CN114112628A - Sample detection system, heating device, heating assembly and use method of heating device - Google Patents
Sample detection system, heating device, heating assembly and use method of heating device Download PDFInfo
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- CN114112628A CN114112628A CN202111408485.4A CN202111408485A CN114112628A CN 114112628 A CN114112628 A CN 114112628A CN 202111408485 A CN202111408485 A CN 202111408485A CN 114112628 A CN114112628 A CN 114112628A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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Abstract
The invention relates to a sample detection system, a heating device, a heating assembly and a using method of the heating device. The heating device includes a heating assembly and a sample carrier. The sample carrier is used for carrying a sample. The heating assembly includes a first heating member and a second heating member. A placing plane is arranged on the first heating element. The placing plane is provided with a heating hole. One side surface of the second heating member abuts against the first heating member, and the other side surface of the second heating member can penetrate through the heating hole. The outer surface of the second heating member is spaced from the inner wall of the heating hole. The heat of the second heating member is not equal to the heat of the first heating member. The sample carrier is placed on the placement plane and covers the heating aperture. The detection device detects the heated sample. Heating device can guarantee sample detecting system's effective operation in succession to the material of different boiling points thermal desorption in different time windows, has also guaranteed the precision of testing result.
Description
Technical Field
The invention relates to the technical field of sample detection, in particular to a sample detection system, a heating device, a heating assembly and a using method of the heating device.
Background
With the wide application of liquid chromatography-mass spectrometry systems in complex compound system analysis, atmospheric pressure electrospray ion sources and atmospheric pressure chemical ionization sources play an important role. The thermal desorption device is used for increasing the saturated vapor pressure of substances with poor volatility under atmospheric pressure, and is a key component of in-situ ionization mass spectrum. The existing thermal desorption device cannot give consideration to substances with low desorption temperature and high desorption temperature. At lower temperatures, the high boiling point analytes cannot be effectively desorbed and cannot be detected; at higher temperatures, the components of the mixture will be desorbed simultaneously, causing ionization competition of each component and mass spectrum peak congestion. More importantly, the desorption temperature is set too high, and low boiling point analytes are easy to crack and can not be effectively detected. Meanwhile, the film belt is directly contacted with the high-temperature heating assembly, can be melted and broken even releases other unrelated chemical substances when being in a high-temperature environment for a long time, and influences the continuous and effective operation and the detection precision of the whole thermal desorption device.
Disclosure of Invention
In view of the above, it is desirable to provide a sample detection system, a heating device, a heating assembly, and a method for using a heating device that thermally desorb substances with different boiling points.
A heating assembly comprises a first heating element and a second heating element, wherein a placing plane is arranged on the first heating element and used for placing a sample bearing piece and transmitting the heat of the first heating element to the sample bearing piece, and a heating hole is formed in the placing plane; the second heating member can wear to establish in the heating hole, the second heating member is used for the orientation a side that the sample holds the carrier is not higher than in the ascending position of direction of gravity place the plane in the ascending position of direction of gravity, the surface of second heating member with heating hole inner wall looks interval, the heat of second heating member with the heat of first heating member is not equal.
In one embodiment, the first heating member includes a heating body and a first heating portion, the placing plane is disposed on the heating body, the heating body is connected to one end of the second heating member, the first heating portion is disposed in the heating body, and heat of the first heating portion can be transferred to the placing plane through the heating body.
In one embodiment, the second heating member includes a fixing portion and a second heating portion, the fixing portion is abutted to the first heating member, one end of the second heating portion is connected to the fixing portion, and the other end of the second heating portion is inserted into the heating hole.
In one embodiment, the second heating member further includes a heat insulating portion, one side of the heat insulating portion is connected to the fixing portion, the other side of the heat insulating portion facing away from the fixing portion is connected to the first heating member, one end of the second heating portion is connected to the heat insulating portion, and the second heating portion is located between the first heating member and the fixing portion.
In one embodiment, the heat insulation part is provided with a kidney-shaped hole, and the second heating part is movably connected to the heat insulation part through the kidney-shaped hole.
In one embodiment, the diameter of the heating hole is in the range of 2mm to 8mm, and the outer diameter of the second heating part is in the range of 2mm to 3 mm.
