CN118136488A - Sample injection heating device for secondary electrospray ionization source device - Google Patents

Sample injection heating device for secondary electrospray ionization source device Download PDF

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Publication number
CN118136488A
CN118136488A CN202410289625.8A CN202410289625A CN118136488A CN 118136488 A CN118136488 A CN 118136488A CN 202410289625 A CN202410289625 A CN 202410289625A CN 118136488 A CN118136488 A CN 118136488A
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China
Prior art keywords
heating
ionization chamber
source
sample injection
heat insulation
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CN202410289625.8A
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Chinese (zh)
Inventor
罗鑫
胡晓兰
李雪
汤志峰
王慧玲
郑跃丹
赖奕琪
拜特
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Jinan University
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Jinan University
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Priority to CN202410289625.8A priority Critical patent/CN118136488A/en
Publication of CN118136488A publication Critical patent/CN118136488A/en
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Abstract

The invention provides a sample injection heating device for a secondary electrospray ionization source device, and belongs to the technical field of analytical instruments. The invention comprises the following steps: the breathing gas source ionization chamber heating module is arranged on the ionization chamber of the secondary electrospray ionization source device; an expiration source sampling tube heating module, one end of which is connected to the ionization chamber; the expiration source ionization chamber heating module is used for heating the ionization chamber and the expiration source sampling tube heating module. According to the invention, the ionization chamber and the sample injection pipe are heated at high temperature by arranging the breath source ionization chamber heating module and the breath source sample injection pipe heating module, so that low-volatility pollutants accumulated on the sample injection pipe and the inner wall of the ionization chamber can be thoroughly removed, the influence of background noise on a test sample is reduced, and the performance of an instrument is improved.

