A rapid quantitative detection system for solid powder samples based on combined spectroscopy

Abstract

This invention relates to the field of quantitative detection technology, and in particular to a rapid quantitative detection system for solid powder samples based on combined spectroscopy, comprising a sample acquisition module and a detection module. During sample preparation, the raw materials are first sieved using a raw material sieving device, then transported manually or mechanically to a drying device for drying. After drying, the dried raw materials are pulverized using a pulverizing device, and finally, the pulverized raw materials are compressed into tablets / suspended for sample preparation. During detection, the prepared sample is placed at a designated station, and the sample surface is alternately excited using a spectral excitation device. The spectrum is then captured by a signal acquisition device, and after aligning the multispectral data using a data processing device, a pre-trained model is called using an analysis device to output the component concentrations and physical properties.

Description

Technical Field

[0001] This invention relates to the field of quantitative detection technology, and in particular to a rapid quantitative detection system for solid powder samples based on combined spectroscopy. Background Technology

[0002] Spectroscopy is a method system that utilizes the emission, absorption, or scattering spectral characteristics of molecules or atoms undergoing energy level transitions when matter interacts with radiation energy for qualitative and quantitative analysis. Currently, there is a problem that spectroscopic analysis techniques are difficult to use for in-situ, real-time, and accurate quantitative analysis of powder mixture samples. This paper proposes a new spectroscopic analysis technique that combines spectroscopic techniques and instrument structure to establish a quantitative model between changes in optical system parameters (such as laser source power, effective sample irradiation volume, sample calibration, and powder sample physical properties) and changes in sample spectral intensity. This model aims to eliminate the influence of changes in spectroscopic instrument optical system parameters and sample physical properties on sample spectral intensity, and to develop a novel spectroscopic analysis technique to achieve accurate quantitative analysis of the main components of solid powder samples. Furthermore, traditional solid powder detection methods, such as chemical titration, chromatography, and mass spectrometry, rely on complex pretreatment steps, which are time-consuming, costly, and may damage the sample.

[0003] The combined spectroscopy method aims to achieve rapid, non-destructive, and high-precision quantitative detection through the fusion of multispectral information. Therefore, this technology addresses the limitations of traditional detection methods. Traditional detection methods are designed for complex mixed powders, such as pharmaceuticals, minerals, and food additives, where a single spectral technique cannot comprehensively cover the component information. The combined spectroscopy method enhances the sensitivity and specificity for detecting multi-component, low-content components by combining multiple spectral techniques, such as near-infrared, Raman, and infrared spectroscopy. Therefore, this research can improve the ability to simultaneously detect multiple components. Existing detection technologies require significant time and manpower costs and cannot guarantee the accuracy of the results. Therefore, developing supporting portable or online detection systems is crucial to meet the real-time monitoring needs of industrial sites, laboratories, and field scenarios, reducing reliance on large instruments and professional personnel, lowering costs, improving detection efficiency, and promoting the long-term development of intelligent detection equipment. Summary of the Invention

[0004] The purpose of this invention is to provide a rapid quantitative detection system for solid powder samples based on combined spectroscopy, so as to solve the problems mentioned in the background art.

[0005] The technical solution adopted in this invention is: A rapid quantitative detection system for solid powder samples based on combined spectroscopy includes a sample acquisition module and a detection module. The sample acquisition module consists of a raw material sieving device, a drying device, a pulverizing device, and a sample preparation device, which sequentially sieves, dries, pulverizes, and prepares the raw materials. The detection module consists of a spectral excitation device, a signal acquisition device, a data processing device, and an analysis device, which sequentially excites the sample surface, captures the spectrum, aligns the data, and outputs the component concentration and physical properties.

[0006] Optionally, the raw material screening equipment is a vibrating screen.

[0007] Optionally, the drying equipment is a vacuum oven.

[0008] Optionally, the pulverizing equipment is a planetary ball mill.

[0009] Optionally, the sample preparation equipment is an automated tablet press.

[0010] Optionally, the spectral excitation device uses laser and X-rays to excite the sample surface.

[0011] Optionally, the signal acquisition device employs a multi-channel detector to simultaneously capture the emission / heat dissipation spectrum.

[0012] Optionally, the data processing device aligns the multispectral data using a time / space registration algorithm.

[0013] Optionally, the analysis device may call a pre-trained model to output component concentrations and physical properties.

[0014] Compared with the prior art, the beneficial effects of the present invention are: 1. Rapid quantitative detection technology for solid powder samples based on combined spectroscopy not only enables accurate and precise quantitative determination of the main components of solid powder samples, but also allows for the establishment of quantitative models to adapt to the complexity of different matrices and components.

[0015] 2. To solve the problem that existing spectral analysis techniques are insufficient for in-situ, real-time, and accurate quantitative analysis of powder mixture samples.

[0016] 3. Using combined spectroscopic techniques and instrument structure, establish a quantitative model between changes in optical system parameters and physical properties of powder samples and changes in sample spectral intensity. Eliminate the influence of changes in optical system parameters of spectroscopic instruments and physical properties of samples on sample spectral intensity, and develop a new spectroscopic analysis technique to achieve accurate quantitative analysis of the main components of solid powder samples.

