CN114639588A - Sample introduction device for rapidly detecting volatile substances based on ion mobility spectrometry - Google Patents
Sample introduction device for rapidly detecting volatile substances based on ion mobility spectrometry Download PDFInfo
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- CN114639588A CN114639588A CN202011481425.0A CN202011481425A CN114639588A CN 114639588 A CN114639588 A CN 114639588A CN 202011481425 A CN202011481425 A CN 202011481425A CN 114639588 A CN114639588 A CN 114639588A
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- sample
- sealed
- ion mobility
- mobility spectrometry
- volatile substances
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0468—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components with means for heating or cooling the sample
-
- 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
Abstract
The invention discloses a sample introduction device for rapidly detecting volatile substances based on ion mobility spectrometry, which comprises: the device comprises a cavity fixing frame, a sampling mechanism and a heating transmission mechanism, wherein the cavity fixing frame is composed of 4 stainless steel cylinders and used for supporting and fixing the sampling mechanism, the sampling mechanism is used for bearing a sample to be tested and can move within a preset range, so that the sampling mechanism is kept in contact with or separated from the heating transmission mechanism, and the heating transmission mechanism is used for heating the gaseous sample to be tested in cooperation with the sampling mechanism. The invention adopts the design of combining hot carrier gas penetrating purging and thermal analysis, thereby greatly reducing the possible loss of volatile substances in the sampling process, greatly shortening the time length of analyzing all samples from the matrix, realizing the rapid detection of the volatile samples to be detected while ensuring the sample feeding amount of the samples, meeting the requirement of on-site real-time monitoring, enlarging the application range of the ion mobility spectrometry as a quantitative instrument, and having wider application prospect.
Description
Technical Field
The invention relates to the technical field of ion mobility spectrometry detection equipment, in particular to a sample introduction device for rapidly detecting volatile substances based on ion mobility spectrometry.
Background
The ion mobility spectrometry is a technology for separating and detecting gas-phase ions based on different movement rates of the gas-phase ions in an external electric field under the atmospheric pressure state, has the advantages of high detection speed, high sensitivity, low price and the like, and is a real-time dynamic detection technology with great application prospect. The sample injector is an essential part of the ion mobility spectrometry, and the performance of the sample injector directly determines the sample injection efficiency and the overall performance of the ion mobility spectrometry. The products disclosed in 201210563261.5 halogen lamp sample injector for thermal desorption and 201721139511.7 gradient thermal desorption sample injector are the most common thermal desorption sample injectors before the atmospheric pressure ionization source ionizes the gaseous sample in the prior art, and have the advantages of high speed, simple structure, high efficiency and the like. This is because the gaseous sample molecules have higher ionization efficiency than solvation in the solid and liquid states where the intermolecular interaction is great, and are suitable for various atmospheric pressure ionization sources developed at present. However, the sample injector is suitable for detection and analysis of samples with moderate volatility and even difficult volatility, and for samples with extreme volatility, due to the sealing property and the design of the air ports, a part of samples can not enter the ion mobility spectrometry in the sample injection process, so that the detection sensitivity and the quantitative accuracy of volatile substances are influenced.
Therefore, the development of a sample injection device based on ion mobility spectrometry, which can rapidly detect volatile substances such as sevoflurane and accurately quantify the volatile substances has great practical value.
Disclosure of Invention
In view of the above technical problems, the present invention provides a sample injection device for rapidly detecting volatile substances based on ion mobility spectrometry, which aims at the limitations of the existing methods.
