realized by controlling a two-position three-way valve A2, a two-position three-way valve B3 and a two-position three-way valve C4; the inlet end of the air pump 7 is connected with the NC end (normally closed) of the two-position three-way valve C4, and the outlet end of the air pump 7 is connected with the tail gas collecting system 9; the NO end (normally open) of the two-position three-way valve C4 is connected with the sample inlet of the mass spectrometer 8, and the inlet end of the two-position three-way valve C4 is connected with the sample collecting air bag 6; the inlet end of the two-position three-way valve A2 is connected with the sample generating device 1, the NO end is connected with the tail gas collecting system 9, the NC end is connected with the NO end of the two-position three-way valve B3, the outlet end of the two-position three-way valve B3 is connected with the sample collecting air bag 6, and the NC end is connected with the air source 5;
s1: the two-position three-way valve A2 works in an NC state, the two-position three-way valve B3 works in an NO state, and the two-position three-way valve C4 works in the NC state; the sample generating device 1 generates sample gas to be detected, the sample gas to be detected sequentially passes through an NC channel of the two-position three-way valve A2 and an NO channel of the two-position three-way valve B3, the air pump 7 is started, the sample gas to be detected is extracted through the NC channel of the two-position three-way valve C4, and the sample gas to be detected is promoted to enter the sample collecting air bag 6; after the sample to be detected reaches the target amount V3, entering a mass spectrometer detection stage S2;
s2: the two-position three-way valve A2 works in the NO state, the two-position three-way valve B3 works in the NO state, and the two-position three-way valve C4 works in the NO state; the sample generating device 1 generates sample gas to be detected and is connected with the tail gas collecting system 9 through an NO channel of a two-position three-way valve A2; the air pump 7 is closed, and a sample to be detected collected in the sample collection air bag 6 enters the mass spectrometer 8 through the NO channel of the two-position three-way valve C4 for detection and analysis; after the detection process of the mass spectrometer 8 is finished, entering an air bag emptying stage S3;
s3: the two-position three-way valve A2 works in the NO state, the two-position three-way valve B3 works in the NO state, and the two-position three-way valve C4 works in the NC state; the sample generating device 1 generates sample gas to be detected and is connected with the tail gas collecting system 9 through an NO channel of a two-position three-way valve A2; the air pump 7 is started, and under the action of the air pump 7, the residual sample to be detected in the sample collection air bag 6 enters the tail gas collection system 9 through an NC channel of the two-position three-way valve C4; after the air bag is emptied, the air bag cleaning stage S4 is entered;
s4: the two-position three-way valve A2 works in a NO state, the two-position three-way valve B3 works in an NC state, and the two-position three-way valve C4 works in the NC state; the sample generating device 1 generates sample gas to be detected and is connected with the tail gas collecting system 9 through an NO channel of a two-position three-way valve A2; the air pump 7 is started, the carrier gas in the gas source 5 enters the sample collecting air bag 6 through the NC channel of the two-position three-way valve B3, and enters the tail gas collecting system 9 through the NC channel of the two-position three-way valve C4 under the action of the air pump 7.
The sample generating device 1 comprises one or more than two sample generating devices in a plurality of fields such as fermentation process, catalytic reaction process, flue gas combustion process, animal and plant metabolic process and the like.
The gas source 5 is one or more of high-purity nitrogen, helium, argon or air.
The mass spectrometer 8 is a quadrupole mass spectrometer, an ion trap mass spectrometer, a magnetic mass spectrometer or a time-of-flight mass spectrometer.
