A detection device and method capable of quickly detecting the content of a cooling agent of an electronic atomizer

Abstract

The present application belongs to the technical field of electronic atomizer detection, and particularly relates to a detection device and method capable of rapidly detecting the content of a cooling agent of an electronic atomizer, the detection steps comprising: sealingly butting the electronic atomizer with a micro cyclone sampler, inputting aerosol into the micro cyclone sampler, and forming uniform aerosol beams inside the micro cyclone sampler; then starting a Raman (SERS) detection module, irradiating the SERS substrate after contacting with the aerosol beams by a laser source, and collecting the Raman scattering signals subjected to collision frequency shift by a micro spectrometer; processing the collected Raman scattering signals, eliminating the interference of propylene glycol and glycerol matrix and the environmental fluorescence background, and extracting the characteristic peak data of the cooling agent; based on the SERS characteristic peak library of the cooling agent, comparing the extracted characteristic peak positions of the cooling agent to identify the type of the cooling agent; and according to the area of the characteristic peak and a pre-constructed correction curve, calculating the content of the cooling agent; the present application does not require complex pretreatment, and is rapid, accurate and strong in anti-interference ability.

Description

Technical Field

[0001] This invention belongs to the field of electronic atomizer detection technology, specifically relating to a detection device and method for rapidly detecting the content of cooling agent in electronic atomizers. Background Technology

[0002] Cooling agents are the core functional ingredients in e-liquids that determine the vaping experience. They enhance user comfort by simulating a cooling sensation. Common types include WS-23 (N,2,3-trimethyl-2-isopropylbutyramide), WS-3 (mentholamide), and DL-menthol. However, excessive amounts of cooling agents can irritate and damage the respiratory mucosa, and long-term inhalation may lead to health risks such as throat discomfort and coughing. Therefore, the content of cooling agents in e-liquids needs to be precisely controlled.

[0003] Existing technologies for detecting cooling agents in electronic atomizers have many insurmountable shortcomings: 1. The pretreatment process is cumbersome. Traditional detection methods rely on a complex process of "filter capture - solvent extraction - chromatographic separation". A single detection takes more than 2 hours. In addition, the cooling agent is prone to volatilization or residue during sample transfer, which leads to distorted detection results. 2. Poor equipment adaptability: Traditional testing devices are mostly desktop structures, which are bulky and dependent on a fixed laboratory environment, and cannot meet the needs of mobile scenarios such as rapid sampling and quality control on the production line.

[0004] In view of this, the present invention proposes a detection device and method for rapidly detecting the content of cooling agent in electronic atomizers. Summary of the Invention

[0005] In view of the above-mentioned shortcomings in the prior art, the present invention provides a detection device and method for rapidly detecting the content of cooling agent in electronic atomizers, so as to solve the problems in the background art.

[0006] To solve the above-mentioned technical problems, the present invention adopts the following technical solution: Firstly, a method for rapidly detecting the cooling agent content in an electronic atomizer includes the following steps: S1: Sampling preparation: Select a disposable universal sampling head and seal it with the micro cyclone sampler. The disposable universal sampling head has a built-in silicone sealing sleeve and an anti-backflow valve, and can be used with electronic nebulizer nozzles with a diameter of 6-18mm. The leakage rate is <0.05mL / min. For non-contact aerosol sampling, hold the sampling head and align it with the electronic nebulizer nozzle, maintaining a non-contact gap of ≤2mm. Start the micro suction pump and set the sampling parameters: suction flow rate 15-25mL / s, single suction duration 2-3s, suction interval 20-25s, and a total of 3-5 suctions. The aerosol enters the micro cyclone sampler through the sampling head and forms a uniform aerosol bundle through the spiral guide channel. S2: Raman spectroscopy signal acquisition. The surface-enhanced Raman spectroscopy (SERS) detection module is activated. This module includes a 785nm semiconductor laser source, a SERS-enhanced substrate, and a miniature spectrometer. The laser source irradiates the SERS substrate after it has come into contact with aerosol micelles at a power of 30–80mW. The miniature spectrometer acquires the Raman scattering signal with an integration time of 0.3–0.5s and a detection wavelength range of 400–2000cm. -1 ; S3: Signal processing and interference elimination. The collected Raman scattering signal is processed by intelligent algorithm to automatically remove the interference of propylene glycol and glycerol matrix and the background of ambient fluorescence, and extract the characteristic peak data of cooling agent. S4: Qualitative and quantitative analysis, based on the built-in SERS characteristic peak library of cooling agents, identifies the types of cooling agents by comparing the positions of characteristic peaks; the content of cooling agents is calculated by substituting the characteristic peak areas into the pre-constructed calibration curve.

