CN218631910U - Sample carrying device for solid or liquid thermal desorption sample injection of ion mobility spectrometer - Google Patents
Sample carrying device for solid or liquid thermal desorption sample injection of ion mobility spectrometer Download PDFInfo
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- CN218631910U CN218631910U CN202222675635.4U CN202222675635U CN218631910U CN 218631910 U CN218631910 U CN 218631910U CN 202222675635 U CN202222675635 U CN 202222675635U CN 218631910 U CN218631910 U CN 218631910U
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Abstract
The utility model belongs to the analytical chemistry instrument field, concretely relates to a carry appearance device that is used for ionic migration spectrometer solid or liquid thermal desorption to advance kind. The sampling slide comprises a sample carrying table and a sampling slide, wherein the sample carrying table is provided with a cylindrical groove for placing the sampling slide, the sampling slide consists of an upper-layer annular metal sheet, a middle-layer sampling paper and a lower-layer circular metal sheet which are coaxially arranged, the upper, middle and lower layers of the sampling slide are laminated into an integral structure, and the part where the annular metal sheet and the sampling paper are not overlapped is a sample area. The utility model is used for the thermal desorption of analysis appearance solid or liquid advances kind, simple structure, and convenient to use can improve thermal desorption efficiency, and the good reliability.
Description
Technical Field
The utility model belongs to the analytical chemistry instrument field, concretely relates to carry appearance device that is used for ionic migration spectrum analysis appearance solid or liquid thermal desorption to advance appearance.
Background
The Ion Mobility Spectrometry (IMS) technology is a separation and detection technology appearing in the 70 th 20 th century, and compared with the traditional mass Spectrometry and chromatography instruments, the IMS separation and detection technology has the characteristics of simple structure, high sensitivity, high analysis speed and reliable result. The thermal desorption sample injector is an essential component used in a multifunctional ion mobility spectrometry rapid detector, the performance of the thermal desorption sample injector is good and bad, the sampling efficiency and the overall performance of the ion mobility spectrometry are directly determined, the heating is realized by controlling the temperature through a heating rod, and the heating temperature belongs to a constant temperature control mode.
The sample injection device for the thermal desorption sample injector does not have a commercialized instrument at present, and each research unit is designed and improved correspondingly according to the use requirements of different instruments. The existing sample injection assembly has low thermal desorption efficiency, synchronous desorption of a sample when the sample is tiled with a substrate, and interference influence when the sample is repeatedly used; for example, in patent CN201721139511.7, a sample is directly placed on the surface of a sample loading table, and the desorption process is affected, in patent CN201220715903.4, the sample loading device has a complex structure, and although accurate sample injection can be realized, the thermal desorption efficiency is low; some sample carriers can only be suitable for gas, and the sample carrier is inconvenient to replace, which is not beneficial to repeated tests, for example, in patent CN201721443983.1, when liquid sample injection is needed, the sample carrier cannot be replaced, which is inconvenient to perform other tests. Therefore, it is necessary to design and research a novel sample injector structure to improve the thermal desorption efficiency, and the sample injector is widely applicable to solid or liquid samples.
SUMMERY OF THE UTILITY MODEL
For solving the problem that prior art exists, the utility model provides a carry appearance device that is used for ionic migration spectrometer solid or liquid thermal desorption to advance kind.
In order to realize the purpose of the utility model, the utility model adopts the following technical scheme:
the utility model provides a sample carrying device, which comprises a sample carrying platform and a sample carrying slide; the sample carrying table is provided with a cylindrical groove for placing a sample carrying slide; the sample-feeding slide consists of an upper-layer circular metal sheet, a middle-layer sampling paper and a lower-layer circular metal sheet which are coaxially arranged, the upper layer of annular metal sheet and the lower layer of annular metal sheet are occluded and sealed into an integral structure through the periphery.
In the above technical scheme, further, the cylindrical groove is coaxial with the sample injection slide.
In the above technical solution, further, the inner diameter of the cylindrical groove is 8-12mm; the thickness of the groove is 0.5-2mm; the outer diameter of the sample injection slide is equal to the inner diameter of the groove or the outer diameter of the sample injection slide is smaller than the inner diameter of the groove, so that the sample injection slide is just arranged in the sample loading table and is prevented from moving.
In the above technical scheme, further, the outer diameter of the sample injection slide is 0.5-2mm smaller than the inner diameter of the groove.
In the above technical scheme, further, the difference between the outer circle and the inner circle of the annular radius of the circular metal sheet is 1-3mm.
In the above technical scheme, further, the part of the circular metal sheet which is not overlapped with the sampling paper is a sample area, and the inner diameter of the sample area is 5-11mm.
In the technical scheme, the sample carrying platform is made of iron, aluminum and stainless steel, heat conduction for a sample carrying slide is easy to realize, and heat of the sample carrying platform comes from the thermal desorption sample injector; the circular metal sheets and the circular metal sheets are made of aluminum sheets or iron sheets.