Description

Sample injection heating device for secondary electrospray ionization source device
Technical Field
The invention relates to the technical field of analytical instruments, in particular to a sample injection heating device for a secondary electrospray ionization source device.
Background
The secondary electrospray ionization (Secondary electrospray ionization, SESI) technique is an atmospheric pressure ionization technique derived from electrospray ionization techniques, the principle of which can be summarized as: high voltage is applied to the solvent, charged sol particles (such as charged solvent liquid drops and protonated solvent molecule ions) are generated through coulomb explosion, the charged particles are in direct contact with the sample, neutral to-be-detected objects are charged through ion-molecule reaction or after being fused into the charged liquid drops through coulomb explosion, and the to-be-detected object ions enter a mass spectrometer from a mass spectrum interface under the combined action of a flow field and an electric field to be detected. SESI has the following advantages: real-time ionization, abundant ionized species, high ionization efficiency and soft ionization are particularly suitable for direct mass spectrometry of chemically active organic matters such as aldehyde ketone, unsaturated hydrocarbon and the like, but SESI cannot ionize low-polarity and nonpolar compounds such as alkane and the like. Currently, SESI and heterogeneous mass spectrometer coupling can be used to detect trace amounts of complex volatile metabolites, explosives, and secondary organic contaminants formed by atmospheric chemistry and room air chemistry in real-time in exhaled breath.
In the long-term use process of the SESI source, low-volatile substances residues caused by analyzing a sample can be accumulated in the sample injection tube and the ionization chamber, and the low-volatile substances are difficult to remove in the normal use process, so that the accuracy and the stability of an analysis result can be influenced for a long time. In order to solve the problem of low volatile matter residue, several measures are generally taken: the sample inlet pipe and the ionization chamber are made of mirror polishing grade 316L stainless steel material to eliminate micro stagnation areas; inert material coating is adopted on the inner walls of the sample injection pipe and the ionization chamber, so that the adsorption of substances is reduced.
Disclosure of Invention
In view of the above, in order to solve the technical problems that low volatile substances remain and gather in the sample injection pipe and the ionization chamber and are difficult to clean, the invention provides a sample injection heating device for a secondary electrospray ionization source device, which heats an ionization chamber and the sample injection pipe at high temperature by arranging an expiration source ionization chamber heating module and an expiration source sample injection pipe heating module, so that low volatile pollutants gathered in the sample injection pipe and the inner wall of the ionization chamber can be thoroughly cleaned, the influence of background noise on a test sample is reduced, and the performance of an instrument is improved.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a sample injection heating device for a secondary electrospray ionization source device, comprising:
The breathing gas source ionization chamber heating module is arranged on the ionization chamber of the secondary electrospray ionization source device;
An exhalation source sampling tube heating module, one end of which is connected to the ionization chamber;
The expiration source ionization chamber heating module is used for heating the ionization chamber and the expiration source sampling tube heating module.
Preferably, the expiratory source ionization chamber heating module comprises:
an ionization chamber heating block disposed on the ionization chamber;
The heating rod is arranged on the ionization chamber heating block and is used for heating the ionization chamber heating block;
and the temperature safety switch is fixed on the ionization chamber heating block through the temperature safety switch.
Preferably, the ionization chamber heating block comprises an ionization chamber upper heating block and an ionization chamber lower heating block which are respectively fixed at the upper end and the lower end of the ionization chamber.
Preferably, the heating rods are respectively arranged on the ionization chamber upper heating block and the ionization chamber lower heating block.
Preferably, the exhalation source sampling tube heating module comprises:
one end of the stainless steel sampling tube is connected to the ionization chamber, and the other end of the stainless steel sampling tube is sleeved with a front heating tube heat insulation sleeve;
the sample injection pipe heating belt is wound on the stainless steel sample injection pipe;
the heat insulation sleeve is sleeved outside the sample injection pipe heating band and is used for sealing the sample injection pipe heating band;