[0007] In step S2, the Raman scattering signal is generated by the inelastic collision between laser photons emitted by the laser source and the cooling agent molecules, resulting in the molecules absorbing / releasing a small amount of energy, which causes a shift in the frequency of the scattered light.

[0008] Secondly, the SERS substrate in step S2 is a quartz sheet modified with a silver nanorod array, and the laser source is a 785nm near-infrared laser.

[0009] Simultaneously, in step S3, the Raman scattering signal is decomposed into a multi-scale wavelet decomposition based on the interference library data composed of the spectral signals of "blank SERS substrate + pure propylene glycol / glycerol aerosol". This separates the high-frequency characteristic peak signal of the cooling agent from the low-frequency matrix interference and fluorescence background signal, retains the wavelet coefficients corresponding to the characteristic peak of the cooling agent, and obtains a preliminary denoised spectrum after reconstruction. Through multi-characteristic peak fusion technology, the exclusive characteristic peak range of the cooling agent is locked, and the residual matrix interference in this range is eliminated by comparing with the interference library data, finally obtaining a pure spectrum containing only the characteristic peak signal of the cooling agent.

[0010] Furthermore, in step S4, based on the fact that the peak area of ​​the Raman characteristic peak of the cooling agent is proportional to the concentration of the cooling agent, the formula for calculating the calibration curve is Y=kX+b, where Y represents the net peak area between the characteristic peak of the cooling agent and the baseline signal, X represents the actual content of the cooling agent, k is the sensitivity coefficient of the calibration curve, and b is a systematic error correction term.

[0011] In step S4, the net peak area is calculated using the integral formula, as follows: Where n is the number of spectral data points within the integral interval of the characteristic peak. , These represent the net signal strengths of the i-th and (i+1)-th data points, respectively. The Raman shift interval between two adjacent data points. The baseline area within the integration interval is used to substitute the net peak area into the calibration curve formula to calculate the actual content of the cooling agent.

[0012] Meanwhile, when testing refillable e-cigarettes, it is necessary to collect blank aerosol (atomizing liquid without cooling agent) for background subtraction. E-cigarettes can be sampled and tested directly without pretreatment.

[0013] Secondly, a detection device capable of rapidly detecting the cooling agent content in an electronic atomizer includes: The micro sampling module includes a disposable universal sampling head, a micro cyclone sampler, and a suction pump. The disposable universal sampling head has a built-in silicone sealing sleeve and an anti-backflow valve, and can be adapted to electronic atomizer mouthpieces with a diameter of 6-18mm. The SERS Raman detection module includes an integrated Raman probe, a semiconductor laser source, and a miniature spectrometer. The integrated Raman probe incorporates a SERS-enhancing substrate (silver nanorod array), and the laser focusing spot diameter is ≤0.5mm. The semiconductor laser source has a wavelength of 785nm (anti-fluorescence interference) and an adjustable power of 30–80mW. The miniature spectrometer has a detection wavelength range of 400–2000cm². -1 Resolution ≤ 3cm -1 Data acquisition rate ≥100Hz; The data processing module includes an embedded main control chip, a built-in SERS characteristic peak library for cooling agents and a noise reduction algorithm, which can automatically deduct matrix interference and support real-time display of detection results and data upload. The power supply module is a rechargeable lithium battery.