A heating device comprising a heating assembly as described above and a sample carrier for carrying a sample, the sample carrier being placed on the placement plane and covering the heating well.
A sample detection system comprises a detection device and the heating device, wherein the detection device is used for detecting a sample heated by the heating device.
A method of using a heating device, comprising the steps of:
placing a sample bearing member on the placing plane and covering the sample bearing member on the heating hole;
placing a sample on the sample carrier;
controlling the temperature of the heating hole to a first temperature, heating the sample bearing piece, and keeping a preset low-temperature heating time;
controlling the temperature of the heating hole to a second temperature; wherein the second temperature is less than the first temperature;
and finishing heating.
In one embodiment, the maintaining of the preset low temperature heating time further includes:
controlling the temperature of the central area of the heating hole to a third temperature, and keeping a preset high-temperature heating time; wherein the third temperature is higher than the first temperature;
controlling the temperature of the heating hole to a second temperature; wherein the second temperature is less than the first temperature;
and finishing heating.
In one embodiment, the controlling the temperature of the heating hole to a first temperature includes:
controlling the temperature of the first heating member to the first temperature; or
Controlling the temperature of the first and second heating members to the first temperature.
In one embodiment, the temperature of the heating hole is controlled to a first temperature, and the first temperature is not greater than 200 ℃.
In one embodiment, the temperature of the central region of the heating hole is controlled to a third temperature, and the third temperature is not greater than 800 ℃.
According to the sample detection system, the heating device, the heating assembly and the use method of the heating device, when detection is needed, a sample is placed on the sample bearing piece, and the sample bearing piece is placed on the placing plane and covers the heating hole. When the liquid sample is heated, the first heating member and the second heating member are heated, respectively. Because the heat of the second heating member is not equal to the heat of the first heating member, and the outer surface of the second heating member is spaced apart from the inner wall of the heating hole. Can make the inner wall temperature of heating hole be higher than the temperature of second heating member through heat regulation, then make liquid sample at the in-process of being heated, the directional removal is regional to relative low temperature, second heating member top promptly, simultaneously with liquid sample restriction in relative microthermal second heating member top, avoid the outside region of sample smooth high temperature heating hole, thereby realize fixing a position liquid sample in the heating process, guarantee the position uniformity of liquid sample, make the stability difference that detects little. The repeatability of the detection device in the detection process is improved, and the detection precision is improved. The temperature of the inner wall and the edge of the heating hole is constant by keeping the heat of the first heating element, so that the constant-temperature heating function can be realized, the Leidenfrost effect of a liquid sample is avoided, and the safety and the reliability of the heating process are ensured.
The sample can be heated, detected and analyzed with different boiling points by only adjusting the heat of the first heating element or the second heating element. The sample can also be heated to the first temperature by controlling the heat of the first heating element, so that the temperature near the heating hole reaches the first temperature, the temperature of the second heating element reaches the first temperature, and the temperature of the first heating element and the temperature of the second heating element are consistent and constant, so that most of the low-boiling-point components can be desorbed without cracking. And then controlling the heat of the second heating element to quickly raise the temperature of the second heating element to a third temperature which is higher than the temperature of the edge of the heating hole, carrying out desorption analysis on the components with high boiling point, quickly reducing the temperature of the second heating element to restore the temperature to the second temperature, and finishing heating or preparing for next analysis. Because the preset high-temperature heating time of the second heating element is short, the sample bearing part cannot be damaged. The preset high-temperature heating time is usually 3s-10 s.
The sample detection system can meet the desorption and detection requirements of complex analyte systems with different desorption temperatures. Heating device and heating element can realize the material of different boiling points and thermal desorption in different time windows, reduce the ionization competition effect that traditional single subassembly brought, provide certain degree's separation function, improve qualitative and quantitative accuracy, have guaranteed sample detecting system's continuous effective operation, have also guaranteed the precision of testing result.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention.
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a heating apparatus according to an embodiment;
fig. 2 is a schematic structural diagram of the heating assembly in the embodiment of fig. 1.
