Infrared in-situ transmission sample holder and infrared transmission detection system

Abstract

The application discloses an infrared in-situ transmission sample assembly and an infrared transmission detection system. The infrared in-situ transmission sample assembly comprises a temperature-controllable heating tube, a metal tube sleeve and a sample support. The temperature-controllable heating tube comprises a tube main body. The metal tube sleeve comprises a main tube sleeve which is inserted into the tube main body and is electrically connected with a temperature controller. The sample support comprises a support main body which is inserted into the main tube sleeve and has a tubular structure with open ends. A groove is formed in one end of the support main body along the side surface, and the groove is used for inserting a sample to be measured so that the sample to be measured is in the pipeline of the support main body. The sample assembly can directly place the sample without loading or clamping other window materials, can avoid the breakage of the sample, is beneficial to the evaporation of a small amount of water vapor in the heating process, and thus can avoid the interference of water vapor in the measurement process. The application provides a more accurate and reliable sample accessory for the measurement and analysis of the infrared transmission spectrum.

Description

Technical Field

[0001] This application belongs to the field of infrared transmission detection technology, specifically relating to an infrared in-situ transmission sample assembly for variable temperature infrared detection and an infrared transmission detection system containing the infrared in-situ transmission sample assembly. Background Technology

[0002] Temperature-controlled infrared spectroscopy (TCIR) is a temperature-regulated infrared spectroscopy method that dynamically monitors changes in the absorption, reflection, or transmission spectra of samples under different temperature conditions to reveal the dynamic response of materials in terms of microstructure, molecular motion, and interactions. Its core principle is based on the changes in molecular vibrational modes, conformational states, or chemical bond stability induced by temperature variations. These changes directly affect the position, intensity, and shape of infrared absorption peaks. For example, in polymer research, this technique can sensitively capture abrupt changes in chain segment motion during the glass transition, and by analyzing specific spectral bands (such as 2922 cm⁻¹), it can reveal the dynamic response of materials in terms of microstructure, molecular motion, and interactions. -1 1600cm -1 Thermodynamic parameters are determined by the peak area inflection point of (e.g., [missing information]). Currently, this technique is widely used in materials science, polymer chemistry, and pharmaceutical analysis, demonstrating unique advantages, particularly in phase transition studies, reaction kinetic monitoring, and plasticizer effect assessment.

[0003] For variable-temperature infrared spectroscopy, sample preparation and accessory selection directly affect spectral quality. Currently, transmission spectrum measurement accessories for infrared spectrometers are easily affected by moisture during in-situ heating tests, influencing the spectral results. Therefore, vacuuming or nitrogen purging is generally required during testing. Furthermore, in solid-state testing, the potassium bromide pellet method is commonly used for sample preparation. While mechanical clamping is necessary to ensure optical path stability during measurement, the fragility of the sample complicates the measurement process. Utility Model Content

[0004] In view of this, the primary objective of this application is to provide an infrared in-situ transmission sample assembly that allows for direct placement of samples without the need for additional window materials for loading or clamping, thus preventing sample breakage. Furthermore, this sample assembly facilitates the evaporation of small amounts of water vapor during the heating process, thereby avoiding interference from water vapor during measurement.

[0005] To achieve the above objectives, this application adopts the following technical solution:

[0006] One aspect of this application discloses an infrared in-situ transmission sample assembly, comprising:

[0007] A temperature-controlled heating element, comprising a tube body;

[0008] A metal tube sleeve includes a main tube sleeve, the main tube sleeve being inserted into the tube body, and the main tube sleeve being electrically connected to a temperature controller;

[0009] And a sample holder, which includes a holder body inserted into the main body tube sleeve. The holder body is a tubular structure with open ends. A groove is provided along the side of one end of the holder body for inserting the sample to be tested, so that the sample to be tested is in the tube of the holder body.

[0010] The infrared in-situ transmission sample assembly of this application allows the sample to be placed directly in the groove of the support body. Infrared light is transmitted through the pipes in the support body to the sample, enabling sample testing. No additional window material is required for sample placement, avoiding the problem of sample fragility. Simultaneously, a metal sleeve is fitted over the sample support. This sleeve serves two purposes: it achieves heat transfer and temperature control, and it facilitates the evaporation of small amounts of water vapor during heating, thus preventing interference from water vapor. This ensures accurate and reliable infrared transmission spectrum measurement results.