[0014] In this invention, the Raman spectrometer is the core detection component for identifying and quantifying the types and content of cooling agents. When the laser of the Raman spectrometer irradiates the cooling agent molecules in the aerosol, some photons undergo inelastic collisions with the molecules, causing changes in photon energy. This phenomenon is called Raman scattering. The Raman spectrometer can directly acquire spectra from the aerosol without pretreatment steps such as filter trapping and solvent extraction, enabling online real-time analysis of cooling agents. Based on the uniqueness of the Raman characteristic peaks of different cooling agent molecules, it can simultaneously identify structurally similar cooling agent types such as WS-3, WS-23, and menthol, overcoming the technical deficiency of current gas chromatography detection methods that cannot distinguish between types.

[0015] Compared with the prior art, the present invention has the following beneficial effects: 1. This invention requires no complex pretreatment throughout the entire process, which greatly improves efficiency compared to traditional testing methods and can meet the needs of high-speed quality control and batch sampling inspection in electronic atomizer production lines; 2. This invention eliminates matrix interference by comparing data from an interference library, reducing the relative standard deviation of the detection results and achieving high detection accuracy, thus meeting the accuracy requirements for quantitative analysis of cooling agents; 3. The detection device of this invention adopts an integrated design, is compact in size, and can be operated by hand. It does not rely on a fixed laboratory environment and power supply, and is suitable for mobile scenarios such as on-site sampling inspection, logistics traceability, and store compliance inspection. Attached Figure Description

[0016] Figure 1 This is a schematic flowchart of an embodiment of a detection method for rapidly detecting the cooling agent content in an electronic atomizer according to the present invention. Figure 2 This is a schematic diagram of the system structure of an embodiment of the device for detecting the content of cooling agent in an electronic atomizer according to the present invention. Detailed Implementation

[0017] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below in conjunction with specific embodiments.

[0018] The accompanying drawings are for illustrative purposes only and are schematic diagrams, not actual pictures. They should not be construed as limiting the invention. To better illustrate the embodiments of the invention, some parts in the drawings may be omitted, enlarged, or reduced, and do not represent the actual product dimensions. It is understandable to those skilled in the art that some well-known structures and their descriptions may be omitted in the drawings.

[0019] In the accompanying drawings of the embodiments of the present invention, the same or similar reference numerals correspond to the same or similar components. In the description of the present invention, it should be understood that if terms such as "upper," "lower," "left," "right," "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 present invention 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 and operated in a specific orientation. Therefore, the terms used to describe positional relationships in the accompanying drawings are only for illustrative purposes and should not be construed as limiting the present invention. For those skilled in the art, the specific meaning of the above terms can be understood according to the specific circumstances.

[0020] In the description of this invention, unless otherwise explicitly specified and limited, the term "connection" or similar designation indicating a connection between components should be interpreted broadly. For example, it can refer to a fixed connection, a detachable connection, or an integral part; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium; it can refer to the internal communication between two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0021] Example 1: like Figure 1-2 As shown, this invention employs a synergistic technical approach of "non-contact rapid sampling + surface-enhanced Raman spectroscopy (SERS) + intelligent analysis" to propose a detection device and method capable of rapidly detecting the cooling agent content in electronic atomizers. Specific technical details are as follows: This system employs a combination of a disposable universal sampling head and a miniature cyclone sampler. The sampling head incorporates a built-in silicone sealing sleeve and an anti-backflow valve. Utilizing the elastic deformation properties of the silicone sealing sleeve, it can adaptively fit disposable or refillable electronic atomizer nozzles with diameters ranging from 6 to 18 mm. After docking, the leakage rate is <0.05 mL / min, ensuring leak-free aerosol collection. During sampling, a contactless gap of ≤2 mm is maintained to avoid the risk of contamination from direct contact between the sampling head and the atomizer nozzle. By starting the miniature diaphragm pump, setting a suction flow rate of 15–25 mL / s, a single suction time of 2–3 seconds, and a suction interval of 20–25 seconds, 3–5 suctions are sufficient to complete sample collection, achieving an aerosol capture efficiency >98%. The miniature cyclone sampler features an internal spiral flow channel, allowing aerosols to form a uniform aerosol bundle within 3 seconds of entry. This ensures sufficient contact between the cooling agent molecules and the subsequent SERS-enhanced substrate, replacing the complex flow equalization structure of traditional dynamic simulation chambers and significantly improving sampling efficiency.

