Sample detection accessory and coupled detection system

Abstract

The utility model discloses a kind of sample detection accessory and combined detection system, sample detection accessory includes sample bin;Sample bin is provided with sample inlet and sample outlet, sample inlet and sample outlet are respectively communicated with sample bin inside;Located at one end of sample bin is provided with incident light path unit, incident light path unit is used to collimate the light that is shot into sample bin inside;Located at the other end of sample bin is provided with emergent light path unit, emergent light path unit is used to focus the light that is shot out of sample bin.Processing. Through the coupling of gas path and light path on sample detection accessory, GC, MS and absorption spectrum detection can be combined through the sample detection accessory, so that the combined detection system can simultaneously realize the spectral and mass spectrum analysis of electrolyte components, comprehensive qualitative and quantitative analysis of electrolyte components is realized, the efficiency of analysis is improved, and the accuracy of spectral and mass spectrum analysis is well guaranteed.

Description

Technical Field

[0001] This utility model belongs to the field of detection technology, and specifically relates to a sample detection accessory and a combined detection system. Background Technology

[0002] With the development of the new energy industry, the study of battery performance has become an important direction, and various analytical and characterization methods are now widely used in battery performance research. Electrolyte, as the "blood" of a battery, has a significant impact on its thermal, electrical, and chemical properties. Different battery systems, different application scenarios, and different battery manufacturers all have different electrolyte formulations; therefore, the analysis of battery electrolyte components has become an important research direction for new energy batteries. Utility Model Content

[0003] The purpose of this invention is to provide a sample testing accessory and a combined testing system to achieve comprehensive and accurate qualitative and quantitative analysis of electrolyte components.

[0004] This utility model is achieved through the following technical solution:

[0005] Sample testing accessories, including sample compartment;

[0006] The sample chamber is provided with a sample inlet and a sample outlet, and the sample inlet and sample outlet are respectively connected to the interior of the sample chamber;

[0007] An incident light path unit is provided at one end of the sample chamber, which is used to collimate the light rays entering the sample chamber.

[0008] An outgoing light path unit is provided at the other end of the sample chamber, which is used to focus the light emitted from the sample chamber.

[0009] In some embodiments, the sample chamber is provided with a sample channel, the sample inlet and the sample outlet are respectively connected to the sample channel, and the incident optical path unit and the outgoing optical path unit are respectively disposed at both ends of the sample channel.

[0010] In some embodiments, the incident optical path unit includes a collimating lens, and the exit optical path unit includes a condensing lens.

[0011] In some embodiments, an optical path plunger is provided at the end of the sample chamber, and the optical path plunger is provided with mounting holes for mounting incident optical fibers or outgoing optical fibers, and the mounting holes are connected to the sample chamber.

[0012] In some embodiments, a gas path plunger is provided at the sample inlet and sample outlet, and the gas path plunger is provided with a connection hole for setting up a pipeline, the connection hole communicating with the interior of the sample chamber.

[0013] In some embodiments, the inner wall of the sample chamber is provided with a coating.

[0014] On the other hand, this utility model also provides a combined detection system, including:

[0015] A gas chromatograph, which is used to separate the components in a sample;

[0016] An absorption spectroscopy unit, comprising a light source and a spectral detector, wherein the spectral detector is used for spectral analysis of various components of the sample;

[0017] A mass spectrometer, which is used for mass spectrometric analysis of various components of a sample;

[0018] And, the aforementioned sample testing accessories;

[0019] The gas chromatograph is connected to the sample inlet, the mass spectrometer is connected to the sample outlet, and the light from the light source is processed by the incident light path unit and then enters the sample chamber. The light in the sample chamber is processed by the outgoing light path unit and then received by the spectrometer detector.

[0020] In some embodiments, the sample detection accessory is disposed inside the column oven of the gas chromatograph, and the column oven is provided with a temperature control unit for adjusting the temperature inside the column oven.

[0021] In some embodiments, the length of the sample channel in the sample chamber is 10-100cm.

[0022] In some embodiments, the inner diameter of the sample channel of the sample chamber is matched with the inner diameter of the chromatographic column of the gas chromatograph.

[0023] Compared with the prior art, this utility model has the following advantages and beneficial effects:

[0024] By coupling the gas path and optical path in the sample detection accessory, GC, MS, and absorption spectroscopy detection can be combined through this accessory. This allows the coupled detection system to simultaneously perform spectral and mass spectrometric analysis of electrolyte components, achieving comprehensive qualitative and quantitative analysis of electrolyte components and improving analytical efficiency. At the same time, it is precisely because of the coupling of the gas path and optical path in the sample detection accessory that the accuracy of spectral and mass spectrometric analysis is well guaranteed.

