CN113960151A - Gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry - Google Patents

Gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry Download PDF

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Publication number
CN113960151A
CN113960151A CN202010632539.4A CN202010632539A CN113960151A CN 113960151 A CN113960151 A CN 113960151A CN 202010632539 A CN202010632539 A CN 202010632539A CN 113960151 A CN113960151 A CN 113960151A
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control device
gas
calibration
sampling
path
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李京华
李东明
李海洋
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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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
    • G01N27/622—Ion mobility spectrometry
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0422—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for gaseous samples
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/26—Mass spectrometers or separator tubes

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  • Analytical Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

The gas circuit comprises a control device I-control device IV, a quantitative tube cavity, a calibration liquid cavity and a migration tube; the control device I-the control device IV is respectively provided with at least one inlet end and two outlet ends; when the control device I-control device IV works, the inlet end is communicated with the first path of outlet end or the inlet end is communicated with the second path of outlet end; the first path outlet end of the control device I is sequentially communicated with the control device II, the quantitative tube cavity, the control device III and the transfer tube; the second path of outlet end of the control device I is communicated with the calibration liquid cavity, the control device IV and the transfer pipe in sequence; the control device II is also connected with an air extraction sampling pump; and the calibration liquid cavity is filled with calibration liquid and used for releasing calibration liquid gas. By switching gas circuits for automatic analysis, sampling and calibration of the ion mobility spectrometry, the analysis function, the sampling process and the calibration function can be respectively realized.