The technical means adopted by the invention are as follows:
a sample introduction device for rapidly detecting volatile substances based on ion mobility spectrometry comprises a sample introduction mechanism and a heating transmission mechanism;
the sample feeding mechanism comprises a sealed sample feeding chamber, a sample carrying disc with a handle and a sealing strip; an opening is formed in one side of the sealed sample injection cavity, and a sample carrying disc with a handle enters the sealed sample injection cavity from the opening; the sample carrying disc with the handle is of a flat plate structure, and a through hole is formed in the middle of the sample carrying disc;
the sample carrying disc with the handle is used for carrying a sample to be tested and can move within a preset range, so that the sample carrying disc is kept in contact with or separated from the heating transmission mechanism; the sealing strip is used for sealing the contact part of the hand-held sample carrying disc and the sealed sample feeding cavity so as to ensure the sealing performance of the sealed sample feeding cavity;
the heating transmission mechanism is used for being matched with the sample injection mechanism to transmit and heat the gaseous sample to be detected and comprises an upper tetrafluoride tube and a lower tetrafluoride tube which are respectively inserted into the upper side and the lower side of the sealed sample injection chamber and a heating sleeve arranged on the outer side of the upper tetrafluoride tube; the heating sleeve is preferably arranged at the middle section of the upper tetrafluoro pipe;
the lower end of the upper tetrafluoride tube and the upper end of the lower tetrafluoride tube are respectively inserted into the upper side and the lower side of the sealed sample introduction chamber and are coaxial with the center of the sample carrying area with the handle in the vertical direction; the other end of the upper tetrafluoride pipe is connected with the ion migration pipe, and an O-shaped ring seal is arranged at the joint; and the other end of the lower tetrafluoride tube is used for introducing preheated clean air to be used as a hot carrier gas, and the hot carrier gas carries the gaseous sample to be detected into the heating transmission mechanism through a through hole in the middle of the sample carrying disc with the handle.
Furthermore, the sample feeding device also comprises a chamber fixing frame; the sealed sample injection cavity is fixed above the cavity fixing frame; preferably, the chamber holder is comprised of four stainless steel cylinders.
Furthermore, a groove matched with the sample carrying disc with the handle in size is formed in the sealed sample feeding cavity, circular through holes with the same diameter and coaxial vertical directions are formed in the centers of the upper plane and the lower plane of the sealed sample feeding cavity and used for inserting the tetrafluoro tube, and the diameter of each circular through hole is 2-8 mm; the sample carrying disc with the handle can enter the sealed sample feeding cavity through the sealing strip, and the position of the sample carrying disc with the handle is determined through the groove of the sealed sample feeding cavity.
Furthermore, the through hole of the sample carrying disc with the handle is circular, and the diameter of the through hole is 10-30 mm; in the through-hole, on same horizontal plane, inlay a plurality of corrosion-resistant, insulating and heat conduction's narrow thin slice of equidistant range on two directions of mutually perpendicular, the thin slice can make hot carrier gas pass through on the one hand, and on the other hand plays the effect of bearing the weight of the sample and heating sample, and the thin slice width is at 0.5 ~ 2mm, and length is at 3 ~ 30mm, and thickness is at 0.1 ~ 1mm, and adjacent thin slice interval is at 0.05 ~ 2 mm.
Furthermore, the sample carrying disc with the handle is made of a corrosion-resistant, insulating and heat-conducting material;
if the sample carrying disc with the handle is a circular flat plate, the diameter of the annular part outside the middle circular through hole is 15-40 mm, the thickness of the annular part is 1-8 mm, and the annular part can be perfectly matched with a groove embedded in the sealed sample introduction cavity so as to realize the function of positioning the sample carrying disc.
Furthermore, the sample carrying disc with the handle can move along a specific direction, and the sample to be detected can be obtained and fed by pushing and pulling.
Furthermore, a heating rod and a sensor can be embedded in the sealed sample injection chamber, so that the sealed sample injection chamber can be used for samples with poor volatility or samples needing heating to improve the analysis speed, and the heating temperature range is 40-200 ℃; the inner wall is made of heat-conducting material of stainless steel or aluminum, and the outer wall is made of heat-insulating material of polytetrafluoroethylene or Peek material.
Further, the heating sleeve is a hollow cylindrical structure, a heating rod and a sensor can be embedded in the heating sleeve, the heating sleeve is used for samples with poor volatility or when the analytic speed needs to be improved by heating, and the heating temperature range is 40-200 ℃.
Furthermore, the joints of the tetrafluoride tube, the sampling mechanism and the ion migration tube which are directly contacted with each other in the sampling device are sealed by corrosion-resistant, insulating and heat-resistant O-shaped rings, so that the sealing performance of the sampling device is ensured.
Compared with the prior art, the invention has the following advantages:
1. the invention provides a sample introduction device capable of rapidly detecting volatile substances in an ion mobility spectrometry, which enlarges the application range of the ion mobility spectrometry as a quantitative instrument and has wider application prospect.