[0022] A 785nm near-infrared semiconductor laser source was selected. This wavelength of laser light can effectively suppress fluorescence interference from matrix components such as propylene glycol and glycerol in the electronic atomization liquid, reducing the influence of impurity peaks on the characteristic signal of the cooling agent. The SERS-enhanced substrate is a quartz sheet modified with a silver nanorod array. Its surface plasmon resonance effect can enhance the Raman signal of the cooling agent molecules by 10%. 6 This significantly reduces the detection limit; the detection wavelength range of the miniature spectrometer is set to 400–2000 cm⁻¹. -1 Resolution ≤ 3cm -1 With a data acquisition rate ≥100Hz and an integration time of only 0.3–0.5s, the detection time is minimized while ensuring signal acquisition accuracy. The integrated Raman probe integrates the laser source, SERS enhancement substrate, and spectrometer acquisition port, with a laser focusing spot diameter ≤0.5mm, ensuring the targeting and concentration of signal acquisition.

[0023] An innovative algorithm combining "multi-feature peak fusion + wavelet transform denoising" is adopted to construct a full-process intelligent signal processing system, achieving accurate extraction of cooling agent feature signals and efficient removal of interference. Based on the exclusive characteristic peak library of cooling agents, the core peak combination of the target cooling agent is locked through multi-characteristic peak fusion technology. Combined with the multi-dimensional collaborative verification logic of peak position matching and peak shape determination, the qualitative misjudgment caused by matrix interference and background noise interference of a single characteristic peak is completely avoided, and the differentiation accuracy of structurally similar cooling agents is greatly improved. Wavelet transform denoising algorithm is used to decompose and reconstruct the spectral signal at multiple scales, accurately separating the high-frequency effective cooling agent feature signal from the low-frequency ambient fluorescence background and propylene glycol / glycerol matrix interference signal, efficiently removing non-target interference, and extracting pure cooling agent feature peak data; The algorithm has a built-in environment adaptive compensation model that can dynamically adjust parameters based on signal characteristics to automatically compensate for signal offset and intensity fluctuations caused by temperature fluctuations of 15-40℃ and humidity changes of 30%-70%. It does not require additional temperature and humidity control devices and is perfectly adapted to complex environments in various scenarios such as laboratories, production lines, and outdoor sampling inspections, ensuring the stability and reliability of test results.

[0024] It features a built-in dedicated SERS characteristic peak library for cooling agents, including characteristic peak data for common cooling agents such as WS-3, WS-23, and DL-menthol. Accurate identification of cooling agent types can be quickly achieved by comparing the positions of characteristic peaks. Pre-constructed calibration curves are built using standard solutions of cooling agents with concentration gradients from 0.02 to 50 mg / L, following the same sampling and signal acquisition process as for samples, covering low, medium, and high concentration ranges. The extracted characteristic peak areas can be substituted into the calibration curve for rapid calculation of cooling agent content. For refillable e-nebulizers, background subtraction is performed by collecting an additional breath of blank aerosol without cooling agents, further improving quantitative accuracy. Disposable e-nebulizers can be directly sampled and detected without complex pretreatment.

[0025] The detection device consists of a micro-sampling module, a SERS Raman detection module, a data processing module, and a power supply module. The micro-sampling module enables contactless and rapid aerosol acquisition. The SERS Raman detection module enhances and acquires the signal. The data processing module has a built-in characteristic peak library and algorithm model, which automatically performs signal analysis, qualitative identification, and quantitative calculation, and supports real-time display of detection results and data upload. The power supply module uses a rechargeable lithium battery with a capacity of ≥5000mAh, which can continuously detect ≥100 samples on a single charge and supports Type-C fast charging to ensure continuous use in mobile scenarios.