Description

Gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry
Technical Field
The invention belongs to the field of chemical substance field detection, and particularly relates to an air path for automatic analysis, sampling and calibration of ion mobility spectrometry.
Background
The Ion Mobility Spectrometry (IMS) technology is a qualitative separation technology for ions based on the difference in ion mobility time, detects and identifies different species of substances based on the difference in mobility of gas phase ions in a weak electric field, and is suitable for trace detection of some volatile organic compounds, such as drugs, explosives, chemical warfare agents, and atmospheric pollutants. The ion mobility tube is a core component of ion mobility spectrometry.
Besides the analysis process of the sample, the ion mobility spectrometer also comprises a sampling process of the sample gas and a process of introducing a certain amount of calibration liquid into the instrument and calibrating the peak position of the ion peak. The operation of the ion mobility spectrometry needs to provide a drift gas and a carrier gas, wherein the carrier gas is used for carrying a sample gas or a calibration solution of a standard substance, and the calibration solution is input into an ion mobility tube for analysis or calibration. Therefore, the gas path of the carrier gas relates to various gas paths such as analysis, sampling and calibration due to different analysis purposes, and the crossing of the gas paths is avoided, so that the residue and the interference are reduced.
An ion mobility spectrometer and its gas circuit control method (patent number ZL201310692819.4) invented by Liyang et al, the gas circuit control method mainly adopts air pump to drive clean gas, adjust the flow meter of the multi-channel regulating valve to make it reach the required flow respectively, after the differential ion mobility spectrometry 12, flight time ion mobility spectrometry 10 run stably, can open the first membrane sample injection device 13, the second membrane sample injection device 14 at the same time, can open the first membrane sample injection device 13, the second membrane sample injection device 14 to carry out sampling analysis under certain sampling flow rate separately. And provides another two paths of air flows which are respectively used as drift air for the differential ion mobility spectrometry 12 and the time-of-flight ion mobility spectrometry 10. The gas flow is controlled for carrying the sample of the membrane sample introduction device for analysis. The invention does not relate to a gas circuit for quantitative sampling and a gas circuit for standard liquid calibration.
The invention relates to a thermal desorption sample injector ion mobility spectrometry gas circuit (patent number ZL201210508587.8) invented by Binheyingwen and the like, wherein the thermal desorption sample injector ion mobility spectrometry gas circuit is a gas circulation system consisting of an ion migration tube, a gas driving device and a purifying device, and comprises the ion migration tube and a sample injector, and the ion migration tube is sequentially provided with a sample inlet, a gas outlet and a gas floating port; the sample injector is provided with a gas outlet and a gas inlet; the invention can realize the basic functions of analysis, detection, standby, back flushing and the like, and prolongs the service life of the purifying agent.
The ion mobility spectrometer (patent number ZL201410315716.0) with the double-circulation gas path is invented by Guo Hewarong and the like, and adopts the ion mobility spectrometer with the double-circulation gas path, and the sample gasification chamber, the external circulation active carbon filter tip, the external circulation pump, the two-position three-way electromagnetic valve and the sample molecule collection chamber are communicated through a gas transmission pipeline in sequence to form the external circulation gas path; the tail gas outlet of the migration pipe, the internal circulation pump, the internal circulation drying unit and the internal circulation doping unit are sequentially communicated, the outlet of the internal circulation doping unit is divided into two pipelines, one pipeline is communicated with the carrier gas inlet on the inner side of the diaphragm in the sample molecule collector, and the other pipeline is communicated with the migration gas inlet of the migration pipe to form an internal circulation gas path. The inner circulation gas circuit and the outer circulation gas circuit are separated by a diaphragm, so that the ion mobility spectrometer can keep dry and clean for a long time in the operation process, and the sampling detection is accurate. The invention designs an external circulation gas path for sample gasification conveying and an internal circulation gas path for the operation of a migration tube, which are used for conveying and analyzing samples. And the gas circuit of quantitative sampling and standard calibration is not involved.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: in the process of automatic analysis, sampling and calibration, the ion mobility spectrometry relates to various different gas paths such as analysis, sampling and calibration, avoids the crossing of the gas paths, and reduces residue and interference.
In view of the above technical problems, the present invention provides an air path for automatic analysis, sampling and calibration of ion mobility spectrometry, which can respectively realize the functions of analysis, sampling and calibration by switching the air paths for automatic analysis, sampling and calibration of ion mobility spectrometry.
The technical scheme of the invention is as follows:
the invention provides an air path for automatic analysis, sampling and calibration of ion mobility spectrometry, which comprises a control device I-control device IV, a quantitative tube cavity, a calibration liquid cavity and a migration tube;