The elements in the figure are labeled as follows:
10. a heating device; 100. a sample carrier; 110. a first plate; 120. a second plate; 200. a heating assembly; 210. a first heating member; 211. a fixed block; 212. heating plates; 2121. placing a plane; 213. heating the hole; 214. mounting holes; 220. a second heating member; 221. a fixed part; 222. a second heating section; 230. a heat insulating part; 300. and (4) a mounting piece.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Referring to fig. 1 and 2, a sample testing system in one embodiment includes a testing device and a heating device 10. The heating device 10 includes a heating assembly 200 and a sample carrier 100. The sample carrier 100 is used to carry a sample. The heating assembly 200 includes a first heating member 210 and a second heating member 220. The first heating member 210 is provided with a placing plane 2121. The placement plane 2121 is used for placing the sample carrier 100 and for transferring heat of the first heating element 210 to the sample carrier 100. The placing plane 2121 is provided with a heating hole 213. The second heating member 220 can be inserted into the heating hole 213. The second heating member 220 is for facing a side of the sample carrier 100 at a position not higher than a position of the placement plane 2121 in the direction of gravity. The outer surface of the second heating member 220 is spaced apart from the inner wall of the heating hole 213. The heat of the second heating member 220 is not equal to the heat of the first heating member 210. The sample carrier 100 is placed on the placement plane 2121 and covers the heating aperture 213. The detection device is used for detecting the sample heated by the heating device 10.
When a test is required, a sample is placed on the sample carrier 100, the sample carrier 100 is placed on the placement plane 2121, and is covered on the heating hole 213. When the sample in the liquid state is heated, the first heating member 210 and the second heating member 220 are heated, respectively. Since the heat of the second heating member 220 is not equal to the heat of the first heating member 210, the outer surface of the second heating member 220 is spaced apart from the inner wall of the heating hole 213. Can make the inner wall temperature of heating hole 213 be higher than the temperature of second heating member 220 through heat regulation, then make liquid sample at the in-process of being heated, the directional removal is regional to relative low temperature, second heating member 220 top promptly, simultaneously with liquid sample restriction in relative microthermal second heating member 220 top, avoid the sample to slide to the outside region of high temperature heating hole 213, thereby realize fixing a position liquid sample in the heating process, guarantee the position of liquid sample unanimity, make the stability difference of detection little. The repeatability of the detection device in the detection process is improved, and the detection precision is improved. The temperature of the inner wall and the edge of the heating hole 213 is kept constant by keeping the heat of the first heating element 210, so that the constant-temperature heating function can be realized, the occurrence of the Leidenfrost effect on a liquid sample is avoided, and the safety and the reliability of the heating process are ensured.
In one embodiment, a method of using the heating device 10 of any of the above embodiments, comprises the steps of:
placing the sample carrier 100 on the placement plane 2121 and covering the heating aperture 213;
placing a sample on the sample carrier 100;
controlling the temperature of the heating hole 213 to a first temperature, heating the sample carrier 100, and maintaining a preset low-temperature heating time;
controlling the temperature of the heating hole 213 to a second temperature; wherein the second temperature is less than the first temperature;
and finishing heating.
The second heating member 220 is inserted into the heating hole 213 and is located in a central region of the heating hole 213. The side of the second heating element 220 facing the sample carrier 100 may be flush with the rest plane 2121 or may be lower than the rest plane 2121.
In one embodiment, the maintaining of the preset low temperature heating time further includes:
controlling the temperature of the central region of the heating hole 213 to a third temperature, and maintaining a preset high temperature heating time; wherein the third temperature is higher than the first temperature;
controlling the temperature of the heating hole 213 to a second temperature; wherein the second temperature is less than the first temperature;
and finishing heating.
In one embodiment, controlling the temperature of the heating aperture 213 to a first temperature comprises:
controlling the temperature of the first heating member 210 to a first temperature; or
The temperatures of the first and second heating members 210 and 220 are controlled to a first temperature.
The manner of controlling the heating hole 213 to the first temperature can be selectively adjusted according to the actual detection requirement.
In one embodiment, the temperature of the heating hole 213 is controlled to a first temperature, and the first temperature is not greater than 200 ℃.
In one embodiment, the temperature of the central region of the heating hole 213 is controlled to a third temperature, and the third temperature is not greater than 800 ℃.