the front heating pipe heat insulation sleeve is sleeved on the stainless steel sampling pipe and then connected with the heat insulation sleeve.
Preferably, the inner diameter of the front heating pipe heat insulation sleeve is matched with the outer diameter of the stainless steel sample feeding pipe, and the front heating pipe heat insulation sleeve is used for limiting the shaking space of the stainless steel sample feeding pipe in the heat insulation sleeve.
Preferably, the heat insulation sleeve comprises a lower part of the heat insulation sleeve of the rear heating pipe and a heat insulation sleeve of the rear heating pipe which are buckled with each other;
the sample injection pipe heating belt is arranged in a groove below the rear heating pipe heat insulation sleeve, and the rear heating pipe heat insulation sleeve is buckled on the lower part of the heating pipe heat insulation sleeve.
Preferably, the heat insulation sleeve further comprises a heating pipe heat insulation sleeve fixing sleeve;
the heating pipe heat insulation sleeve fixing sleeve is sleeved below the heating pipe heat insulation sleeve and on the rear heating pipe heat insulation sleeve and is used for fixing the heating pipe heat insulation sleeve below and the rear heating pipe heat insulation sleeve above and then fixing the heating pipe heat insulation sleeve on the front decorative palm plate shell of the breathing gas source.
Preferably, one end of the stainless steel sample feeding pipe is fixed on the ionization chamber through a stainless steel sample feeding pipe clamping joint.
Preferably, a heat insulation module is arranged between the ionization chamber and a mass spectrum interface adapter on the secondary electrospray ionization source device.
Compared with the prior art, the invention has the following beneficial effects:
According to the sample injection heating device for the secondary electrospray ionization source device, provided by the invention, the ionization chamber and the sample injection pipe are heated at high temperature by arranging the breath source ionization chamber heating module and the breath source sample injection pipe heating module, so that low-volatility pollutants accumulated on the sample injection pipe and the inner wall of the ionization chamber can be thoroughly removed, the influence of background noise on a test sample is reduced, and the performance of an instrument is improved.
The sample injection heating device for the secondary electrospray ionization source device provided by the invention has the advantages of ingenious and compact structure, very convenient disassembly and assembly, and convenience in industrialization and cost control.
Drawings
FIG. 1 is a perspective view of a secondary electrospray ionization source apparatus;
FIG. 2 is a perspective view of the secondary electrospray ionization source device after removal of the front decorative palm panel housing of the respiratory source;
FIG. 3 is a front view of a secondary electrospray ionization source apparatus;
FIG. 4 is a cross-sectional view taken along the direction A-A in FIG. 3;
FIG. 5 is a cross-sectional view taken along the direction B-B in FIG. 3;
FIG. 6 is a first partial exploded view of the breath source sample tube heating module of the present invention;
FIG. 7 is a second partial exploded view of the breath source sample tube heating module of the present invention;
FIG. 8 is a first partial exploded view of the expiratory source ionization chamber heating module of the present invention;
FIG. 9 is a second partial exploded view of the expiratory source ionization chamber heating module of the present invention;
FIG. 10 is an exploded view of a third portion of the heating module of the exhalation source ionization chamber of the present invention;
In the figure, 1, an expiration source main hand plate shell; 1-2, decorating a hand plate shell in front of an expiration source; 2. an exhalation source sampling tube heating module; 2-1, a front heating pipe heat insulation sleeve; 2-2, stainless steel sample feeding pipe; 2-3, a sample injection pipe heating belt; 2-4, heating the pipe under the heat insulation sleeve; 2-5, a rear heating pipe is arranged on the heat insulation sleeve; 2-6, fixing the heating pipe heat insulation sleeve; 3. an exhalation source ionization chamber heating module; 3-1, a mass spectrum interface adapter; 3-2, a heat insulation module; 3-3, ionization chamber; 3-4, heating blocks on the ionization chamber; 3-5, a temperature safety switch; 3-6, heating rod; 3-7, pressing a temperature safety switch block; 3-8, heating blocks under the ionization chamber; 3-9, a stainless steel sampling tube clamping sleeve joint; 3-10, fixing parts of capillary sample injection devices; 3-11, capillary sample introduction device; 3-12, O-shaped ring; 3-13, auxiliary gas fixing parts; 3-14, r1/8 quick connector; 3-15, M5 quick connector.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention; it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments, and that all other embodiments obtained by persons of ordinary skill in the art without making creative efforts based on the embodiments in the present invention are within the protection scope of the present invention.
