CN212411998U

CN212411998U - Capillary heating element and mass spectrometer

Info

Publication number: CN212411998U
Application number: CN202020591368.0U
Authority: CN
Inventors: 刘思雨; 张丽平
Original assignee: Kunshan Nier Precision Instrument Co ltd
Current assignee: Kunshan Nier Precision Instrument Co ltd
Priority date: 2020-04-20
Filing date: 2020-04-20
Publication date: 2021-01-26
Anticipated expiration: 2030-04-20

Abstract

The utility model provides a capillary heating element and mass spectrograph, wherein, capillary heating element includes: the device comprises an installation base, a heating base, a ceramic heating element, a pressing element, a sample injection capillary tube and a cover cap; the heating base assembles in the one side of installation base, is provided with adiabatic seal structure between the two, ceramic heating member assembles on the heating base to compress tightly fixedly by compressing tightly the piece, advance a kind capillary and pass the block according to advancing the kind direction in proper order, compress tightly the piece, ceramic heating member, heating base and installation base, and form heat conduction with ceramic heating member, advance the entrance point of kind capillary and be totally by the block cladding, its exit end stretches out from the installation base. The utility model discloses a capillary heating element adopts ceramic heating element to heat advancing kind capillary, and it has small, the low power dissipation, heats advantage even, with adjustable temperature fast. The sample injection capillary tube is completely wrapped in the heating assembly, so that the heating efficiency can be improved, and the temperature uniformity of the whole capillary tube can be ensured.

Description

Capillary heating element and mass spectrometer

Technical Field

The utility model relates to a mass spectrometry detects technical field, especially relates to a capillary heating element and mass spectrograph.

Background

The mass spectrometry technology has the advantages of high detection sensitivity, high analysis speed, strong specificity and the like, and is widely applied to the aspects of chemical analysis, life science analysis, clinical detection and the like. For diverse analytes, different ionization methods can be used, including electrospray ionization, analytical electrospray ionization, atmospheric pressure chemical ionization, extractive electrospray ionization, real-time direct analysis, matrix-assisted laser analytical ionization, and the like. For liquid samples, the ionization efficiency of the ion source is closely related to the desolvation effect. Taking electrospray ionization as an example, a liquid sample forms a Taylor cone at the tip of a spray needle under the action of a high-voltage electric field in an open environment, atomized charged liquid drops enter air, the liquid drops are continuously reduced along with the continuous volatilization of a solvent, when the coulomb acting force of charges on the inner surface of the liquid drops is greater than the surface tension of the liquid drops, coulomb explosion can be generated to form smaller charged liquid drops, the solvent is continuously volatilized, the process is repeated, and finally gas-phase ions are formed.

Because the solvent removing effect of the atomized liquid drops is poor, the liquid drops generated by spraying can not be completely converted into target ions, and the detection efficiency of the mass spectrum is influenced, so that the conventional mass spectrometer usually uses a heating mode of dry auxiliary gas flow to improve the solvent removing effect. However, the traditional method needs an instrument to be additionally provided with a gas channel, so that the structure is not compact enough. The gas flow rate needs to be adjusted according to different methods, and meanwhile, the gas allowance of the gas cylinder needs to be noticed at any time, so that the operation is inconvenient. In addition, the heating wire usually adopts an integral wrapping sample feeding structure mode, so that the energy consumption of an instrument system is increased. Therefore, it is necessary to provide a further solution to the above problems.

SUMMERY OF THE UTILITY MODEL

The utility model aims at providing a capillary heating element and mass spectrograph to overcome the not enough that exists among the prior art.

In order to solve the technical problem, the technical scheme of the utility model is that:

a capillary heating assembly, comprising: the device comprises an installation base, a heating base, a ceramic heating element, a pressing element, a sample injection capillary tube and a cover cap;

the heating base assemble in the one side of installation base is provided with adiabatic seal structure between the two, ceramic heating member assemble in on the heating base, and by it compresses tightly fixedly to compress tightly the piece, the block forms with the heating base and is used for ceramic heating member and the airtight space that compresses tightly an assembly, advance the kind capillary and pass in proper order according to advancing the kind direction the block, compress tightly a piece, ceramic heating member, heating base and installation base, and with ceramic heating member forms the heat conduction, advance the kind capillary entrance point completely by the block cladding, its exit end is certainly the installation base stretches out.

As the utility model discloses a capillary heating element's improvement, it is used for making to offer on the installation base capillary heating element assembles a plurality of pilot holes fixed.