In one embodiment, controlling the temperature of the central region of the heating hole 213 to a third temperature includes:
the temperature of the second heating member 220 is increased to a third temperature.
In one embodiment, if the sample is in a liquid state, the first heating element 210 is controlled to a first temperature; alternatively, the sample carrier 100 is heated by controlling the first heating element 210 to a first temperature and the second heating element 220 to a second temperature.
When the sample is liquid, can only control first heating member 210 and heat, second heating member 220 does not heat, then near the temperature of heating hole 213 is higher than second heating member 220, and liquid sample restriction is in the relatively microthermal second heating member 220 top, avoids the sample to slide to the outside region of high temperature heating hole 213 to realize fixing a position liquid sample in the heating process, guarantee that the position of liquid sample is unanimous, make the stability difference of detection little.
In one embodiment, if the sample is in a solid state, the first heating element is controlled to a first temperature; alternatively, the second heating member is controlled to the first temperature. The solid sample can be heated by a single heating element, and the heating efficiency is improved.
In one embodiment, reducing the temperature of the first heating member 210 and the temperature of the second heating member 220 to the second temperature previously comprises:
and detecting the heated sample by using a detection device.
The sample can be heated, detected and analyzed for samples of different boiling points only by adjusting the heat of the first heating member 210 or the second heating member 220. The sample may be also heated to the first temperature in the vicinity of the heating hole 213 and the first temperature of the second heating member 220 by controlling the heat of the first heating member 210, and the temperature of the first heating member 210 and the temperature of the second heating member 220 may be the same and may be kept constant, so that most of the low-boiling components may be desorbed without being cracked. Then, the heat of the second heating member 220 is controlled to rapidly increase the temperature of the second heating member 220 to a third temperature higher than the temperature of the edge of the heating hole 213, and after the desorption analysis of the high boiling point component, the temperature of the second heating member 220 is rapidly reduced to return to the second temperature, and the heating is terminated or the next analysis is prepared. Since the preset high-temperature heating time of the second heating member 220 is short, the sample carrier 100 is not damaged.
It should be noted that the first temperature, the third temperature and the second temperature in the above embodiments are not fixed temperatures, nor are they specified temperatures of a certain value, and may be modified and adjusted according to actual detection needs or heating needs of sample components. Meanwhile, the high-temperature heating time is usually preset to be 3s to 10 s. The preset high temperature heating time may be increased for 12s, 20s or 30s according to the sample heating requirement as long as the sample carrier 100 is not damaged.
The sample detection system can meet the desorption and detection requirements of complex analyte systems with different desorption temperatures. Heating device 10 and heating element 200 can realize the material of different boiling points thermal desorption in different time windows, reduce the ionization competition effect that traditional single subassembly brought, provide the separation function of certain degree, improve qualitative and quantitative accuracy, have guaranteed sample detecting system's continuous effective operation, have also guaranteed the precision of testing result.
The heating device 10 may also heat the sample in a solid state. A solid sample in a powder or block form is directly placed on the sample carrier 100 and then heated and resolved by the first and second heating members 210 and 220.
In one embodiment, the heating device 10 further comprises a mount 300. The mount 300 is used to mount the heating assembly 200 within the instrument. Instruments including but not limited to mass spectrometers, other instruments requiring heating functionality may also be equipped with the heating assembly 200.
Further, the sample carrier 100 and the second heating element 220 are spaced apart. If the resting plane 2121 is a horizontal plane, the second heating element 220 is located below the horizontal plane and the sample carrier 100 is located on the horizontal plane. The placement plane 2121 may be other planes as long as the spacing between the second heating member 220 and the sample carrier 100 is provided. The non-contact between the second heating element 220 and the sample carrier 100 can prevent the sample carrier 100 from melting, breaking and releasing other unnecessary components when the second heating element 220 generates high temperature, thereby ensuring the continuous and effective operation of the sample detection system. Meanwhile, the high-boiling-point components can not be lost during low-temperature desorption; when the low-boiling-point components are desorbed at high temperature, the cracking of the low-boiling-point components is not caused. The accuracy of the detection result is also ensured. In one embodiment, if the resting plane 2121 is a horizontal plane, a side of the second heating element 220 facing the sample carrier 100 is flush with the horizontal plane, and the sample carrier 100 can contact both the resting plane 2121 and a side of the second heating element 220. Whether the sample carrier 100 and the second heating member 220 are spaced apart, that is, the positional relationship between the placement plane 2121 and a side surface of the second heating member 220 can be adjusted as necessary according to actual detection conditions.