In the description of the present invention, it should be noted that the positional or positional relationship indicated by the terms such as "upper", "lower", "inner", "outer", "top/bottom", etc. are based on the positional or positional relationship shown in the drawings, are merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the apparatus or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "configured to," "engaged with," "connected to," and the like are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention will be understood in specific cases by those of ordinary skill in the art.
The invention provides a sample injection heating device for a secondary electrospray ionization source device, which comprises:
A respiratory gas source ionization chamber heating module 3 which is arranged on an ionization chamber 3-3 of the secondary electrospray ionization source device;
an exhalation source sampling tube heating module 2, one end of which is connected to the ionization chamber;
The expiration source ionization chamber heating module 3 is used for heating the ionization chamber 3-3 and the expiration source sampling tube heating module 2.
According to the invention, the breath source ionization chamber heating module 3 is arranged on the ionization chamber, the breath source sampling tube heating module 2 is fixedly connected with the ionization chamber 3-3, and the ionization chamber 3-3 and the sampling tube are heated at high temperature through the breath source ionization chamber heating module, so that low-volatility pollutants accumulated on the sampling tube and the inner wall of the ionization chamber can be thoroughly removed, the influence of background noise on a test sample is reduced, and the performance of an instrument is improved.
As shown in fig. 1-5, the secondary electrospray ionization source device comprises an exhalation source main hand plate shell 1, an exhalation source sampling tube heating module 2 and an exhalation source ionization chamber heating module 3;
As shown in fig. 8-10, the present invention provides a preferred embodiment of an exhalation source ionization chamber heating module 3, specifically as follows:
The source ionization chamber heating module may comprise: the mass spectrum interface adapter 3-1, the heat insulation module 3-2, the ionization chamber 3-3, the ionization chamber upper heating block 3-4, the temperature safety switch 3-5, the heating rod 3-6, the temperature safety switch pressing block 3-7, the ionization chamber lower heating block 3-8 and the stainless steel sampling tube cutting sleeve connector 3-9;
The ionization chamber 3-3 is provided with a capillary sample injection device fixing piece 3-10, a capillary sample injection device 3-11, an O-shaped ring 3-12, an auxiliary gas fixing piece 3-13, an r1/8 quick connector 3-14 and an M5 quick connector 3-15;
The connection relation among the components is as follows:
The heat insulation module 3-2 is interposed between the mass spectrometry interface adapter 3-1 and the ionization chamber 3-3 in order to prevent excessive conduction of the temperature of the mass spectrometer interface to the ionization chamber 3-3, affecting the heated temperature; the temperature safety switch 3-5 is respectively fixed on the ionization chamber upper heating block 3-4 and the ionization chamber lower heating block 3-8 through the temperature safety switch voltage 3-7; the heating rods 3-6 are respectively arranged on the upper heating block 3-4 of the ionization chamber and the lower heating block 3-8 of the ionization chamber and are fixed through set screws; the capillary sample injection device fixing piece 3-10 is fixed on the ionization chamber 3-3, so as to facilitate the fixing of the capillary sample injection device 3-11; the auxiliary air fixing piece 3-13 is respectively provided with an r1/8 quick connector 3-14 and an M5 quick connector 3-15 which are fixed at the upper part thereof; the total number of O-shaped rings 3-12 is 3, so that the purpose of sealing between the auxiliary gas fixing piece 3-13 and the ionization chamber 3-3 is achieved;
As shown in fig. 6-7, the present invention provides a preferred embodiment of an exhalation source sampling tube heating module 2, specifically as follows:
The expiration source sampling tube heating module 2 can preferably comprise a front heating tube heat insulation sleeve 2-1, a stainless steel sampling tube 2-2, a sampling tube heating belt 2-3, a rear heating tube heat insulation sleeve lower 2-4, a rear heating tube heat insulation sleeve upper 2-5 and a heating tube heat insulation sleeve fixing sleeve 2-6;
The connection relation among the components is as follows:
The breath source sampling tube heating module 2 is fixed on the breath source ionization chamber heating module 3 through a stainless steel sampling tube clamping sleeve connector 3-9, and meanwhile, the breath source sampling tube heating module 2 and the breath source ionization chamber heating module 3 are core modules of the patent; firstly, an expiration source sampling tube heating module 2 consists of a front heating tube heat insulation sleeve 2-1, a stainless steel sampling tube 2-2, a sampling tube heating belt 2-3, a rear heating tube heat insulation sleeve lower 2-4, a rear heating tube heat insulation sleeve upper 2-5 and a heating tube heat insulation sleeve fixing sleeve 2-6; the sample tube heating belt 2-3 is uniformly wound on the stainless steel sample tube 2-2, so that the sample tube is uniformly heated; the lower part 2-4 of the heat insulation sleeve of the rear heating pipe is that a sample injection pipe heating belt 2-3 wound on a stainless steel sample injection pipe 2-2 is placed in a groove of the sample injection pipe heating belt, and the upper part 2-5 of the heat insulation sleeve of the rear heating pipe is sleeved on the lower part 2-4 of the heat insulation sleeve of the heating pipe, so that a closed heat insulation sleeve is formed; the front heating pipe heat insulation sleeve 2-1 is screwed on the lower part 2-4 of the rear heating pipe heat insulation sleeve by virtue of threads, and the inner diameter of the front heating pipe heat insulation sleeve 2-1 is slightly larger than that of the stainless steel sample feeding pipe 2-2, so that the shaking space of the stainless steel sample feeding pipe 2-2 in the heat insulation sleeve can be limited; the heating pipe heat-insulating sleeve fixing sleeve 2-6 is a fixing piece designed to be provided with a notch, firstly, the fixing piece is sleeved between the lower part 2-4 of the rear heating pipe heat-insulating sleeve and the upper part 2-5 of the rear heating pipe heat-insulating sleeve, the lower part 2-4 of the rear heating pipe heat-insulating sleeve and the upper part 2-5 of the rear heating pipe heat-insulating sleeve are firmly fixed through screws on the upper part of the heating pipe heat-insulating sleeve fixing sleeve 2-6, and at the moment, the stainless steel sampling pipe 2-2 can be firstly fixed on the ionization chamber 3-3 through the stainless steel sampling pipe cutting sleeve joint 3-9, and then the whole expiration source sampling pipe heating module 2 is fixed on the expiration source front decorative hand plate shell 1-2.
The working principle and the beneficial effects of the invention are as follows:
The breath source sampling tube heating module 2 and the breath source ionization chamber heating module 3 are core modules of the invention. The heating module 3 of the ionization chamber of the breathing gas source heats, the heat is conducted to the ionization chamber 3-3 and the stainless steel sample feeding tube 2-2, the stainless steel sample feeding tube 2-2 can uniformly transfer the temperature to each part of the inner wall of the stainless steel sample feeding tube 2-2 through the sample feeding tube heating belt 2-3, the heating is very uniform, and the heating temperature of the stainless steel sample feeding tube 2-2 is set to be 130 ℃ under the normal condition; meanwhile, the fixing structure of the stainless steel sampling tube 2-2 is very ingenious, firstly, the mode that the lower 2-4 part of the rear heating tube heat insulation sleeve is buckled with the upper 2-5 part of the rear heating tube heat insulation sleeve is adopted, the fixing sleeve 2-6 part of the rear heating tube heat insulation sleeve is utilized for fixing, the stainless steel sampling tube is very convenient to install, the problem of errors of the stainless steel sampling tube 2-2 in the processing process is solved, and clamping grooves are designed on the lower 2-4 part of the rear heating tube heat insulation sleeve and the upper 2-5 part of the rear heating tube heat insulation sleeve, so that the assembly precision is guaranteed conveniently. Meanwhile, the whole air source sample injection tube heating module 2 is very convenient to disassemble and assemble, and the whole air source sample injection tube heating module 2 can be disassembled only by screwing off 4 screws fixed on the front decorative palm plate shell 1-2 of the air source and unscrewing the stainless steel sample injection tube clamping sleeve joint 3-9, and the operation is reversed during the installation.
The ionization chamber heating module 3 has simpler structure and is easy to install; firstly, the temperature of the mass spectrometer interface can be effectively prevented from being transferred to the ionization chamber by the heat insulation module 3-2, and the temperature of the mass spectrometer interface is not expected to be conducted excessively because the heating temperature of the ionization chamber is usually set at 90 ℃; the ionization chamber 3-3 is heated by the heating rods fixed in the upper and lower heating blocks 3-6, and the ionization chamber 3-3 is heated relatively uniformly because the upper and lower heating blocks are respectively provided with a heating rod for heating the heating rods, so that the problem of removing low-volatility pollutants is well solved.
The above is only a preferred embodiment of the present invention; the scope of the invention is not limited in this respect. Any person skilled in the art, within the technical scope of the present disclosure, may apply to the present invention, and the technical solution and the improvement thereof are all covered by the protection scope of the present invention.