[0026] Example 2: like Figure 1-2 The rapid detection device described in this invention is prepared, wherein the micro-sampling module includes a disposable universal sampling head, a micro-cyclone sampler, and a micro-diaphragm pump; the laser source wavelength of the SERS Raman detection module is 785nm, and the power is adjustable in the range of 30-80mW; the SERS enhancement substrate is a quartz sheet modified with a silver nanorod array; the data processing module has a built-in SERS characteristic peak library of cooling agents and a "multi-characteristic peak fusion + wavelet transform denoising" algorithm; the pre-constructed calibration curve (Y=kX+b) is as follows: WS-23: Y = 0.825X + 0.0031; WS-3: Y = 0.798X + 0.0028; DL-Menthol: Y = 0.856X + 0.0042; Where Y represents the net peak area of ​​the characteristic peak of the cooling agent and the baseline signal, that is, the effective signal intensity (unit: dimensionless, quantized output by the spectrometer detection system) of the characteristic peak of the cooling agent in the Raman signal collected by the miniature spectrometer after deducting matrix interference and background noise; X represents the actual concentration of the cooling agent (unit: mg / L), corresponding to the concentration of the prepared standard solution (gradient range of 0.02~50mg / L); k is the sensitivity coefficient of the calibration curve, representing the change in the net peak area of ​​the corresponding Raman characteristic peak when the concentration of the cooling agent changes by 1mg / L. The larger the value of k, the more sensitive the detection method is to the concentration change of the cooling agent. b (intercept) is a systematic error correction term, mainly determined by the baseline noise of the detection system, the background signal of the SERS substrate, the residual solvent signal, etc. The closer the value is to 0, the smaller the background interference of the system (the b value of this curve is ≤0.0042, the interference is extremely low).

[0027] Implementation of detection method: S1: Sampling preparation, select a brand new disposable universal sampling head, insert it into the interface of the micro cyclone sampler and tighten the seal, and confirm the leakage rate is <0.05mL / min through air tightness test; For non-contact aerosol sampling, a disposable electronic nebulizer containing WS-23 was selected. The sampling head was held and aligned with the nebulizer nozzle, maintaining a 1mm non-contact gap. The micro diaphragm pump was started, and the sampling parameters were set as follows: aspiration flow rate of 20mL / s, single aspiration duration of 2.5s, and aspiration interval of 22s. A total of 4 aspirations were performed. The aerosol entered the micro cyclone sampler through the sampling head and formed a uniform aerosol bundle through the spiral guide channel. S2: Raman spectral signal acquisition. Start the SERS Raman detection module, set the laser source power to 50mW, and the miniature spectrometer acquires the Raman scattering signal with an integration time of 0.4s. S3: Signal processing and interference cancellation. Intelligent algorithms automatically process the acquired spectral signals, removing matrix interference from propylene glycol and glycerol, as well as ambient fluorescence background, and extracting the characteristic peak data of WS-23 (915 cm⁻¹). -1 / 1302cm -1 ); S4: Qualitative and quantitative analysis: By comparing the positions of characteristic peaks, the cooling agent in the electronic atomizer was identified as WS-23. The area of ​​the characteristic peak was extracted and substituted into the calibration curve Y=0.825X+0.0031, and the content of WS-23 was calculated to be 3.25mg / L. Disposal of the sampling head: After the test is completed, remove the disposable universal sampling head and put it into a special sealed recycling bag for subsequent centralized processing.

[0028] Detection limit verification: A series of low-concentration cooling agent standard aerosols were prepared. With a signal-to-noise ratio (S / N) ≥3 as the judgment criterion, the detection limit of WS-23 was 0.05 mg / L, the detection limit of WS-3 was 0.06 mg / L, and the detection limit of DL-menthol was 0.02 mg / L, all of which meet the detection requirements of low-concentration cooling agents.

[0029] Accuracy verification: A mixed cooling agent standard aerosol with a concentration of 5 mg / L (WS-23, WS-3, and DL-menthol were all 5 mg / L) was tested 10 times according to the detection method of this invention. The relative standard deviation (RSD) of WS-23 was 1.3%, the RSD of WS-3 was 1.5%, and the RSD of DL-menthol was 1.1%, all ≤1.8%, indicating that the repeatability of this method is good.