2. In the sealed sample injection cavity adopted by the invention, hot carrier gas penetration blowing and thermal analysis are combined, so that possible loss of volatile substances in the sample injection process is reduced to a great extent, the time for analyzing all samples from a matrix is greatly shortened, the rapid detection of the sample to be detected is realized while the sample injection quantity of the sample is ensured, the requirement of on-site real-time monitoring can be met, and the application scene of the ion mobility spectrometry is widened.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 shows a sample introduction device according to the present invention.
Fig. 2 is a schematic view of a sample carrying plate with a handle.
In the figure, (1) a chamber fixing frame, (2) a lower tetrafluoride tube, (3) a sealed sample introduction chamber, (4) a sample carrying disc with a handle, (5) a sealing strip, (6) an upper tetrafluoride tube, and (7) a heating sleeve.
Detailed Description
The present invention is described in further detail below with reference to the attached drawings.
As shown in fig. 1, the present application provides a sample injection device for rapidly detecting volatile substances based on ion mobility spectrometry, which includes a chamber fixing frame, a sample injection mechanism and a heating transmission mechanism; the chamber fixing frame consists of 4 stainless steel cylinders, the sampling mechanism comprises a sealed sampling chamber, a sample carrying disc with a handle and a sealing strip, and the heating transmission mechanism comprises an upper tetrafluoride tube, a lower tetrafluoride tube and a heating sleeve;
the lower end of the upper tetrafluoride tube and the upper end of the lower tetrafluoride tube are respectively inserted into the upper side and the lower side of the sealed sample introduction chamber and are coaxial with the center of the sample carrying area with the handle in the vertical direction; the other end of the upper tetrafluoride tube is connected with the ion migration tube; and the other end of the lower tetrafluoride pipe is filled with preheated clean air which is used as a heat carrier gas.
A groove matched with the sample carrying disc with the handle in size is formed in the sealed sample feeding cavity and used for determining the position of the sample carrying disc with the handle; the centers of the upper plane and the lower plane of the sealed sample injection cavity are provided with circular through holes with the same diameter and coaxial vertical direction for inserting the tetrafluoro tube, and the diameter of each circular through hole is 4 mm.
The sample carrying disc with the handle is of a circular flat plate structure, a circular through hole is formed in the middle of the sample carrying disc, and the diameter of the circular through hole is 15 mm; in the circular through hole, a plurality of corrosion-resistant, insulating and heat-conducting narrow sheets which are arranged at equal intervals are embedded in the same horizontal plane and in two mutually perpendicular directions, the width of each sheet is 1mm, the length of each sheet is 3-15 mm, the thickness of each sheet is 0.2mm, and the distance between every two adjacent sheets is 0.5 mm.
The sample carrying disc with the handle is made of a material which is corrosion-resistant, insulating and heat-conductive; the inner wall of the sealed sample injection cavity is made of stainless steel heat-conducting material, and the outer wall of the sealed sample injection cavity is made of polytetrafluoroethylene heat-insulating material.
Optionally, a heating rod and a sensor are embedded in the sealed sample introduction chamber, and the heating temperature is 100 ℃.
The heating sleeve is a hollow cylindrical structure, a heating rod and a sensor are embedded in the heating sleeve, and the heating temperature is 100 ℃.
The joints of the tetrafluoride tube, the sample feeding mechanism and the ion migration tube which are directly contacted with each other in the sample feeding device are sealed by corrosion-resistant, insulating and heat-resistant O-shaped rings so as to ensure the sealing performance of the whole sample feeding device.
When sampling, connecting the upper end of the upper tetrafluoride tube with an ion migration tube, and sealing the joint by an O-shaped ring; then, dropwise adding a sample to be detected to the center of a sample loading area of a sample loading disc with a handle, penetrating the sample loading disc with the handle through a sealing strip, pushing the sample loading disc into a sealed sample injection cavity, and sealing the sample injection cavity by using the sealing strip to ensure the sealing property of the sealed sample injection cavity; after the molecules of the sample to be detected are carried by the hot carrier gas and pass through the lower tetrafluoride tube, the sealed sample introduction chamber and the upper tetrafluoride tube, the sample to be detected is ensured to be in a gaseous state, and then the sample enters the ion migration tube to realize the separation and detection of the sample.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. A sample introduction device for rapidly detecting volatile substances based on ion mobility spectrometry is characterized by comprising a sample introduction mechanism and a heating transmission mechanism;
the sample feeding mechanism comprises a sealed sample feeding cavity, a sample carrying disc with a handle and a sealing strip; an opening is formed in one side of the sealed sample injection cavity, a sample carrying disc with a handle enters the sealed sample injection cavity from the opening, and the opening is sealed by a sealing strip; the sample carrying plate with the handle is of a flat plate structure, and a through hole is formed in the middle of the sample carrying plate;
the heating and conveying mechanism comprises an upper tetrafluoride pipe, a lower tetrafluoride pipe and a heating sleeve; the upper tetrafluoride pipe and the lower tetrafluoride pipe are respectively inserted into the upper side and the lower side of the sealed sample introduction chamber; the heating sleeve is sleeved outside the upper polytetrafluoroethylene tube; the position of the upper tetrafluoride tube and the lower tetrafluoride tube inserted into the sealed sample introduction chamber is coaxial with the center of the sample carrying area with the handle in the vertical direction.