[0017] This application addresses the shortcomings of single-spectral techniques, such as insufficient sensitivity or poor anti-interference capabilities, through multi-source spectral data fusion and algorithm optimization, including machine learning and deep learning. It also establishes novel quantitative analysis models to improve the reliability of trace component detection in complex matrices. Particularly in the pharmaceutical industry, it enables rapid detection of active pharmaceutical ingredients (APIs), excipient ratios, and illegal additives, ensuring drug quality. In the food safety field, it facilitates on-site screening of additives and contaminants, such as heavy metals and pesticide residues. In the environmental monitoring industry, it allows for rapid analysis of pollutant components in soil and dust, such as microplastics and industrial waste. In materials science, it enables the optimization of functional materials, such as battery materials and catalysts, focusing on component design and quality control. Furthermore, this technology can effectively reduce detection costs, reagent consumption, and manpower, shortening the detection cycle from hours to minutes; it supports green chemistry principles, reduces wastewater generation, and contributes to the sustainable development of the industry. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 This is a schematic diagram of the application; Figure 2 This is a diagram illustrating the steps involved in obtaining the sample in this application; Figure 3 This is a schematic diagram of the testing process for this application; Figure 4 This is a schematic diagram of the critical process route in this application. Figure 1 ; Figure 5 This is a schematic diagram of the critical process route in this application. Figure 2 ; Figure 6 This is a schematic diagram of the critical process route in this application. Figure 3 .

[0020] Figure label: 100. Rapid quantitative detection system for solid powder samples; 110. Sample acquisition module; 120. Detection module; 111. Raw material screening equipment; 112. Drying equipment; 113. Crushing equipment; 114. Sample preparation equipment; 121. Spectroscopic excitation equipment; 122. Signal acquisition equipment; 123. Data processing equipment; 124. Analysis equipment. Detailed Implementation

[0021] In the description of this invention, it should be understood that the terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," and "circumferential" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship commonly used when the product of this invention is in use, or the orientation or positional relationship commonly understood by those skilled in the art. They are only used to facilitate the description of this invention and to 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 invention.

[0022] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of this invention, "a plurality of" means two or more, unless otherwise explicitly specified.

[0023] Given that current technologies require significant time and manpower costs and cannot guarantee the accuracy of test results, it is necessary to develop supporting portable or online testing systems to meet the real-time monitoring needs of industrial sites, laboratories, and field scenarios. This would reduce reliance on large instruments and professional personnel, lower costs, improve testing efficiency, and promote the long-term development of intelligent testing equipment.

[0024] like Figure 1-6 As shown, this embodiment of the invention provides a rapid quantitative detection system for solid powder samples based on combined spectroscopy, including a rapid quantitative detection system 100 for solid powder samples. The rapid quantitative detection system 100 for solid powder samples includes a sample acquisition module 110 and a detection module 120. The sample acquisition module 110 consists of a raw material sieving device 111, a drying device 112, a pulverizing device 113, and a sample preparation device 114. The sample acquisition module 110 sequentially performs sieving, drying, pulverizing, and sample preparation on the raw materials. The detection module 120 consists of a spectral excitation device 121, a signal acquisition device 122, a data processing device 123, and an analysis device 124. It sequentially excites the sample surface, captures the spectrum, aligns the data, and outputs the component density and physical properties.

[0025] During sample preparation, the raw materials are first screened using the raw material screening equipment 111. Then, the screened raw materials are placed in the drying equipment 112 by manual or mechanical means (such as a transfer vehicle) for drying. After drying, the dried raw materials are crushed using the pulverizing equipment 113. Finally, the crushed raw materials are pressed into tablets or suspended for sample preparation using the sample preparation equipment 114 to complete the sample preparation. During testing, the prepared sample is placed at the designated station, and the sample surface is alternately excited by the spectral excitation device 121. The spectrum is then captured by the signal acquisition device 122. After the multispectral data is aligned by the data processing device 123, the analysis device 124 calls the pre-trained model to output the component concentration and physical properties.

[0026] Research methods and technological routes I. Research Methods 1. Joint Spectroscopic Technology Fusion Strategy By combining Fourier Transmission Infrared Spectroscopy (FTIR) (functional group identification) with X-ray Fluorescence Spectroscopy (XRF) (elemental analysis), or Raman spectroscopy (Raman) (functional group identification) with Laser-Induced Breakdown Spectroscopy (LIBS) (trace element detection), the detection accuracy is improved through multi-dimensional data complementarity.

[0027] Multimodal data fusion algorithms (such as principal component analysis (PCA), partial least squares regression (PLSR), and fuzzy neural networks) are used to eliminate spectral interference and establish a joint quantitative model.

[0028] 2. Sample processing and standardization Powder pretreatment: Uniformity is improved by ball milling and sieving (particle size <75μm), and scattering interference is reduced by using binders (such as KBr tableting).

[0029] Dynamic sample introduction technology: Design a pneumatic suspension or vibrating fluidized bed sample introduction system to achieve continuous powder delivery and avoid batch errors in static sample preparation.