Claims (4)
1. The utility model provides a trace volatile component mass spectrum detection method, the device that relates to include sample generating device (1), sample collection air pocket (6), air supply (5), aspiration pump (7) and mass spectrograph (8), its characterized in that: the mass spectrometry detection method of the trace volatile components is used for detecting the volatile components of which the volatilization volume V1 of the sample to be detected generated by the sample generation device (1) is less than the sample injection volume V2 of the mass spectrometer (8);
a detection process comprising a sample gas collection stage S1, a mass spectrometer detection stage S2, an air bag emptying stage S3 and an air bag emptying stage S4 in that order;
the high-efficiency mass spectrum detection and analysis of trace volatile components are realized through the cyclic work of each stage; the working state and switching of each stage are realized by controlling a two-position three-way valve A (2), a two-position three-way valve B (3) and a two-position three-way valve C (4); the inlet end of the air pump (7) is connected with the NC end of the two-position three-way valve C (4), and the outlet end of the air pump (7) is connected with the tail gas collecting system (9); the NO end of the two-position three-way valve C (4) is connected with a sample inlet of a mass spectrometer (8), and the inlet end of the two-position three-way valve C (4) is connected with a sample collecting air bag (6); the inlet of the two-position three-way valve A (2) is connected with the sample generating device (1), the NO end is connected with the tail gas collecting system (9), the NC end is connected with the NO end of the two-position three-way valve B (3), the outlet of the two-position three-way valve B (3) is connected with the sample collecting air bag (6), and the NC end is connected with the air source (5);
s1: the two-position three-way valve A (2) works in an NC state, the two-position three-way valve B3 works in an NO state, and the two-position three-way valve C (4) works in the NC state; the sample generating device (1) generates sample gas to be detected, the sample gas sequentially passes through an NC channel of the two-position three-way valve A (2) and an NO channel of the two-position three-way valve B (3), the air pump (7) is started, the sample gas to be detected is extracted through the NC channel of the two-position three-way valve C (4), and the sample gas to be detected is promoted to enter the sample collecting air bag (6); after the sample to be detected reaches the target amount V3, entering a mass spectrometer detection stage S2;
s2: the two-position three-way valve A (2) works in an NO state, the two-position three-way valve B (3) works in the NO state, and the two-position three-way valve C (4) works in the NO state; the sample generating device (1) generates sample gas to be detected and is connected with the tail gas collecting system (9) through an NO channel of the two-position three-way valve A (2); the air pump (7) is closed, and a sample to be detected collected in the sample collection air bag (6) enters the mass spectrometer (8) through the NO channel of the two-position three-way valve C (4) for detection and analysis; after the detection process of the mass spectrometer (8) is finished, entering an air bag emptying stage S3;
s3: the two-position three-way valve A (2) works in an NO state, the two-position three-way valve B (3) works in the NO state, and the two-position three-way valve C (4) works in an NC state; the sample generating device (1) generates sample gas to be detected and is connected with the tail gas collecting system (9) through an NO channel of the two-position three-way valve A (2); the air pump (7) is started, and under the action of the air pump (7), the residual sample to be detected in the sample collection air bag (6) enters the tail gas collection system (9) through an NC channel of the two-position three-way valve C (4); after the air bag is emptied, the air bag cleaning stage S4 is entered;
s4: the two-position three-way valve A (2) works in an NO state, the two-position three-way valve B (3) works in an NC state, and the two-position three-way valve C (4) works in the NC state; the sample generating device 1 generates sample gas to be detected and is connected with a tail gas collecting system (9) through an NO channel of a two-position three-way valve A (2); the air pump (7) is started, the carrier gas in the gas source (5) enters the sample collecting air bag (6) through the NC channel of the two-position three-way valve B (3), and enters the tail gas collecting system (9) through the NC channel of the two-position three-way valve C (4) under the action of the air pump (7).
2. The mass spectrometry detection method of trace volatile components according to claim 1, characterized in that:
the sample generating device 1 comprises one or more than two sample generating devices in a plurality of fields such as fermentation process, catalytic reaction process, flue gas combustion process, animal and plant metabolic process and the like.
3. The mass spectrometry detection method of trace volatile components according to claim 1, characterized in that:
the gas source (5) is one or more than two of high-purity nitrogen, helium, argon or air.
4. The mass spectrometry detection method of trace volatile components according to claim 1, characterized in that:
the mass spectrometer (8) is a quadrupole mass spectrometer, an ion trap mass spectrometer, a magnetic mass spectrometer or a time-of-flight mass spectrometer.
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Cited By (1)
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| CN116878966A (en) * | 2023-09-07 | 2023-10-13 | 美康盛德医疗科技(苏州)有限公司 | Mass spectrum microsampling device |
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Application publication date: 20210618 |