When in use, the sample loading slide is arranged in the groove of the sample loading table, the sample loading table is arranged in the support of the thermal desorption sample injector, the heat of the sample loading device comes from the thermal desorption sample injector, the temperature range of the heat source is 25-200 ℃, the ultrahigh temperature causes the sampling paper to generate a thermal desorption signal, and the upper layer circular metal sheet and the lower layer circular metal sheet of the sample loading piece are heated.
The sampling slide is internally provided with a sampling paper loaded sample table, a sampling slide lower layer metal sheet and a sampling slide upper layer annular metal sheet which are heated up and down in a triple mode, so that the heat efficiency is improved.
Compared with the prior art, the invention has the following beneficial effects: the sample carrier has simple structure, the design of the sample carrier is suitable for solid or liquid thermal desorption sample injection, the sample diffusion area can be effectively increased, and the sample introduction efficiency is improved; in the process of the thermal desorption, the upper and lower metal sheets of the sample loading plate and the metal cavity of the sample loading table are heated and transferred at the same time, the thermal desorption efficiency can be improved, the thermal desorption time is shortened, the thermal desorption signal is enhanced, and the detection sensitivity is favorably improved; the sample injection slide three-layer integrated structure is simple and convenient to use and good in reliability.
Drawings
FIG. 1 is a schematic view of the loading device;
FIG. 2 is a top view of a sample slide;
FIG. 3 is a schematic longitudinal sectional view of a sample slide;
in the figure, 1, a sample loading table, 2, a sample loading slide, 3, a groove, 4, a circular metal sheet, 5, middle layer sampling paper and 6, a circular metal sheet;
FIG. 4 is a graph of an analyzer for detecting propofol ion mobility spectrometry spectra in 10 μ L and 10ppm blood by using direct sampling paper;
FIG. 5 is a graph of a sample injection spectrum of Propofol ion in blood of 10 μ L and 10ppm detected by the analyzer using the sample loading device of the present application.
Detailed Description
The invention is further illustrated but is not in any way limited by the following specific examples.
Example 1
The utility model relates to a sample carrying device for solid or liquid thermal desorption sample introduction of an ion mobility spectrometer, which comprises a sample carrying platform 1 and a sample introduction slide 2; the upper surface of the sample carrying table is provided with a cylindrical groove 3, and a sample carrying slide 2 is placed in the groove; the inner diameter of a cylindrical groove arranged in the upper surface of the sample loading platform is 11mm; the heat of the sample carrying table comes from the thermal desorption sample injector layer top (temperature controlled heating by heating rod and sensor). The temperature of the thermal desorption sample injector is set to be 150 ℃. When in use, the sample carrying table is placed in the thermal desorption sample injector bracket.
The use of two materials for the comparative sample support, firstly, the stainless steel plate material which is easy to conduct heat and secondly, the polytetrafluoroethylene material.
The balance temperature of the sample carrying table for testing the stainless steel plate is 150 ℃, the balance temperature of the sample carrying table for testing the polytetrafluoroethylene material is lower than 150 ℃, and the balance temperature is related to the heating time length. Obviously, the sample carrying table made of stainless steel is more beneficial to improving the thermal desorption efficiency in the thermal desorption sample introduction.
Example 2
A sample carrying device for solid or liquid thermal desorption sample injection of an ion mobility spectrometer comprises a sample carrying table 1 and a sample injection slide 2; the upper surface of the sample carrying table is provided with a cylindrical groove 3, a sample carrying slide is placed in the groove, and the cylindrical groove is coaxial with the sample carrying slide; the inner diameter of a circular groove arranged in the upper surface of the sample loading platform is 11mm; the thickness of the groove is 1mm; the sample carrying table is made of stainless steel plate easy to conduct heat, and the heat of the sample carrying table comes from the top of the upper layer of the thermal desorption sample injector (heated to 150 ℃ by a heating rod and a sensor under the controlled temperature). The sample introduction carrier is composed of an upper layer circular metal sheet 4, a middle layer sampling paper 5 and a lower layer circular metal sheet 6 which are coaxially arranged, and the upper layer, the middle layer and the lower layer of the sample introduction carrier are laminated into an integral structure. When the sample carrier is used, the sample carrier is placed in the thermal desorption sample injector bracket, and the sample injection slide is placed in the groove of the sample carrier.
The lower surface of the sample slide is contacted with the cylindrical groove, and the sample slide is a three-layer semi-surrounding structure; the bottom layer structure of the sample carrier is that a layer of sampling paper is pressed on a circular metal sheet such as an aluminum foil sheet, a circular metal sheet with a hollow middle is arranged on the sampling paper, the sample carrier is viewed from the upper layer, and a layer of sampling paper is arranged below the circular metal aluminum foil sheet; the sample injection slide is the same piece from the upper and lower structures, and the bottom layer metal aluminum foil (lower) and the annular metal aluminum foil (upper) are pressed together through the periphery to form an integral structure.