As an improvement of the capillary tube heating assembly of the present invention, the heat insulating seal comprises: the heat insulation ring, set up in first seal groove on the heating base, set up in second seal groove on the installation base, be provided with in the first seal groove support lean on in the first sealing washer of the last one side of heat insulation ring, be provided with in the second seal groove support lean on in the second sealing washer of another side on the heat insulation ring.

As the utility model discloses an improvement of capillary heating element, the third seal groove has still been seted up to the another side of installation base, be provided with in the third seal groove support by in the third sealing washer of capillary heating element's assembly surface.

As an improvement of the capillary heating element of the present invention, the ceramic heating element is a ceramic heating ring, which is assembled in a fixing groove on the heating base.

As the utility model discloses a capillary heating element's improvement, it has the face that compresses tightly to compress tightly one end, the peripheral edge of the face that compresses tightly is fixed in through the screw on the heating base, the other end forms and is used for the fixed link of block spiro union.

As the utility model discloses an improvement of capillary heating element, advance kind of capillary sealed fixed by capillary sealing joint, capillary sealing joint be located by the block, compress tightly a piece, ceramic heating member and heat the cavity that the base encloses.

As the utility model discloses a capillary heating element's improvement, still be provided with a temperature sensor on the heating base, its with ceramic heating member is connected with a temperature controller.

a mass spectrometer, comprising: the inner part of the shell is divided into a primary vacuum cavity and a secondary vacuum cavity by a partition plate; the mass spectrometer further comprises: a capillary heating assembly as described above;

the capillary heating assembly is fixed on the panel on one side of the shell, and the outlet end of the sample injection capillary extends into the primary vacuum cavity.

As an improvement of the mass spectrometer of the present invention, the ion funnel of the mass spectrometer is located in the primary vacuum cavity, the quadrupole guide rod, the ion trap and the detector of the mass spectrometer are located in the secondary vacuum cavity, and the separator is further provided with a cone lens;

the exit end, ion funnel, taper lens, quadrupole guide rod, the ion trap of advance kind capillary are located a measuring path in proper order, the detector is located one side of ion trap, mechanical pump suction inlet has still been seted up on the one-level vacuum cavity, molecular pump suction inlet has still been seted up on the second grade vacuum cavity.

Compared with the prior art, the beneficial effects of the utility model are that: the utility model discloses a capillary heating element adopts ceramic heating element to heat advancing kind capillary, and it has small, the low power dissipation, heats advantage even, with adjustable temperature fast. The sample injection capillary tube is completely wrapped in the heating assembly, so that the heating efficiency can be improved, and the temperature uniformity of the whole capillary tube can be ensured. Capillary heating element still has the sealed design of adiabatic, can guarantee self and with the applied leakproofness between the mass spectrograph, and then guarantee the vacuum requirement of mass spectrograph rear end.

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 described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.

Fig. 1 is an exploded perspective view of a capillary tube heating assembly according to a first embodiment of the present invention;

fig. 2 is a cross-sectional view of a capillary tube heating assembly according to a first embodiment of the present invention;

fig. 3 is a front view of a mass spectrometer according to a second embodiment of the present invention;

FIG. 4.1 is a mass spectrum of a rhodamine B molecule with a mass-to-charge ratio 443 under room temperature conditions, which is detected by a mass spectrometer without the first embodiment;

FIG. 4.2 is a mass spectrum of rhodamine B molecule with a mass-to-charge ratio 443 detected by a mass spectrometer of the first embodiment under a heating condition of 200 ℃.

Detailed Description

The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.

As shown in fig. 1 and 2, a first embodiment of the present invention provides a capillary tube heating assembly 100, which includes: the device comprises a mounting base 2, a heating base 4, a ceramic heating element 5, a pressing element 7, a sample injection capillary 9 and a cover cap 8.

The mounting base 2 is used for mounting and fixing the capillary tube heating assembly 100 of the present embodiment. Correspondingly, the mounting base 2 is provided with a plurality of mounting holes for mounting and fixing the capillary tube heating assembly 100. In one embodiment, the number of the mounting holes is four, and the four mounting holes are distributed at four corners of the mounting base 2, so that the mounting base can be fixed on the applied mass spectrometer through screws. Meanwhile, the mounting base 2 is also provided with a through hole for the sample injection capillary 9 to pass through, and a protruding part for keeping the capillary extending into the mass spectrometer is arranged on the through hole in a protruding mode.