[0025] This sample detection accessory has a simple structure and can be easily set directly into the GC. It is easy to connect with the GC, MS and spectral detection unit, thus facilitating its application in existing detection equipment and reducing the need for modifications to existing detection equipment, making application and detection more convenient. Attached Figure Description

[0026] To more clearly illustrate the technical solutions of the embodiments of this utility model, the accompanying drawings in the embodiments will be briefly described below. It should be understood that the following drawings only show some embodiments of this utility model and should not be regarded as a limitation on the scope. For those skilled in the art, other related drawings can be obtained based on these drawings without creative effort.

[0027] Figure 1 This is a structural block diagram of the combined detection system of this utility model.

[0028] Figure 2 This is a schematic diagram illustrating the working principle of the sample testing accessory of this utility model.

[0029] Figure 3 This is a schematic diagram of the sample testing accessory structure of this utility model.

[0030] Figure 4 This is a front view of the sample testing accessory structure of this utility model.

[0031] Figure 5 This is a cross-sectional view of the sample chamber in the sample testing accessory of this utility model.

[0032] Figure 6 for Figure 3 A partial schematic diagram of point A in the middle.

[0033] in:

[0034] 11. Sample introduction system; 12. Separation system;

[0035] 21. Light source; 22. Spectrometer detector; 23. Incident fiber; 24. Outgoing fiber.

[0036] 31. Ion source; 32. Mass analyzer; 33. Mass spectrometer detector;

[0037] 41. Sample chamber; 411. Sample channel; 412. Sample inlet; 413. Sample outlet; 414. Optical path plunger; 415. Mounting hole; 416. Gas path plunger; 417. Connection hole; 418. Sealing gasket; 419. Sealing gasket; 42. Incident optical path unit; 43. Outgoing optical path unit. Detailed Implementation

[0038] To make the objectives, technical solutions, and advantages of the embodiments of this utility model clearer, the technical solutions of the embodiments of this utility model will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are some embodiments of this utility model, but not all embodiments.

[0039] In the field of materials composition analysis, mass spectrometry analysis of materials components can be achieved by using GC-MS coupled with GC-MS.

[0040] GC: Gas Chromatography, which separates mixtures by utilizing differences in boiling point, polarity, and adsorption properties of substances.

[0041] MS: Mass spectrometer. It works by ionizing the components in a sample in an ion source to generate charged ions with different charge-to-mass ratios. These ions are then accelerated by an electric field to form an ion beam that enters the mass analyzer. In the mass analyzer, electric and magnetic fields are used to cause opposite velocity dispersion, which focuses the ion beam to obtain a mass spectrum, thereby determining the mass of each component.

[0042] By using GC-MS coupled with the separation capability of GC and the analytical capability of MS, mass spectrometry analysis of most organic compounds can be achieved.

[0043] Since MS spectra provide information on ion fragments of a substance, relying solely on the interpretation of MS spectra is often insufficient for a comprehensive and accurate analysis of the substance. Therefore, it is often necessary to combine them with other analytical methods to analyze the composition of the substance, resulting in low analytical efficiency and difficulty in achieving accurate analysis of the substance's components.

[0044] FTIR (Fourier Transform Infrared) spectrometers, or spectrometers employing other absorption spectroscopy techniques, are important analytical tools for detecting organic components. Absorption spectroscopy can provide a wealth of information in the qualitative and semi-quantitative analysis of organic components.

[0045] Utilizing the property that molecules absorb light when a sample is illuminated by a light source, information about the molecular structure can be obtained by detecting the absorption of light at different wavelengths. For example, the spectrum actually measured by an infrared spectrometer is a summation of the vibrational and rotational motions of molecules. The peak position, number of peaks, and peak intensity information provided by the infrared spectrum can be used for the identification and analysis of organic components. However, the object of absorption spectroscopy needs to be a pure substance or a substance with a relatively simple composition; otherwise, when the absorption spectra of multiple components are superimposed, the interpretation of the spectrum will be very complex or even impossible.

[0046] Electrolytes are often composite systems containing multiple components. Direct infrared spectroscopy testing cannot identify each component, and appropriate separation methods are often required to obtain an ideal infrared spectrum.