The maximum outer diameter of sampling paper of the sample carrying slide aluminum foil bag is 10mm, the sampling paper is just placed in the sample carrying table to avoid moving, and the part where the circular ring-shaped metal sheet and the sampling paper are not overlapped is a sample area, namely, the area of the sampling paper exposed on the upper layer of the sample carrying slide is a sample area, and the radius is 8mm.
Compared with a sample carrying slide, the sample carrying slide has a structure that three layers of aluminum foils surround sampling paper, and direct sampling paper (10 mm) is respectively arranged in a sample carrying table for sample introduction.
The pipettor takes 10 muL and 10ppm propofol samples in blood to drop into the sample area, and records the change of the thermal desorption time of two different sample slides. The detection of the direct sampling paper reduces the signal intensity to 50mv when the analysis time is 200S, as shown in FIG. 4; the signal intensity is reduced to 50mv when the sample introduction slide glass detection is carried out for the analysis time of 150S, and as shown in figure 5, the desorption time is improved by 25 percent.
Example 3
Compared with the liquid sampling efficiency of different sampling slides, the sampling slide in the embodiment 2 of the application is directly used, and the sampling paper (10 mm) is directly used and is respectively placed in the sample carrying table for sampling.
Parameters set by the ion mobility spectrometer: the temperature of the transfer tube is 100 ℃, and the temperature of the sample injector is 150 ℃; the air source is a purified air source, the flow rate of the bleaching gas is 500sccm, the flow rate of the dopant carrier gas is 100sccm, the flow rate of the sample carrier gas is 400sccm, the propofol samples in 10 muL and 10 ng/muL blood are dripped into the sample area by a pipette, and ion mobility spectrograms of propofol thermal desorption curves of two different sample injection slides are recorded, as shown in figures 4 and 5.
The highest signal intensity of 360mv in the thermal desorption interval of the direct sampling paper sample injection (figure 4) and the highest signal intensity of 450mv in the three-layer sample injection slide injection (figure 5). Cumulatively calculating the peak area of the propofol doublet in 120S, which is 84608mv in FIG. 4 and 93252mv in FIG. 5; the total amount of the desorbed propofol is consistent with that of the desorbed propofol after the desorption time is prolonged. But the spectrogram and experimental data obviously show that the three-layer sample injection slide sample injection (figure 4) has high desorption speed, the desorption signal is enhanced, and the thermal desorption efficiency is improved.
It will be apparent to those skilled in the art that many changes and modifications can be made, or equivalents employed, to the presently disclosed embodiments without departing from the intended scope of the invention. Therefore, any simple modification, equivalent change and modification made to the above embodiments according to the technical essence of the present invention shall still fall within the protection scope of the technical solution of the present invention.
Claims (7)
1. The sample carrying device is characterized by comprising a sample carrying table (1) and a sample carrying slide (2); the sample carrying table is provided with a cylindrical groove (3) for placing a sample carrying slide; the sample introduction slide glass is composed of an upper-layer circular metal sheet (4), a middle-layer sampling paper (5) and a lower-layer circular metal sheet (6) which are coaxially arranged, and the upper layer, the middle layer and the lower layer of the sample introduction slide glass are laminated into an integral structure.
2. The sample loading device according to claim 1, wherein the cylindrical recess (3) is coaxial with the sample slide.
3. The sample loading device of claim 1, wherein the cylindrical recess has an inner diameter of 8-12mm; the thickness of the groove is 0.5-2mm; the outer diameter of the sample injection slide is equal to the inner diameter of the groove (3) or the outer diameter of the sample injection slide is smaller than the inner diameter of the groove (3).
4. The sample carrier device according to claim 3, characterized in that the outer diameter of the sample carrier is 0.5-2mm smaller than the inner diameter of the recess (3).
5. The sample loading device of claim 1, wherein the difference between the outer circle and the inner circle of the annular radius of the circular ring-shaped metal sheet is 1-3mm.
6. The sample loading device according to claim 1, wherein the non-coincident part of the upper annular metal sheet of the sample loading plate and the sampling paper is a sample area, and the inner diameter of the sample area is 5-11mm.
7. The sample loading device according to claim 1, wherein the sample loading platform is made of iron, aluminum or stainless steel; the circular metal sheets and the circular metal sheets are made of aluminum sheets or iron sheets.
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CN202222675635.4U CN218631910U (en) | 2022-10-11 | 2022-10-11 | Sample carrying device for solid or liquid thermal desorption sample injection of ion mobility spectrometer |
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CN202222675635.4U CN218631910U (en) | 2022-10-11 | 2022-10-11 | Sample carrying device for solid or liquid thermal desorption sample injection of ion mobility spectrometer |
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