CN114264539A - Solvent-assisted thermal desorption apparatus - Google Patents
Solvent-assisted thermal desorption apparatus Download PDFInfo
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- CN114264539A CN114264539A CN202010971221.9A CN202010971221A CN114264539A CN 114264539 A CN114264539 A CN 114264539A CN 202010971221 A CN202010971221 A CN 202010971221A CN 114264539 A CN114264539 A CN 114264539A
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Abstract
The present invention provides a solvent-assisted thermal analysis apparatus comprising: a primary air source; a thermal desorption apparatus comprising: a sample-receiving chamber having a cavity for receiving a sample, a carrier gas inlet and a carrier gas outlet formed at opposite ends thereof and communicating with the cavity, the carrier gas outlet being connected to an analysis instrument; and a heating element disposed on a wall of the sample-receiving chamber; and at least one gas phase solvent adding device, which comprises a solvent tank, a solvent filling port at the top, a first gas conduit and a second gas conduit, wherein one end of the first gas conduit is connected to the main gas source, the other end of the first gas conduit extends to the position below the liquid level of the solvent in the solvent tank, one end of the second gas conduit extends to the position above the liquid level, and the other end of the second gas conduit is communicated with the carrier gas inlet. According to the thermal desorption equipment, the gas-phase solvent adding device is arranged at the front end of the thermal desorption cavity, so that the collection of semi-volatile or difficultly-volatile components in the sample can be realized at a lower temperature with the aid of the gas-phase solvent.
Description
Technical Field
The invention relates to the field of analytical chemistry sample collection, in particular to thermal analysis equipment for collecting semi-volatile or nonvolatile components in a cigarette sample under the assistance of a gas phase solvent.
Background
In-situ sampling is an important development direction in the field of analysis at present, and thermal analysis is a relatively mature technology for collecting target analysis compounds in a sample. Conventional thermal analysis devices generally heat the sample by means of heat transfer, light, microwave, or electromagnetism, and raise the temperature of the sample to achieve the purpose of rapidly converting the target analyte from a solid phase or a liquid phase to a gas phase.
Theoretically, the higher the heating temperature, the more sufficient the target compound is resolved, but the higher the heating temperature is, the higher the thermal stability requirement of the sample is generally. Furthermore, for complex sample systems, a higher heating temperature means more interfering substances are released. Thus, conventional thermal analysis devices are generally suitable for the collection of volatile components from samples that are more thermally stable, and conventional thermal analysis devices are generally less efficient at resolving semi-volatile or less volatile compounds.
Disclosure of Invention
In order to solve the above problems, the present invention provides a solvent-assisted thermal analysis apparatus, in which a gas-phase solvent adding device is disposed at a front end of a thermal analysis cavity, so that collection of semi-volatile or non-volatile components in a sample can be achieved even at a low temperature with the aid of a gas-phase solvent.
According to the present invention, the thermal resolution apparatus comprises: a primary air source; a thermal desorption apparatus comprising: a sample-receiving chamber having a cavity for receiving a sample, a carrier gas inlet and a carrier gas outlet formed at opposite ends of the sample-receiving chamber in a length direction, respectively, and communicating with the cavity, wherein the carrier gas outlet is connected to an analysis instrument; and a heating element surrounding the sample-receiving chamber and disposed on a wall of the sample-receiving chamber; and at least one gas phase solvent adding device, wherein the gas phase solvent adding device comprises a solvent tank, a solvent filling port formed at the top of the solvent tank, a first gas conduit and a second gas conduit, one end of the first gas conduit is connected to the main gas source, the other end of the first gas conduit extends below the liquid level of the solvent in the solvent tank, one end of the second gas conduit extends above the liquid level in the solvent tank, and the other end of the second gas conduit is communicated with the carrier gas inlet.
According to an embodiment of the present invention, the thermal desorption apparatus may include a plurality of gas-phase solvent addition devices, the first gas conduit of each of the plurality of gas-phase solvent addition devices being connected to a main gas source, and the thermal desorption apparatus further includes a gas mixing chamber including a turbulent structure for mixing the gas-phase solvents generated by the plurality of gas-phase solvent addition devices, a gas inlet end of the gas mixing chamber being connected to the second gas conduit of each of the plurality of gas-phase solvent addition devices, and a gas outlet end being connected to the carrier gas inlet.
Optionally, the thermal analysis apparatus may further comprise a temperature control element disposed around an outside of the vapor phase solvent addition device.