the control device I-the control device IV is respectively provided with at least one inlet end and two outlet ends; when the control device I-control device IV works, the inlet end is communicated with the first path of outlet end or the inlet end is communicated with the second path of outlet end;
the first path outlet end of the control device I is sequentially communicated with the control device II, the quantitative tube cavity, the control device III and the transfer tube; the second path of outlet end of the control device I is communicated with the calibration liquid cavity, the control device IV and the transfer pipe in sequence;
the control device II is also connected with an air extraction sampling pump;
and the calibration liquid cavity is filled with calibration liquid and used for releasing calibration liquid gas.
Preferably, when the gas path is used for realizing an analysis function, the inlet end of the control device I is used for introducing carrier gas, the first outlet end of the control device I is communicated with the first outlet end of the control device II, the inlet end of the control device II is communicated with one end of the quantitative tube cavity, the other end of the quantitative tube cavity is communicated with the inlet end of the control device III, and the first outlet end of the control device III is communicated with the migration tube.
Preferably, when the gas path is used for realizing a sampling function, the pumping port of the pumping sampling pump is communicated with the second path of outlet port of the control device II, the inlet port of the control device II is communicated with one end of the quantitative tube cavity, the other end of the quantitative tube cavity is communicated with the inlet port of the control device III, and the second path of outlet port of the control device III is used for communicating the sampling port.
Preferably, when the gas path is used for realizing a calibration function, the inlet end of the control device I is used for introducing carrier gas, the outlet end of the second path of the control device I is communicated with one end of a calibration liquid cavity, the other end of the calibration liquid cavity is communicated with the inlet end of the control device IV, and the outlet end of the second path of the two-position three-way electromagnetic valve IV is communicated with the transfer pipe; and the first outlet end of the control device IV is closed.
Preferably, the sample gas collected by the sampling port is a gas sample in the natural state in the air or a gas sample after a liquid or solid sample is heated and vaporized.
Preferably, the control device I-control device IV is independently selected from one or the combination of a two-position three-way electromagnetic valve, a two-position two-way electromagnetic valve, a three-position four-way electromagnetic valve and a one-way valve.
Preferably, the quantitative pipe cavity has a heating and heat-preserving function, and the temperature range is 10-90 ℃.
Preferably, the calibration liquid cavity has a heating and heat-preserving function, and the temperature range is 10-70 ℃.
The invention also provides a using method of the gas circuit, which comprises the following steps:
when the gas path is used for realizing the sampling function, the gas extraction sampling pump extracts gas, the sample gas enters the gas extraction sampling pump through the control device III, the quantitative tube cavity and the control device II in sequence after being extracted through the sampling port, and the sample gas is extracted into the quantitative tube cavity to complete the sampling process;
when the gas circuit is used for realizing an analysis function, the carrier gas entering from the inlet end of the control device I passes through the control device I and the control device II, and the sample in the quantitative tube cavity is sent into the migration tube through the control device III for analysis;
when the gas path is used for realizing the calibration function, the carrier gas entering from the inlet end of the control device I sequentially passes through the control device I, the calibration liquid cavity and the control device IV, and the calibration liquid gas in the calibration liquid cavity is sent into the migration pipe for calibration.
Advantageous effects
1. The gas circuit for automatic analysis, sampling and calibration of the ion mobility spectrometry provided by the invention can respectively realize the functions of analysis, sampling and calibration by switching the gas circuits for automatic analysis, sampling and calibration of the ion mobility spectrometry.
2. The gas sample sampled by the invention enters the migration pipe for analysis through the analysis carrier gas carrier in the quantitative pipe, and the sample in the quantitative pipe is cleaned and emptied while the gas sample is analyzed, so that the instrument can be timely recovered, the sample residue of each time is reduced, and the interference on the next sampling and analysis is reduced.
3. The calibration analysis gas path provided by the invention utilizes the analysis carrier gas to carry, and the calibration liquid gas is sent to the migration tube, so that the volume and the residue of the gas path are reduced.
4. The gas path of the invention adopts one path of analysis carrier gas, and realizes the functions of analysis, sampling and calibration after switching, has compact structure and small volume, can reduce the residue of the sample and the calibration liquid, and ensures the accuracy of the analysis result.
Drawings
FIG. 1 is a gas path diagram for automatic analysis, sampling and calibration of ion mobility spectrometry;
FIG. 2 is a gas flow diagram of an ion mobility spectrometry analysis process;
FIG. 3 is a gas flow diagram of a sampling process for ion mobility spectrometry;
FIG. 4 is a gas flow diagram of a calibration process for ion mobility spectrometry;
in the figure, 1-4, a two-position three-way electromagnetic valve; 5. an air extraction sampling pump; 6. a dosing tube cavity; 7. a transfer tube; 8. and calibrating the liquid cavity.