The heating base 4 is used for realizing the installation and fixation of the heating base 4. Specifically, the heating base 4 is fitted to one surface of the mounting base 2, and in order to ensure heat insulation sealing property, a heat insulation sealing structure is provided therebetween, the heat insulation sealing structure including: the heat insulating ring 3, a first seal groove 12 provided in the heating base 4, and a second seal groove 11 provided in the mounting base 2. Wherein, a first sealing ring which is abutted against one surface of the heat insulating ring 3 is arranged in the first sealing groove 12, and a second sealing ring which is abutted against the other surface of the heat insulating ring 3 is arranged in the second sealing groove 11.

Meanwhile, the vacuum requirement at the rear end of the mass spectrometer is further ensured in order to ensure the sealing performance between the mass spectrometer and the applied mass spectrometer. A third sealing groove 10 is further formed in the other surface of the mounting base 2, and correspondingly, a third sealing ring abutting against the mass spectrometer mounting surface is arranged in the third sealing groove 10.

In one embodiment, the first, second, and third seal rings are made of high-temperature-resistant fluororubber seal rings.

The ceramic heating element 5 is used for heating the sample injection capillary 9 to replace a heating mode of adopting dry auxiliary gas flow in the prior art, and has the advantages of small volume, low power consumption, rapid and uniform heating and adjustable temperature.

Specifically, the ceramic heating element 5 is assembled on the heating base 4 and is pressed and fixed by the pressing member 7, so that the ceramic heating element 5 is closely attached to the heating base 4. In one embodiment, the ceramic heating element 5 is a ceramic heating ring that fits into a retaining groove on the heating base 4, the retaining groove being sized and shaped to accommodate the ceramic heating ring. One end of the pressing piece 7 is provided with a pressing surface, the peripheral edge of the pressing surface is fixed on the heating base 4 through screws, and the other end of the pressing surface forms a connecting end for fixing the cap 8 in a threaded manner.

The cap 8 and the heating base 4 form a closed space for assembling the ceramic heating element 5 and the pressing element 7. The cap 8 has a tapered structure, and as described above, when the other end of the pressing member 7 is a threaded end, the tapered cap 8 is assembled on the pressing member 7 in a threaded connection manner, and the end surface of the tapered cap abuts against the heating base 4 to form the above-mentioned sealed space.

The sample injection capillary 9 is used for sample injection and can be made of stainless steel. Specifically, the sample injection capillary 9 sequentially passes through the cap 8, the pressing member 7, the ceramic heating member 5, the heating base 4 and the mounting base 2 according to a sample injection direction, an inlet end of the sample injection capillary 9 is completely covered by the cap 8, and an outlet end of the sample injection capillary extends out of the mounting base 2. So, advance appearance capillary 9 and wrap up in heating element completely, can improve heating efficiency and guarantee that whole capillary temperature is homogeneous.

Further, the sample injection capillary 9 and the ceramic heating element 5 form heat conduction. Meanwhile, the sample injection capillary 9 is sealed and fixed by a capillary sealing joint 6, the capillary sealing joint 6 is located in a cavity surrounded by the cap 8, the pressing piece 7, the ceramic heating piece 5 and the heating base 4, and one end of the capillary sealing joint is screwed into the heating base 4. Therefore, the ceramic heating element 5 transfers heat to the cap 8, the pressing element 7, the capillary sealing joint 6 and the heating base 4, and further transfers the sample injection capillary 9, so that the sample injection capillary 9 is integrally heated, and the heating efficiency is high.

In addition, a temperature sensor is arranged on the heating base 4, and is connected with the ceramic heating element 5 and a temperature controller, so that the heating temperature of the ceramic heating element 5 can be controlled and adjusted. The temperature sensor and the temperature controller can be made of existing products, and are combined and applied to the technical scheme of the embodiment, the embodiment does not relate to the improvement of the temperature sensor and the temperature controller, and for example, the temperature controller with the model number of TLPY-TL4 can be used.

Based on the same technical concept, the utility model discloses still provide a mass spectrometer.

As shown in fig. 3, a second embodiment of the present invention provides a mass spectrometer, which includes: a housing, an ion funnel 302, a quadrupole guide rod 306, an ion trap 307, a detector 308.

The shell is internally divided into a primary vacuum cavity 301 and a secondary vacuum cavity 305 by a partition plate; characterized in that the mass spectrometer further comprises: the capillary heating assembly 100 as described above. The capillary heating assembly 100 is fixed on a panel 311 on one side of the housing, and the outlet end of the sample injection capillary 9 extends into the primary vacuum cavity 301.

An ion funnel 302 of the mass spectrometer is positioned in a primary vacuum cavity 301, a quadrupole guide rod 306, an ion trap 307 and a detector 308 of the mass spectrometer are positioned in a secondary vacuum cavity 305, and a conical hole lens 303 is further arranged on a partition plate.