In one embodiment, the sample carrier 100 includes a first plate 110 and two second plates 120 attached to either side of the first plate 110. The first plate 110 is placed on a placement plane 2121 and is used to carry a sample, and the second plate 120 is located in an area outside the placement plane 2121. In this way, when the first plate 110 is placed on the placing plane 2121, under the action of the gravity of the second plate 120, the first plate 110 can be tightly attached to the placing plane 2121, so that the first plate 110 is in good contact with the placing plane 2121, which is beneficial for the placing plane 2121 to uniformly transfer heat to the first plate 110. Further, the second plate 120 is disposed obliquely relative to the first plate 110, that is, an included angle is formed between the second plate 120 and the first plate 110, and a height position of the second plate 120 away from the first plate 110 is lower than the placing plane 2121, which is equivalent to that the sample carrier 100 is fastened on the placing plane 2121, on one hand, the sample carrier can be stably mounted on the placing plane 2121, and on the other hand, the sample carrier 100 can be well contacted with the placing plane 2121, so as to achieve close fitting.
In particular, the sample carrier 100 is a membrane tape structure. The film bag is a flat film belt. The membrane tape includes, but is not limited to, a polytetrafluoroethylene film. The material of the membrane strip can also be polyether ketone, aluminum foil or copper foil. The width of the film strip ranges from 8mm to 12 mm. The thickness of the film strip ranges from 0.08mm to 0.12 mm. In one embodiment, the width of the membrane strip is 10 mm. The thickness of the film tape was 0.1 mm. The membrane belt structure has continuity, is convenient to replace, does not have sample cross contamination, and ensures the detection precision. The sample carrier 100 may also be a carrier plate structure. The carrier plate includes, but is not limited to, a glass plate. As long as the heating operation is convenient and the detection precision is ensured.
Further, the first heating member 210 includes a heating body and a first heating part. The heating body is provided with a placing plane 2121. The heating body is connected to one end of the second heating member 220. The first heating part is disposed in the heating main body. The heat of the first heating part can be transferred to the placing plane 2121 through the heating body. Specifically, the heating body includes a fixing block 211 and a heating plate 212. The fixing block 211 is for mounting on the mounting member 300. The heating plate 212 is mounted on the fixing block 211. The first heating part is disposed inside the heating plate 212. The side of the heating plate 212 facing away from the mount 300 is a resting plane 2121. The fixing block 211 and the heating plate 212 are made of a material having high heat resistance and thermal conductivity. Specifically, the fixing block 211 includes, but is not limited to, a copper block, an aluminum block, or a stainless steel block. The heating plate 212 includes, but is not limited to, a copper plate, an aluminum plate, or a stainless steel plate. The fixing block 211 can provide stable support for the heating plate 212, and ensure structural stability of the heating assembly 200. The heating plate 212 can make the sample carrier 100 placed more stably, and the heating plate 212 can also ensure that the heat dissipation of the first heating part is more uniform, ensuring the practicability and reliability of the heating assembly 200.
The heating plate 212 is configured to maintain a uniform temperature at each portion of the placement plane 2121 during heating operation. The heat distribution on the placing plane 2121 is uniform, so that the sample on the sample bearing member 100 is heated more uniformly, and the sliding phenomenon is not easy to occur in the heating process, thereby improving the stability of the detection result. Further, the first heating unit has a rod shape. The heating plate 212 is provided with a mounting hole 214. The rod-shaped first heating unit is inserted into the mounting hole 214. The heat distribution on the placing plane 2121 can be more uniform, so that the sample is heated more uniformly and is not easy to slide in the heating process. The rod-shaped first heating unit is specifically, for example, an electric heating rod. The electric heating rod is connected with external equipment through a first lead, when the external equipment is started, the electric heating rod is powered through the first lead, and the electric heating rod works to generate heat and transmits the heat to the heating plate 212. Of course, the heating rod is not limited to the mode of electric heating, and it is also possible to transfer heat from an external heat source to the heating rod, and then transfer heat to the heating plate 212 through the heating rod. In addition, in this embodiment, the heating rod is not limited to heating the heating plate 212, for example, an electric resistance wire may be disposed inside the heating plate 212, and the heating plate 212 may be heated when the electric resistance wire is powered on, for example, heat generated by combustion or heat generated by chemical reaction may be directly transferred to the heating plate 212, or heat may be transferred to the heating plate 212 by other methods, which is not limited herein.