According to another embodiment of the present invention, the thermal resolution device may further comprise a three-way solenoid valve having a first inlet, a second inlet, and an outlet, wherein the first inlet is connected to the second gas conduit, the second inlet is connected to the additional gas source, and the outlet is connected to the carrier gas inlet.
Optionally, the thermal desorption apparatus may further comprise a heat-retaining element, which is arranged outside the heating element.
Further, a gas line channel may be provided between the heating element and the keep warm element, the first gas duct being connected to the main gas source via a gas line passing through the gas line channel.
According to a further embodiment of the invention, a stop element for limiting the position of the sample within the cavity may be provided within the sample-receiving chamber.
Optionally, the thermal resolution device may further comprise a gas mass flow meter disposed between the primary gas source and the first conduit to control the carrier gas flow rate.
According to one example, the thermal desorption apparatus may further comprise a flow diversion member disposed between the carrier gas outlet and the analysis instrument.
According to another embodiment of the present invention, the thermal analysis device may further include a gate that is provided at an end of the sample-receiving chamber where the carrier gas outlet is formed, and that can be opened or closed with respect to the sample-receiving chamber.
Further, a carrier gas outlet may be formed on a wall of the sample-receiving chamber adjacent the gate.
Alternatively, the carrier gas outlet may also be formed on the door.
Drawings
The above and other aspects and features of the present invention will become apparent from the following description of the embodiments with reference to the accompanying drawings, in which:
FIG. 1 is a schematic structural view of a thermal analysis apparatus according to a first embodiment of the present invention;
FIG. 2 is a schematic view of the structure of the thermal analysis apparatus of the thermal analysis device shown in FIG. 1;
FIG. 3 is a schematic view of a vapor phase solvent addition apparatus according to one embodiment of the present invention;
FIG. 4 is a schematic view showing a plurality of vapor phase solvent addition means of a thermal analysis apparatus according to a second embodiment of the present invention;
FIG. 5 is a schematic view of a part of the structure of a thermal analysis apparatus according to a third embodiment of the present invention;
FIG. 6 is a schematic structural view of a thermal analysis apparatus according to a fourth embodiment of the present invention;
FIG. 7 is a schematic structural view of a thermal analysis apparatus according to a fifth embodiment of the present invention; and
FIG. 8 is a schematic structural view of the thermal analysis apparatus of the thermal analysis device according to another embodiment of the present invention.
Detailed Description
Illustrative, non-limiting examples of the present invention are described in detail below with reference to the accompanying drawings, which further illustrate a solvent-assisted thermal analysis apparatus according to the present invention.
According to the thermal analysis equipment disclosed by the invention, the gas phase solvent adding device is arranged at the front end of the thermal analysis cavity, so that the collection of semi-volatile or difficultly volatile components in the sample can be realized at a lower temperature. In particular, the thermal analysis apparatus according to the present invention comprises a main gas source 1, a thermal analysis device 2 and at least one gas phase solvent addition device 3, as shown in fig. 1.
The thermal analysis device 2 comprises a sample-receiving chamber 21 and a heating element 22, as shown in fig. 2. The sample-receiving chamber 21 is a cylinder or cartridge having a cavity 210 for receiving a sample. The sample-receiving chamber 21 also has a carrier gas inlet 211 and a carrier gas outlet 212 formed at opposite ends thereof in the length direction and communicating with the cavity 210, respectively, wherein the carrier gas outlet 212 is connected to an analysis instrument. Optionally, the thermal analysis apparatus may further comprise a flow dividing member (not shown) disposed between the carrier gas outlet 212 and the analysis instrument to control the flow dividing ratio of the sample into the analysis instrument. The heating element 22 surrounds the sample-receiving chamber 21 and is arranged on a wall of the sample-receiving chamber 21 in order to heat the latter. Preferably, a stop element 26 for defining the position of the sample 9 within said cavity may be provided within the sample-receiving chamber 21, as shown in fig. 1.