[0011] In some examples, a heat dissipation section is provided at the lower end of the tube body. This section accelerates heat dissipation from the sample assembly, facilitating subsequent temperature-controlled experiments and allowing for easier storage of the sample assembly after the experiment. The specific connection method for the heat dissipation section is not particularly limited. As an example, a connecting plate is provided at the lower end of the tube body, and the connecting plate and the heat dissipation section are connected and fixed using methods well-known in the art, such as threaded fastening. It is understood that the heat dissipation section can be electrically connected to a controller to achieve a switch; those skilled in the art possess this capability, and therefore, it will not be elaborated upon here.

[0012] In some examples, the main tube sleeve has a connecting portion at the end near the groove of the support body, and the connecting portion electrically connects the main tube sleeve to the temperature controller via a circuit. As a preferred example, the connecting portion extends vertically outward from the tube wall of the main tube sleeve. In this case, the connecting portion not only serves to electrically connect to the temperature controller, but also limits the movement of the main tube sleeve. When the main tube sleeve is inserted into the tube body, because the connecting portion is perpendicular to the tube wall of the main tube sleeve, it forms a stop, allowing the main tube sleeve to be inserted precisely into the tube body, while also facilitating the removal of the metal tube sleeve.

[0013] It is understood that the groove of the support body is located inside the tube body, and can be configured accordingly by designing specific dimensions. Those skilled in the art possess this capability, and therefore will not elaborate further. The groove's location inside the tube body ensures that the sample to be tested is precisely within the heating zone of the tube body, achieving better heating and temperature control, and ensuring the accuracy and reliability of the measurement results.

[0014] In some examples, a limiting member is provided at the end of the support body away from the groove, and the limiting member extends vertically outward from the side wall of the support body. The limiting member facilitates control over the insertion of the sample holder, and, in conjunction with appropriate dimensional design, ensures controllable insertion depth of the sample holder, avoiding over-insertion.

[0015] In other examples, the limiting member has a protrusion at its end away from the support body, the protrusion being perpendicular to the surface of the limiting member and extending away from the support body. This protrusion design facilitates the insertion and removal of the sample holder by the operator.

[0016] It is understood that in the sample assembly of this application, the inner wall of the tube body is fitted with the outer wall of the main tube sleeve, and the inner wall of the main tube sleeve is fitted with the outer wall of the support body.

[0017] Another aspect of this application discloses an infrared transmission detection system comprising the infrared in-situ transmission sample assembly described above.

[0018] In some examples, the infrared transmission detection system includes:

[0019] Infrared light source;

[0020] An infrared in-situ transmission sample assembly, wherein infrared light emitted by the infrared light source is transmitted to the sample to be tested through a tubular sample holder;

[0021] The infrared detection module is used to detect the infrared transmission spectrum of the sample to be tested.

[0022] And a data acquisition and processing module, used to acquire and process the detection data in the infrared detection module and output an infrared transmission spectrum.

[0023] Specifically, after assembling the infrared in-situ transmission sample assembly, it is placed in an infrared spectrometer, heated in a heating mode, and the infrared light source is turned on. The infrared light is transmitted through the pipes of the sample holder onto the sample to be tested, thereby obtaining the transmitted infrared light of the sample and measuring the infrared transmission information of the sample.

[0024] The beneficial effects of this application are:

[0025] The infrared in-situ transmission sample assembly provided in this application features simple sample placement, eliminates the need for additional window materials, and avoids the risk of sample breakage. Furthermore, the metal sleeve design facilitates the evaporation of small amounts of water vapor during heating, preventing water vapor interference and improving the accuracy and reliability of the test.

[0026] The infrared in-situ transmission sample assembly provided in this application can realize the changes in sample structure and composition from room temperature to high temperature under programmed temperature control, and has the advantages of high measurement accuracy, wide spectral range, and high spectral resolution. This sample assembly provides reliable testing and metrological assurance, enabling extensive in-situ transmission spectroscopy measurements. It can objectively and accurately reflect the relevant information on molecular structure changes with temperature, providing necessary scientific data for research on the pyrolysis reaction mechanism of materials and the analysis of complex internal interactions of materials. Attached Figure Description

[0027] Figure 1 This is a schematic diagram of the structure of the infrared in-situ transmission sample assembly 200 in a preferred embodiment of this application.

[0028] Figure 2 for Figure 1 A schematic diagram of the explosive decomposition structure of the mid-infrared in-situ transmission sample assembly 200.