[0047] As mentioned above, GC can effectively separate the components in an organic system, thus meeting the requirements for absorption spectroscopy testing. Furthermore, the carrier gas for GC-MS can be an atomic gas, which has minimal interference with the absorption spectrum. By detecting the absorption spectra of the components separated by GC and combining them with MS spectra, accurate qualitative and quantitative analysis of the organic system can be achieved.

[0048] Based on the above detection principle, coupling absorption spectroscopy with GC-MS can utilize the separation function of GC to separate mixed samples into individual components. Then, absorption spectroscopy is used to analyze the absorption spectra of each individual component after separation, while MS is used to analyze the mass spectra of each component after separation. This allows for the simultaneous analysis of the absorption spectra and mass spectra of organic samples, enabling comprehensive and accurate qualitative and quantitative detection of samples.

[0049] Therefore, the key to realizing the coupling of absorption spectroscopy and GC-MS is to simultaneously send the components separated by GC into absorption spectroscopy and MS for detection.

[0050] In some embodiments, a sample detection accessory is used, which integrates both gas and optical paths, enabling the integration and joint use of GC, absorption spectroscopy unit and MS.

[0051] The sample testing accessories include a sample compartment;

[0052] The sample chamber is equipped with a sample inlet and a sample outlet, which are connected to the interior of the sample chamber.

[0053] An incident light path unit is located at one end of the sample chamber. The incident light path unit is used to collimate the light rays entering the sample chamber.

[0054] An outgoing light path unit is located at the other end of the sample chamber. The outgoing light path unit is used to focus the light emitted from the sample chamber.

[0055] The following explanation of the sample testing accessory, based on its working principle in conjunction with the combined detection system, refers to... Figure 1 and Figure 2 The combined detection system includes:

[0056] GC is used to separate the components in a sample; it includes an injection system 11 and a separation system 12. The injection system 11 typically includes an injection needle / autosampler and an injection port for feeding the sample, and the separation system 12 typically includes a column oven and a chromatographic column.

[0057] The absorption spectroscopy unit is used to detect the absorption spectra of the separated components. It includes a light source 21 and a spectrometer 22. The spectrometer 22 is used for spectral analysis of each component of the sample.

[0058] MS is used for mass spectrometry analysis of various components of a sample; it includes an ion source 31, a mass analyzer 32, and a mass spectrometer detector 33.

[0059] And sample testing accessories, for reference Figure 3 , Figure 4 , Figure 5 and Figure 6 The system includes a sample chamber 41, which has a sealed space inside. The sample chamber 41 is provided with a sample inlet 412 and a sample outlet 413 that are respectively connected to the sealed space inside the sample chamber. The gas chromatograph is connected to the sample inlet, and the mass spectrometer is connected to the sample outlet. The components separated by GC enter the sample chamber through the sample inlet and are then sent to the ion source of the mass spectrometer through the sample outlet for mass spectrometry analysis of the sample by MS.

[0060] One end of the sample chamber 41 is connected to the incident optical fiber 23 of the light source of the absorption spectroscopy unit. The incident optical path unit 42 located at this end of the sample chamber is used to collimate the light emitted from the incident optical fiber and then send it into the sample chamber. The other end of the sample chamber is provided with an outgoing optical path unit 43, which is used to focus the light emitted from the other end of the sample chamber. The focused light is received by the outgoing optical fiber 24 of the spectrometer located at the other end of the sample chamber and sent to the spectrometer for processing to perform spectral analysis of the sample.

[0061] Here, the incident light path unit 42 can be a collimating lens, and the exit light path unit 43 can be a condensing lens.

[0062] The gas path and optical path of the coupled detection system are coupled through the sample detection accessory. While the sample is transmitted through the gas path, the sample detection accessory also conducts light. This allows the sample to be transmitted to the MS for detection through the gas path, while the light passes through the sample molecules to achieve spectral detection of the sample. Thus, the spectral and mass spectrometric detection of the sample can be achieved simultaneously.

[0063] Reference Figure 1 and Figure 2 The combined detection system consists of a gas injection system, a separation system, a sample chamber, an ion source, a mass analyzer, and a mass spectrometer detector.

[0064] The optical path of the combined detection system consists of a light source, an incident optical path unit, a sample chamber, an outgoing optical path unit, and a spectral detector.

[0065] The detection principle of the combined detection system based on the above structure is as follows:

[0066] After the sample and carrier gas are separated by the GC separation system, they enter the sample chamber through the sample inlet and flow out through the sample outlet. The separated components of the sample are then sent to MS for mass spectrometry analysis.