[0030] Accuracy verification: Three electronic atomizer samples with known cooling agent content were selected (Sample 1 containing WS-23, Sample 2 containing WS-3, and Sample 3 containing DL-menthol). Corresponding cooling agent standards at low, medium, and high concentration levels were added, and spiked recovery tests were conducted. The results showed that the spiked recoveries of WS-23 were 95.3%–103.8%, WS-3 were 96.1%–104.0%, and DL-menthol were 95.7%–103.2%, all meeting the accuracy requirements for quantitative analysis.

[0031] Detection efficiency verification: Ten different types of electronic atomizer samples (five disposable and five refillable) were continuously tested. The time taken for a single test (from sample preparation to result output) was calculated. The results showed that the average test cycle was 2.5 minutes, and 24 samples could be tested per hour, which meets the requirements for rapid batch testing.

[0032] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for rapidly detecting the cooling agent content in an electronic atomizer, characterized in that, Includes the following steps: S1: Seal and connect the electronic atomizer to the micro cyclone sampler, and input the aerosol into the micro cyclone sampler to form a uniform aerosol bundle inside the micro cyclone sampler. S2: Activate the Raman (SERS) detection module. The laser source irradiates the SERS substrate after it comes into contact with the aerosol beam, and the miniature spectrometer collects the Raman scattering signal that has undergone frequency shift due to the collision. S3: Process the collected Raman scattering signals to eliminate interference from propylene glycol and glycerol matrix and ambient fluorescence background, and extract characteristic peak data of the cooling agent; S4: Based on the SERS characteristic peak library of cooling agents, the type of cooling agent is identified by comparing the position of the characteristic peaks of the extracted cooling agents; the content of cooling agents is calculated based on the area of ​​the characteristic peaks and the pre-constructed calibration curve.

2. The detection method according to claim 1, characterized in that: The Raman scattering signal mentioned in step S2 is generated by the inelastic collision between laser photons emitted by the laser source and the cooling agent molecules, resulting in the molecules absorbing / releasing a small amount of energy, which causes a shift in the frequency of the scattered light.

3. The detection method according to claim 1, characterized in that: In step S2, the SERS substrate is a quartz sheet modified with a silver nanorod array, and the laser source is a 785nm near-infrared laser.

4. The detection method according to claim 1, characterized in that: In step S3, the Raman scattering signal is decomposed into multi-scale wavelet decomposition to separate the high-frequency cooling agent characteristic peak signal from the low-frequency matrix interference and fluorescence background signal, retain the wavelet coefficients corresponding to the cooling agent characteristic peak, and obtain the preliminary denoised spectrum after reconstruction.

5. The detection method according to claim 1, characterized in that: In step S4, the formula for calculating the calibration curve is Y=kX+b, where Y represents the net peak area between the characteristic peak of the cooling agent and the baseline signal, X represents the actual content of the cooling agent, k is the sensitivity coefficient of the calibration curve, and b is a systematic error correction term.

6. The detection method according to claim 1, characterized in that: In step S4, the net peak area is calculated using the integral formula, as follows: Where n is the number of spectral data points within the integral interval of the characteristic peak. , These represent the net signal strengths of the i-th and (i+1)-th data points, respectively. The Raman shift interval between two adjacent data points. The baseline area within the integration interval is used to substitute the net peak area into the calibration curve formula to calculate the actual content of the cooling agent.

7. The detection method according to claim 1, characterized in that: When testing the electronic atomizer, the atomized liquid without cooling agent needs to be collected for background subtraction.

8. A detection device capable of rapidly detecting the cooling agent content in an electronic atomizer, characterized in that, include: A micro sampling module, which uses a sampling head and a suction pump to deliver aerosol drawn from an electronic atomizer into a micro cyclone sampler; The SERS Raman detection module includes an integrated Raman probe, a semiconductor laser source, and a miniature spectrometer, used to acquire Raman scattering signals. The data processing module includes an embedded main control chip, a built-in SERS characteristic peak library for cooling agents and a noise reduction algorithm, which can automatically deduct matrix interference and support real-time display of detection results and data uploading. A power supply module that supplies power to the entire detection device.

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