[0029] Figure 3 for Figure 1 A schematic diagram of the structure of the sample holder 30.

[0030] Figure 4 This is a schematic diagram of the infrared transmission detection system in a preferred embodiment of this application.

[0031] Figures 5-7 The infrared spectrum of the hydrogel sample detected using the infrared in-situ transmission sample assembly described in this application is shown in Example 2.

[0032] In the figure: 100 - Infrared light source, 200 - Infrared in-situ transmission sample assembly, 300 - Infrared detection system, 400 - Computer acquisition and processing system;

[0033] 10-Controllable heating tube, 11-Tube body, 12-Heat dissipation part; 20-Metal tube sleeve, 21-Main tube sleeve, 22-Connecting part; 30-Sample holder, 31-Holder body, 32-Groove, 33-Limiting part, 34-Protrusion; 40-Temperature controller. Detailed Implementation

[0034] The infrared in-situ transmission sample assembly provided by this utility model will now be described in further detail with reference to the accompanying drawings.

[0035] It should be noted that when a component is referred to as "fixed to," "set on," or "mounted to" another component, it can be directly on or indirectly on the other component. However, when a component is referred to as "connected to" or "attached to" another component, it can be directly connected to or indirectly connected to the other component. Furthermore, "connection" generally refers to a method of fixing, and this fixing can be any method of fixing conventional in the art, such as "threaded connection," "riveting," or "welding."

[0036] It should be understood that the terms "length", "width", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", and "outer" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing the embodiments of this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed or operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.

[0037] Example 1

[0038] This embodiment discloses an infrared in-situ transmission sample assembly, the structure of which can be found in [reference needed]. Figure 1 and Figure 2 The infrared in-situ transmission sample assembly includes a temperature-controlled heating tube 10, a metal sleeve 20, and a sample holder 30. The sample holder 30 is inserted into the metal sleeve 20, which is in turn inserted into the temperature-controlled heating tube 10. The outer wall of the sample holder 30 is in contact with the inner wall of the metal sleeve 20, and the outer wall of the metal sleeve 20 is in contact with the inner wall of the temperature-controlled heating tube 10. The metal sleeve 20 is electrically connected to a temperature controller 40.

[0039] In this embodiment, the temperature-controlled heating tube 10 includes a tube body 11, with a metal sleeve 20 inserted inside the tube body 11. The outer wall of the metal sleeve 20 is fitted against the inner wall of the tube body 11. In this embodiment, the tube body 11 is also made of metal, without any special limitations. The heating method of the tube body 11 is not particularly limited and can be any method well-known in the art, such as resistance heating. In this embodiment, the tube body 11 can be heated using either programmed heating or direct heating (achieved through an external controller). It is recommended that the operating temperature not exceed 600℃, and different heating ranges and heating curves can be set according to usage requirements, with a maximum of thirty heating ranges. Preferably, the temperature controller 40 uses PID control algorithm technology to collect and adjust the heating temperature in real time, with a control accuracy within ±5℃.

[0040] A heat dissipation section 12 is provided at the lower end of the tube body 11 for dissipating heat from the sample assembly. Specifically, in this embodiment, a connecting plate is provided on the lower end face of the tube body 11, and the connecting plate is fixedly connected to the heat dissipation section 12 by means of thread fastening or other methods well known in the art.

[0041] In this embodiment, the metal sleeve 20 includes a main sleeve 21, which is inserted into the interior of the tube body 11, with the outer wall of the main sleeve 21 fitting against the inner wall of the tube body 11. One end of the main sleeve 21 has a connecting portion 22, which electrically connects the main sleeve 21 to the temperature controller 40 via a circuit. In this embodiment, the connecting portion 22 extends vertically outward from the tube wall of the main sleeve 21, allowing it to not only connect electrically to the temperature controller 40 but also limit the movement of the main sleeve 21. When the main sleeve 21 is inserted into the temperature-controlled heating tube 10, the perpendicularity of the connecting portion 22 to the tube wall of the main sleeve 21 creates a stop, ensuring the main sleeve 21 is properly inserted into the tube body 11, and also facilitating the removal of the metal sleeve 20.