[0067] The light source is transmitted to the sample detection accessory via the incident optical fiber. After being collimated by the incident optical path unit, it enters the sample chamber. The incident light is absorbed by the sample in the sample chamber. The outgoing light after being absorbed by the sample is focused by the outgoing optical path unit and enters the outgoing optical fiber. It is then sent to the spectrometer detector to realize the detection of the sample absorption spectrum.

[0068] In some embodiments, optical path plungers 414 are respectively provided at both ends of the sample chamber 41. The optical path plungers 414 are provided with mounting holes 415 for setting the incident optical fiber or the outgoing optical fiber. The mounting holes 415 are connected to the sample chamber, so that light can enter the sample chamber through the incident light and the light in the sample chamber can be received by the outgoing optical fiber.

[0069] In some embodiments, an incident light path unit 42 is provided between the light path plunger at one end and the sample inlet in the sample chamber 41. The incident light path unit 42 is a collimating lens for collimating the incident light. An exit light path unit 43 is provided between the light path plunger at the other end and the sample outlet. The exit light path unit 43 is a condensing lens for focusing the exit light.

[0070] Collimating lenses and condensing lenses are made of materials with high light transmittance. Since the lens is in direct contact with the sample, to prevent the sample from affecting the lens's light transmission and to avoid the lens introducing contaminants into the sample, the lens material is made of a material that is relatively inert to the target component of the sample and will not introduce other impurities. For example, if infrared spectroscopy is required, materials such as calcium fluoride, potassium bromide, zinc selenide, and single-crystal silicon can be selected for the lens material.

[0071] In some embodiments, gas path plungers 416 are respectively provided on the sample inlet 412 and the sample outlet 413. A connection hole 417 for connecting pipelines is provided on the gas path plunger 416. The connection hole 417 communicates with the inside of the sample chamber to facilitate the connection of the sample chamber with the pipelines of GC and MS.

[0072] In some embodiments, the inner wall of the sample chamber 41 may be coated to reflect stray light. The material of the coating is also determined according to the light source, and generally a coating with high reflectivity to the light source can be used. Since the sample is transported within the sample chamber, the coating material should be inert relative to the target components of the sample and should not introduce other impurities. Simultaneously, since the sample chamber is a high-temperature environment, the coating material needs to be able to withstand temperatures up to 300°C. For example, if infrared spectroscopy is required, materials such as gold, chromium, silver, and aluminum can be used as the coating material.

[0073] To ensure the airtightness of the gas path for sample testing accessories, the sample chamber needs to be sealed. Specifically, this can be achieved by installing seals, such as gaskets and gaskets, between the connecting components. For example, a gasket 418 can be installed between the collimating lens, condenser lens, and the sample chamber to seal both ends of the sample chamber, creating a sealed space inside. Gaskets 419 can be installed between the gas plunger and the sample inlet and outlet to seal the sample inlet and outlet. Graphite can be used for the gaskets and gaskets, as it provides excellent sealing, does not introduce impurities that interfere with the test, and can withstand temperatures up to 300°C.

[0074] In some embodiments, a sample channel 411 is provided within the sample chamber 41, with a sample inlet 412 and a sample outlet 413 respectively connected to the sample channel 411. An incident light path unit 42 and an exit light path unit 43 are respectively disposed at both ends of the sample channel 411. The diameter of the sample channel 411 is set to be as small as possible to reduce the volume of the sample channel. Generally, the diameter of the sample channel 411 is set to be the same as or close to the inner diameter of the GC column.

[0075] When using this sample detection accessory to test samples, different sample components have different absorption properties to the light source, resulting in varying sensitivities. Furthermore, the sample concentration within the sample channel is relatively low. Therefore, the influence of the sample channel length on the test needs to be considered. Generally, the length of the sample channel 411 is set to 10-100 cm. Increasing the optical path length optimizes the sensitivity of the sample detection accessory. In this case, the MS spectral acquisition can also be integrated to superimpose spectra acquired over a period of time, further increasing detection sensitivity and facilitating the installation of the sample detection accessory.

[0076] In some embodiments, the sample detection accessory is placed in the column oven of the GC. The internal temperature can be adjusted by the temperature regulation unit installed in the column oven. The temperature regulation unit can adjust the temperature within the range of room temperature to 350°C and maintain the temperature inside the column oven at a stable temperature, so that the sample in the sample chamber can always be kept in a stable temperature environment during the test.