Detailed Description
Example 1
The gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry (as shown in figures 1 and 2) comprises a two-position three-way electromagnetic valve 1, a two-position three-way electromagnetic valve 2, a quantitative pipe cavity, a two-position three-way electromagnetic valve 3 and a migration pipe;
in the analysis gas path, the inlet end of the two-position three-way solenoid valve 1 is used for introducing carrier gas, the first path of outlet end of the two-position three-way solenoid valve 1 is communicated with the first path of outlet end of the two-position three-way solenoid valve 2, the inlet end of the two-position three-way solenoid valve 2 is communicated with one end of the quantitative pipe cavity, the other end of the quantitative pipe cavity is communicated with the inlet end of the two-position three-way solenoid valve 3, and the first path of outlet end of the two-position three-way solenoid valve 3 is communicated with the migration pipe. In the analysis mode, the carrier gas sends the sample in the quantitative tube cavity into the transfer tube for analysis through a two-position three-way electromagnetic valve 1, a two-position three-way electromagnetic valve 2, the quantitative tube cavity and a two-position three-way electromagnetic valve 3 of the analysis gas circuit; the quantitative pipe cavity is heated and insulated, and the temperature is 10 ℃; in the ion mobility spectrometry of the negative ion mode, a lamp ionization mode is adopted, the temperature of an ion mobility tube is 100 ℃, the flow rate of a drift gas is 400ml/min, the flow rate of a carrier gas is 200ml/min, acetone is used as a reactant ion, and the signal intensity is about 2.5V.
Example 2
The gas path for automatic analysis, sampling and calibration of the ion mobility spectrometry comprises a two-position three-way electromagnetic valve 1, a calibration liquid cavity, a two-position three-way electromagnetic valve 4 and a migration tube, wherein carrier gas sends calibration liquid gas in the calibration liquid cavity into the migration tube through the calibration gas path for calibration.
In the calibration gas path, the inlet end of the two-position three-way electromagnetic valve 1 is used for introducing carrier gas, the second path of outlet end of the two-position three-way electromagnetic valve 1 is communicated with one end of the calibration liquid cavity, the other end of the calibration liquid cavity is communicated with the inlet end of the two-position three-way electromagnetic valve 4, and the second path of outlet end of the two-position three-way electromagnetic valve 3 is communicated with the transfer pipe. When the calibration mode is switched, the carrier gas sequentially passes through the two-position three-way electromagnetic valve 1, the calibration liquid cavity and the two-position three-way electromagnetic valve 4, and the calibration liquid gas in the calibration liquid cavity is sent into the transfer pipe for calibration; the first path of outlet end of the two-position three-way electromagnetic valve 4 is closed; in the ion mobility spectrometry of the negative ion mode, a lamp ionization mode is used, the temperature of an ion mobility tube is 100 ℃, the flow rate of a drift gas is 400ml/min, the flow rate of a carrier gas is 200ml/min, and acetone is used as a reaction reagent ion.
Methyl salicylate is used as standard calibration liquid, and the migration constant of the methyl salicylate is 1.47; the calibration liquid cavity is heated and insulated, and when the temperature is 10 ℃, the strength of the methyl salicylate peak is about 0.05V; the intensity of the methyl salicylate peak was about 1.3V at a temperature of 70 ℃.
Example 3
The gas circuit for automatic analysis, sampling and calibration of the ion mobility spectrometry comprises an air extraction sampling pump, a two-position three-way electromagnetic valve 2, a quantitative pipe cavity, a two-position three-way electromagnetic valve 3 and a sampling port; in the sampling gas path, an air exhaust port of an air exhaust sampling pump is communicated with a second path of outlet end of the two-position three-way electromagnetic valve 2, an inlet end of the two-position three-way electromagnetic valve 2 is communicated with one end of a quantitative tube cavity, the other end of the quantitative tube cavity is communicated with an inlet end of the two-position three-way electromagnetic valve 3, and a second path of outlet end of the two-position three-way electromagnetic valve 3 is communicated with a sampling port.
When the sampling mode is switched, the air extraction sampling pump extracts air, sample gas enters the air extraction sampling pump from the sampling port, the two-position three-way electromagnetic valve 3, the quantitative pipe cavity and the two-position three-way electromagnetic valve 2 in sequence, and the sample gas is extracted into the quantitative pipe cavity to complete the sampling process;
in the ion mobility spectrometry of the negative ion mode, a lamp ionization mode is used, the temperature of an ion mobility tube is 100 ℃, the flow rate of a drift gas is 400ml/min, the flow rate of a carrier gas is 200ml/min, acetone is used as a reaction reagent ion, and the air extraction flow rate is 5L/min.
The quantitative pipe cavity is heated and insulated, and the temperature is 90 ℃; the sample is safflower oil, which comprises methyl salicylate, oleum Terebinthinae, white camphor oil, cinnamic aldehyde oil, and cinnamon leaf oil. In the sampling mode, the bottle mouth of the safflower oil sample is pumped and sampled for 6-15 seconds, and the sample gas is collected into the quantitative pipe cavity; and switching to an analysis mode for analysis.
When the sample of n-safflower oil was analyzed, there were several peak patterns including a peak having a migration constant of 1.47 and a signal intensity of about 0.2V, and it was judged as a component of methyl salicylate.