The thermal analysis apparatus 2 further comprises at least one gas phase solvent addition apparatus 3. According to a first embodiment of the present invention, the thermal analysis apparatus 2 may comprise a vapor phase solvent addition apparatus 3, as shown in FIG. 1. However, a plurality of gas-phase solvent adding apparatuses 3 may be provided as necessary. FIG. 3 shows a schematic of a vapor phase solvent addition apparatus according to an embodiment of the present invention. The gas-phase solvent adding apparatus includes a solvent tank 31, a solvent filling port 32 formed at the top of the solvent tank, a first gas conduit 33, and a second gas conduit 34. The first gas conduit 33 has one end connected to the main gas source 1 and the other end extending below the liquid level 35 of the solvent in the solvent tank 31, and the second gas conduit 34 has one end extending above the liquid level 35 in the solvent tank 31 and the other end communicating with the carrier gas inlet 211, as shown in fig. 1. Referring to fig. 3, orifice 330 of first gas conduit 33 is located below liquid level 35 and orifice 340 of second gas conduit 34 is located above liquid level 35.
The thermal desorption apparatus according to the present invention introduces gas phase solvent assistance on the basis of thermal desorption, thus enabling desorption of semi-volatile or less volatile compounds at lower heating temperatures. In addition, the thermal analysis equipment is also suitable for collecting the target compound in the sample with poor thermal stability, so that the application range of the thermal analysis technology is widened, and the analysis efficiency of the target analysis compound is effectively improved. The thermal analysis equipment has a simple structure, is easy to operate, has strong universality, and can be adapted to various analysis instruments or analysis equipment because the analyzed target compound is in a gaseous state. In addition, the gas lines employed in the thermal desorption apparatus of the present invention all have good thermal stability, i.e., do not significantly deform or release interfering compounds at high temperatures.
According to the second embodiment of the present invention, the thermal analysis apparatus includes a plurality of vapor phase solvent addition devices 2, the first gas conduit 33 of each of which is connected to the main gas source 1 through the gas line 36, as shown in fig. 4. The primary gas source may be, for example, a gas cylinder, an air compressor, or other gas sources commonly used in the art. In the second embodiment, the thermal desorption apparatus further includes a gas mixing chamber 4 including a turbulent flow structure 40 for mixing the vapor phase solvents generated by the plurality of vapor phase solvent adding devices 2. The gas mixing chamber 40 has a gas inlet end connected to the second gas conduit 34 of each of the plurality of vapor phase solvent addition devices through a gas line 37 and a gas outlet end connected to the carrier gas inlet 211 through a gas line 38.
According to the third embodiment of the present invention, the thermal analysis apparatus may further include a gas mass flow meter 5 provided on the gas line between the main gas source 1 and the first duct 33 to control the carrier gas flow rate, as shown in fig. 5. Preferably, the thermal desorption apparatus may further include a temperature control element 6 disposed around an outer side of the vapor phase solvent adding device 2 for controlling heating, temperature control and heat preservation of the vapor phase solvent.
According to a fourth embodiment of the invention, the thermal analysis apparatus may further comprise a three-way solenoid valve 7, as shown in fig. 6. The three-way solenoid valve 7 has a first inlet 71, a second inlet 72 and an outlet 73, wherein the first inlet 71 is connected to the second gas conduit 34, the second inlet 72 is connected to the additional gas source 8 and the outlet 73 is connected to the carrier gas inlet 211. When the three-way electromagnetic valve 7 is in communication with the first inlet 71 and the outlet 73, the whole thermal analysis device is in a working mode; and when the three-way solenoid valve 7 is in communication with the second inlet 72 and the outlet 73, the whole thermal analysis device is in a cleaning residue removing mode.
According to a fifth embodiment of the invention, the thermal analysis device 2 may further comprise a heat-retaining element 23, which is arranged outside the heating element 22, as shown in fig. 7. The insulating element 23 serves to insulate the heating element 22 while protecting the operator from high temperatures. According to an alternative embodiment, a gas line channel 24 may be provided between the heating element 22 and the heat retaining element 23. The first gas conduit 33 is connected to the main gas source 1 via a gas line 25 passing through the gas line channel 24. That is, the main gas source 1 is disposed on the side of the thermal analysis apparatus where the load gas outlet is formed, and the gas line 25 extends from the first gas conduit through the gas line channel 24, i.e., through the entire sample-receiving chamber 21 to the main gas source 1. Therefore, the gas line 25 is preheated by the heating element 22, thereby reducing fluctuation in the concentration of the gas-phase solvent due to the difference in the temperature of the carrier gas and the temperature of the solvent, while also enabling energy saving.