[0042] Please continue reading. Figure 1 , Figure 2 At the same time, combined Figure 3 The sample holder 30 includes a holder body 31, which is a tubular structure open at both ends. The holder body 31 is inserted into the main tube sleeve 21, and the outer wall of the holder body 31 fits against the inner wall of the main tube sleeve 21. A groove 32 is formed along the side of the holder body 31 near the connecting portion 22 of the metal tube sleeve 20. This groove 32 is used to place the sample to be tested. A limiting member 33 is provided at the end of the holder body 31 away from the groove 32. The limiting member 33 extends vertically outward from the side wall of the holder body 31. The limiting member 33 facilitates control of the insertion of the sample holder 30, thereby ensuring that the insertion depth of the sample holder is controllable and avoiding over-insertion. Further, in this preferred embodiment, a protrusion 34 is provided at the end of the limiting member 33 away from the holder body 31. The protrusion 34 is perpendicular to the surface of the limiting member 33 and extends away from the holder body 31. The design of the protrusion 34 facilitates the operator to insert or remove the sample holder 30.

[0043] It is understood that after the groove 32 on the support body 31 is inserted into the tube body 11, it is located inside the tube body 11. The insertion depth of the support body 31 can be designed by designing specific dimensions to ensure that the groove 32 is located inside the tube body 11. Those skilled in the art have this ability, so it will not be described in detail here.

[0044] The dimensions of the sample components in this application are not particularly limited. Those skilled in the art can design or adjust the dimensions according to actual needs based on the structural disclosure of this application. As an example, in this embodiment, the length of the temperature-controlled heating tube 10 is 40–45 mm, and the inner diameter is 25–32 mm. The length of the metal sleeve 20 is 46–52 mm, and the inner diameter is 15–20 mm. The length of the sample holder 30 is 30–36 mm, and the inner diameter is 12–14 mm. The width of the groove 32 is 2 mm to facilitate sample insertion.

[0045] Furthermore, there are no particular limitations on the materials of the temperature-controlled heating tube 10, the metal sleeve 20, and the sample holder 30. Any conventional metal material in the art is acceptable. As an example, in this embodiment, the temperature-controlled heating tube 10, the metal sleeve 20, and the sample holder 30 are all made of stainless steel.

[0046] Based on the infrared in-situ transmission sample assembly in this embodiment, this embodiment further provides an infrared transmission detection system, the composition of which is as follows: Figure 4 The system shown includes an infrared light source 100, an infrared in-situ transmission sample assembly 200, an infrared detection system 300, and a computer acquisition and processing system 400.

[0047] The infrared light source 100 is used to generate infrared light, which enters the infrared in-situ transmission sample assembly 200. Specifically, it is transmitted to the sample to be tested through the pipe of the support body 31 of the sample holder 30. The infrared detection system 300 and the computer acquisition and processing system 400 detect the sample to be tested and collect and process the detection results.

[0048] Example 2

[0049] This embodiment takes a hydrogel sample as an example to further illustrate the working process and detection method of the infrared in-situ transmission sample assembly 200 in Example 1.

[0050] Those skilled in the art know that polymer materials possess multi-level microstructures and complex interactions, which are key to determining their properties. To investigate these interactions, molecular spectroscopy (such as infrared spectroscopy) is often used as a common technique. On one hand, the chemical structure of polymers can be identified by observing the positions and intensities of different characteristic peaks, corresponding to different functional groups on the polymer chain. On the other hand, the physical or chemical environment of these functional groups can be determined based on changes in the positions and intensities of their characteristic absorption peaks, thus enabling the analysis of the complex interactions within the polymer material.

[0051] Therefore, this application uses common poly(N-isopropylacrylamide) hydrogel as the research object and measures its transmission infrared spectrum during in-situ heating and cooling processes. The specific steps are as follows:

[0052] S1. Sample assembly installation: The sample assembly is installed according to the structural composition of Example 1. The installation structure is as follows: Figure 1 As shown in the image.

[0053] S2, Empty Test: Without adding a sample, first set the predicted temperature value and heating rate, then scan the empty background to obtain the background image of the sample.

[0054] S3. Sample preparation: Dissolve an appropriate amount of N-isopropylpropionamide monomer and photoinitiator (monomer content 1%) in deionized water, remove air bubbles by ultrasonication, transfer the above prepolymer solution to a glass mold, initiate polymerization under ultraviolet light (365nm), and take out the gel sample (thickness about 1mm) after half an hour.

[0055] S4. Place the hydrogel sample prepared in step S3 into the groove 32 of the sample holder 30, and assemble the sample assembly according to step S1.

[0056] S5. Test the infrared transmission spectrum of the sample. Set the temperature to 25-45℃, collect data every 2℃, and the heating rate is 1℃ / min. The actual test temperature error should not exceed ±0.1℃.