2. The ion mobility spectrometry-based sample introduction device for rapid detection of volatile substances according to claim 1, further comprising a chamber holder; the sealed sample introduction cavity is fixed above the cavity fixing frame; preferably, the chamber holder is composed of four stainless steel cylinders.
3. The sampling device for rapidly detecting the volatile substances based on the ion mobility spectrometry as claimed in claim 1, wherein a groove matched with the sample carrying disc with the handle in size is arranged inside the sealed sampling chamber, and the position of the sample carrying disc with the handle is determined by the groove of the sealed sampling chamber; the centers of the upper plane and the lower plane of the sealed sample injection cavity are provided with circular through holes which have the same diameter and are coaxial in the vertical direction, so that the tetrafluoro tube can be inserted into the circular through holes, and the diameter of each circular through hole is 2-8 mm.
4. The sample introduction device for rapidly detecting volatile substances based on ion mobility spectrometry according to claim 1, wherein the through hole of the sample carrying disc with the handle is circular and has a diameter of 10-30 mm; a plurality of thin slices are embedded in the through holes, the width of each thin slice is 0.5-2 mm, the length of each thin slice is 3-30 mm, the thickness of each thin slice is 0.1-1 mm, and the distance between every two adjacent thin slices is 0.05-2 mm; the slices are arranged on the same horizontal plane in two mutually vertical directions at equal intervals; the sheet is corrosion resistant, insulating and thermally conductive.
5. The sampling device for rapid detection of volatile substances based on ion mobility spectrometry according to claim 1, wherein the sample carrying tray with the handle is made of a corrosion-resistant, insulating and heat-conductive material.
6. The sampling device for rapidly detecting the volatile substances based on the ion mobility spectrometry as claimed in claim 1, wherein a heating rod and a sensor are arranged in the sealed sampling chamber, and the heating temperature is 40-200 ℃; the inner wall of the sealed sample injection chamber is made of heat-conducting materials, and the outer wall of the sealed sample injection chamber is made of heat-insulating materials.
7. The ion mobility spectrometry-based sample introduction device for rapid detection of volatile substances according to claim 6, wherein the heat conductive material is stainless steel or aluminum; the heat-insulating material is polytetrafluoroethylene or a Peek material.
8. The sampling device for rapidly detecting the volatile substances based on the ion mobility spectrometry as claimed in claim 1, wherein a heating rod and a sensor are embedded in the heating sleeve, and the heating temperature is 40-200 ℃.
9. The sampling device for rapid detection of volatile substances based on ion mobility spectrometry according to claim 1, wherein the interfaces of the upper and lower tetrafluoride tubes and the sealed sampling cavity are sealed by corrosion-resistant, insulating and heat-resistant O-rings.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011481425.0A CN114639588A (en) | 2020-12-15 | 2020-12-15 | Sample introduction device for rapidly detecting volatile substances based on ion mobility spectrometry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011481425.0A CN114639588A (en) | 2020-12-15 | 2020-12-15 | Sample introduction device for rapidly detecting volatile substances based on ion mobility spectrometry |
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| Publication Number | Publication Date |
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| CN114639588A true CN114639588A (en) | 2022-06-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011481425.0A Pending CN114639588A (en) | 2020-12-15 | 2020-12-15 | Sample introduction device for rapidly detecting volatile substances based on ion mobility spectrometry |
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| CN (1) | CN114639588A (en) |
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2020
- 2020-12-15 CN CN202011481425.0A patent/CN114639588A/en active Pending
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