Further, the second heating member 220 abuts on the first heating member 210. The second heating member 220 includes a fixing part 221 and a second heating part 222. The fixing portion 221 abuts against the first heating member 210. One end of the second heating unit 222 is connected to the fixing unit 221. The other end of the second heating part 222 is inserted into the heating hole 213. The second heating part 222 may also be an electric heating rod. Specifically, the second heating part 222 is a high-temperature microcrystalline ceramic heating rod. Other possibilities of the second heating part 222 are the same as the first heating part, and are not described herein. The upper limit of the temperature of the high-temperature microcrystalline ceramic heating rod is 800 ℃, and the upper limit of the temperature of the first heating unit is 200 ℃. The temperature of the first heating part and the temperature of the second heating part 222 are obviously different, which is beneficial to positioning a liquid sample and desorbing components with different boiling points. The second heating part 222 and the fixing part 221 are point-contacted. The second heating part 222 is prevented from transferring heat to the fixing part 221. It is ensured that heat can be accumulated on the second heating part 222 to achieve rapid high-temperature heating.
If the sample carrier 100 is directly heated at high temperature by the placement plane 2121, even instantaneous high temperature heating may cause damage to the sample carrier 100. In this embodiment, the rod-shaped second heating part 222 is inserted into the heating hole 213 to heat the sample carrier 100, and the second heating part 222 heats the sample carrier 100 at a high temperature point, so that the sample carrier 100 is not damaged by instantaneous high temperature point heating. The second heating section is generally capable of making its own temperature higher than that of the first heating section in a time range of 3s to 10 s.
Specifically, a communication hole is opened at one end of the fixing portion 221. The communication hole communicates with the heating hole 213. The other end of the fixing portion 221 abuts against the first heating member 210. The other end of the second heating part 222 is inserted into the heating hole 213 through the communication hole. The communication hole can increase the length of the heating hole 213 to facilitate the insertion and installation of the second heating unit 222.
In one embodiment, the second heating element 220 further includes an insulating portion 230. One side of the heat insulating part 230 is connected to the fixing part 221, and the other side of the heat insulating part 230 opposite to the fixing part 221 is connected to the first heating member 210. One end of the second heating part 222 is connected to the heat insulating part 230, and the second heating part 222 is positioned between the first heating member 210 and the fixing part 221. When the temperature of the second heating part 222 is higher than that of the first heating part, the heat insulating part 230 can insulate the heat of the second heating part 222 from being transferred from the fixing part 221 to the second heating part 222. The temperature of the first heating part and the second heating part 222 is stable, and the heating process is reliable. Specifically, the heat insulating part 230 is made of a high temperature heat insulating material. The upper limit of the adiabatic temperature of the adiabatic part 230 is not less than the upper limit of the temperature of the second heating part 222. When the second heat insulating part 230 is a high-temperature microcrystalline ceramic heating rod, the upper limit of the heat insulating temperature of the heat insulating part 230 is 800 ℃.
Further, the heat insulation part 230 is provided with a kidney-shaped hole. The second heating part 222 is movably connected to the heat insulating part 230 through a kidney-shaped hole. Since the heat insulating part 230 is formed with a kidney-shaped hole, a bolt may be inserted through the kidney-shaped hole, and the second heating part 222 abuts against the bolt. The height position of the bolt in the kidney-shaped hole is adjustable up and down, thereby enabling adjustment of the mounting position of the second heating part 222. Other high temperature resistant members may be inserted into the waist-shaped hole, as long as the structural stability and safety of the second heating part 222 can be ensured.