[0057] The results are as follows Figure 5-7 As shown, Figure 5 This example shows the full wavelength range (4000-800cm) of the poly-N-isopropylacrylamide (NIPAM) hydrogel sample. -1 Under varying temperature infrared spectroscopy, the molecular chain of poly(N-isopropylacrylamide) (NIPAM) simultaneously possesses hydrophilic amide groups and a hydrophobic carbon chain backbone, as well as isopropyl side groups, with the most significant differences observed in the 1750-1500 cm⁻¹ range. -1 ( Figure 6 ) and 3800-3000cm -1 ( Figure 7 The range reflects the change in the hydrophilic amino groups in poly(N-isopropylacrylamide) (NIPAM). It can be seen that with increasing temperature (1649 and 1625 cm⁻¹), the changes in the hydrophilic amino groups are observed. -1 The interconversion of absorption peaks indicates the formation of intermolecular / internal hydrogen bonds (C=O…H―N) within the polymer chain. Experimental results show that temperature is a functional factor regulating the hydrogen bond interactions of C=O…H―N in the polymer and the dehydration of the polymer carbon chain, thereby driving their dynamic phase separation transitions in the hydrogel system.

[0058] The above embodiments demonstrate that the infrared in-situ transmission sample assembly provided in this application can accurately and reliably perform infrared transmission detection and reverse analysis on samples. It is understood that, using hydrogel samples as an example, the infrared in-situ transmission sample assembly and infrared transmission detection system provided in this application can accurately detect infrared transmission spectra and analyze changes in molecular structure during temperature variations, regardless of the molecular structure of any organic or polymeric compound.

[0059] It should be noted that this application is not limited to the above-described embodiments. The above embodiments are merely examples, and any embodiments with the same structure and effect as the technical concept within the scope of this application are included in the technical scope of this application. Furthermore, various modifications that can be conceived by those skilled in the art to the embodiments, and other ways of constructing by combining some of the constituent elements of the embodiments, without departing from the spirit of this application, are also included in the scope of this application.

Claims

1. An infrared in-situ transmission sample assembly, comprising: include: A temperature-controlled heating element, comprising a tube body; A metal tube sleeve includes a main tube sleeve, the main tube sleeve being inserted into the tube body, and the main tube sleeve being electrically connected to a temperature controller; And a sample holder, which includes a holder body inserted into the main body tube sleeve. The holder body is a tubular structure with open ends. A groove is provided along the side of one end of the holder body for inserting the sample to be tested, so that the sample to be tested is in the tube of the holder body.

2. The infrared in-situ transmission sample assembly as described in claim 1, characterized in that, The lower end of the tube body is provided with a heat dissipation section.

3. The infrared in-situ transmission sample assembly as described in claim 1, characterized in that, The main tube sleeve has a connecting part at the end near the groove of the support body, and the connecting part electrically connects the main tube sleeve to the temperature controller through a circuit.

4. The infrared in-situ transmission sample assembly as described in claim 3, characterized in that, The connecting portion extends vertically outward from the wall of the main tube sleeve.

5. The infrared in-situ transmission sample assembly as described in claim 1, characterized in that, The groove of the support body is located inside the tube body.

6. The infrared in-situ transmission sample assembly as described in claim 1, characterized in that, A limiting member is provided at the end of the support body away from the groove, and the limiting member extends vertically outward from the side wall of the support body.

7. The infrared in-situ transmission sample assembly as described in claim 6, characterized in that, The limiting member has a protrusion at its end away from the support body. The protrusion is perpendicular to the surface of the limiting member and extends away from the support body.

8. The infrared in-situ transmission sample assembly as described in any one of claims 1-7, characterized in that, The inner wall of the tube body is fitted with the outer wall of the main tube sleeve, and the inner wall of the main tube sleeve is fitted with the outer wall of the support body.

9. An infrared transmission detection system, characterized in that, It contains the infrared in-situ transmission sample assembly as described in any one of claims 1-8.

10. The infrared transmission detection system as described in claim 9, characterized in that, include: Infrared light source; An infrared in-situ transmission sample assembly, wherein infrared light emitted by the infrared light source is transmitted to the sample to be tested through a tubular sample holder; The infrared detection module is used to detect the infrared transmission spectrum of the sample to be tested. And a data acquisition and processing module, used to acquire and process the detection data in the infrared detection module and output an infrared transmission spectrum.

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