According to another embodiment of the invention, the thermal analysis device may further comprise a door 27, as shown in fig. 1. The gate 27 is provided at the end of the sample-receiving chamber 21 forming the carrier gas outlet 212 and can be opened or closed with respect to the sample-receiving chamber. When door 27 is closed, a seal is maintained between the door and the walls of sample-receiving chamber 21. Further, a carrier gas outlet 212 is formed on the wall of the sample-receiving chamber 21 adjacent to the gate 27, as shown in fig. 1. Optionally, the thermal analysis device may further include a gate 27 ', wherein the carrier gas outlet 212 ' is formed directly on the gate 27 ', so that the structure of the thermal analysis device may be simplified, as shown in fig. 8.
Although exemplary embodiments of the present invention have been described, it will be apparent to those skilled in the art that changes may be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the claims and their equivalents.
Claims (12)
1. A solvent-assisted thermal analysis apparatus comprising:
a primary air source;
a thermal desorption apparatus comprising:
a sample-receiving chamber having a cavity for receiving a sample, a carrier gas inlet and a carrier gas outlet formed at opposite ends of the sample-receiving chamber in a length direction and communicating with the cavity, respectively, wherein the carrier gas outlet is connected to an analysis instrument; and
a heating element surrounding the sample-receiving chamber and disposed on a wall of the sample-receiving chamber; and
at least one gas phase solvent adding device, wherein the gas phase solvent adding device comprises a solvent tank, a solvent filling port formed at the top of the solvent tank, a first gas conduit and a second gas conduit, one end of the first gas conduit is connected to the main gas source, the other end of the first gas conduit extends below the liquid level of the solvent in the solvent tank, one end of the second gas conduit extends above the liquid level in the solvent tank, and the other end of the second gas conduit is communicated with the carrier gas inlet.
2. The thermal analysis apparatus of claim 1, wherein the thermal analysis apparatus comprises a plurality of vapor phase solvent addition devices, the first gas conduit of each of the plurality of vapor phase solvent addition devices being connected to the main gas source, and the thermal analysis apparatus further comprises:
the gas mixing chamber, the gas mixing chamber includes the vortex structure that is used for being directed at by the gaseous phase solvent that a plurality of gaseous phase solvent adds the device and produces mixes, the inlet end of gas mixing chamber with the second gas conduit of each of a plurality of gaseous phase solvent adds the device links to each other, the end of giving vent to anger is connected to the carrier gas entry.
3. The thermal analysis apparatus of claim 1 or 2, further comprising:
a temperature control element disposed around an outside of the vapor phase solvent addition device.
4. The thermal analysis apparatus of claim 1, further comprising:
a three-way solenoid valve having a first inlet connected to the second gas conduit, a second inlet connected to an additional gas source, and one outlet connected to the carrier gas inlet.
5. The thermal desorption apparatus of claim 1, wherein the thermal desorption device further comprises a heat retention element disposed outside the heating element.
6. The thermal analysis apparatus of claim 5, wherein a gas line channel is provided between the heating element and the holding element, the first gas conduit being connected to the primary gas source via a gas line passing through the gas line channel.
7. The thermal analysis apparatus of claim 1, wherein a stop element is provided within the sample-receiving chamber for defining the position of the sample within the cavity.
8. The thermal analysis apparatus of claim 1, further comprising:
a gas mass flow meter disposed between the main gas source and the first conduit to control a carrier gas flow rate.
9. The thermal analysis apparatus of claim 1, further comprising:
a diverter component disposed between the carrier gas outlet and the analytical instrument.
10. The thermal analysis apparatus of claim 1, wherein the thermal resolution device further comprises a gate disposed at an end of the sample-receiving chamber forming the carrier gas outlet and openable or closable relative to the sample-receiving chamber.
11. The thermal analysis apparatus of claim 10, wherein the carrier gas outlet is formed on a wall of the sample-receiving chamber adjacent the door.
12. The thermal analysis apparatus of claim 10, wherein the carrier gas outlet is formed on the door.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010971221.9A CN114264539A (en) | 2020-09-16 | 2020-09-16 | Solvent-assisted thermal desorption apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010971221.9A CN114264539A (en) | 2020-09-16 | 2020-09-16 | Solvent-assisted thermal desorption apparatus |
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| Publication Number | Publication Date |
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| CN114264539A true CN114264539A (en) | 2022-04-01 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202010971221.9A Pending CN114264539A (en) | 2020-09-16 | 2020-09-16 | Solvent-assisted thermal desorption apparatus |
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| CN (1) | CN114264539A (en) |
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- 2020-09-16 CN CN202010971221.9A patent/CN114264539A/en active Pending
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