In one embodiment, the heating assembly 200 further comprises a temperature sensing element. The temperature sensing member is used to sense the temperatures of the first and second heating parts 222. Therefore, the temperature of the first heating part and the second heating part 222 is sensed by the temperature sensing element, and the heating rod is correspondingly controlled to work according to the sensed temperature of the temperature sensing element, so that the temperature of the supporting plane of the first heating part and the second heating part 222 is controlled within a preset range. Specifically, the temperature measurement sensing element is connected with the external device through the second wire, and of course, the temperature measurement sensing element can also send signals to the external device in a wireless transmission mode.
Specifically, the temperature sensing element includes a PT100 temperature sensor and a type K thermocouple temperature sensor. The PT100 temperature sensor is used to monitor the temperature of the first heating part. The K-type thermocouple temperature sensor is used for monitoring the temperature of the second heating part 222, and the K-type thermocouple temperature sensor can be used for setting a gradient temperature program, so that the second heating part 222 can be controlled to rapidly increase the temperature more conveniently.
In one embodiment, the heating holes 213 are through holes. The shape of the heating hole 213 is a circular hole, an elliptical hole, a square hole, or a triangular hole. Other shapes of apertures are also possible and are not limited herein. The diameter of the heating hole 213 is in the range of 2mm to 8mm, and the outer diameter of the second heating part 222 is in the range of 2mm to 3 mm. In one embodiment, the diameter of the heating hole 213 is 4 mm.
Besides the electric thermal desorption device, the constant-temperature thermal desorption device with a single component also has other desorption modes, such as an ultrasonic vibration desorption device and a halogen light pyrolysis device, which cannot take into account substances with low desorption temperature and high desorption temperature. At lower temperatures, the high boiling point analytes cannot be effectively desorbed and cannot be detected; at higher temperatures, the components of the mixture will be desorbed simultaneously, causing ionization competition of each component and mass spectrum peak congestion. Desorption temperature is set too high, and low boiling point analytes are easily cracked and cannot be effectively detected. However, in practical use, for example, a complicated analysis system having a large variety of types and large differences in physicochemical properties such as pesticide and veterinary drug residues in foods often contains both a substance having a low desorption temperature and a substance having a high desorption temperature. Generally, in order to simultaneously solve the problems of substance desorption and cross contamination, a disposable, thin and chemically stable membrane strip is adopted. If the film strip is directly contacted with the high-temperature heating assembly 200, the film strip can be melted and broken even other irrelevant chemical substances are released under the high-temperature environment for a long time, and the continuous and effective operation of the whole heating device 10 is influenced. Some combined thermal desorption devices in the prior art are generally selected from one of the combination of an electrothermal desorption device, a photothermal desorption device and an acoustic desorption device, however, the photothermal desorption device or the acoustic desorption device inevitably causes the disadvantages of complex, bulky and difficult control of the desorption device, and especially the core heating assembly 200 cannot be heated for a long time due to the limitation of the service life.
The embodiment provides a combined efficient thermal desorption device. The device can be used for heating liquid or solid samples, is beneficial to mass spectrum detection of more types of samples, can realize thermal desorption of substances with different boiling points in different time windows, reduces ionization competitive effect caused by a traditional single component, provides a certain separation function, and improves qualitative and quantitative accuracy. Meanwhile, the electric heating desorption device is stable in control, simple in structure, convenient to process and easy for batch production.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the present invention, unless otherwise expressly stated or limited, the terms "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; they may be directly connected or indirectly connected through intervening media, or they may be connected internally or in any other suitable relationship, unless expressly stated otherwise. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
In the present invention, unless otherwise expressly stated or limited, the first feature "on" or "under" the second feature may directly conflict with the first and second features, or the first and second features may indirectly conflict with each other through intervening media. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
It will be understood that when an element is referred to as being "secured to" or "disposed on" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "upper," "lower," "left," "right," and the like as used herein are for illustrative purposes only and do not denote a unique embodiment.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (11)
1. A heating assembly, characterized in that the heating assembly comprises:
the heating device comprises a first heating element, a second heating element and a heating element, wherein a placing plane is arranged on the first heating element and used for placing a sample bearing piece and transmitting heat of the first heating element to the sample bearing piece, and a heating hole is formed in the placing plane; and
the second heating member, the second heating member can wear to establish in the heating hole, the second heating member is used for the orientation a side that sample holds the thing is not higher than in the ascending position of direction of gravity place the plane in the ascending position of direction of gravity, the surface of second heating member with heating hole inner wall looks interval, the heat of second heating member with the heat inequality of first heating member.