The outlet end of the sample capillary 9, the ion funnel 302, the tapered hole lens 303, the quadrupole guide rod 306 and the ion trap 307 are sequentially located on a detection path, the detector 308 is located on one side of the ion trap 307, the primary vacuum cavity 301 is further provided with a mechanical pumping port 304, and the secondary vacuum cavity 305 is further provided with a molecular pumping port 309.

When the mass spectrometer works, the ion source is an electrospray ion source, and the electrospray ion source 310 is over against the mass spectrum sample injection capillary 9. Setting the heating temperature of the heating assembly according to the sample property information, starting the ion source after the set temperature is reached, starting sample introduction, enabling the sample ionized by the electrospray ion source 310 to enter the capillary heating assembly 100, further desolvating under the action of high temperature, then flying out from the other end of the capillary, entering the ion funnel 302, performing primary focusing on the ion funnel 302, entering the ion trap 307 for mass analysis under the guiding action of the four-stage guide rod 306 through the conical hole lens 303, and finally ejecting ions with different mass-to-charge ratios out of the ion trap 307 at different times to enter the detector 308 to finish ion detection.

In order to verify the detection effect of the mass spectrometer adopting the second embodiment, as shown in fig. 4.1 and 4.2, fig. 4.1 is a mass spectrum of the rhodamine B molecule with the mass-to-charge ratio 443, which is detected by the mass spectrometer not adopting the first embodiment under the room temperature condition; FIG. 4.2 is a mass spectrum of rhodamine B molecule with a mass-to-charge ratio 443 detected by a mass spectrometer of the first embodiment under a heating condition of 200 ℃. As can be seen from the two groups of mass spectrum detection results, the desolvation effect of the sample ions is obviously enhanced and the ion signal intensity is obviously improved under the heating condition.

To sum up, the utility model discloses a capillary heating element adopts ceramic heating element to heat advance kind capillary, and it has small, the low power dissipation, heats advantage even, that the temperature is adjustable fast. The sample injection capillary tube is completely wrapped in the heating assembly, so that the heating efficiency can be improved, and the temperature uniformity of the whole capillary tube can be ensured. Capillary heating element still has the sealed design of adiabatic, can guarantee self and with the applied leakproofness between the mass spectrograph, and then guarantee the vacuum requirement of mass spectrograph rear end.

It is obvious to a person skilled in the art that the invention is not restricted to details of the above-described exemplary embodiments, but that it can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims

1. A capillary heating assembly, comprising: the device comprises an installation base, a heating base, a ceramic heating element, a pressing element, a sample injection capillary tube and a cover cap;

2. The capillary heating element of claim 1, wherein the mounting base defines a plurality of mounting holes for mounting and fixing the capillary heating element.

3. The capillary heating assembly of claim 1, wherein the thermally insulating seal comprises: the heat insulation ring, set up in first seal groove on the heating base, set up in second seal groove on the installation base, be provided with in the first seal groove support lean on in the first sealing washer of the last one side of heat insulation ring, be provided with in the second seal groove support lean on in the second sealing washer of another side on the heat insulation ring.

4. The capillary tube heating element according to any one of claims 1 to 3, wherein a third sealing groove is further formed in the other surface of the mounting base, and a third sealing ring abutting against the assembling surface of the capillary tube heating element is disposed in the third sealing groove.

5. The capillary heating assembly of claim 1, wherein the ceramic heating element is a ceramic heating ring that fits into a retaining groove on the heating base.

6. The capillary heating element according to claim 1 or 5, wherein the pressing member has a pressing surface at one end, the peripheral edge of the pressing surface is fixed to the heating base by screws, and the other end forms a connecting end for screw-fixing the cap.

7. The capillary heating assembly of claim 1, wherein the sample capillary is sealingly secured by a capillary seal fitting located in a cavity enclosed by the cap, the compression member, the ceramic heating element, and the heating base.

8. The capillary heating assembly of claim 1, wherein the heating base further comprises a temperature sensor coupled to the ceramic heating element and a temperature controller.

9. A mass spectrometer, comprising: the inner part of the shell is divided into a primary vacuum cavity and a secondary vacuum cavity by a partition plate; characterized in that the mass spectrometer further comprises: the capillary tube heating assembly of any one of claims 1 to 8;

10. The mass spectrometer of claim 9, wherein an ion funnel of the mass spectrometer is located in the primary vacuum chamber, a quadrupole guide rod, an ion trap and a detector of the mass spectrometer are located in the secondary vacuum chamber, and a conical hole lens is further arranged on the partition plate;