[0077] Based on the aforementioned sample testing accessories and the combined testing system using these accessories, the testing procedure for the samples is as follows:

[0078] 1) Pre-treatment of test samples;

[0079] 2) The sample is transferred to the GC injection system. The sample is treated appropriately in the GC injection system, such as by high temperature, so that the components in the sample are converted into gaseous state in sequence and then transferred to the GC separation system with the carrier gas.

[0080] 3) The sample and carrier gas are continuously distributed in the GC separation system. After multiple distributions, the sample is separated. Each component of the sample enters the sample chamber through the sample inlet in sequence, and the absorption spectrum of the sample is detected by the absorption spectroscopy unit.

[0081] 4) Simultaneously, the sample in the sample chamber enters the ion source through the sample outlet. The ion source breaks the sample molecules into charged ion fragments, which are then transported to the mass analyzer. In the mass analyzer, the ion fragments undergo opposite velocity dispersion using electric and magnetic fields, and are focused to obtain mass spectra, thus completing the mass spectrometry analysis of the sample.

[0082] In the description of this utility model, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", and "outer" used to indicate the orientation or positional relationship are based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship that the utility model product is usually placed in during use. They are only used to facilitate the description of this utility model and simplify the description, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.

[0083] Furthermore, the use of terms such as "horizontal" and "vertical" in the description of this utility model does not imply that the components are required to be absolutely horizontal or suspended, but rather that they can be slightly tilted. For example, "horizontal" simply means that its direction is more horizontal relative to "vertical," and does not mean that the structure must be completely horizontal, but can be slightly tilted.

[0084] In the description of this utility model, it should also be noted that, unless otherwise explicitly specified and limited, the terms "set," "install," "connect," and "link" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this utility model based on the specific circumstances.

[0085] The above description is merely a preferred embodiment of the present utility model and is not intended to limit the present utility model in any way. Any simple modifications or equivalent changes made to the above embodiments based on the technical essence of the present utility model shall fall within the protection scope of the present utility model.

Claims

1. Sample testing accessories, characterized in that, Includes sample compartment; The sample chamber is provided with a sample inlet and a sample outlet, and the sample inlet and sample outlet are respectively connected to the interior of the sample chamber; An incident light path unit is provided at one end of the sample chamber, which is used to collimate the light rays entering the sample chamber. An outgoing light path unit is provided at the other end of the sample chamber, which is used to focus the light emitted from the sample chamber.

2. The sample testing accessory according to claim 1, characterized in that, The sample chamber is provided with a sample channel, and the sample inlet and sample outlet are respectively connected to the sample channel. The incident light path unit and the outgoing light path unit are respectively located at both ends of the sample channel.

3. The sample testing accessory according to claim 1 or 2, characterized in that, The incident optical path unit includes a collimating lens, and the outgoing optical path unit includes a condensing lens.

4. The sample testing accessory according to claim 1 or 2, characterized in that, An optical path plunger is provided at the end of the sample chamber. The optical path plunger is provided with mounting holes for setting the incident optical fiber or the outgoing optical fiber. The mounting holes are connected to the sample chamber.

5. The sample testing accessory according to claim 1 or 2, characterized in that, Gas path plungers are provided at the sample inlet and sample outlet, and the gas path plungers are provided with connection holes for setting up pipelines. The connection holes are connected to the inside of the sample chamber.

6. The sample testing accessory according to claim 1 or 2, characterized in that, The inner wall of the sample chamber is coated.

7. A combined detection system, characterized in that, include: A gas chromatograph, which is used to separate the components in a sample; An absorption spectroscopy unit, comprising a light source and a spectral detector, wherein the spectral detector is used for spectral analysis of various components of the sample; A mass spectrometer, which is used for mass spectrometric analysis of various components of a sample; And, the sample testing accessory according to any one of claims 1-6; The gas chromatograph is connected to the sample inlet, the mass spectrometer is connected to the sample outlet, and the light from the light source is processed by the incident light path unit and then enters the sample chamber. The light in the sample chamber is processed by the outgoing light path unit and then received by the spectrometer detector.

8. The combined detection system according to claim 7, characterized in that, The sample detection accessory is installed inside the column oven of the gas chromatograph, and the column oven is equipped with a temperature control unit for adjusting the temperature inside the column oven.

9. The combined detection system according to claim 7, characterized in that, The sample channel of the sample chamber is 10-100cm in length.

10. The combined detection system according to claim 7, characterized in that, The inner diameter of the sample channel in the sample chamber is matched with the inner diameter of the chromatographic column of the gas chromatograph.

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