2. The heating assembly according to claim 1, wherein the first heating member includes a heating body on which the placement plane is provided, and a first heating portion that is connected to one end of the second heating member, the first heating portion being provided in the heating body, and heat of the first heating portion being transmittable to the placement plane through the heating body.
3. The heating assembly according to claim 1, wherein the second heating member includes a fixing portion and a second heating portion, the fixing portion is abutted against the first heating member, one end of the second heating portion is connected to the fixing portion, and the other end of the second heating portion is inserted into the heating hole.
4. The heating assembly as claimed in claim 3, wherein the second heating element further includes a heat insulating portion, one side of the heat insulating portion is connected to the fixing portion, the other side of the heat insulating portion facing away from the fixing portion is connected to the first heating element, one end of the second heating portion is connected to the heat insulating portion, and the second heating portion is located between the first heating element and the fixing portion.
5. The heating assembly as claimed in claim 4, wherein the heat insulating part is provided with a kidney-shaped hole, and the second heating part is movably connected to the heat insulating part through the kidney-shaped hole; and/or
The aperture range of the heating hole is 2mm-8mm, and the outer diameter range of the second heating part is 2mm-3 mm.
6. A heating device, characterized in that the heating device comprises:
the heating assembly of any one of claims 1-5; and
the sample bearing piece is used for bearing a sample, and the sample bearing piece is placed on the placing plane and covers the heating hole.
7. A sample detection system, characterized in that the sample detection system comprises:
a detection device; and
a heating device as claimed in claim 6, wherein the detection means is arranged to detect the sample after heating by the heating device.
8. A method of using a heating device, the method comprising the steps of:
placing a sample bearing member on the placing plane and covering the sample bearing member on the heating hole;
placing a sample on the sample carrier;
controlling the temperature of the heating hole to a first temperature, heating the sample bearing piece, and keeping a preset low-temperature heating time;
controlling the temperature of the heating hole to a second temperature; wherein the second temperature is less than the first temperature;
and finishing heating.
9. The method of using a heating device as claimed in claim 8, wherein the maintaining of the preset low temperature heating time further comprises:
controlling the temperature of the central area of the heating hole to a third temperature, and keeping a preset high-temperature heating time; wherein the third temperature is higher than the first temperature;
controlling the temperature of the heating hole to a second temperature; wherein the second temperature is less than the first temperature;
and finishing heating.
10. The method of using a heating device of claim 9, wherein said controlling the temperature of the heating aperture to a first temperature comprises:
controlling the temperature of the first heating member to the first temperature; or
Controlling the temperature of the first and second heating members to the first temperature.
11. The method of using a heating device of claim 9, wherein said controlling the temperature of said heating aperture to a first temperature, said first temperature being no greater than 200 ℃; and/or
The temperature of the central region of the heating hole is controlled to a third temperature, and the third temperature is not more than 800 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111408485.4A CN114112628A (en) | 2021-11-19 | 2021-11-19 | Sample detection system, heating device, heating assembly and use method of heating device |
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| CN202111408485.4A CN114112628A (en) | 2021-11-19 | 2021-11-19 | Sample detection system, heating device, heating assembly and use method of heating device |
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| US20210151305A1 (en) * | 2018-04-20 | 2021-05-20 | Shimadzu Research Laboratory(Shanghai) Co. Ltd. | Ionization device, mass spectrometer, ion mobility spectrometer, and ionization method |
| CN112834603A (en) * | 2019-11-22 | 2021-05-25 | 中国科学院大连化学物理研究所 | Combined efficient thermal desorption device |
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| CN107167334A (en) * | 2016-03-08 | 2017-09-15 | 莫福探测仪器有限责任公司 | The chemical vapor of the temperature influence of compound with low volatility and detection |
| US20210151305A1 (en) * | 2018-04-20 | 2021-05-20 | Shimadzu Research Laboratory(Shanghai) Co. Ltd. | Ionization device, mass spectrometer, ion mobility spectrometer, and ionization method |
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