Claims (9)

1. The gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry is characterized by comprising a control device I-control device IV, a quantitative tube cavity, a calibration liquid cavity and a migration tube;
the control device I-the control device IV is respectively provided with at least one inlet end and two outlet ends; when the control device I-control device IV works, the inlet end is communicated with the first path of outlet end or the inlet end is communicated with the second path of outlet end;
the first path outlet end of the control device I is sequentially communicated with the control device II, the quantitative tube cavity, the control device III and the transfer tube; the second path of outlet end of the control device I is communicated with the calibration liquid cavity, the control device IV and the transfer pipe in sequence;
the control device II is also connected with an air extraction sampling pump;
and the calibration liquid cavity is filled with calibration liquid and used for releasing calibration liquid gas.
2. The gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry according to claim 1, wherein: when the gas path is used for realizing an analysis function, the inlet end of the control device I is used for introducing carrier gas, the first path outlet end of the control device I is communicated with the first path outlet end of the control device II, the inlet end of the control device II is communicated with one end of a quantitative pipe cavity, the other end of the quantitative pipe cavity is communicated with the inlet end of the control device III, and the first path outlet end of the control device III is communicated with the migration pipe.
3. The gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry according to claim 1, wherein: when the gas path is used for realizing a sampling function, an air suction opening of the air suction sampling pump is communicated with a second path of outlet end of the control device II, an inlet end of the control device II is communicated with one end of the quantitative tube cavity, the other end of the quantitative tube cavity is communicated with an inlet end of the control device III, and the second path of outlet end of the control device III is used for being communicated with the sampling opening.
4. The gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry according to claim 1, wherein: when the gas path is used for realizing a calibration function, the inlet end of the control device I is used for introducing carrier gas, the second path of outlet end of the control device I is communicated with one end of a calibration liquid cavity, the other end of the calibration liquid cavity is communicated with the inlet end of the control device IV, and the second path of outlet end of the control device IV is communicated with the migration pipe; and the first outlet end of the control device IV is closed.
5. The gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry according to claim 3, wherein: the sample gas collected by the sampling port is a gas sample in the natural state in the air or a gas sample obtained after a liquid or solid sample is heated and vaporized.
6. The gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry according to claim 1, wherein: the control device I-the control device IV are respectively and independently selected from one or the combination of a two-position three-way electromagnetic valve, a two-position two-way electromagnetic valve, a three-position four-way electromagnetic valve and a one-way valve.
7. The gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry according to claim 1, wherein: the quantitative pipe cavity has the heating and heat preservation functions, and the temperature range is 10-90 ℃.
8. The gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry according to claim 1, wherein: the calibration liquid cavity has the heating and heat preservation functions, and the temperature range is 10-70 ℃.
9. A method of using a gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry according to any one of claims 1 to 8, characterized by: the method comprises the following steps:
when the gas path is used for realizing the sampling function, the gas extraction sampling pump extracts gas, the sample gas enters the gas extraction sampling pump through the control device III, the quantitative tube cavity and the control device II in sequence after being extracted through the sampling port, and the sample gas is extracted into the quantitative tube cavity to complete the sampling process;
when the gas circuit is used for realizing an analysis function, the carrier gas entering from the inlet end of the control device I passes through the control device I and the control device II, and the sample in the quantitative tube cavity is sent into the migration tube through the control device III for analysis;
when the gas path is used for realizing the calibration function, the carrier gas entering from the inlet end of the control device I sequentially passes through the control device I, the calibration liquid cavity and the control device IV, and the calibration liquid gas in the calibration liquid cavity is sent into the migration pipe for calibration.
CN202010632539.4A 2020-07-03 2020-07-03 Gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry Pending CN113960151A (en)

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CN202010632539.4A CN113960151A (en) 2020-07-03 2020-07-03 Gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry

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Application Number Priority Date Filing Date Title
CN202010632539.4A CN113960151A (en) 2020-07-03 2020-07-03 Gas circuit for automatic analysis, sampling and calibration of ion mobility spectrometry

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CN113960151A true CN113960151A (en) 2022-01-21

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