Claims (10)

1. A sample injection heating device for a secondary electrospray ionization source device, comprising:
The breathing gas source ionization chamber heating module is arranged on the ionization chamber of the secondary electrospray ionization source device;
An exhalation source sampling tube heating module, one end of which is connected to the ionization chamber;
The expiration source ionization chamber heating module is used for heating the ionization chamber and the expiration source sampling tube heating module.
2. The sample injection heating apparatus for a secondary electrospray ionization source apparatus of claim 1, wherein the expiratory source ionization chamber heating module comprises:
an ionization chamber heating block disposed on the ionization chamber;
The heating rod is arranged on the ionization chamber heating block and is used for heating the ionization chamber heating block;
and the temperature safety switch is fixed on the ionization chamber heating block through the temperature safety switch.
3. The sample-feeding heating device for a secondary electrospray ionization source device according to claim 2, wherein the ionization chamber heating block comprises an ionization chamber upper heating block and an ionization chamber lower heating block which are respectively fixed at the upper end and the lower end of the ionization chamber.
4. A sample injection heating apparatus for a secondary electrospray ionization source as recited in claim 3, wherein the heating rods are disposed on the ionization chamber upper heating block and the ionization chamber lower heating block, respectively.
5. The sample injection heating apparatus for a secondary electrospray ionization source apparatus of claim 1, wherein the exhalation source sample injection tube heating module comprises:
one end of the stainless steel sampling tube is connected to the ionization chamber, and the other end of the stainless steel sampling tube is sleeved with a front heating tube heat insulation sleeve;
the sample injection pipe heating belt is wound on the stainless steel sample injection pipe;
the heat insulation sleeve is sleeved outside the sample injection pipe heating band and is used for sealing the sample injection pipe heating band;
the front heating pipe heat insulation sleeve is sleeved on the stainless steel sampling pipe and then connected with the heat insulation sleeve.
6. The sample injection heating apparatus for a secondary electrospray ionization source device as recited in claim 5, wherein an inner diameter of the front heating tube insulating sleeve is adapted to an outer diameter of the stainless steel sample injection tube for limiting a shaking space of the stainless steel sample injection tube in the insulating sleeve.
7. The sample injection heating apparatus for a secondary electrospray ionization source apparatus as recited in claim 5, wherein the heat shield comprises a back heating tube heat shield and a back heating tube heat shield which are buckled with each other;
the sample injection pipe heating belt is arranged in a groove below the rear heating pipe heat insulation sleeve, and the rear heating pipe heat insulation sleeve is buckled on the lower part of the heating pipe heat insulation sleeve.
8. The sample injection heating apparatus for a secondary electrospray ionization source apparatus as recited in claim 7, wherein the insulating sleeve further comprises a heating tube insulating sleeve fixing sleeve;
the heating pipe heat insulation sleeve fixing sleeve is sleeved below the heating pipe heat insulation sleeve and on the rear heating pipe heat insulation sleeve and is used for fixing the heating pipe heat insulation sleeve below and the rear heating pipe heat insulation sleeve above and then fixing the heating pipe heat insulation sleeve on the front decorative palm plate shell of the breathing gas source.
9. The sample-feeding heating device for a secondary electrospray ionization source device as recited in claim 1, wherein one end of the stainless steel sample-feeding tube is fixed on the ionization chamber through a stainless steel sample-feeding tube clamping joint.
10. The sample heating device for a secondary electrospray ionization source as recited in any one of claims 1-9, wherein a thermal insulation module is disposed between the ionization chamber and a mass spectrometry interface adapter on the secondary electrospray ionization source.
CN202410289625.8A 2024-03-13 2024-03-13 Sample injection heating device for secondary electrospray ionization source device Pending CN118136488A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202410289625.8A CN118136488A (en) 2024-03-13 2024-03-13 Sample injection heating device for secondary electrospray ionization source device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202410289625.8A CN118136488A (en) 2024-03-13 2024-03-13 Sample injection heating device for secondary electrospray ionization source device

Publications (1)

Publication Number Publication Date
CN118136488A true CN118136488A (en) 2024-06-04

Family

ID=91246861

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202410289625.8A Pending CN118136488A (en) 2024-03-13 2024-03-13 Sample injection heating device for secondary electrospray ionization source device

Country Status (1)

Country Link
CN (1) CN118136488A (en)

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