[0030] 3. Development of Spectral Detection System It adopts a modular design: integrating multispectral light sources (such as lasers and X-ray tubes), detectors (CCD / PMT) and optical path switching devices, supporting multispectral parallel or rapid switching detection.

[0031] Miniaturized optical path design: Utilizing fiber optic coupling technology to reduce the size of the equipment and adapt to industrial environments (such as dustproof and vibration-resistant).

[0032] 4. Data Processing and Algorithms Spectral noise reduction: Background noise is eliminated based on wavelet transform or Savitzky-Golay filtering.

[0033] Quantitative modeling: Combining machine learning (such as random forest and support vector machine) with traditional chemometrics methods, a dynamic calibration model is trained using a standard sample library.

[0034] Real-time analysis: Develop edge computing modules (such as embedded GPUs) to achieve millisecond-level parsing of spectral data.

[0035] II. Critical Process Path (See instruction manual attached) Figure 4-6 ) III. Key Technologies 1. Multispectral collaborative calibration technology By combining internal standard methods (such as adding Y2O3 as an XRF internal standard) with an external standard sample library, the matrix effect and instrument drift problems can be solved.

[0036] 2. Dynamic sample introduction anti-interference design Ultrasonic vibration dispersion combined with carrier gas purging (argon) is used to reduce signal fluctuations caused by powder agglomeration.

[0037] 3. Lightweight Algorithm Deployment The quantitative model is compressed into TensorRT format to enable low-power real-time computation on embedded devices.

[0038] 4. Optimization Methods Improved spectral resolution: Optimized grating line density; Model iteration: Adapting to new sample types through incremental learning.

[0039] IV. Process Flow Diagram stage Key technologies Output results Sample preparation process Vibrating screen + ball mill optimization Standardized Sample Preparation Parameter Library Spectral detection Multispectral excitation and synchronous signal acquisition Joint spectral database (including 100+ standards) Algorithm Development PCA-PLSR fusion model training Quantitative analysis software V1.0 System Integration Modular hardware assembly and industrial protection design Prototype (testing cycle < 1 minute / sample) Industrialization verification Metallurgical / Chemical Scenarios Pilot Testing standards (enterprise level) stage Key technologies Output results Sample preparation process Vibrating screen + ball mill optimization Standardized Sample Preparation Parameter Library By employing the aforementioned research methods and process routes, we can systematically advance technological research and development, ultimately leading to a highly efficient and precise rapid detection solution for solid powders.

[0040] Technology Risks and Countermeasures Spectral interference: Correction is performed using a multi-spectral-line fitting algorithm and internal standard method, referencing the anti-interference design of the E5000 spectrometer.

[0041] Sample heterogeneity: Introduce vibrators and automated sieving devices to optimize the sample preparation process.

[0042] Insufficient real-time performance: Improve CCD data acquisition speed and algorithm parallel processing capabilities, referencing the fast response solution of LIPS technology.

[0043] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A rapid quantitative detection system for solid powder samples based on combined spectroscopy, characterized in that, The system includes a rapid quantitative detection system for solid powder samples (100), which includes a sample acquisition module (110) and a detection module (120). The sample acquisition module (110) consists of a raw material screening device (111), a drying device (112), a pulverizing device (113), and a sample preparation device (114). The sample acquisition module (110) sequentially screens, dries, pulverizes, and prepares the raw materials. The detection module (120) consists of a spectral excitation device (121), a signal acquisition device (122), a data processing device (123), and an analysis device (124). It sequentially excites the sample surface, captures the spectrum, aligns the data, and outputs the component density and physical properties.

2. The rapid quantitative detection system for solid powder samples based on combined spectroscopy according to claim 1, characterized in that, The raw material screening equipment (111) is a vibrating screen.

3. The rapid quantitative detection system for solid powder samples based on combined spectroscopy according to claim 1, characterized in that, The drying equipment (112) is a vacuum oven.

4. The rapid quantitative detection system for solid powder samples based on combined spectroscopy according to claim 1, characterized in that, The pulverizing equipment (113) is a planetary ball mill.

5. The rapid quantitative detection system for solid powder samples based on combined spectroscopy according to claim 1, characterized in that, The sample preparation equipment (114) is an automated tablet press.

6. The rapid quantitative detection system for solid powder samples based on combined spectroscopy according to claim 1, characterized in that, The spectral excitation device (121) uses laser and X-rays to excite the sample surface.

7. The rapid quantitative detection system for solid powder samples based on combined spectroscopy according to claim 1, characterized in that, The signal acquisition device (122) uses a multi-channel detector to synchronously capture the emission / heat dissipation spectrum.

8. The rapid quantitative detection system for solid powder samples based on combined spectroscopy according to claim 1, characterized in that, The data processing device (123) aligns the multispectral data using a time / space registration algorithm.

9. The rapid quantitative detection system for solid powder samples based on combined spectroscopy according to claim 1, characterized in that, The analytical device (124) calls the pre-trained model to output the components of sepsis and physical properties.

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